Hollow cathode target and methods of making same.
Abstract
Sputtering targets and methods of making sputtering targets are described. The method includes the steps of: providing a sputtering metal workpiece made of a valve metal; transverse cold-rolling the sputtering metal workpiece to obtain a rolled workpiece; and cold-working the rolled workpiece to obtain a shaped workpiece. The sputtering targets exhibits a substantially consistent grain structure and/or texture on at least the sidewalls.

Term
Term ended
Expired 20 November 2021, 4.8 years ago.
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12 claims: 1 independent, 11 dependent
- 1NOVEDAD DE LA INVENCION Habiéndose descrito la invención como antecede, se reclama como propiedad lo contenido en las siguientes:REIVINDICACIONES 5 . 1. Un método para fabricar un objetivo o anticátodo de deposición electrónica, caracterizado porque comprende los pasos de: proporcionar una pieza de trabajo de metal de 10 deposición electrónica que comprende al menos un metal de válvula;laminar transversalmente la pieza de trabajo de metal de deposición electrónica para obtener una pieza de trabajo laminada;y 15 trabajar en frío la pieza de trabajo laminada para obtener una pieza de trabajo formada.
- 2El método de conformidad con la reivindicación 1, caracterizado porque incluye además el paso de relevar de esfuerzos la pieza de trabajo de metal 20 de deposición electrónica entre los pasos de laminación transversal y trabajo en frió.
- 3El método de conformidad con la reivindicación 2, caracterizado porque el paso de relevo de esfuerzos es a una temperatura de aproximadamente 25 600°C hasta aproximadamente 850°C.
- 4El método de conformidad con la reivindicación 1, caracterizado porque la pieza de trabajo de metal de deposición electrónica no es recocida o relevada de esfuerzos entre los pasos de laminación 5 transversal y trabajo en frío.
- 5El método de conformidad con la reivindicación 1, caracterizado porque incluye además el paso de recocer la pieza de trabajo de metal de deposición electrónica entre los pasos de laminación 10 transversal y trabajo en frío.
- 6El método de conformidad con la reivindicación 2 caracterizado porque el paso de recocido es a una temperatura de aproximadamente 950°C hasta aproximadamente 1300°C. 15
- 7El método de conformidad con la reivindicación 2 caracterizado porque el paso de relevos de esfuerzos comprende el paso de relevo de esfuerzos la pieza de trabajo de metal de deposición electrónica durante aproximadamente 2 horas. 20
- 8El método de conformidad con la reivindicación 6 caracterizado porque el paso de recocido comprende el paso de recocer la pieza de trabajo de metal de deposición electrónica durante aproximadamente 2 horas.
- 9El método de conformidad con la reivindicación 1, caracterizado porque el metal de válvula es tantalio, niobio o una aleación de los mismos. reivindicación 1, caracterizado porque comprende además el paso de limpiar con máquina la pieza de trabajo 10 formada para obtener el objetivo o anticátodo de deposición electrónica. 12. El método de conformidad con la reivindicación 1, caracterizado porque el paso de proporcionar una pieza de trabajo de metal de deposición 15 electrónica comprende los pasos de:forjar plano un lingote que comprende al menos un metal de válvula;cortar el lingote forjado en placas;y limpiar con máquinas las placas. 20 13. El método de conformidad con la reivindicación 1, caracterizado porque el paso de laminación transversal comprende el paso de laminar la pieza de trabajo de deposición electrónica como una pieza de trabajo de laminación un número de veces en una primera dirección y un número de veces en una segunda dirección perpendicular a la primera dirección. 14. El método de conformidad con la reivindicación 1, caracterizado porque el paso de 5 laminación transversal comprende el paso de laminar la pieza de trabajo de deposición electrónica como una pieza de trabajo de laminación tantas veces en la primera dirección como en la segunda dirección. 15. El método de conformidad con la
- 1010 reivindicación 13, caracterizado porque el paso de laminación transversal comprende los pasos de:laminar la pieza de trabajo de deposición electrónica un número de veces en la primera dirección, y posteriormente laminar la pieza de trabajo de 15 laminación un número de veces en la segunda dirección. 16. El método de conformidad con la reivindicación 1, caracterizado porque la pieza de trabajo laminada tiene un espesor de laminación predeterminado. 20 17. El método de conformidad con la reivindicación 16, caracterizado porque el espesor de laminación predeterminado es de aproximadamente 0.63 centímetros (0.25 pulgadas) hasta aproximadamente un calibre de 5 centímetros (2). ' 18. El método de conformidad con la reivindicación 1, caracterizado porque incluye además el paso de recocer la pieza de trabajo de metal de deposición electrónica antes del paso de laminación 5 transversal. 19. El método de conformidad con la reivindicación 18, caracterizado porque el paso de recocido antes del paso de laminación transversal es a una temperatura de aproximadamente 1050°C hasta 10 aproximadamente 1300°C. ' 20. El método de conformidad con la reivindicación 1, caracterizado porque el paso de laminación de la pieza de trabajo laminada comprende el estirado profundo de la pieza de trabajo laminada, la 15 formación por torneado de la pieza de trabajo laminada, o la formación por flujo de la pieza de trabajo laminada, o combinaciones de los mismos. . 21. El método de conformidad con la ' reivindicación 1, caracterizado porque el paso de 20 trabajar en frío la pieza de trabajo laminada comprende primero el estiramiento profundo de la pieza de trabajo laminada para formar una preforma, y a continuación formar por flujo la preforma sobre un mandril. 22. El método de conformidad con la 25 reivindicación 17, caracterizado porque el paso de recocido antes del paso de la laminación transversal comprende los pasos de recocer la pieza de trabajo de metal de deposición electrónica durante aproximadamente 2 horas. 5 23. El método de conformidad con la reivindicación 1, caracterizado porque la pieza de trabajo formada exhibe al menos 50% de reducción en frío Λ con respecto a la pieza de trabajo de metal de deposición electrónica (SMW) laminada. 10 24. El método de' conformidad con la reivindicación 1, caracterizado porque la pared lateral de la pieza de trabajo formada exhibe una reducción de menos del 50% en frío con respecto a la pieza de trabajo laminada.
- 1115 25. El método de conformidad con la reivindicación 1, caracterizado porque la pieza de trabajo formada es de forma cilindrica o de copa. 26. El método de conformidad con la reivindicación 1, caracterizado porque el paso para 20 trabajar en frío la pieza de trabajo laminada comprende 25 reivindicación 1, caracterizado porque comprende además 49 w 9 el paso de relevar de esfuerzos la pieza de trabajo formada después del paso de trabajo en frío. - 28. El método de conformidad con la reivindicación 1, caracterizado porque comprende además ' 5 el paso de recocer la pieza de trabajo formada después del paso de trabajo en frío. 29. El método de conformidad con .la reivindicación 27, caracterizado porque el paso de relevo de esfuerzo después del paso de trabajo en frió ocurre a 10 una temperatura de aproximadamente 600 °C hasta aproximadamente 850°C. 30. El método de conformidad con la reivindicación 28, caracterizado porque el paso de recocer después del paso de trabajar en frío ocurre a una 15 temperatura de aproximadamente 900 °C hasta aproximadamente 1300°C. 31. .El método de conformidad con la reivindicación 1, caracterizado porque el objetivo o anticátodo de deposición electrónica tiene forma de copa 20 o cilindrica y tiene una altura de aproximadamente 26.67 centímetros (10.5 pulgadas), un diámetro interno de aproximadamente 24.49 centímetros (9.25 pulgadas), un diámetro externo de aproximadamente 24.13 centímetros (9.50 pulgadas) y un espesor de la pared lateral de 1 25 aproximadamente 0.63 centímetros (0.25 pulgadas). 32. Un método para recuperar metal de válvula de un objetivo o anticátodo de deposición electrónica usado o gastado hecho de conformidad con el método de la reivindicación 1, caracterizado porque comprende el paso 5 de hidratar el metal de válvula para obtener metal de válvula hidratado. 33. El método de conformidad con la reivindicación 32, caracterizado porque comprende además los pasos de:10 moler el metal de válvula hidratado para obtener polvo hidratado de metal de válvula;separar un metal de válvula hidratado del blindaje de metal no hidratado, desgasificar el polvo hidratado del metal de 15 válvula para obtener polvo de metal de válvula desgasificado;y procesar el polvo de metal de válvula desgasificado para obtener un lingote de metal de válvula.
