Method and Apparatus for Rapid Preparation of Multiple Specimens for Transmission Electron Microscopy
Claim Score by NHIP
Abstract
A method and apparatus for in-situ lift-out rapid preparation of TEM samples. The invention uses adhesives and/or spring-loaded locking-clips in order to place multiple TEM-ready sample membranes on a single TEM support grid and eliminates the use of standard FIB-assisted metal deposition as a bonding scheme. Therefore, the invention circumvents the problem of sputtering from metal deposition steps and also increases overall productivity by allowing for multiple samples to be produced without opening the FIB/SEM vacuum chamber.

Term
4.6 yearsto projected expiry
Projected expiry 26 April 2031, counted from filing; an application has no term until it is granted.
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29 claims: 2 independent, 27 dependent
- 1A method for in-situ lift-out preparation of samples for electron microscopy in a microscopy chamber having at least one viewing window, using a micro gripping and manipulation device and a microprobe assembly having an adhesive or a spring loaded locking clip at an end, the method comprising:a) placing a wafer, microprobe assemblies and a support grid into an electron microscopy chamber;b) placing the microscopy chamber under vacuum;c) grasping the microprobe assembly with the micro gripping and manipulation device;d) creating a sample membrane by etching out portions of the wafer using an ion beam;e) using the micro gripping and manipulation device to move the microprobe assembly so that the adhesive or spring loaded locking clip will touch and attach to the sample membrane;f) severing the sample membrane from the wafer;g) moving the microprobe assembly with the attached sample membrane to the support grid, so that the sample membrane is over a viewing window;i) securing the microprobe assembly to the support grid;and j) releasing the microprobe assembly from the micro gripping and manipulation device.
- 8Broadest claimClaim Score 79, broad(NHIP)An apparatus for in-situ lift-out preparation of electron microscopy samples comprising:a) a micro gripping and manipulation device;b) a microprobe assembly having a first end for gripping by the micro gripping and manipulation device, and a second end;and c) an attachment element at the second end of the microprobe assembly.
Independent claims2
62 paragraphs in 5 sections, as filed
REFERENCE TO RELATED APPLICATIONS
0001This application claims one or more inventions which were disclosed in Provisional Application No. 61/413,083, filed Nov. 12, 2010, entitled “METHOD AND APPARATUS FOR RAPID PREPARATION OF MULTIPLE SPECIMENS FOR TRANSMISSION ELECTRON MICROSCOPY”. The benefit under 35 USC §119(e) of the United States provisional application is hereby claimed, and the aforementioned application is hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
00021. Field of the Invention
0003The present invention is in the technical field of methods of sample preparation and manipulation for preparing a specimen for transmission electron microscopy (TEM) examination. More particularly, the present invention is in the technical field of sample preparation and manipulation by methods of in-situ lift-out techniques.
00042. Description of Related Art
0005The standard in-situ lift-out method involves moving a micromanipulator probe to a sample membrane that was previously milled from a wafer by use of a focused ion beam/scanning electron microscope (FIB/SEM) or similar machine. This leaves the sample membrane approximately 1-2 microns thick with varying length and height (typically 5-15 micron length and 5-15 micron height). The micromanipulator probe is then welded to the sample membrane by ion beam assisted metal deposition. When the weld is secured, the sample membrane is then cut from the wafer by a focused ion beam (FIB) and extracted from the wafer.
0006The probe then moves the sample to a transmission electron microscope (TEM) grid where it is welded to the TEM grid by ion beam assisted metal deposition. When the sample membrane is secured to the TEM grid, the probe is cut from the sample by FIB. The sample membrane is then milled again by FIB until it is thin enough for use in a TEM, typically between 50-200 nanometers thick. The entire method is done within the FIB/SEM machine chamber while it is activated and under vacuum.
0007The current method of in-situ lift-out has a low productivity, as the number of samples that are produced is relatively low in comparison to the total amount of time and effort that is used for this purpose. Features that shorten the time of preparing a sample and/or increase user productivity are highly desirable in this field.
0008The current method also has problems in metal deposition steps where excess material may sputter on, and contaminate unintended objects.
