Lead-free solder composition.

(54) Title: LEAD-FREE WELDING COMPOSITION.

(54) Title: LEAD-FREE SOLDER COMPOSITION.

(57) Summary

A solder composition includes about 4% to about 25% by weight of tin, about 0.1% to about 8% by weight of antimony, about 0.03% to about 4% by weight of copper, about 0.03% to about 4% by weight of nickel, about 66% to about 90% by weight of indium, and about 0.5% to about 9% by weight of silver; the composition may further include about 0.2% to about 6% by weight of zinc, and, independently, about 0.01% to about 0.3% by weight of germanium; The composition can be used to solder an electrical connector to an electrical contact surface on a glass component.

(57) Abstract

A solder composition includes about 4% to about 25% by weight tin, about 0.1% to about 8% or by weight antimony, about 0.03% to about 4% by weight copper, about 0.03% to about 4% by weight nickel, about 66% to about 90% by weight indium, and about 0.5% to about 9% by weight silver. The composition can further inelude about 0.2% to about 6% by weight zinc, and, independently, about 0.01% to about 0.3% by weight germanium. The composition can be used to solder an electrical connector to an electrical contact surface on a glass component.

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PATENT TITLE NO. 344239

ANTA YA TECHNOLOGIES CORP.

Fenner Street, Cranston, Rhode Island, USA

LEAD-FREE WELDING COMPOSITION lnt.CI.8: B23K35 / 24; C22C28 / 00

JENNIE S. HWANG; JOHN PEREIRA: ALEXANDRA M. MACKIN; JOSEPH C. GONSALVES

REQUEST

International filing date:

MX / a / 2013/0090 February 14, 2012

PRIORITY

Country:

Date;

US US February 2011 September 28, 2011

Number:

61/439,538

61/540,213

Validity: Twenty year;

Expiration Date: February 1, 2032 &amp;

The s® reference patent grantsf based on articles 1^or, 2nd fraction V, 6th fraction III, and 59 of the Industrial Property Law. In accordance with article 23 of the Law on Industrial Property, this patent is valid for twenty years, non-extendable, Assembled from the date of filing of the International application and will be paid for the fee to maintain rights in force. ?

Who subscribes to the present title efo makes Jo based on nes lll and 7 ° bis 2 efe the Law of the

Industrial Property (Official Gazette of the Federation (D 0 F.) 27 ^ 6 (19®1, fápW 4. 25/10/1996, 12/26/19 ^ 7, 05/17/1999,&gt; 06/01/ 2004, 06/16/2005, 01/25 / 20D6, 06/05/2009, 06/01/2010, 1 28β / 2010, 28 / 0ΒΛ., _ ______12 and 04/09/2012); articles 1 »3^or fraction V subsection a), 4^or and 12 ° sections I and lll of the Regulation of the MeXica Institute ^ -of ^ 'Industrial Property (DOF 14/12 / 199®, amended on 07/01/2002, 07/15/2004, 07/28/2004 and 7 / 09/2007), articles 1^or, 3^or, 4^or, 5th fraction VjnasO-4), 16 fractions I and lil and 30 of the Organic Law of the Mexican Institute of Industrial Property (DOF 27/1271999, amended erWTO / 2002, 07/29/2004, 08/04/2004 and 09/13/2007); 1 », 3“ and 5th paragraph a) of the Agreement that delegates powers to the Deputy Directors General, Coordinator, Divisional Directors, Head of the Regional Offices, Divisional Deputy Directors, Departmental Coordinators and other subordinates of the Mexican Institute of Industrial Property. (DOF 12/15/1999, amended on 02/04/2000, 07/29/2004, 08/04/2004 and 09/13/2007).

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Issue Date: December 7, 2016

THE DIVISIONAL DIRECTOR OF PATENTS

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NAHANNY CANAL REYES

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RELATED REQUESTS

This application claims the benefit of US provisional application No. 61 / 439,538, filed on February 4, 2011 and US provisional application No. 61 / 540,213 filed on September 28, 2011. The full content of the previous applications are incorporated herein by reference.

BACKGROUND OF THE INVENTION

The windshields and rear windows of vehicles such as automobiles often include electrical devices located inside or on the glass. Typically, electrical appliances are antennas or defrosters. In order to provide an electrical connection to an electrical device, a small area of ​​metallic coating is applied to the glass to make the metallized surface that is electrically connected to the electrical device. Then an electrical connector is soldered onto the metalized surface. The electrical connector (i.e. power) is commonly soldered to the metalized glass surface with a lead (Pb) containing solder. Due to environmental concerns and / or regulatory mandates in various countries, most industries are currently using or planning to use

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Lead-free solders in soldering applications. A common lead-free solder used in some industries contains a high content of tin (Sn), such as more than 80% tin. Lead-free solders used in automotive glass as described herein are described in US Patent No. 6,253,988 issued to John Pereira on July 3, 2001 (hereinafter Pereira). Among several lead-free solders, Pereira describes a solder composition with a weight percentage of 64.35-65.65% indium (In), 29.7% - 30.3% tin (Sn), 4.05% - 4.95% silver (Ag), 0.250.75% copper (Cu) (hereinafter the indium 65 solder).

There are difficulties encountered when welding devices for automotive glass that are not present in other applications. Automotive glass tends to be brittle, and common high-tin lead-free solders that are suitable for use in other applications can typically cause cracking of automotive glass. Although materials such as ceramic and silicon may appear similar in some respects to automotive glass, some welds that are suitable for welding to ceramic or silicon devices are not suitable for welding automotive glass. Welding two materials with a substantial difference in the coefficient of thermal expansion (CTE) between them, such as glass and copper in this case, imposes stress on the weld, during cooling of the weld joint, or during excursions rear temperature. The weld composition must have a melting point (liquidus) that is low enough not to

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causing automotive glass cracking during the welding procedure, since a higher melting point and consequently higher processing temperature increases the adverse effects of CTE mismatch, imposes more load during cooling. The melting point of the solder composition, however, needs to be high enough not to melt during normal car use, for example when the car is in the sun with windows closed or under other harsh environmental conditions extreme. Indium-containing welds, however, typically have much lower melting points than other welds. The indium 65 solder, for example, has a solidus temperature of 109 ° C, compared to 160 ° C for the lead solder, and a liquidus temperature of 127 ° C, compared to 224 ° C for the lead solder. Some vehicle manufacturers wish that glass products must be able to survive high temperatures, for example 110 ° C for an original equipment manufacturer (OEM) and 120 ° C on the other hand, without any deterioration in performance.

Therefore, there is a need for a suitable lead-free solder composition for use on glass that can withstand higher elevated temperatures than currently available compositions, while delivering all other desired properties for this sector of application.

BRIEF DESCRIPTION OF THE INVENTION

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Generally, the invention is directed to a welding composition.

One embodiment includes about 4% to about 25% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.03% to about 4% by weight of copper, of about 0.03% to about 4% by weight of nickel, from about 66% to about 90% by weight of indium, and about 0.5% to about 9% by weight of silver. The weld composition can have a solidus temperature in a range of between 120 ° C and 145 ° C and a liquidus temperature in a range of between 130 ° C and 155 ° C.

In certain embodiments, the composition further includes about 0.2% to about 6% by weight of zinc. In certain other embodiments, the composition further includes about 0.01% to about 0.3% by weight of germanium. In these specific embodiments, the composition can include about 70% to about 86% by weight of indium.

In some embodiments, the composition includes about 7% to about 19% by weight of tin, from about 0.2% to about 8% by weight of antimony, from about 0.1% to about 1.5% by weight of copper , from about 0.1% to about 4% by weight of nickel, from about 70% to about 80% by weight of indium and about 4% to about 8% in

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silver weight.

In some other modalities, the composition includes about

4% to about 20% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.1% to about 4% by weight of copper, from about 0.1% to about 3% by weight of nickel, from about 71% to about 86% by weight of indium and from about 1% to about 6% by weight of silver.