- 1220 34. El método de conformidad con la reivindicación 1, caracterizado porque la pieza de trabajo formada tiene un borde donde el borde es sometido a laminado para formar un reborde. 35. El método de conformidad con la 25 reivindicación 1, caracterizado porque la pieza de trabajo de metal dé deposición electrónica es una placa y se une una segunda placa de refuerzo de metal sobre la primera placa antes de someter la pieza de trabajo laminada al trabajo en frío. 5 36. El método de conformidad con la reivindicación 35, caracterizado porque la unión es por unión explosiva, unión mecánica, unión por laminación, o combinaciones de las mismas. 37. El método de conformidad con la 10 reivindicación 35, caracterizado porque la segunda placa de refuerzo de metal es de cobre. 38. ’ El método de conformidad con la reivindicación 35, caracterizado porque la segunda placa de refuerzo de metal es de un metal diferente al de la 15 pieza de trabajo de metal de deposición electrónica. 39. El método de conformidad con la reivindicación 1, caracterizado porque comprende además cortar una pieza de trabajo en forma de disco para la pieza de trabajo laminada antes de trabajar en frío la 20 pieza de trabajo laminada. 40. Un objetivo o anticátodo de deposición electrónica, caracterizado porque se fabrica de conformidad con el método de la reivindicación 1. 41. Un montaje de objetivo o ' anticátodo de 25 deposición electrónica, caracterizado porque comprende el objetivo o anticátodo de deposición electrónica de conformidad con la reivindicación 40, y porque comprende además una porción superior hecha de un material no depositado electrónicamente unido a las paredes laterales 5 del objetivo o anticátodo de deposición electrónica, o un blindaje externo de un material que no puede ser depositado electrónicamente donde el objetivo o anticátodo de deposición electrónica está asegurado al blindaje externo o ambos. 10 42. El montaje de objetivo o anticátodo de deposición electrónica de conformidad con la reivindicación 41, caracterizado porque la porción superior está hecha de un material base de metal de válvula que tiene una textura fuerte (100). 15 43. El montaje de objetivo- o anticátodo de deposición . electrónica de conformidad con la reivindicación 42, caracterizado porque el material base de metal de válvula es un material basado en tantalio, un material basado en niobio, o ambos. 20 44. El montaje de objetivo o anticátodo de deposición electrónica de conformidad con la reivindicación 42, caracterizado porque el material base de metal de válvula es un metal de válvula o aleación del mismo que tiene una textura fuerte (100). 45. El montaje de objetivo o anticátodo, de deposición electrónica de conformidad con la reivindicación 44, caracterizado porque la aleación de metal de válvula comprende tantalio y tungsteno. 5 46. El montaje de objetivo o anticátodo de deposición electrónica de conformidad con la' reivindicación 41, caracterizado porque la porción superior está hecha de un material no hidratado. 47. El montaje de objetivo o anticátodo de 10 deposición electrónica de conformidad con la reivindicación 41, caracterizado porque el blindaje externo está hecho de un material no hidratante. 48. El montaje de objetivo o anticátodo de deposición electrónica de conformidad con la 15 reivindicación 47, caracterizado porque el blindaje externo comprende aluminio, cobre o ambos. 49. Un objetivo o anticátodo, caracterizado porque comprende al menos un metal de válvula, donde el objetivo o anticátodo tiene un diseño HCM y el objetivo o 20 anticátodo tiene a) un tamaño de grano de 5 ASTM o más fino;b) una textura global mezclada (111)—(100);c) un tamaño de grano uniforme, donde la varianza del tamaño de grano es +/-2 ASTM;o 25 combinaciones de los mismos. 50. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque el objetivo o anticátodo tiene al menos dos de las tres propiedades. 51. El objetivo o anticátodo de conformidad con 5 la reivindicación 49, caracterizado porque el objetivo o anticátodo tiene las tres propiedades. 52. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque el objetivo o anticátodo está al menos parcialmente recristalizado. 10 53. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque el objetivo o anticátodo está al menos 95% recristalizado. 54. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque el objetivo o 15 anticátodo está completamente recristalizado. 55. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque está presente la propiedad a) y la textura global tipo primaria (111) está libre de bandas puntiagudas, localizadas de textura 20 (100). 56. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque está presente la propiedad a) y el tamaño de grano es de aproximadamente 5 ASTM hasta aproximadamente 13 ASTM. 57. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque está presente la propiedad a) y el tamaño de grano es de aproximadamente 5 ASTM hasta aproximadamente 10 ASTM. 5 58. El objetivo o anticátodo de conformidad con la reivindicación 49, caracterizado porque está presente la propiedad a) y el tamaño de grano es de aproximadamente 7 ASTM hasta aproximadamente 9 ASTM. 59. El método de conformidad con la 10 reivindicación 1, caracterizado porque el trabajo en frío es un trabajo en frío multidireccional. I 56 j
Independent claims12
150 paragraphs in 9 sections, as filed
(54) Title: HOLE CATHODE OBJECTIVE AND METHODS FOR MANUFACTURING THE SAME.
(54) Title: HOLLOW CATHODE TARGET AND METHODS OF MAKING SAME.
(57) Summary
Electronic deposition targets and methods are described for manufacturing electronic deposition targets. The method includes the steps of: providing an electron deposition metal workpiece made of a valve metal; transversely roll the work piece of metal of electronic deposition to obtain a rolled piece; and cold working the rolled part to obtain a formed workpiece. Electron deposition targets exhibit a substantially consistent grain structure and / or texture on at least the side walls.
(57) Abstract
Sputtering targets and methods of making sputtering targets are described. The method includes the steps of: providing a sputtering metal workpiece made of a valve metal; transverse cold-rolling the sputtering metal workpiece to obtain a rolled workpiece; and cold-working the rolled workpiece to obtain a shaped workpiece. The sputtering targets exhibits a substantially consistent grain structure and / or texture on at least the sidewalls.