SUMMARY OF THE INVENTION
0009The present invention provides a method and apparatus for in-situ lift-out rapid preparation of samples for electron microscopy. The invention uses adhesives and/or spring-loaded locking-clips in order to place multiple sample membranes on a single support grid and eliminates the use of standard FIB-assisted metal deposition as a bonding scheme. Therefore, the invention circumvents the problem of sputtering from metal deposition steps and also increases overall productivity by allowing for multiple samples to be produced without opening the FIB/SEM vacuum chamber.
BRIEF DESCRIPTION OF THE DRAWING
0010<figref idref="DRAWINGS">FIG. 1</figref> is a flowchart demonstrating the method.
0011<figref idref="DRAWINGS">FIG. 2</figref> is a perspective view of a lift-out system.
0012<figref idref="DRAWINGS">FIG. 3</figref> is a perspective view of the continuation of a lift-out system from <figref idref="DRAWINGS">FIG. 2</figref>.
0013<figref idref="DRAWINGS">FIG. 4</figref> is a perspective view of the continuation of a lift-out system from <figref idref="DRAWINGS">FIG. 3</figref>.
0014<figref idref="DRAWINGS">FIG. 5-A</figref> is a perspective view of an alternate embodiment of a lift-out system.
0015<figref idref="DRAWINGS">FIG. 5-B</figref> is a perspective view of an alternate embodiment of a lift-out device.
0016<figref idref="DRAWINGS">FIG. 5-C</figref> is a side view of an alternate embodiment of a lift-out device of <figref idref="DRAWINGS">FIG. 5-B</figref>.
0017<figref idref="DRAWINGS">FIG. 6</figref> is a wide perspective view of a continuation of a lift-out system from <figref idref="DRAWINGS">FIG. 4</figref>.
0018<figref idref="DRAWINGS">FIG. 7</figref> is a close up perspective view of <figref idref="DRAWINGS">FIG. 6</figref> and continuation of a lift-out system from <figref idref="DRAWINGS">FIG. 6</figref>.
0019<figref idref="DRAWINGS">FIG. 8</figref> is a close up perspective view of <figref idref="DRAWINGS">FIG. 6</figref> and continuation of a lift-out system from <figref idref="DRAWINGS">FIG. 7</figref>.
0020<figref idref="DRAWINGS">FIG. 9-A</figref> is a wide perspective view of a repetition of a lift-out system.
0021<figref idref="DRAWINGS">FIG. 9-B</figref> is a wide perspective view of an alternate embodiment of <figref idref="DRAWINGS">FIG. 9-A</figref>.
0022<figref idref="DRAWINGS">FIG. 9-C</figref> is a wide perspective view of an alternate embodiment of <figref idref="DRAWINGS">FIG. 9-A</figref>.
0023<figref idref="DRAWINGS">FIG. 10-A</figref> is a wide perspective view of an alternate embodiment of <figref idref="DRAWINGS">FIG. 9-A</figref>.
0024<figref idref="DRAWINGS">FIG. 10-B</figref> is a close up cross sectional view of <figref idref="DRAWINGS">FIG. 10-A</figref>.