In still other modalities, the composition includes about 11% to about 17% by weight of tin, from about 0.5% to about 3% by weight of antimony, from about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 5% by weight of nickel, from about 72% to about 77% by weight of indium, about 4% to about 8.5% by weight of silver, and about 0.3% to about 1.5% by weight of zinc. In these specific modalities, the composition may include from about 13% to about 15% by weight of tin, from about 0.5% to about 2.5% by weight of antimony, from about 0.5% to about 1.5% in weight of copper, from about 1% to about 4% by weight of nickel, from about 74% to about 75% by weight of indium, from about 5% to about 8.5% by weight of silver, and about 0.3% to about 1.5% by weight of zinc. Examples of these specific embodiments may include from about 15% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of

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copper, about 1% by weight nickel, about 75% by weight indium, about 6% by weight silver, and about 0.5% to about 1.5% by weight zinc, like about 15 wt% tin, about 1 wt% antimony, about 1 wt% copper, about 1 wt% nickel, about 75 wt% indium, about 6% by weight of silver, and about 1% by weight of zinc. Other examples of these specific modalities may include about 14% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 3 % by weight nickel, about 75% by weight indium, about 5% by weight silver, and about 0.5% to about 1.5% by weight zinc, about 14% by weight tin , about 1% by weight of antimony, about 1% by weight of copper, about 3% by weight nickel, about 75% by weight indium, about 5% by weight silver, and about 1% by weight zinc. Still other examples of these specific embodiments may include about 13% by weight of tin, about 1.5% to about 2.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 4% by weight nickel, about 74% by weight indium, about 5% by weight silver, and about 0.5% to about 1.5% by weight zinc, about 13% by weight tin, about 2% by weight of antimony, about 1% by weight copper, about 4% by weight nickel, about 74% by weight indium, about 5% by weight silver, and

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MEXICAN INSTITUTE

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about 1% by weight of zinc.

In still other modalities, the composition essentially includes from about 11% to about 17% by weight of tin, from about 0.5% to about 3% by weight of antimony, from about 0.5% to about 1.5% in weight of copper, from about 0.5% to about 5% by weight of nickel, from about 72% to about 77% by weight of indium, about 4% to about 8.5% by weight of silver, and about 0.3 % to about 1.5% by weight of zinc. In these specific modalities, the composition may consist essentially of about 13% to about 15% by weight of tin, from about 0.5% to about 2.5% by weight of antimony, from about 0.5% to about 1.5% by weight of copper, from about 1% to about 4% by weight of nickel, from about 74% to about 75% by weight of indium, about 5% to about 8.5% by weight of silver, and about 0.3% to about 1.5% by weight of zinc. Examples of these specific embodiments may consist essentially of about 15% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, of about 1% by weight of nickel, about 75% by weight of indium, about 6% by weight of silver, and about 0.5% to about 1.5% by weight of zinc, such as about 15% by weight of tin, about 1% by weight of antimony, about 1% by weight copper, about 1% by weight nickel, about 75% by weight indium, about 6% by weight silver, and about 1% by weight zinc. Others

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Examples of these specific embodiments may consist essentially of about 14% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, of about 3% by weight nickel, about 75% by weight indium, about 5% by weight silver, and about 0.5% to about 1.5% by weight zinc, such as about 14% by weight tin , about 1% by weight of antimony, about 1% by weight copper, about 3% by weight nickel, about 75% by weight indium, about 5% by weight silver, and about 1% by weight zinc. Still other examples of these specific embodiments may consist essentially of about 13% by weight of tin, about 1.5% to about 2.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 4% by weight nickel, about 74% by weight indium, about 5% by weight silver, and about 0.5% to about 1.5% by weight zinc, such as about 13% by weight tin, about 2% by weight of antimony, about 1% by weight copper, about 4% by weight nickel, about 74% by weight indium, about 5% by weight silver, and about 1% by weight zinc. In these specific embodiments, the weld composition can have a solidus temperature in a range of between about 120 ° C and about 145 ° C, such as in a range of between 120 ° C and 135 ° C and a liquidus temperature in a range of between 130 ° C and about 155 ° C, as in a range of between about 130 ° C and about 145 ° C.

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The invention is also directed to an electrical connection in a glass component including a glass component, a silver-containing electrical contact surface on the glass component, and an electrical connector soldered to the electrical contact surface on the glass component with a layer of a solder composition with a mixture of elements comprising about 4% to about 25% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.03% to about 4% by weight of copper, from about 0.03% to about 4% by weight of nickel, about 66% to about 90% by weight of indium and about 0.5% to about 9% by weight of silver. In other embodiments, an electrical connection in a glass component includes a glass component, a silver-containing electrical contact surface on the glass component, and an electrical connector soldered to the electrical contact surface on the glass component with a coating. of a solder composition comprising essentially from about 4% to about 25% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.03% to about 4% by weight of copper, from about 0.03% to about 4% by weight of nickel, from about 66% to about 90% by weight of indium and about 0.5% to about 9% by weight of silver.

The invention is also directed to a method of forming the solder composition that includes the mixture of indium, nickel, copper,

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silver, antimony, and tin to form an alloy that includes about 4% to about 25% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.03% to about 4% by weight copper, from about 0.03% to about

4% by weight of nickel, from about 66% to about 90% by weight of indium and about 0.5% to about 9% by weight of silver. In some embodiments, indium and tin are mixed in a first molten mixture, and at least nickel, copper, and silver are mixed in solution in a second mixture that is added to the first molten mixture. In other embodiments, tin and nickel are mixed in a molten mixture, and at least copper, indium, and silver are added to the molten mixture. In these specific modalities, zinc can be added after all other metals have been added to the molten mixture.

In some embodiments, tin is mixed at a rate of about 7% to about 19% by weight, antimony is mixed at a rate of about 0.2% to about 8% by weight, copper is mixed at a rate of about 0.1% to about 1.5% by weight, nickel is mixed in a ratio of about 0.1% to about 4% by weight, the indium is mixed in a ratio of about 70% to about 80% by weight, and silver is mixed in a ratio of about 4% to about 8% by weight.

In other modalities, a method of training the

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antimony and tin to form an alloy that includes approximately

11% to about 17% by weight of tin, from about 0.5% to about 3% by weight of antimony, from about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 5 % by weight of nickel, from about 72% to about 77% by weight of indium and about 0.5% to about 1.5% by weight of zinc. In these specific modalities, the composition may include from about 13% to about 15% by weight of tin, from about 0.5% to about 2.5% by weight of antimony, from about 0.5% to about 1.5% in weight of copper, from about 1% to about 4% by weight of nickel, from about 74% to about 75% by weight of indium, from about 5% to about 6% by weight of silver, and about 0.5% to about 1.5% by weight of zinc. Examples of these specific modalities may include about 15% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 1% by weight of nickel, about 75% by weight of indium, about 6% by weight of silver, and about 0.5% to about 1.5% by weight of zinc, such as about 15% by weight of tin, about 1% by weight of antimony, about 1% by weight of copper, about 1% by weight nickel, about 75% by weight indium, about 6% by weight silver, and about 1% by weight zinc. Other examples of these specific modalities may include about 14% by weight of tin,

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INtUSTUAL about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 3% by weight of nickel, about 75% by weight of indium, of about 5% by weight of silver, and about 0.5% to about 1.5% by weight of zinc, like about 14% by weight of tin, about 1% by weight of antimony, about 1% in copper weight, about 3% by weight nickel, about 75% by weight indium, about 5% by weight of silver, and about 1% by weight of zinc. Still other examples of these specific embodiments may include about 13% by weight of tin, about 1.5% to about 2.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 4%_?by weight of nickel, about 74% by weight of indium, about 5% by weight of silver, and about 0.5% to about 1.5% by weight of zinc, such as about 13% by weight of tin, about 2% by weight antimony, about 1% by weight copper, about 4% by weight nickel, about 74% by weight indium, about 5% by weight silver, and about 1% by weight of zinc.

In addition to providing environmentally friendly lead-free materials, the solder compositions of the invention have many advantages, such as providing a lead-free composition that can be used in automotive glass, offering necessary mechanical properties in strength and ductility and that withstand desired high service temperatures, while keeping the desired and low manufacturing process temperature.

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BRIEF DESCRIPTION OF THE DRAWINGS

The foregoing will be evident from the following more particular description of the exemplary embodiments of the invention, as illustrated in the accompanying drawings in which the same reference characters refer to the same parts through different views. The drawings are not necessarily to scale, but emphasis is instead placed on the illustrative embodiments of the present invention.

Figure 1 is an internal view of a rear window of an automobile including an electrically powered defroster.

FIG. 2 is a side view of an electrical connector soldered to an electrical contact in the rear window of FIG. 1, with the rear window, electrical contact, and solder shown in section.

Figure 3A is a schematic illustration of a flow chart of a method of forming modalities of solder compositions in the invention.

Figure 3B is a schematic illustration of a flow chart of another method of forming modalities of solder compositions in the invention.