MñY-23-2003 10:14
CABOT LALJ - IP GROUP
97Θ 670 Θ027 P.03 / 32 (13) INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPKRATION TRIATV (PCD (U) World Intellcetanl Proparty ΟιχιηίζΑίίΟΛ unnecessaryrnitlonal Butwu (43) Internal uncle my Publication Data 3OMeylOO2Q0.O5.2001)
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PCT (10) International Publication Numbor WO 02/42513 A2 (31) lulriiutlonal Patent CWuifiotioA C13C ILOU (XI) Infernitlonvl Applk'KÜou Nainber: PCT / US0LM337Í (W) Iniernirlnaal Filing Date:
2 (1 November 2001 (20.112001) (35) Fifint LMjaac *<sup>1</sup> English (24) Publication L ^ ntMtei tngüth (3 *) Prlurlty Dula;
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j (71) JineiKoit FORD, Robert, D .; 316 Playgoond Οπ / ο, West Rcañíni. PA 19011 (US). MICHALÜK Chrialuph ”r, A .; 2306 UM "" ni CtmIA ftjlhnrttvilte, TA 19525 (74) Alano LANDO, Michtlle, D. (Cabal Corporntloti, 157 * Contad Roed. PO Box 7001. Blllerici MA 01821-7001 = (US) (VI) Daaignat "t Sratwi ( hn (iono (): AE, AG, aL AM, AT, AU, AÁ, ΒΛ, BB, BG, m, B Y. HZ, CA. “.Ή, pN, CO CR. C7. DE. DK, DM , DZ, EC, BE ES. FL GB, GD, GE GH, CJM, HR. HU. ID. IL IN Ja. JP, KE, KO, KP, KR. KZ, LC. LE VR. 15, i. T, 1.11. LV. MA, MD.M0.MK. MH MW, MX, ΜΣ, NO, NZ, OM. PH. Pl „Mr, kO. RU. SD, SE, SO. SL SK. SL, TJ, TM, TR, ΤΓ, TE UA, UG. UZ, VN, ϊ U. 2a. ZW.
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HOLLOW CATHODE OBJECTIVE AND METHODS TO MANUFACTURE THE SAME? BACKGROUND OF THE INVENTION, The present invention relates to an objective or target of electronic deposition and to methods for manufacturing the same.
• Its used various techniques of electronic deposition to affect the deposition of a film by restraining the surface of a substrate. The deposited metal films, like metal films on a thin film semiconductor device, can be formed by a magnetron electron deposition apparatus or other electron deposition techniques. The magnetron electron deposition apparatus induces 15 plasma ions from a gas to bombard a target or target, causing the surface particles of the target or target material to be ejected from it, and to be deposited as a film or layer over the area of to substrate. Conventionally, an electron deposition source in the form of a flat disk or rectangle is used as the target or target, and the ejected atoms travel along an optical horizon path to deposit on top of a disc whose deposition face 25 is parallel to the erosion of the target face or target. A hollow cathode magnetron electron deposition (HCM) target or target in the form of a crucible or inverted cup can be used as the target or target material. An internal chamber or electron deposition cavity defined by the target or target contains a plasma that erodes the surfaces of the interior wall of the target or target in the manner mentioned above. An attribute of an electron deposition system that employs a hollow cathode target or target is its ability to deposit a film that is capable of filling deep and narrow channels in the substrate. This is accomplished when the atoms of the target or target, ejected from the anterior walls of the target or target, are ionized as they pass through the plasma. The magnetic fields then direct the ions in a direction perpendicular to the substrate.
The electronic CD magnetron deposition or standard magnetron electronic deposition involves the 20 well-known principles of cross-field electric gas discharges to give very high deposition rates, as well as other highly desirable parameters. The high deposition rates simply result from the fact that the magnetically enhanced discharge plasmas allow a very high power density under available conditions. With this technique, high deposition rates at low pressures are typical, and good uniformity and gradual coverage are possible. It is also possible to use alternating voltage FR 5 (radio frequency) instead of DC voltage in magnetron electron deposition. A disadvantage of the prior art, however, is that the good deposition uniformity it provides is at the expense of not very uniform erosion of the target or target. In this way, the life of the target or target suffers.
Examples of its electron deposition devices and methods described in US Patent Number 5,693,197 to Lal et al., US Patent Number 5,997,697 to Guenenfelder et al., US Patent Number et al. , US Patent Number 6,033,536 from Ichihara et al., US Patent Number 5,529,674 from Hedgeoth, US Patent Number 5,656,138 from Scobey et al., US Patent Number 6,063,245 to Frach et al. ', US Patent Number 5,437,778 to Hedgooth, US Patent Number 6,077,407 to Lichr et al., US Patent Number 5,770,025 to Kiyadent8,178,178 US Patent Number 5,770,025 to Kiyadent8,178 US Patent Number 5,770,025 Estadent8,17,178,07825 Patent Number Kiyadent8,17,178,07825 No. 5,171,415 from Miller et al., US Patent No. 6,083,364 from Ikeda et * al., US Patent No.o unidense Number 3,884,793 from Penfold et al., and US Patent Number 5,393,398 of
Sugano, all of which are incorporated herein by reference in their entirety.
The tantalum hollow cathode magnetron (HCM) electron deposition targets are conventionally manufactured using crucibles that have been manufactured by welding and / or deep drawing. Those techniques tend to impart metallurgical homogeneities to the cathode, which have a damaging impact on the performance of the electronic deposition. For example, weld beads and the surrounding heat affected zone exhibit a। structure and texture of grain that differs from the remaining of the material. These metallurgical inhomogeneities can create parasitic magnetic fields that impede the electron deposition process. Similarly, deep drawing or turning of an annealed or stress-relaxed plate can generate lower amounts of stress that are unevenly distributed around the workpiece, resulting in an annealing and / or erosion response from the deposition of the variables. Consequently, a
One of the disadvantages of the HCM targets or targets produced as described above is that they erode non-uniformly, resulting in a low number of acceptable discs from each tantalum HCM target due to non-uniform deposition of the target. or target on substrate.
In him. design of the target and its associated magnetic field, two main targets are a uniform erosion of the target and a uniform deposition of the target material on the substrate.
The techniques of electronic deposition that are intended to resolve the above objectives involve the use of the electronic deposition with a gyratory magnet CD magnetron, or of additional stationary constituents to be used in the electronic deposition device. The first technique mentioned is responsible for the question of efficiency of use of the. material by moving the magnet structure over the surface of the target or target to simultaneously obtain the uniform use of the material and a gradual adequate coverage. An example of the first technique is described in US Patent Number 5,770,025 to Kiyota, US Patent Number
5,188,717 from Broadbent et al., US Patent
Number 5,171,415 of Miller et al., And US Patent Number 6,083,364 of Ikeda et al., All * incorporated herein by reference in their entirety. An example of the second technique is described in Patent
Sugano, US No. 5,393,398, where a particle interceptor is deposited between the target or target and the substrate to produce a uniform deposited layer on the substrate. However, the above techniques are disadvantageous since they imply the need to use complete equipment and / or expensive with an electronic deposition apparatus.
All patents and publications mentioned above and therein are incorporated in their entirety herein by reference.
SUMMARY OF THE INVENTION
The present invention relates to an electronic deposition target or target, such as an HCM target or target, that exhibits, preferably a structure and texture of 'grain substantially uniformly at least on the side walls thereof. Preferably, any stress within the electron deposition target or target is substantially uniformly distributed through at least the side walls thereof. The electron deposition target or target exhibits, preferably, substantially uniform erosion of electron deposition.