Figures 4A and 4B are schematic illustrations of power connectors that can be soldered with compositions of

Figure 5 is a schematic illustration of a connector

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welding of the invention.

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supply welded to a windshield with welding compositions of the invention.

Figure 6 is a schematic illustration of a windshield mount employing welding compositions of the invention.

Figure 7 is a graph of temperature versus time during one cycle of a temperature cycling test of modalities of solder compositions of the invention.

Figure 8 is a schematic illustration of a tensile test, using a dynamometer to test the performance of the weld compositions of the invention.

Figure 9 is a schematic illustration of a tensile test using a weight to test the performance of the weld compositions of the invention.

DETAILED DESCRIPTION OF THE INVENTION

The present invention provides a soldering composition that is suitable for soldering electrical components to glass to electrically connect electrical devices in or on glass. Referring to Figure 1, the rear window 10 of an automobile (also called a backlight, for example, in Europe) is used as an example

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illustrative. Window (glass component) 10 includes a window defroster 12 consisting of resistive electrical defrost lines 14 embedded within or deposited on the inner surface of window 10. Defrost lines 14 are electrically connected to a pair of strips of electrical contact (the electrical contact surfaces, also known as bus bars) 16 located on the inner surface of the window

10. The electrical contact strips 16 consist of a conductive layer deposited on the inner surface of the window 10. Typically, electrical contact strips 16 are formed from silver containing material.

There are difficulties encountered when welding devices for automotive glass that are not present in other applications. To address some original equipment manufacturer (OEM) concerns about the use of lead-free solders in automotive glass, automotive glass suppliers such as CLEPA (European Association of Automotive Suppliers) have developed various tests, including temperature cycling, constant climate humidity , climatic temperature with humidity and high storage temperature. To address OEM concerns about the melting point of the solder, one test included glass samples soldered to the connectors with indium solder 65 that were stored at 105 ° C for 500 hours, during which time the weights of 500 grams were hung from each of the connectors, however, there were no connectors detached from the glass during the trial period. OEMs such as the Association of

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The composition of the weld of the present invention was developed to address the aforementioned OEM problems.

Referring to Figure 2, the layer of solder composition 20 of the present invention is employed to solder an electrical (i.e., power) connection Ί 8 to each electrical contact strip (i.e., bus bar) 16 in the window 10, using standard welding techniques, such as resistance, flame, micro-flame, hot iron, hot air and induction heating welding device. Welding can be performed in an ambient air atmosphere, without the need for an inert gas environment. The power lines 22 can then be electrically connected to electrical connectors 18 to provide power to the window defroster 12 (Figure 1). Welding performance test and results are provided below.

In one embodiment, the present solder composition 20 includes about 4% to about 25% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.03% to about 4% by weight of copper, from about 0.03% to about 4% by weight of nickel, from about 66% to about 90% by weight of indium and about 0.5% to about 9% by weight of silver.

In certain embodiments, composition 20 includes about 1% to about 7% by weight of silver. In certain modalities, the

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Composition 20 includes about 0.2% to about 8% by weight of antimony. In other embodiments, composition 20 includes about 3% to about 7% by weight of silver. In still other embodiments, composition 20 includes about 1% to about 4% by weight of silver.

In certain embodiments, composition 20 further includes about 0.2% to about 6% by weight of zinc. In certain other embodiments, composition 20 further includes about 0.3% to about 6% by weight of zinc. In still other embodiments, composition 20 further includes about 3% to about 5% by weight of zinc.

In certain other embodiments, composition 20 further includes about 0.01% to about 0.3% by weight of germanium. In these specific embodiments, composition 20 can include about 70% to about 86% by weight of indium.

In some embodiments, composition 20 includes about 7% to about 19% by weight of tin, from about 0.2% to about 8% by weight of antimony, from about 0.1% to about 1.5% by weight of copper, from about 0.1% to about 4% by weight of nickel, from about 70% to about 80% by weight of indium and about 4% to about 8% by weight of silver.

In certain embodiments, composition 20 includes about 74% to about 78% by weight of indium. In these

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specific modalities, composition 20 may include approximately

5% to about 10% by weight of tin, or about 12% to about 19% by weight of tin, or about 12% to about 16% by weight of tin In certain other embodiments, composition 20 includes about 74% to about 80% by weight of indium. In still other embodiments, composition 20 includes about 0.1% to about 3% by weight nickel. In still other embodiments, composition 20 includes about 0.2% to about 5% by weight of antimony.

In still other embodiments, composition 20 includes about 11% to about 17% by weight of tin, from about 0.5% to about 3% by weight of antimony, from about 0.5% to about 1.5% by weight copper, from about 0.5% to about 5% by weight of nickel, from about 72% to about 77% by weight of indium, about 4% to about 7% by weight of silver, and about 0.5% to about 1.5% by weight of zinc. In these specific embodiments, composition 20 may include from about 13% to about 15% by weight of tin, from about 0.5% to about 2.5% by weight of antimony, from about 0.5% to about 1.5% by weight of copper, from about 1% to about 4% by weight of nickel, from about 74% to about 75% by weight of indium, from about 5% to about 6% by weight of silver, and about 0.5% to about 1.5% by weight of zinc. Examples of these specific modalities may include about 15% by weight of

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MEXICAN INSTITUTE OF LA PROMEDAD

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tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 1% by weight of nickel, about 75% by weight of indium, about 6% by weight silver, and about 0.5% to about 1.5% by weight zinc, about 15% by weight tin, about 1% by weight antimony, about 1 wt% copper, about 1 wt% nickel, about 75 wt% indium, about 6% by weight of silver, and about 1% by weight of zinc. Other examples of these specific modalities may include about 14% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 3 % by weight nickel, about 75% by weight indium, about 5% by weight silver, and about 0.5% to about 1.5% by weight zinc, about 14% by weight tin , about 1% by weight of antimony, about 1% by weight of copper, about 3% by weight nickel, about 75% by weight indium, about 5% by weight silver, and about 1% by weight zinc. Still other examples of these specific embodiments may include about 13% by weight of tin, about 1.5% to about 2.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, about 4% by weight nickel, about 74% by weight indium, about 5% by weight silver, and about 0.5% to about 1.5% by weight zinc, about 13% by weight tin, about 2% by weight of

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antimony, about 1% by weight copper, about 4% by weight nickel, about 74% by weight indium, about 5% by weight silver, and about 1% by weight zinc.

Solder composition 20 can have a solidus temperature in a range of between about 120 ° C and about 145 ° C and a liquidus temperature in a range of between 130 ° C and about 155 ° C. Solidus temperature is practically defined as the temperature at which an alloy begins to melt. Below the solidus temperature, the substance is completely solid, with no molten phase. Liquidus temperature is the maximum temperature at which crystals (unmelted metal or alloy) can coexist with the melt. Above the liquidus temperature, the material is homogeneous, consisting of melt only. The welding processing temperature is higher than the liquidus temperature, by a number of degrees that is determined by the welding technique.

In a specific embodiment, composition 20 includes from about 14% to about 16% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper , from about 0.5% to about 1.5% by weight of nickel, from about 74% to about 76% by weight of indium, and from about 6% to about 8% by weight of silver, such as about 15% by weight of tin, about 1.0% by weight of antimony, about 1.0% by weight of

IMPI

MEXICAN INSTITUTE OF THE INDUSTRIAL TRprnDAC

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copper, about 1.0 wt% nickel, about 75 wt% indium, and about 7 wt% silver. Other compositions in this embodiment may include from about 14% to about 21% by weight of tin, from about 0.2% to about 3% by weight of antimony, from about 0.1% to about 4.0% by weight copper, from about 0.1% to about 3.0% by weight of nickel, from about 72% to about 80% by weight of indium and about 1% to about 8% by weight of silver.

In a second specific embodiment, composition 20 includes from about 14% to about 16% by weight of tin, about 2% to about 4% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 74% to about 76% by weight of indium, and from about 4% to about 6% by weight of silver, such as about 15 % by weight of tin, about 3.0% by weight antimony, about 1.0% by weight copper, about 1.0% by weight nickel, about 75% by weight indium, and about 5% by weight silver .

In a third specific embodiment, composition 20 includes from about 12% to about 14% by weight of tin, about 2% to about 4% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 2% to about 4% by weight nickel, from about 74% to

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DB U INDUSTRIAL DIFFICULTY about 76% by weight of indium, and about 4% to about 6% by weight of silver, such as about 13% by weight of tin, about 3.0% by weight of antimony, closely 1.0% by weight copper, about 3.0% by weight nickel, about 75% by weight indium, and about 5% by weight silver, or about 14% by weight tin, about 3.0 wt% antimony, about 1.0 wt% copper, about 2.0% by weight nickel, about 75% by weight indium, and about 5% by weight silver.

In a fourth specific embodiment, composition 20 includes from about 7% to about 9% by weight of tin, about 4% to about 6% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 2% to about 4% by weight of nickel, from about 74% to about 76% by weight of indium, from about 4% to about 6% by weight of silver, and about 2% to about 4% by weight of zinc, such as about 8% by weight tin, about 5.0% by weight antimony, about 1.0% by weight copper, about 3.0% by weight nickel, about 75% by weight indium, about 5% by weight of silver, and about 3.0% by weight of zinc.

In a fifth specific embodiment, composition 20 includes from about 7% to about 9% by weight of tin, about 4% to about 6% by weight of antimony, about

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0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 74% to about 76% by weight of indium, from about 4% to about

6% by weight of silver, and about 4% to about 6% by weight of zinc, such as about 8% by weight of tin, about 5.0% by weight of antimony, about 1.0% by weight of copper, about 1.0% by weight nickel, about 75% by weight indium, about 5% by weight silver, and about 5.0% by weight zinc.

In a sixth specific embodiment, composition 20 includes from about 7% to about 9% by weight of tin, about 4% to about 6% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 2% to about 4% by weight of nickel, from about 74% to about 76% by weight of indium, from about 4% to about 6% by weight of silver, from about 2% to about 4% by weight of zinc, and from about 0.05% to about 0.2% by weight of germanium, such as about 8% by weight of tin, about 4.9% by weight of antimony, about 1.0% by weight of copper, about 3.0% in nickel weight, about 75% by weight indium, and about 5% by weight silver, about 3.0% by weight zinc and about 0.1% by weight germanium.

In some other modalities, composition 20 includes about 4% to about 20% by weight of tin, from about 0.2% to

<img file="MX344239B_D0033.tif" />

IMPI

INSTITUTO MAXJCANO OE LA MKtntDAD industrial about 8% by weight of antimony, from about 0.1% to about 4% by weight of copper, from about 0.1% to about 3% by weight of nickel, about 71% to about 86% by weight of indium and about 1% to about 6% by weight of silver. In certain embodiments, composition 20 includes about 10% to about 19% by weight of tin. In certain other embodiments, composition 20 includes about 74% to about 80% by weight of indium. In these specific embodiments, composition 20 can include about 1% to about 7% by weight of silver. In certain embodiments, composition 20 can include approximately 3.5% by weight of copper. In certain other embodiments, composition 20 includes about 0.1% to about 1% by weight of nickel. In still other embodiments, composition 20 includes about 1% to about 2% by weight nickel. In still other embodiments, composition 20 includes about 0.2% to about 2% by weight of antimony. In still other embodiments, composition 20 includes approximately

2% to about 6% by weight of antimony.

In a seventh specific embodiment, composition 20 includes from about 18% to about 20% by weight of tin, about 0.2% to about 1.0% by weight of antimony, about 0.1% to about 1.0% by weight of copper, from about 0.1% to about 1.0% by weight of nickel, from about 77% to about 80% by weight of indium, and from about 1% to

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about 3% by weight silver, such as about 1R 99% pn Hp tin, about 0.24% by weight antimony, about 0.18% by weight copper, about 0.30% by weight nickel, from about 78.70% by weight of indium, and about 1.48% by weight of silver. The melting point or temperature (liquidus) of this specific modality was approximately 135 ° C and the solidus was approximately 124 ° C.

In an eighth specific embodiment, composition 20 includes from about 13% to about 16% by weight of tin, about 1.0% to about 3.0% by weight of antimony, about 3.0% to about 4.0% by weight of copper, from about 0.2% to about 1.5% by weight of nickel, from about 74% to about 76% by weight of indium, and from about 3% to about 5% by weight of silver, such as about 14.77 % by weight of tin, about 1.93% by weight antimony, about 3.50% by weight copper, about 0.60% by weight nickel, about 74.91% by weight indium, and about 3.87% by weight silver . The melting point or temperature (liquidus) of this specific modality was approximately 135 ° C and the solidus was approximately 123 ° C.

In a ninth specific embodiment, composition 20 includes from about 11% to about 14% by weight of tin, about 2.0% to about 4% by weight of antimony, about 0.5% to about 2% by weight of copper, from about 1.0% to about 3% by weight nickel, from about 76% to

IMPI

MEXICAN INSTITUTE OF INDUSTRIAL OWIDA

<img file="MX344239B_D0035.tif" />

about 79% by weight of indium, and from about 2% to about 5% by weight of silver, such as about 12.68% by weight of tin, about 2.91% by weight of antimony, about 1.22% in copper weight, about 1.87% by weight nickel, about 77.30% by weight indium, and about 3.54% by weight silver. The melting point or temperature (liquidus) of this specific modality was approximately 138 ° C and the solidus was approximately 127 ° C.

In a tenth specific embodiment, composition 20 includes from about 6% to about 9% by weight of tin, about 3.0% to about 5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 1.0% to about 3% by weight of nickel, from about 76% to about 79% by weight of indium, from about 4% to about 6% by weight of silver, and about 2% to about 4% by weight of zinc, such as about 7.66 wt% tin, about 3.75 wt% antimony, about 0.92 wt% copper, about 1.88 wt% nickel, about 77.30 wt% indium, approximately 5.21% by weight of silver, and approximately 3.17% by weight of zinc. The melting point or temperature (liquidus) of this specific modality was approximately 143.4 ° C and the solidus was approximately 129 ° C.

In an eleventh specific embodiment, composition 20 includes from about 7% to about 9% by weight of tin, about 4% to about 6% by weight of antimony,

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about 0.2% to about 1.0% by weight of copper, from about 0.2% to about 1.5% by weight of nickel, from about 73% to about 76% by weight of indium, from about 4% to about 6 % by weight of silver, and about 4% to about 6% by weight of zinc, such as about 8.45% by weight of tin, about 5.42% by weight of antimony, about 0.40% by weight copper, about 0.54% by weight nickel, about 74.21% by weight indium, approximately 5.54% by weight of silver, and approximately 4.86% by weight of zinc. The melting point or temperature (liquidus) of this specific modality was approximately 139.4 ° C and the solidus was approximately

127 ° C.

In a specific embodiment number twelve, composition 20 includes from about 4% to about 6% by weight of tin, about 1.0% to about 2.0% by weight of antimony, about 0.1% to about 2% by weight copper, from about 0.1% to about 1.0% by weight of nickel, from about 84% to about 86% by weight of indium, from about 1% to about 2% by weight of silver, from about 0.2% to about 1% by weight of zinc, and less than about 0.001% to about 0.15% by weight of germanium, such as about 5.31% by weight of tin, about 1.52% by weight of antimony, about 1.07% by weight of copper, about 0.15% by weight of nickel, approximately 85.56% by weight of indium, and approximately 1.45% by weight of silver, approximately

INSTTRJTOMÜtlGANO OF THE "INDUSTRIAL CITY ** *

0.46 wt% zinc and approximately 0.001 wt% germanium. The melting point or temperature (liquidus) of this specific modality was approximately 140 ° C and the solidusftie approximately 132.4 ° C.

In a specific embodiment thirteen, composition 20 includes from about 18% to about 20% by weight of tin, about 0.2% to about 2% by weight of antimony, about 0.1% to about 4.0% by weight of copper, from about 0.1% to about 3.0% by weight of nickel, from about 72% to about 75% by weight of indium, and from about 1% to about 4% by weight of silver, such as about 19.49 % by weight of tin, about 1.03 wt% antimony, about 2.84 wt% copper, about 1.26 wt% nickel, about 73.62 wt% indium, and about 2.79 wt% silver . The melting point or temperature (liquidus) of this specific modality was approximately 134.71 ° C and the solidus was approximately 123.74 ° C.

In a specific fourteen embodiment, composition 20 includes from about 16% to about 19% by weight of tin, about 3.0% to about 6.0% by weight of antimony, about 2.0% to about 4.0% by weight of copper, from about 0.5% to about 3.0% by weight of nickel, from about 70% to about 73% by weight of indium, and from about 1% to about 4% by weight of silver, such as about 18.23 % by weight of tin, about 4.57% by weight of antimony, about 2.7% by weight

IMPI MEXICAN INSTITUTE OF INDUSTRIAL FHOWEDAD

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copper, about 1.49% by weight nickel, about 71.05% by weight indium, and about 2.60% by weight silver. The melting point or temperature (liquidus) of this specific modality was approximately

135.52 ° C and the solidus was approximately 122.98 ° C.