The present invention is also directed to a method of fabricating a hollow cathode magnetron electron deposition target or target that is suitable for causing a uniform film of electronically deposited material to be deposited on a substrate, and with a target of or target. electronic deposition done according to the method. The present invention can be used in different ways suitable to give deposition of a thin film on substrates of different geometries. The objective or target of the present invention preferentially erosion uniformly during the operation and does not require moving parts or additional components, thus providing a simple, cheap and reliable system of electronic deposition of magnetron.
The present invention further provides a method of fabricating a target or target of electronic deposition that involves the steps of providing an electron deposition metal workpiece made of a valve metal; rolling 25 transversely the work piece of metal of electronic deposition to obtain a rolled piece; and cold working the rolled workpiece to obtain a formed workpiece. Optionally, the method includes the additional step to anneal the part of 5 metal work of electronic deposition between the cross-rolling and cold work steps.
The present invention further includes within its scope an electron deposition target or target assembly that contains the electron deposition target described above, and further includes at least one of an upper portion made of a non-deposition or corrosion resistant material. deposition or deposition resistant or can be electronically deposited attached to the side walls of the target or electron deposition target, There is a 15 external shield made of a material that cannot be deposited electronically, where the target or target of electron deposition is secured to the external shield.
The present invention further relates to 20 targets or targets, such as HCM targets or targets.
You should understand that both the above general description and the following detailed description are exemplary and explanatory only and are not intended to provide an additional explanation of the present invention, as claimed. The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate various exemplary embodiments of the present invention and, together with the description, serve to explain the principles of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention may comprise of 10 more complete with reference to the accompanying Figures. Claim that the Figures illustrate exemplary embodiments of the present invention without limiting the scope of the invention.
The Figure 1 is a schematic representation 15 of an embodiment of a magnetron electronic deposition apparatus that uses an objective or target of electronic deposition made according to the method of the present invocation;
Figure 2 is a perspective view of the target or target of electronic deposition of Figure 1;
Figure 3 is a view similar to Figure 2, showing one embodiment of an electron deposition target assembly made in accordance with the present invention;
Figures 4a and 4b are schematic representations of the transverse laminating step according to the method of the present invention; Y
Figure 5 is a flow diagram showing 5 steps of the method according to the method of the present invention.
Figures 6 to 9 are graphs showing graphs of the grain size distribution of the samples used in the examples.
DETAILED DESCRIPTION OF THE PRESENT INVENTION
The present invention provides a method for fabricating an electronic deposition target or target. The method includes providing a workpiece of metal of electronic deposition made of a metal of valve, preferably of tantalum or niobium or alloys thereof. Subsequently, the workpiece of metal of electronic deposition is cross-laminated to obtain a laminated workpiece. The rolled workpiece is then cold worked to obtain a formed workpiece. According to the present invention, the workpiece of metal of electronic deposition can be optionally annealed between the steps of cross rolling and cold working. In certain embodiments, this optional annealing step is avoided.
- The present invention also includes an electron deposition target or target. The 5 targets or targets of electron deposition preferentially exhibiting a structure and / or texture of grain substantially consistent or uniform at least on the side walls thereof. Any stress within the electron deposition target or target is preferably substantially uniformly distributed through at least the side walls of the target or target. The target or target of electron deposition therefore preferably exhibits substantially uniform erosion by electron deposition.
As an option, the present invention further includes within its scope an electron deposition target or target assembly that contains the electron deposition target or target described above and further includes at least one of a top portion can be deposited. electronically attached to the side walls of the electron deposition target or target, There is a high-quality external shield of material that cannot be deposited electronically. The electron deposition target is secured to the outer shield.
Referring now to Figure 1, an embodiment of a magnetron electron deposition apparatus that uses an electron deposition target produced by the present invention is schematically exemplified. As described in Figure 1, a magnetron 1 electron deposition apparatus includes an electronic 3 crucible-shaped deposition target or target, i.e., an elongated, hollow cup-shaped member, as shown in Perspective in Figure. 2. The electron deposition target or target 3 includes interior walls 9, exterior walls 11, and an upper portion 15. In the
Figure 1, the electron deposition target 3 is shown as having been placed in an outer shield or cladding 20 to form the electron deposition assembly 4 as shown. The apparatus 1 further includes a substrate 5 positioned on a substrate holder 6 located adjacent to the electron deposition cavity 1 defined by the interior walls 9 of the electrodeposition target or target 3. Adjacent to the outer walls 11 of the target or electrodeposition target 3 are means 13, such as magnets or electromagnets.
Ί permanent, to provide MF magnetic flux lines that its substantially parallel to the longitudinal axis L of the target or electron deposition target and continuous with the inner walls 9 thereof. The 5 MF magnetic flux lines create a physical trap to contain the bright discharge electrons from the target or electron deposition target 3, as would be easily recognized by one skilled in the art. The means 13 can take any variety of forms, 10 such as a plurality of bar magnets, a plurality of toroidal magnets, or any other means to generate the magnetic flux lines MF as shown in Figure 1. The form of operation of An apparatus such as apparatus 1 in Figure 1 is within the knowledge 15 of one skilled in the art. The electron deposition process, carried out with the apparatus of Figure 1 in a vacuum chamber in the presence of an inert gas, such as argon, (Ar), involves the ionization of the molecules, of the inert gas in cavity 7. This Ionization is brought about under the effect of an electronic field created by applying voltage across the target lens 3 and the substrate holder 6 to produce ionized plasma or inert gas molecules. The ions of plasma then collide with the internal walls 9 of the target or 25 electronic deposition target 3, causing the atoms to be ejected from the internal surface of the target. The ejected target atoms then travel through the plasma, during which a substantial fraction of the ejected target or target atoms are themselves ionized by the plasma.
Once ionized, the target anions are directed to travel along a path perpendicular to the surface of the substrate 5 by an external magnetic field, after which they are deposited on the substrate to form a deposited layer. about him. According to the present invention, the target or target of electronic deposition 3 is formed in such a way that it provides good uniformity of deposition with respect to the substrate while also eroding additionally, without the need to use moving parts in the apparatus of comelronica magnets or rotating substrates, and without the need for additional components as part of the electronic deposition apparatus. Although not necessary, those techniques can optionally be used in the present invention.
The present invention preferably provides an electronic deposition target or target suitable for an HCM assembly that has a substantially homogeneous microstructure at least —--- ---- --- - - - ..... .... | around its inner side walls, that is, a substantially consistent grain structure and texture at least around its inner side walls. The present invention further provides a method for forming the above electronic deposition target or target.
One embodiment of the method of the present invention is described in the form of a flow chart in Figure 5, where some optional steps have been indicated by discontinuous direction arrows. From according to the present invention, as observed in Figure 5, an electron deposition metal workpiece made of a valve metal, such as niobium (Nb), tantalum (la), aluminum (Al), titanium (Ti ), vanadium (V), circumio (Zr), or alloys thereof (hereinafter electron-deposited metals) is provided in step 100. For the purposes of this invention, a valve metal includes copper (Cu). Before step 100, any of the conventional, standard steps such as melting and flat forging and the like can be used. In order to provide the electrodeposition workpiece, a made ingot of a metal of valve is preferably flat forged first, plate cut and machine cleaned to provide the electrodeposition workpiece are conventional, describes oneself in C. Pokross, Controlling the Texture of Tantalum Píate, Journal of Metals, October 1989, pp. 4649; JB Clark, RK Garrett, Jr., TL Jungling, and RI
Asfahani, Influence of Transverse Rolling on the Microstructural and Textural Development in Puré
Tantalum, Metallurgical Transactions A, 23A, pp. 21832191, and the like, all incorporated herein by reference in their entirety.