In a specific embodiment fifteen, composition 20 includes from about 15% to about 18% by weight of tin, about 1.0% to about 4% by weight of antimony, about 1.5% to about 3.5% by weight of copper, from about 1.0% to about 4% by weight of nickel, from about 71% to about 75% by weight of indium, and from about 2% to about 5% by weight of silver, such as about 16.95 % by weight of tin, about 2.69% by weight antimony, about 2.4% by weight copper, about 2.82% by weight nickel, about 72.84% by weight indium, and about 3.31% by weight silver . The melting point or temperature (liquidus) of this specific modality was approximately 139.01 ° C and the solidus was approximately 125.39 ° C.

In a specific sixteen embodiment, composition 20 includes from about 7% to about 11% by weight of tin, about 3.0% to about 5% by weight of antimony, about 1.5% to about 3.5% by weight of copper, from about 0.5% to about 3% by weight of nickel, from about 79% to about 82% by weight of indium, from about 1.0% to about 4% by weight of silver, and about 0.01% to about 1% in

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zinc weight, such as about 9.02 wt% tin, about

4.12 wt% antimony, about 2.21 wt% copper, about 1.09 wt% nickel, about 80.12 wt% indium, about 2.80 wt% silver, and about 0.05 wt% zinc. The melting point or temperature (liquidus) of this specific modality was approximately 142.11 ° C and the solidus was approximately

130.91 ° ​​C.

In a specific seventeen embodiment, composition 20 includes from about 9% to about 12% by weight of tin, about 4% to about 6% by weight of antimony, about 1.5% to about 3.5% by weight of copper, from about 0.5% to about 3.0% by weight of nickel, from about 75% to about 78% by weight of indium, from about 1% to about 3% by weight of silver, and about 0.01% to about 1% by weight of zinc, such as about 10.69 wt% tin, about 5.32 wt% antimony, about 2.58 wt% copper, about 1.55 wt% nickel, about 76.03 wt% indium, approximately 2.11% by weight of silver, and approximately 0.05% by weight of zinc. The melting point or temperature (liquidus) of this specific modality was approximately 140.37 ° C and the solidus was approximately 126.93 ° C.

In a specific embodiment number eighteen, composition 20 includes from about 8% to about 10% by weight of tin, about 2.0% to about 5.0% by weight of antimony, _____

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about 2% to about 4% by weight of copper, from about 0.5% to about 3.0% by weight of nickel, from about 79% to about 82% by weight of indium, from about 2% to about 4 % by weight of silver, from about 0.01% to about 1% by weight of zinc, and less than about 0.001% to about 0.15% by weight of germanium, such as about 9.03% by weight of tin, closely of

3.43% by weight antimony, about 3% by weight copper, about 0.95% by weight nickel, about 80.57% by weight indium, and about 3.32% by weight silver, about

0.1% by weight of zinc and approximately 0.001% by weight of germanium. The melting point or temperature (liquidus) of this specific modality was approximately 141.67 ° C and the solidus was approximately 130.30 ° C.

In a specific embodiment nineteen, composition 20 includes from about 10% to about 14% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 73% to about 77% by weight of indium, from about 5% to about 9% by weight of silver, and about 2% to about 4% by weight of zinc, such as about 12% by weight of tin, about 1% by weight of antimony, about 1% by weight of copper, about 1% by weight of nickel, about 75% by weight of indium, approximately

7% by weight of silver, and approximately 3% by weight of zinc.

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In a specific embodiment twenty, composition 20 includes from about 6% to about 10% by weight of tin, about 3% to about 7% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 2% to about 4% by weight of nickel, from about 73% to about 77% by weight of indium, from about 3% to about 7% by weight of silver, and about 2% to about 4% by weight of zinc, such as about 8% by weight of tin, about 5% by weight of antimony, about 1% by weight of copper, about 3% by weight of nickel, about 75% by weight of indium, about 5% by weight of silver, and about 3% by weight of zinc.

In a specific embodiment twenty-one, composition 20 includes from about 12% to about 16% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 0.5% to about 1.5% by weight of zinc, from about 73% to about 77% by weight of indium, and about 5% to about 9% by weight of silver, such as about 14% by weight of tin, about 1% by weight of antimony, about 1% by weight of copper, about 1% by weight of nickel, about 1% by weight of zinc, about 75% by weight of indium, and about 7% by weight of silver.

In a specific embodiment twenty two, composition 20 includes

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from about 20% to about 24% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5 % by weight of nickel, from about 66% to about 70% by weight of indium, and from about 5% to about 9% by weight of silver, such as about 22% by weight of tin, of about 1 wt% antimony, about 1 wt% copper, about 1% by weight nickel, about 68% by weight indium, and about 7% by weight silver.

In a specific embodiment twenty-three, composition 20 includes from about 18% to about 22% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 2% to about 4% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 66% to about 70% by weight of indium, and from about 5% to about 9% by weight of silver, such as about 20 % by weight of tin, about 1% by weight antimony, about 3% by weight copper, about 1% by weight nickel, about 68% by weight indium, and about 7% by weight silver .

In a specific twenty-four embodiment, composition 20 includes from about 12% to about 16% by weight of tin, from about 1% to about 3% by weight of antimony,

<img file="MX344239B_D0042.tif" />

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about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 73% to about 77% by weight of indium, and from about 5% to about 9% by weight of silver, such as about 14% by weight of tin, about 2% by weight of antimony, about 1% by weight of copper, about 1% by weight of nickel, close-up 75% by weight of indium, and about 7% by weight of silver.

In a specific twenty-five embodiment, composition 20 includes from about 11% to about 15% by weight of tin, about 2% to about 4% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 73% to about 77% by weight of indium, and from about 5% to about 9% by weight of silver, such as about 13 % by weight of tin, about 3% by weight antimony, about 1% by weight copper, about 1% by weight nickel, about 75% by weight indium, and about 7% by weight silver .

In a specific embodiment twenty-six, composition 20 includes from about 14% to about 18% by weight of tin, about 2% to about 4% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 70% to about 74% by weight of indium, and from about 5% to

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about 9% by weight of silver, such as about 16% by weight of tin, about 3% by weight of antimony, about 1% by weight of copper, about 1% by weight of nickel, of about 72% by weight of indium, and about 7% by weight of silver.

In a specific embodiment twenty-seven, composition 20 includes from about 18% to about 22% by weight of tin, about 2% to about 4% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 66% to about 70% by weight of indium, and from about 5% to about 9% by weight of silver, such as about 20 % by weight of tin, about 3% by weight antimony, about 1% by weight copper, about 1% by weight nickel, about 68% by weight indium, and about 7% by weight silver .

In a specific embodiment twenty-eight, composition 20 includes from about 13% to about 17% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 73% to about 77% by weight of indium, and from about 5% to about 9% by weight of silver, such as about 15 % by weight of tin, about 1% by weight antimony, about 1% by weight copper, about 1% by weight nickel, about 75% by weight indium,

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and about 7% by weight of silver. ............................—

In a specific embodiment twenty-nine, composition 20 includes from about 13% to about 17% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 0.5% to about 1.5% by weight of zinc, from about 73% to about 77% by weight of indium, and about 5% to about 8.5% by weight of silver, such as about 14.05 wt% tin, about 0.98 wt% antimony, about 0.87 wt% copper, about 0.70 wt% nickel, about 0.63 wt% zinc , about 74.74% by weight of indium, and about 7.98% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 133.18 ° C and the solidus was approximately 123.94 ° C.

In a specific embodiment thirty, composition 20 includes from about 12% to about 16% by weight of tin, about 0.5% to about 1.5% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 2% to about 4% by weight of nickel, from about 0.5% to about 1.5% by weight of zinc, from about 73% to about 77% by weight of indium, and about 3% to about 7% by weight of silver, such as about 14.14 wt% tin, about

<img file="MX344239B_D0046.tif" />

IMPI

MEXICAN INSTHVTO

INDUSTRIAL DEIAnOMlTY

0.76 wt% antimony, about 0.64 wt% copper, about 2.24 wt% nickel, about 0.75 wt% zinc, about 76.07 wt% indium, and about 5.81 wt% silver . The melting point or temperature (liquidus) of this solder composition was approximately 137.58 ° C and the solidus was approximately 125.92 ° C.