. The electron deposition metal workpiece is then used as a rolling workpiece and transversely rolled in step 110 has a predetermined rolling thickness to obtain a rolled workpiece. Preferably, the default lamination thickness is from about 0.63 centimeter (1/4 inch) to about 2.54 centimeter (1 inch) or more, although other thicknesses can be easily utilized. The rolling workpiece in the context of the electroplated metal workpiece is used until, from the first rolling step where the electroplated metal workpiece is used until the rolled workpiece is produced. with the predetermined lamination thickness. In the transverse rolling step, as observed in Figures 4a and 4b, a rolling workpiece 19 is rolled by a conventional rolling device 17 in a direction perpendicular to the axis (center line) of the ingot defined as A to form another thinner rolling workpiece 21. Later, each successive rolling workpiece 21 is rotated 90 degrees and then rolled in a parallel direction to the central line of the ingot until it reaches the predetermined thickness. Preferably, the rolling is first performed in a first direction A a number of times, and subsequently continued in a second direction B perpendicular to direction A a number of times until the rolling workpiece reaches predetermined to produce a rolled workpiece 23 as seen in Figure 4b. Preferably, the lamination in direction A imparts a true stress of approximately -1.3 and the lamination in direction B imparts a true stress of approximately -1.4. The transverse lamination of the lamination workpiece endures uniformly the workpiece there promotes a favorable response to annealing. The technique described in JB Clark, RK
Garrett, Jr., TL Jungling, and RI Asfahani, Influence of Transverse Rolling on the Microstructural and Textural Development in Puré Tantalum, Metallurgical Transactions Ά, 23A, pp. 2183-2191; and JB Clark, RK Garrett, Jr., TL Jungling, RA Vandermeer, and CL Vold, Effect of 5 Processing Variables on the Texture and Texture Gradients in Tantalum, Metallurgical Transactions A, 22A, pp. 2039. 2048 may be used and those articles are incorporated herein by reference in their entirety.
Preferably, the electrowinning metal workpiece is annealed in the step
105, as indicated by the discontinuous direction arrows, prior to the transverse lamination step described above. Annealing is carried out preferably in a vacuum of 5xl0 ~<sup>4</sup> torr or more, and a sufficient temperature and for a sufficient time to ensure complete partial recrystalization of the flat forged lamination plate. Preferably, the temperature of annealing is from about 950 ° C to about 1300 ° C, and preferably from about two hours, although other temperatures and / or annealing times may be used. This annealing step advantageously allows any work-hardened grains to be recrystallized or recovered, which, in turn, allows the stresses imparted by subsequent intensive rolling of the finished plate to be distributed in an efficient and enhances manner. the microstructural homogeneity and texture in the laminated and annealed plate. The intermediate annealing techniques used during tantalum processing and that can be used here are described in JB Clark, RK Garrett, Jr., TL Jungling, and RI Asfahani, Influence of Transverse Rolling on the Microstructural and Textural Development in Pure Tantalum, Metallurgical
Transactions A, 23A, pp. 2183-2191; and CA Michaluk, Factors Affecting the Mechanical Properties and Texture of Tantalum, Tantalum, E. Chen, A. Crowson, E. Lavemis, W. Eblhara, and P. Kumar (eds.) The Minerals, Metals, and Materials Society, Warrendale , PA, 1996, pp. 205-217;
CA Michaluk, DB Smathcrs and DP Field, Affect of Localized Texture on the Sputter Performance of Tantalum, Procedures of the Twelfth International Conference on Textures of Materials, JA Szpunar (ed.), NRC Research Press, Ottawa, 1999, pp. 1357,1362, all incorporated herein by reference in their entirety.
In one embodiment, after the transverse rolling step 110, the final rolled workpiece (FRW) can be annealed or relieved or stress relieved in step 115 to soften the FRW and improve the formability of the FRW. The stress relief or annealing is best done in a vacuum of 5xl0<sup>-4</sup> torr or higher, there is at a sufficient temperature for a sufficient time to ensure complete recovery or recrystallization of the FRW. Preferably, the temperature for relieving or relaxing stress is from about 600 ° C to about 850 ° C, and the annealing temperature is from about 950 ° C to about 1300 ° C, although other temperatures may be used. The stress relief and annealing time is preferably approximately 2 hours, although other times may be used. Another advantage of annealing the rolled workpiece between the cold work and cross rolling steps is that, by virtue of its lower flow stress, the formed workpiece exhibits an improved surface finish, largely because it can be formed much easier than its unannealed counterpart (ie, its counterpart corresponding to the formed workpiece where the rolled workpiece is not annealed in step 115).
Thus, annealing in step 115 advantageously decreases the requirement of the machine cleaning step of the workpiece formed in step 130 since the workpiece formed may already have an acceptable surface finish to as required by the original equipment manufacturer (OEM).
- In a second embodiment of the present • invention, the rolled workpiece is not annealed
I 5 after the transverse rolling step and before the cold working step in the form of a predetermined target or target. This evasion of the annealing step avoided the relaxation of the excessive amount of cold work i I imparted during the transverse rolling of the plate prior to formation. Since the FRW retains the cold work imparted from the cross-roll, the average amount of true stress with which it will contribute to the workpiece through the formation would preferably be less than -0.2. Therefore, the total stress across the length of the workpiece will not vary to significantly affect the annealing response of the formed workpiece, and annealing the formed workpiece will produce a fine grain structure.
After the optional stress relieving and transverse rolling or annealing step (115), the workpiece is used as a mold and formed in step 120 into a predetermined target or target shape corresponding to the shape of the deposition target or target. electronic. This cold work step preferably includes deep drawing and / or may involve rotary forming (e.g. flow forming) of the rolled workpiece on the formed workpiece, so that a minimum amount of stress (eg, a minimum stress of approximately -2.5 in the workpiece) at the lateral wall of the formed workpiece (SW) after formation. By limiting the amount of stress imparted to the side wall during operation 120, the 10 'severity of stresses and non-uniform stress gradients are preferentially minimal and would have a minor influence on the metallurgical properties of the finished electrodeposition target or target. . Preferably, the predetermined target shape or target 15 corresponds to a cup shape or cylindrical shape, as shown in Figures 2 and 3. The general locations of the base (35), radius (33), the middle wall (31) on the upper wall (29) of the target is shown in Figure 3. The shape of the target 20 or electron deposition target according to The present invention does not necessarily need to be cylindrical or cup-shaped, and the cross section of the target or target of electron deposition in a direction perpendicular to the longitudinal axis L does not necessarily have to be circular.
The cold work used in the process of the present invention is preferably multidirectional cold work, which preferably leads to a multitude of benefits such as size and / or good fine and / or uniform grain texture. This multidirectional cold work is preferentially effected by flow formation as previously described.
In a more preferred embodiment, after transverse lamination (preferably, the material that has been transversely laminated is used to be cut into discoidal or rectangular shaped material, which is then used to form the preform), Cold working of the rolled workpiece to obtain a formed workpiece is preferably effected by deep drawing of the rolled workpiece to form a cup-shaped preform. Subsequently, the preformed material is then preferably flow-formed over a mandrel to form the final formed workpiece 20, which is typically the shape of a cup as shown in Figure 3. This multidirectional cold working of the workpiece via flow formation provides numerous advantages, including but not limited to, importing a greater amount of shear formation into the formed workpiece, resulting in size. finer grain and more uniform in the workpiece formed after annealing.
Preferably, the predetermined target or target shape is stress relieved or further annealed after the cold work step in step 125, as indicated by the discontinuous direction arrows preferentially at temperatures of about 600 to about 850 °. C for stress relief and from about 950 ° C to about 1300 ° C for annealing, although other temperatures can be used. The 125 annealing or stress relief operation is conducted in a vacuum or in an inert atmosphere lasting a preferred period of approximately 15 minutes to approximately 2 hours. The homogeneity of the tension in the formed workpiece (SW) assures that the electronically deposited metal is uniformly responsive to annealing, thereby ensuring a substantially consistent grain structure and / or texture around at least one region in the walls. sides of the completed electron deposition target. The formed workpiece can be mag cleaned in step 130 to produce the target or target of electron deposition, so that it conforms to the dimensional requirements specified by the OEM. As mentioned above, - the electronic deposition target can be formed without the machine cleaning step, as long as the formed workpiece satisfies the OEM defined surface finish requirements. In a preferred embodiment, the electron deposition target is cup-shaped or cylindrical, and has a height of approximately 26.6 centimeters (10.5 10 inches), an internal diameter of approximately 23.4 centimeters (9.25 inches aprgámeta) 24.1 centimeters (9.50 inches) and a lateral wall thickness of approximately 0.63 centimeters (0.25 inches).
The target or target of electronic deposition of the present invention preferentially has borders which is a part of the target or target of electronic deposition. In other words, the rims are integral or part of the same unitary piece that the target or target of electronic deposition thus eliminating the solder of separate ledges to the target or target of electronic deposition. Edges can be formed by rolling over the edges of the electronic deposition target to the desired rim length. This lamination can be i
i__. . _ · Achieved by using material of thick caliber in excess in the part of the mouth, or using the shape of wedge
- of a deep drawing process. The edge of the target, for example, is shown by the number 27 as shown in Figure 1.
Performing the method steps according to the present invention to fabricate an electron deposition target advantageously provides a target that is substantially uniformly eroded during electron deposition and which produces a substantially uniform deposition of the target material onto a substrate, which at the same time avoids the need for complex and expensive components, as mobile components and / or additional components in the electronic deposition apparatus to achieve the above advantages. The goal of electronic deposition made by performing the steps of the method according to the present invention preferably exhibits a substantially consistent grain structure and / or texture at least around all regions of the interior side walls thereof. Any stress within the electron deposition target is preferably substantially uniformly distributed across at least the side walls of the
I
I
I
I
- -। itself, resulting in an electronic uniforms deposition annealing and erosion response.
In one embodiment, the target made of at least one metal of valve preferably holds a fine grain size and / or uniform grain size. Also, the। Objective preferentially has a homogeneous texture. In more detail, preferably, the target containing at least one valve metal has a grain size of 5 ASTM or greater (i.e., or finer), more preferably from about 5 ASTM to about 13 ASTM, more preferably from about 5 ASTM to about 10 ASTM, and most preferably from about 7 ASTM to about 9 ASTM. Additionally, or alternatively, the target has a uniform grain size, for example, where the grain size variance across the target is +2 ASTM or + 1 ASTM, or less. In addition, or alternatively, the objective may have<sub>(</sub> an excellent texture, as is an overall mixed texture (111) - (100) which is preferably free from strong textured localized pointed bands (100). In other words, the texture is such that the grain I that maintains the normal orientation (100) in the direction of the area of electronic deposition dispersed in such a way that no localized clumping of the texture detected (100) exists. Preferably, the target or target of the present invention is at least partially recrystallized, so that at least 75% of the target is recrystallized, and more preferably, at least 95% of the target is recrystallized, and thus even more preferably, at least 98% of the target is recrystallized. Most preferably, the target is completely recrystallized (ie 100% recrystallized). Preferably, the target has one or more of all the properties described above with respect to the texture and grain size. The target preferentially holds to the HCM design as described above and has one or more of all of the above characteristics.
In a preferred embodiment, the methods of the present invention orient the target grains in such a way that parasitic magnetic fields are substantially avoided or completely eliminated. Parasitic magnetic fields are preferentially avoided 20 as a result of the minimization of disarranged grains. In other words, in a preferred embodiment, the present invention enhances the alignment of the magnetic field, in the same way that the orientation of the magnetic field is the same or substantially the same. This 25 allows the orientation of the magnetic field to be
I.
parallel to the flow of electronically deposited material thereby avoiding competition or interference from magnetic fields. This preferably results in improved electronic deposition quality and / or efficiency, which is highly desirable by end users.
Preferably, in accordance with the present invention, an electron deposition target produced as described above is placed in an external shield or cladding, such as the external shield 20 in Figure 1. The outer shield is made of a material which is lighter and cheaper than the valve metal of the electron deposition target, thus avoiding unnecessary weight addition to the electron deposition target and thereby making the mounting of the Objective of electronic deposition and mounting of electronic deposition of the outer shield in a relatively easy electronic deposition vacuum chamber, which at the same time saves costs. Preferably, too, the outer shield is made of a non-hydrating material, like non-hydrating metal. Examples of a non-hydrating metal include, but are not limited to, aluminum or copper.
A metal jacket or reinforcement can preferably be part of the target of electronic deposition by joining a metal reinforcement plate such as a copper plate on a valve metal plate 5 before cold working the material. For example, the metal backing plate can be joined by techniques such as explosive bonding, mechanical bonding, roll bonding, and the like. Once the metal backing plate is attached onto the valve metal plate, then the combined plate with the backing can be subjected to the process of the present invention as described above. This particular method of attaching the metal liner or reinforcement over the valve metal target avoids the additional steps used by end users, where end users typically receive a tantalum target, for example, and then must slide it or a liner. of copper metal on a pre-formed electron deposition target (for example, a can-shaped target), resulting in additional labor and manufacturing costs, as well as time delays. Forming the reinforcement as part of the valve metal plate before the formation of the electronic deposition target, manufacturing costs and time delays can be greatly reduced.
One function of the external shield is to impart structural integrity to the electron deposition target. In this way, the presence of an external shield allows the material of the electronic deposition target along with the inner wall of the HCM to be almost completely consumed, for example, up to a coating thickness of less than 0.25 centimeters (0.1). Without the external shielding, the electron deposition target could not be eroded to its desired minimum size without losing its structural integrity.
When the outer shield is made of a non-hydrating material, this allows the recovery of metal from the valve of a used electron deposition target. Exposure of the composite HCM target to a positive pressure hydrogen atmosphere at a higher temperature, about 450 ° C, the inner lining of the tantalum metal will absorb hydrogen and become friable while the material will not hydrate and remain hard. Hydrated valve metals can be reclaimed from the composite HCM target by mechanical means such as vibration or scraping. The outer shield can therefore be reusable, advantageously, and the unused parts of the electron deposition material recovered and recycled.