In a specific embodiment thirty-one, composition 20 includes from about 11% to about 15% by weight of tin, about 1% to about 3% by weight of antimony, about 0.5% to about 1.5% in weight of copper, from about 3% to about 5% by weight of nickel, from about 0.3% to about 1.5% by weight of zinc, from about 72% to about 76% by weight of indium, and about 4 % to about 6% by weight of silver, such as about 13.43 wt% tin, about 1.31 wt% antimony, about 0.94 wt% copper, about 2.65 wt% nickel, about 0.49 wt% zinc, about 72.97% by weight of indium, and about 7.54% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 140.64 ° C and the solidus was approximately 129.24 ° C.

In a specific thirty-two embodiment, composition 20 consists essentially of from about 13% to about 17% by weight of tin, about 0.5% to about 1.5% by weight of

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antimony, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of nickel, from about 0.5% to about 1.5% by weight of zinc, from about 73% to about 77% by weight of indium, and about 5% to about 8.5% by weight of silver, such as about 14.05% by weight of tin, about 0.98% by weight of antimony, about 0.87% by weight of copper, about 0.70% by weight of nickel, about 0.63% by weight of zinc, about 74.74% by weight of indium, and about 7.98% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 133.18 ° C and the solidus was approximately 123.94 ° C. The resistivity of this solder composition was approximately 16.24x1o ·⁶ Q-cm.

As used in the present application, in some embodiments, solder compositions consisting essentially of the aforementioned materials are limited to the specified materials and those that do not materially affect the basic and novel characteristics of the solder compositions and electrical connectors including welding compositions. The basic and novel features of solder compositions include the thermal (eg, liquid and solid temperatures) and mechanical (eg, performance tests described below) properties described herein.

In a specific embodiment thirty-three, composition 20 consists essentially of about 12% to about 16% by weight of

<img file="MX344239B_D0048.tif" />

IMPI tffTTTUTO MEXICANO

DE LA noniDA »INDUSTRIAL tin, approximately 0.5% to approximately 1.5% by weight of antimony, approximately 0.5% to approximately 1.5% by weight of copper, from approximately 2% to approximately 4% by weight of nickel, of near

0.5% to about 1.5% by weight of zinc, from about 73% to about 77% by weight of indium, and about 3% to about 7% by weight of silver, such as about 14.14% by weight of tin, about 0.76% by weight antimony, about 0.64% by weight copper, about 2.24% by weight nickel, about 0.75% by weight zinc, about 76.07% by weight indium, and about 5.81 wt% silver. The melting point or temperature (liquidus) of this solder composition was approximately 137.58 ° C and the solidus was approximately 125.92 ° C.

In a specific embodiment thirty-four, composition 20 consists essentially of about 11% to about 15% by weight of tin, about 1% to about 3% by weight of antimony, about 0.5% to about 1.5% by weight of copper, from about 3% to about 5% by weight of nickel, from about 0.3% to about 1.5% by weight of zinc, from about 72% to about 76% by weight of indium, and about 4% to about 8% by weight of silver, such as about 13.43 wt% tin, about 1.31 wt% antimony, about 0.94 wt% copper, about 2.65 wt% nickel, about 0.49 wt% zinc, approximately 72.97% by weight of indium, and approximately 7.54% in

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silver weight. The melting point or temperature (liquidus) of this solder composition was approximately 140.64 ° C and the solidus was approximately 129.24 ° C.

Other compositions may include about 8% by weight of tin, about 10% by weight of antimony, about 1% by weight of copper, about 1% by weight of nickel, about 75% by weight of indium, and about 5% by weight silver, or about 11% by weight of tin, about 10% by weight of antimony, about 1% by weight of copper, about 1% by weight of nickel, about 72% by weight of indium, and about 5% by weight of silver, or about 14% by weight of tin, about 1% by weight of antimony, about 1% by weight of copper, about 1% by weight of nickel, about 1% by weight of germanium, about 75% by weight of indium, and about 7% by weight of silver, or about 21% by weight of tin, about 1% by weight of antimony, about 1% by weight of copper, about 68% by weight of indium, and about 9% by weight of silver, or about 22% by weight of tin, about 1% by weight of antimony, about 5% by weight of copper, about 1% by weight of nickel, about 68% by weight of indium, and about 7% by weight of silver, or about 16% by weight of tin, about 1% by weight of antimony, about 5% by weight of copper,

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about 1% by weight nickel, about 68% by weight indium, and about 9% by weight silver, or about 17% by weight tin, about 1% by weight antimony, about 5% by weight copper, about 68% by weight of indium, and about 9% by weight of silver, or about 16% by weight of tin, about 3% by weight of antimony, about 1% by weight of copper, about 75% by weight of indium, and about 5% by weight of silver.

The invention also relates to an electrical connection in a glass component, as shown in Figures 1 and 2, which includes a glass component, a silver-containing electrical contact surface on the glass component, and an electrical connector soldered to the electrical contact surface on the glass component with a layer of a solder composition with a mixture of elements comprising about 4% to about 25% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.03% to about 4% by weight of copper, from about 0.03% to about 4% by weight of nickel, about 66% to about 90% by weight of indium and about 0.5% to about 9% by weight of silver. In other embodiments, an electrical connection in a glass component includes a glass component, a silver-containing electrical contact surface on the glass component, and an electrical connector soldered to the electrical contact surface on the glass component with a coating of a welding composition comprising

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essentially from about 4% to about 25% by weight of tin, from about 0.1% to about 8% by weight of antimony, from about 0.03% to about 4% by weight of copper, from about 0.03% to near to

4% by weight of nickel, from about 66% to about 90% by weight of indium and about 0.5% to about 9% by weight of silver.

A method 100, shown in FIG. 3A of solder composition 20 includes mixing indium, nickel, copper, silver, antimony and tin to form an alloy including about 66% to about 90% by weight of indium, from about 0.5% to about 9% by weight of silver, from about 0.03% to about 3% by weight of nickel, from about 0.03% to about 4% by weight of copper, from about 0.1% to about 8% by weight of antimony and about 4% to about 25% by weight of tin. Method 100 includes melting indium and tin in step 110 and adding antimony in step 120. Method 100 may optionally include mixing, in step 130, about 0.3% to about 5% by weight of zinc, and optionally mixing , in step 140 from about 0.01% to about 0.3% by weight of germanium. In some embodiments, indium and tin are mixed together in a first molten mixture in step 110, and at least nickel, copper, and silver were mixed in solution in step 115 in a second mixture, which is then cooled in step 125 , optionally ground in step 135 and then added in step 150 to

IMPI Mexican iHSTmrro de LA ERORIEDAD industrial the first molten mixture. A flow chart of the method for forming the weld composition 20 is shown in Figure 3A. The method can be performed in an ambient air atmosphere, without the need for an inert or empty gas environment.

In some embodiments, indium is mixed at a rate of about 70% to about 80% by weight, silver is mixed at a rate of about 4% to about 8% by weight, nickel is mixed at a rate of about 0.1% to about 4% by weight, copper is mixed in a ratio of about 0.1% to about 1.5% by weight, antimony is mixed in a ratio of about 0.2% to about 8% by weight, and tin is mixed in a ratio of about 7% to about 19% by weight. The resulting alloy has indium, silver, nickel, copper, antimony, tin and optionally zinc and germanium in proportions described above for solder composition 20.