According to another aspect of the present invention, as described by way of example by means of the upper portion 15 'in Figure 3, the upper portion 15' may be different from the electron deposition target 3 'and be made of a material resistant to electronic deposition. The top portion is preferentially welded or otherwise attached to the side walls of the 'electronic cylindrical deposition target 3' to produce a finished electronic deposition target assembly 4 '. Preferably, the upper portion is made of a metal-based valve material that holds a large grain size and a strong texture (100). The speed of electronic deposition can depend on the texture. Since tantalum targets having texture bands (100) are highly resistant to electron deposition, according to a preferred embodiment, the upper portion can be made of a material based on
Ta or based on Nb that has a strong texture (100). The valve metal-based material can be a commercially pure valve metal, such as tantalum or niobium, which has been specially processed to obtain a strong texture (100), or it can be a metal alloy.
Valve I, such as, for example, an alloy of tantaliotungsten and the like, which typically exhibits a strong texture (100) as mentioned in CA Michaluk, Masters Thesls, Drexel University, 1993; GT Gray III,
SR Bingert, SI Wright, and SR Chen, Influent of Tungsten Alloying Additions on the Mechanical Properties and Texture of Tantalum, Material Research Society Symposium Proceedings, Volume 322, Materials Research Society, 1994, pp. 407-412; SI Wright, SR Bingert, and
MD Johnson, Effect of Annealing Temperature on the Texture of Rolled Tantalum and Tantalum 10 wt% Tungsten, Tungsten and Refractory Metals 2, A. Bose and RJ Dowding (eds.) Metal Powder Industries Federation, Princeton, 1995, pp. 501-508, all incorporated herein by reference in their entirety. The upper portion can also be made of other material resistant to the electronic deposit, as is known to one skilled in the art. According to another aspect, the upper portion is made of a non-moisturizing material, resistant to electron deposition, within the knowledge of one skilled in the art, which makes possible a recovery of the valve metal from an electron deposition target used as such. described previously. Providing a non-electronically deposited upper portion for the electron deposition target advantageously limited erosion to the side walls of the electron deposition target, while slowing the rate of electron deposition along the upper interior area thereof. The above advantage is desirable to ensure a better deposition of a uniform layer on the substrate, since atoms ejected from the upper inner surface of the target can pass through the plasma without being ionized and continue on a non-perpendicular path towards the substratum. These atoms will collide with the substrate at an angle, accumulating the walls on the channels of the same, and will create a full hole in the bottom of those channels. On the other hand, if an atom of an ejected side wall is not ionized, it will simply deposit on the opposite inner side wall of the target. For this reason, making the upper inner surface of the target from a material that cannot be electronically deposited substantially avoids impact by atoms of non-ionized substrates at an angle, and therefore a non-uniform deposition of the material on it.
In accordance with one aspect of the present invention, a spent electronic deposition target 25 is processed to allow recovery of the remaining valve metal. Preferably, the spent electron deposition target is first subjected to a hydration step during which the valve metal is hydrated to produce a very brittle material, and the hydrated valve metal is separated from the non-hydrated armor by technical removal. or conventional separation. Later, the hydrated valve metal is ground to produce valve metal hydride powder. The valve metal hydride powder is then preferentially degassed by heating in a vacuum with a temperature above 450 ° C by removing the hydrogen, thereby producing valve metal powder. The powder can then be further processed according to the method of the present invention to produce an electron deposition target.
The present invention will be best declared by the following examples, which are intended to be exemplary of the present invention.
EXAMPLES. It was used commercially available niobium plates and commercially available tantalum plates from Cabot Corporation in the examples. Each of the niobium and tantalum plates 25 were transversely laminated several times as described in the present application. The plates originally held a thickness of 8.8 centimeters (3.5 inches) through the transverse lamination process obtained with a result of 1.27 5 centimeters (0.500 inches). Cross rolling is done so that rolling is done the same number of times in one direction and in a second direction perpendicular to the first direction. There is a disk that had the dimensions of 1.27 cm x 45.7 cm 10 (0.500 x 18.0) of diameter of each of the plates.
In manufacturing the preform, each of the discs was stretched into a preform that was shaped like a cup by using a 1000 ton braid. The cup-shaped preform had the following 15 dimensions after being subjected to the 1000 ton press: a height of approximately 16.7 cm (6.6) with a wall thickness of approximately 1.27 cm (0.500), where the wall had to prime tapered edge. The internal diameter of the cup was approximately 23.6 cm (9.3). The radius of the inner diameter of a cup was approximately 3.04 cm (1.2) on the lower corners with a radius of the outer diameter of approximately 4.06 cm (1.6) on the outer corners.
To manufacture the finished product, the preformed cup 25 was then placed on a mandrel. The
The mandrel was machined to the desired diameter of the final product and surface finished. The preformed cup was then flow formed to the required wall thickness and length as indicated below. The operation of flow formation was completed in Dynamic Machine Works. After flow forming processing the finished part was then machined to the desired finished dimensions.
The dimensions of the finished part were as follows:
height of approximately 25.14 cm (9.9), wall thickness of approximately 0.64 cm (0.255) with first tapered edge, with an internal diameter of approximately 23.3 cm (9.19), with a radius of approximately 3.04 (1.2) over the corners of the lower internal diameter and with a radius of approximately 3.45 cm (1.36) over the corners of the lower external diameter. One of the niobium 20 samples and one of the tantalum samples was annealed between the cross-rolling steps and the formation of the preform while the other niobium and tantalum samples avoided the annealing step between the steps of transverse lamination and the formation of the preform by cold work. The annealing step was carried out at 1050 ° C for tantalum and was thus maintained lasting 2 hours. Annealing for the niobium product. effected at 1150 ° C and maintained thus lasting 2 hours.
For each of the samples, the finished product ▼ that was formed was subjected to final annealing where the annealing for the niobium formed from an unannealed plate was at 1100 ° C and was thus maintained for 2 hours; the final anneal for the niobium formed from the annealed plate was at 1250 ° C and it remained so for 10 lasting 2 hours; the final anneal for the tantalum formed from the unannealed plate was at 1100 ° C and was thus maintained lasting 2 hours; and the final anneal for the tantalum formed from the annealed plate was at 1050 ° C and remained thus lasting 2 hours.
The uniformity of the microtexture was obtained for each of the samples using the test procedure described in the United States Patent Application 09 / 665,845, which is incorporated in its entirety herein by reference in part of the present application. To ensure a good comparison of the texture data, the step distance used to collect the raw electron backscatter diffraction (EBSD) data was 1/5 of the average grain size determined in both the X and YYY directions exposed in In the table below, the percent recrystallization as well as the grain size are shown.