In other embodiments, the method 100 of forming the solder composition 20 includes mixing indium, nickel, copper, zinc, silver, antimony, and tin to form an alloy including about 72% to about 77% by weight of indium, from about 4% to about 8.5% by weight of silver, from about 0.5% to about 5% by weight of nickel, from about 0.5% to about 1.5% by weight of copper, about 0.3% to about 1.5% by weight of zinc, from about 0.5% to about 3% by weight of antimony, and about

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11% to about 17% by weight of tin. In these specific embodiments, composition 20 can include from about 74% to about 75% by weight of indium, from about 5% to about 6% by weight of silver, from about 1% to about 4% by weight of nickel, from about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of zinc, from about 0.5% to about 2.5% by weight of antimony, and about 13% to about 15% by weight of tin. Examples of these specific embodiments may include about 75% by weight of indium, about 6% by weight of silver, about 1% by weight of nickel, about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of zinc, from about 0.5% to about 1.5% by weight of antimony, and about 15% by weight of tin, such as about 15% by weight of indium, about 16% by weight silver, about 1% by weight nickel, about 1% by weight of copper, about 1% by weight of zinc, about 1% by weight of antimony, and about 15% by weight of tin. Other examples of these specific modalities may include about 75% by weight of indium, about 5% by weight of silver, about 3% by weight of nickel, about 0.5% to about 1.5% by weight of copper. , from about 0.5% to about 1.5% by weight of zinc, from about 0.5% to about 1.5% by weight of antimony, and about 14% by weight of tin, such as about 75% by weight indium, about 5% by weight silver, about 3% by weight nickel, about 1% by weight of copper, about 1% by weight of zinc, about 1% by weight of

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antimony, and about 14% by weight of tin. Still other examples of these specific embodiments may include from about 74% by weight indium, about 5% by weight silver, about 4% by weight nickel, from about 0.5% to about 1.5% by weight of copper, from about 0.5% to about 1.5% by weight of zinc, from about 1.5% to about 2.5% by weight of antimony, and about 13% by weight of tin, such as about 74% in weight of indium, about 5% by weight of silver, about 4% by weight of nickel, about 1% by weight of copper, about 1% by weight of zinc, about 2% by weight of antimony, and about 13% by weight of tin.

Another method 200, shown in FIG. 3B, for forming the solder composition 20 described above includes, in step 210, heating the desired amount of tin (Sn) in a high temperature furnace pan, such as a pan induction heated solder (eg SM Manfredy, Model N.481), until the tin has melted. The induction heated solder pot is a convenient oven to heat relatively small batches of solder to a high temperature, but requires subsequent additions of ingredients and stirring of the molten mixture in the pot while the current is turned off (heating), for reasons of security. In step 220, the container is quenched and the desired amount of nickel (Ni) in flake form is added, preferably 0.089 square cm to about 0.0254 cm thick. All other metals described below may

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be added in the form of an ingot. It was observed that, with stirring, nickel flakes adhered to the molten mixture and melted in solution more easily than nickel powder, and melting nickel in solution was relatively difficult in part because nickel had the highest point of melting (mp 1455 ° C) of the metals in this weld composition. After stirring the nickel in solution in step 230, the vessel is activated over high heat for about 10 minutes, until the temperature of the molten material reaches approximately 815.5 ° C (1500 ° F). Then, in step 240, the vessel is quenched and the desired amount of copper (Cu), silver (Ag), indium (In), antimony (Sb) and optionally germanium (Ge) are added and stirred, in step 250 , until they melt in the metal solution. Then, in step 255 the container is ignited over high heat until the temperature of the molten matter reaches about 760 ° C (1400 ° F). In step 260, the container is quenched, and the desired amount (optional) of zinc (Zn) is added and stirred until it is melted in the metal solution. The container is then ignited on low heat for a few minutes to equilibrate the metal solution, after which the alloy is ready to be poured into ingots. It was observed that zinc should be added as the last ingredient, because it has a relatively low melting point (mp 419.5 ° C) and excessive exposure of the zinc containing metal solution at high temperature can cause zinc to evaporate from the metal solution.

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Functions of elements in the weld composition

The composition of the solder of the invention is a lead-free alloy that offers the highest service temperature, as well as the mechanical properties in strength and ductility and physical properties in humectants and stability as necessary for the applications of the subject, while offering the desired manufacturing capacity. Desired manufacturing capacity includes allowing a sufficiently low process temperature so that prone manufacturing defects or failures and the silver leaching (recovery) phenomenon that often occurs on metallized electrical contact surfaces containing silver solder can be alleviated or removed. This is accomplished by an indium-based material that is metallurgically alloyed or precipitated or dispersed with antimony, copper, nickel, silver, tin and, optionally, germanium and zinc.

Nickel and copper, in combination with other elements, contribute to the overall performance, including the desired increase in processing temperature, and also contribute to the mechanical properties under the designated processing conditions. Nickel and copper can be effective when added even in small amounts, such as 0.03% by weight. These amounts are greater than the generally accepted impurity level for nickel (0.01%), and greater than the generally accepted impurity level for copper in an application that does not include a solder to a printed circuit board with copper. Antimony, in combination with other elements, contributes to achieving

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the desired temperature range. Antimony can be effective when added even in small amounts, such as 0.1% by weight. Zinc, in combination with other elements, contributes to increase the strength of the alloy without considerably reducing the processing temperature. Zinc can be effective when added even in small amounts, such as 0.3% by weight, which is greater than the generally accepted impurity level for zinc (0.003%). Germanium, in combination with other elements, may contribute to the processability of the weld composition due to its antioxidation properties, although germanium may in some cases not be readily detectable in the composition. Germanium can be effective when added even in small amounts, such as 0.01% by weight or less.

EXEMPLIFICATION

Specific examples of% by weight resulting from solder composition 20 were obtained by inductively coupled plasma atomic emission spectroscopy (ICP-AEC). Solidus and liquidus temperature results were obtained by differential scanning calorimetry (DSC).

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Results and tests of welding performance

I. Temperature delation test

This test was carried out in accordance with DIN EN ISO 16750-4-H section 5.3.1.2. The test samples were 11 glass windshields (4 large, 4 medium, and 3 small) with welded power connectors with a specific embodiment of the weld composition of the present invention. Schematic illustrations of the jumper terminal power connectors 18a and 18b, each having a raised elongated jumper portion extending between two separate solder pads 19 at opposite ends, are shown in Figures 4A and 4B, respectively. Power connectors 18a and 18b are hereafter referred to as power connectors 18. The area of ​​each solder pad 19 was approximately 64 mm², and, as shown in Figure 5, the weld composition 20 has a thickness of approximately 0.5 mm. The power connectors 18 were soldered onto the windshield 10 by rotating the solder ingot into a solder tape, the solder tape refluxing onto a base copper material in a continuous strip, scraping the solder from the stripe to a uniform dimension, sealing and forming the terminal using standard tool, applying flux to the weld surface and soldering the power connector 18 to the target area of ​​the electrical contact strip 16 on the windshield 10 using a resistance welding device, with a power input at a

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range from approximately 750 watt-seconds to approximately

1050 watt-seconds, such as approximately 900 watt-seconds, followed by cooling while power connector 18 was held in place on windshield 10 for a period of time in an interval of approximately 8 seconds and approximately 12 seconds, such as approximately 10 seconds. The composition of solder 20 consisted essentially of approximately 14.05% by weight of tin, approximately 0.98% by weight of antimony, approximately 0.87% by weight of copper, approximately 0.70% by weight of nickel, approximately 0.63% by weight of zinc, approximately 74.74% by weight of indium, and approximately 7.98% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 133.18 ° C and the solidus was approximately 123.94 ° C. A schematic illustration of the complete assembly including power connectors 18 connected to electrical contact strips 16 and power lines 22 on the windshield 10 is shown in Figure 6.

In this test, illustrated in Figure 7, the temperature of a climate controlled chamber (eg Russells, Netherlands MI, model RDV42-25-25 / 11900955 in relatively dry, but uncontrolled, humidity) is cycled for a period of time. 8 hours total ambient (approximately 20 ° C) at -40 ° C and maintained at -40 ° C for 90 minutes, followed by a ramp to 105 ° C for 120 minutes, before returning to room temperature, with 14 V electric current applied through the

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if IMPI ίΝΤΤΤΠΓΓΟ MUICAHO SAY THE PROPERTY

INDUSTRIAL power line 22 from the end of the -40 ° C step and ends at the end of the 105 ° C step, as indicated by the respective arrows shown in Figure 7. After 20 cycles, each power plug 18 was pulled for 3 seconds in the test shot 300 (at room temperature), as shown in Figure 8, in the generally normal direction for the weld layer 20 and windshield surface 10, at a force of 50 N on a digital force gauge 310 (Mark-10 Long Island, NY, model BG100) connected by a hook 320 to connect power 18 approximately midway between the solder pads 19 and manually actuated by handle 330. No failures (ie, connect disconnects) occurred during this test.