TABLE 1: METALOGRAPHIC RESULTS
<td> 5</td><td>Melting pot</td><td>by Tantalum (Target or</td><td>Anticatode of</td><td>Cathode</td>
<td></td><td>Hole) -</td><td>Laminate Workpiece</td><td>Final, Annealed</td><td>(FRW)</td>
<td></td><td>Temp.</td><td>Wall.</td><td>Wall Radio</td><td>Based</td>
<td></td><td></td><td>Higher</td><td>Half</td><td>Half</td>
<td></td><td>1050 ° C</td><td>% Recrystalized 100</td><td> 100 100</td><td> 100</td>
<td></td><td></td><td>Grain Size ASTM 5.0</td><td> 5.1 7.4</td><td> 6.4</td>
<td> 10</td><td></td><td></td><td></td><td></td>
<td></td><td></td><td>Grain Size in ^ 55</td><td> ~62 ~30</td><td> ~40</td>
Microns
Tantalum Crucible (Target or Anticathode Cathode
<td></td><td>Hollow) - Workpiece</td><td>Laminated</td><td>Final,</td><td>Not Overcooked</td>
<td></td><td>(FRW)</td><td></td><td></td><td></td>
<td> 15</td><td>Temp.</td><td>Wall</td><td>Wall</td><td>Base Radius</td>
<td></td><td></td><td>Higher</td><td>Half</td><td>Half</td>
<td></td><td>1100 ° C% Recrystallized</td><td> 100</td><td> 100</td><td> 96 99</td>
<td></td><td>ASTM Grain Size</td><td> 7.3</td><td> 7.2</td><td> 6.4 6.6</td>
<td></td><td>Grain Size in</td><td> ~30</td><td> ~32</td><td> ~40 ~38</td>
<td></td><td>Microns</td><td></td><td></td><td></td>
<td> 20</td><td colspan="2">Niobium Crucible (Target 0</td><td colspan="2">Cathode Anticathode</td>
<td></td><td>Hollow) - Workpiece</td><td>Laminated</td><td>Final,</td><td>Annealed (FRW)</td>
<td></td><td>Temp,</td><td>Wall</td><td>Wall</td><td>Base Radius</td>
<td></td><td></td><td>Higher</td><td>Half</td><td>Half</td>
<td></td><td>1250 ° C% Recrystalized</td><td> 100</td><td> 100</td><td> 100 100</td>
<td>Temp.</td><td>Wall Higher</td><td>Wall Half</td><td>Radio</td><td>Based Half</td>
<td></td><td>Grain Size ASTM 8.7</td><td> 8.6</td><td> 7.6</td><td> 8.7</td>
<td></td><td>Grain Size in</td><td> ~19 '</td><td> ~19</td><td> ~19</td>
Microns
Niobium Crucible (Target or Anticathode of Cathode '
Hollow) - Final Laminate Workpiece, Not Overcooked
<td></td><td>(FRW)</td><td></td><td></td><td></td><td></td><td></td><td></td>
<td></td><td>Temp,</td><td></td><td></td><td>Wall</td><td>Wall</td><td>Radio</td><td>Based</td>
<td></td><td></td><td></td><td></td><td>Higher</td><td>Half</td><td></td><td>Half</td>
<td></td><td>1100 ° C</td><td colspan="2">% Recrystalized</td><td> 100</td><td> 100</td><td> 100</td><td> 100</td>
<td> 10</td><td></td><td>Size from</td><td>ASTM grain</td><td> 9.3</td><td> 9.3</td><td> 9.3</td><td> 9.3</td>
<td></td><td></td><td>Size from</td><td>Grain in</td><td> -15</td><td> -15</td><td> -15</td><td> ~15</td>
Microns
TABLE II: TEXTURE RESULTS (Middle Wall Samples, Annealing Temperature
Optima)
<td></td><td colspan="2">Diffraction by</td><td>Lambda (λ)</td><td>Omega (Ω)</td>
<td></td><td></td><td>Electrodiffraction</td><td>Rad</td><td>Rad</td>
<td></td><td></td><td></td><td><sup>1</sup></td><td> ——</td>
<td></td><td></td><td>EBSD electronics</td><td>mm</td><td>mm</td>
<td> 20</td><td></td><td>Grain size</td><td></td><td></td>
<td></td><td></td><td>(microns)</td><td></td><td></td>
<td></td><td>Tantalum, SMW Annealed</td><td> 64</td><td> 92</td><td> 15</td>
<td></td><td>Tantalum, SMW Unannealed</td><td> 22</td><td> 238</td><td> 84</td>
<td></td><td>Niobium, SMW Annealed</td><td> 17</td><td> 162</td><td> 92</td>
<td></td><td>Niobium, SMW Unannealed</td><td> 10</td><td> 236</td><td> 198</td>
The analysis of texture showed an improvement in the homogeneity of the texture especially with respect to samples that started with the annealed plate. In particular, the annealed electronic deposition targets or targets formed from the unannealed FRW had a more severe texture gradient as demonstrated by a higher lambda value, and a more severe texture band as revealed by a value of larger omega. The variability in the texture has been 10 reported to correlate it with the variability in the performance of the electronic deposition in tantalum (CA Michaluk, DB Smathers, and DP Field, Affect of Localized Texture on the Sputter Performance of Tantalum, Proceedings of the Twelfth International Conference on 15 Texture of Materials, JA Szpunar (cd.), NRC Research Press, Ottawa, 1999, pp. 1357-1362, incorporated in its entirety by reference). Also, as seen from previous results, the benefit of using a non-annealed plate in the forming process is that the final annealed crucible has a finer grain size. The benefit of starting with an annealed plate is an improvement in the homogeneity of the texture in the final crucible, as well as the ease of forming the part. In addition, the use of an annealed RFW has a more uniform grain structure, as evident from the grain size distribution graphs provided in Figures 6-9, as measured by TSL using an analysis technique of Diffraction by Electronic Backscattering according to what is referred to in US Patent No. 09 / 665,845. Thus, each method has benefits depending on the desired needs of the end user and the present invention provides various options to satisfy the requirements of the end user.
It will be apparent to those skilled in the art that various modifications and variations can be made to the embodiments of the present invention without departing from the spirit or scope of the present invention. In this way, it is intended that the present invention covers other modifications and variations of this invention within the<sup>1</sup> scope of the appended claims and their equivalents.
Contents9
9 sheets
Sheet 1 Sheet 2 Sheet 3 Sheet 4 Sheet 5 Sheet 6 Sheet 7 Sheet 8 Sheet 9
20 members in 11 offices
Priority claims3
| Document | Office | Kind | Date |
|---|---|---|---|
| 25311600 | United States of America | P | |
| 29541701 | United States of America | P | |
| 0143376 | United States of America | W |
Members20
| Document | Office | Kind | |
|---|---|---|---|
| WO0242513A2 | World Intellectual Property Organization (WIPO) | A2 | |
| AU3644502A | Australia | A | |
| US2003019746A1 | United States of America | A1 | |
| WO0242513A3 | World Intellectual Property Organization (WIPO) | A3 | |
| KR20030057557A | Republic of Korea | A | |
| EP1339894A2 | European Patent Office (EPO) | A2 | |
| IL156119A0 | Israel | A0 | |
| TW573032B | Taiwan Province of China | B | |
| MXPA03004635AThis record | Mexico | A | |
| CN1531605A | China | A | |
| JP2004536958A | Japan | A | |
| RU2003119076A | Russian Federation | A | |
| US6887356B2 | United States of America | B2 | |
| US2005167015A1 | United States of America | A1 | |
| RU2261288C2 | Russian Federation | C2 | |
| CN1293229C | China | C | |
| KR100831543B1 | Republic of Korea | B1 | |
| US7468110B2 | United States of America | B2 | |
| JP4828782B2 | Japan | B2 | |
| EP1339894B1 | European Patent Office (EPO) | B1 |
Numbers
- Application
- 3004635
Titles2
- English
- HOLLOW CATHODE TARGET AND METHODS OF MAKING SAME.
- Spanish
- OBJETIVO DE CATODO DE HUECO Y METODOS PARA FABRICAR EL MISMO.
Classification
- CPC, 5
- H01J37/342
- C23C14/34
- C23C14/3407
- C23C14/3414
- H01J37/3491
- IPC, 6
- C22B5 12
- B21B3 00
- C22F1 00
- C22F1 08
- C22F1 18
- C23C14 34