II. Hot dip test

This test was performed in accordance with DIN EN ISO 16750-4-K section 5.1.2.2 on nine windshield samples, including 5 welded power connectors with the same solder composition used in test 1. Two windshield samples use a solder composition consisting essentially of approximately 14.14% by weight of tin, approximately 0.76% by weight of antimony, approximately 0.64% by weight of copper, approximately 2.24% by weight of nickel, approximately 0.75% by weight of zinc, approximately 76.07% by weight of indium and approximately 5.81% by weight of silver. The melting point or temperature (liquidus) of this weld composition was

<img file="MX344239B_D0060.tif" />

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INDUSTRIAL approximately 137.58 ° C and the solidus was approximately 125.92 ° C. Two other windshield samples use a solder composition that consisted essentially of approximately 13.43% by weight of tin, approximately 1.31% by weight of antimony, approximately 0.94% by weight of copper, approximately 2.65% by weight of nickel, approximately 0.49% in zinc weight, approximately 72.97% by weight of indium, and approximately 7.54% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 140.64 ° C and the solidus was approximately 129.24 ° C.

In this test 400, illustrated in Figure 9, the temperature of a climate controlled chamber (A &amp; W Blake Heat Chamber) was held at 105 ° C for 96 hours, with 14 V electric current load applied through power line 22 and 6 N mechanical load in a normal direction generally to the solder layer 20 and the surface of the windshield 10 (applied by the connection of weight 410 to the connector Power 18 per hook 420 located approximately midway between the solder pads 19) directed vertically downward as gravity acceleration for the entire 96 hours. The temperature of the power connectors (measured by 430 thermocouple) increased to a maximum of approximately 120 ° C during the test due to the applied electrical load. After 96 hours of testing, each power connector was pulled (at room temperature) as shown in Figure 8 and described above, at a force of 50N on a digital force gauge for 3

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seconds (Mark-10 Long Island, NY, model BG50).

There are no failures (i.e., the connector disconnects, or microcracks) occurred during this test.

III. High temperature storage test

This test was performed on the same test samples as previously used for Test I. In this test, the temperature of a climate controlled chamber (in relatively dry, but uncontrolled humidity) was kept at a constant of 120 ° C for 24 hours without any electrical or mechanical load from the power connectors. After the end of 24 hours, each power connector was pulled (at room temperature) as shown in Figure 8 and described above, at a force of 50N on a digital force gauge for 3 seconds (Mark-10 Long Island, NY, model BG100). There are no faults (that is, the connector disconnects) occurred during this test.

IV. Long-term test with electric charge

This test was performed on the same test samples as previously used for tests I and III. In this test, the temperature of a climate controlled chamber (relatively dry, but uncontrolled humidity) was held at a constant of 105 ° C for 500 hours under 14 V electric current for the full 500 hours. After the end of 500 hours, each power connector was pulled (at room temperature) as shown in Figure 8 and described

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above, at a force of 50N on a digital force gauge for 3 seconds (Mark-10 Long Island, NY, model BG100). There are no faults (that is, the connector disconnects) occurred during this test.

V. Heat shock test

This test was carried out in accordance with DIN EN ISO 16750-4-H section 5.4.2. The test samples were five 30.48 cmx20.48 cm tempered glass plates with 30 power connectors each. The plates were 4mm thick, stained, enamel printed and overprinted with six 2.54cm wide silver strips. The power connectors were soldered to the silver strips. The two plate power connectors were soldered with a solder composition consisting essentially of approximately 14.05% by weight of tin, approximately 0.98% by weight of antimony, approximately 0.87% by weight of copper, approximately 0.70% by weight of nickel, about 0.63% by weight of zinc, about 74.74% by weight of indium, and about 7.98% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 133.18 ° C and the solidus was approximately 123.94 ° C. The power connectors on one another plate were soldered with a solder composition consisting essentially of approximately 14.14% by weight of tin, approximately 0.76% by weight of antimony, approximately 0.64% by weight of copper, approximately 2.24% by weight of nickel, approximately

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0.75 wt% zinc, about 76.07 wt% indium, and about 5.81 wt% silver. The melting point or temperature (liquidus) of this solder composition was approximately 137.58 ° C and the solidus was approximately 125.92 ° C. The power connectors on an additional board were soldered with a solder composition consisting essentially of approximately 13.43% by weight of tin, approximately 1.31% by weight of antimony, approximately 0.94% by weight of copper, approximately 2.65% by weight of nickel , approximately 0.49% by weight of zinc, approximately 72.97% by weight of indium, and approximately 7.54% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 140.64 ° C and the solidus was approximately 129.24 ° C.

In this test, one cycle consisted of heating the samples in a climate controlled chamber to 105 ° C for one hour without electrical or mechanical load, followed by completely immersing the samples in cold water (approximately 23 ° C or lower, from the refrigerator) . The samples were dried with compressed air after each cycle. After 5 cycles and then after 10 cycles, each power connector was pulled (at room temperature) as shown in Figure 8 and described above, at a force of 50N on a digital force gauge for 3 seconds (Mark -10 Long Island, NY, model BG100). There are no faults (that is, the connector disconnects) occurred during this test.

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SAW. High humidity tests: Constant climate

In this test, carried out in accordance with DIN EN ISO 6270-2CH, eight windshield samples were exposed in an ambient chamber at a constant temperature of 80 ° C and a humidity of&gt; 96% RH (generated steam) for a total of 504 hours, with electric current charging at the 14 V power connectors (approximately 22 A drawing) for 15 minutes from 10 hours after reaching the specified temperature and humidity, and for 15 minutes every 24 hours thereafter until the end of 504 hours. The temperature of the power connectors (measured by thermocouples) increased to a maximum of approximately 95 ° C during the test due to the applied electrical load. After the end of 504 hours, each power connector was pulled (at room temperature) as shown in Figure 8 and described above, at a force of 50N on a digital force gauge for 3 seconds (Mark-10 Long Island, NY, model BG100). If the silver layer (electrical contact surface 16) separates the glass 10, during the 504 hours or during the drag test, then the drag tests and electrical tests cannot be performed, and the contact of the weld was evaluated as good . However, a sample of windshield from each of the three weld compositions described above in Test V completes the high humidity / constant climate test without failure (i.e. connector is disconnected).

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Vile. Resistance to classify washing fluids

The test sample was a 30.48 cm x 30.48 cm glass plate with 30 power connectors each (as described above), soldered with a solder composition consisting essentially of approximately 14.05% by weight tin, approximately 0.98% by weight of antimony, about 0.87% by weight of copper, about 0.70% by weight of nickel, about 0.63% by weight of zinc, about 74.74% by weight of indium, and about 7.98% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 133.18 ° C and the solidus was approximately 123.94 ° C.

In this test, the sample was immersed for 24 hours in a simulated windshield wash solution made of 11 and 1/8 cups of water, 3 and 1/6 cups of ethanol, 1.6 cups of isopropanol, 1 and 1/4 tablespoons of ethylene glycol and a fourth tablespoon of sodium lauryl sulfate. After the end of 24 hours, each power connector was pulled (at room temperature) as shown in Figure 8 and as described above, except that Force Gauge 310 was an Instron Force Gauge operated at a speed of 100 mm / min at a force of 50 N in a force gauge for 2 seconds (Instron, Norwood, MA model 5544). There are no faults (that is, the connector disconnects) occurred during this test.

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Vile. Salt spray test

This test was carried out in accordance with DIN EN ISO 9227 section

8. The test sample was a 30.48 cm x 30.48 cm glass plate with 30 power connectors each (as described above), soldered with a solder composition consisting essentially of approximately 14.05% by weight tin, approximately 0.98% by weight of antimony, about 0.87% by weight of copper, about 0.70% by weight of nickel, about 0.63% by weight of zinc, about 74.74% by weight of indium, and about 7.98% by weight of silver. The melting point or temperature (liquidus) of this solder composition was approximately 133.18 ° C and the solidus was approximately 123.94 ° C.

In this test, the test sample was exposed to a salt spray mist in a test chamber (Harshaw model 22) for 96 hours. The salt concentration was 5% and the pH was between 6.5 and 7.2. The salt mist temperature was set at + 35 ° C + 2 ° C and the tower temperature was set at + 48 ° C, with the air pressure between 16 and 18 psi. After the end of 96 hours, each power connector was pulled (at room temperature) as shown in Figure 8 and described above, except that Force Gauge 310 was an Instron Force Gauge operated at a speed of 100mm / min at a force of 50 N for 2 seconds (Instron, Norwood, MA model 5544). There are no faults (that is, the connector disconnects) occurred during this test.

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The teachings of all patents, published applications and references cited here are incorporated by reference in their entirety.

Although this invention has been particularly shown and described with reference to its exemplary embodiments, it will be understood by those of skill in the art that various changes in form and detail can be made without departing from the scope of the invention as included in the claims attached.