DETAILED DESCRIPTION OF THE INVENTION
The Method
0025Referring now to <figref idref="DRAWINGS">FIG. 1</figref>, there is shown a flowchart <b>100</b> of the method. The method is comprised of the following steps shown in the flowchart <ul id="ul0001" list-style="none"><li id="ul0001-0001" num="0026"><b>101</b>: Place wafer, microprobe assemblies and TEM support grid into FIB/SEM chamber—Set up all the necessary parts in order to do an in-situ lift-out according to the method shown in the flowchart <b>100</b>. A wafer, microprobe assemblies, and TEM support grids are loaded into a FIB/SEM chamber, which is then activated, placing all its contents under vacuum.</li><li id="ul0001-0002" num="0027"><b>102</b>: Place microprobe assembly in micro gripping and manipulation device—a micro gripping and manipulation device reaches and grasps a micromanipulator probe, which has an adhesive or a spring loaded locking clip at the end of it.</li><li id="ul0001-0003" num="0028"><b>103</b>: Ion mill sample membrane from wafer—the FIB/SEM is used to create a sample membrane by etching out portions of the wafer using an ion beam. The sample membrane will be approximately 5-15 microns long, 5-15 microns deep, and less than 200 nanometers thick when the step is completed. The sample membrane will also be partially cut away from the wafer.</li><li id="ul0001-0004" num="0029"><b>104</b>: Attach microprobe assembly to sample membrane—the micro gripping and manipulation device moves the micromanipulator probe so that the adhesive or spring loaded locking clip will touch and attach to the sample membrane. The sample membrane is attached to both the wafer and the microprobe assembly.</li><li id="ul0001-0005" num="0030"><b>105</b>: Detach sample membrane from wafer—the sample membrane is completely severed from the wafer by the FIB/SEM ion beam. The sample membrane is now only attached to the microprobe assembly.</li><li id="ul0001-0006" num="0031"><b>106</b>: Move microprobe assembly with attached sample membrane to a TEM support grid—the microprobe assembly is moved from the wafer to the TEM support grid so that the sample membrane is over a hollow viewing window.</li><li id="ul0001-0007" num="0032"><b>107</b>: Secure microprobe assembly with attached sample membrane to a TEM support grid—the microprobe assembly is attached to the TEM support grid using an adhesive or a spring loaded locking clip so that it is secured to the TEM support grid.</li><li id="ul0001-0008" num="0033"><b>108</b>: Release microprobe assembly from micro gripping and manipulation device—the micro gripping and manipulation device releases the microprobe assembly with sample membrane only attached to the TEM support grid.</li><li id="ul0001-0009" num="0034"><b>109</b>: Repeat Process?—the process may be repeated to create and attach more sample membranes to the TEM support grid.</li></ul>
0035If yes, return to step <b>102</b> and repeat the method;
0036If no, go on to the last step. <ul id="ul0002" list-style="none"><li id="ul0002-0001" num="0037"><b>110</b>: Remove TEM support grid from FIB/SEM for examination—the TEM support grid has as many sample membranes attached to it as required by the user and the FIB/SEM is deactivated, releasing the vacuum chamber. The TEM support grid is removed so that it can by viewed by a TEM.</li></ul>
The Apparatus
0038Referring now to <figref idref="DRAWINGS">FIG. 2</figref> to <figref idref="DRAWINGS">FIG. 4</figref>, there is shown a microprobe assembly <b>1</b> held by a micro gripping and manipulation device <b>2</b>, which is next to a wafer <b>6</b>. The microprobe assembly <b>1</b> consists of a micromanipulator probe <b>3</b> with a sample attachment element—in this embodiment shown as an adhesive <b>4</b>—at the end opposite the end held by device <b>2</b>. A sample membrane <b>5</b> is part of the wafer <b>6</b>.
0039In more detail, still referring to <figref idref="DRAWINGS">FIG. 2</figref> to <figref idref="DRAWINGS">FIG. 4</figref>, the microprobe assembly <b>1</b> is moved by the micro gripping and manipulation device <b>2</b> to the sample membrane <b>5</b>. The sample membrane <b>5</b> was previously ion milled by FIB from the wafer <b>6</b>. The micromanipulator probe <b>3</b> is attached to the sample membrane <b>5</b> by the adhesive <b>4</b>. After the adhesive <b>4</b> bonds the sample membrane <b>5</b> to the micromanipulator probe <b>3</b>, the sample membrane <b>5</b> is detached from the wafer <b>6</b> and moved by the micro gripping and manipulation device <b>2</b> holding the microprobe assembly <b>1</b> with respect to the wafer <b>6</b>.
0040In reference to the flowchart <b>100</b> shown in <figref idref="DRAWINGS">FIG. 1</figref>, <figref idref="DRAWINGS">FIG. 2</figref> is shown after the following steps were previously completed; “Place wafer, microprobe assemblies and TEM support grid into FIB/SEM chamber” <b>101</b>; “Place microprobe assembly in micro gripping and manipulation device” <b>102</b>; “Ion mill sample membrane from wafer” <b>103</b>. <figref idref="DRAWINGS">FIG. 3</figref> is shown after the step, “Attach microprobe assembly to sample membrane” <b>104</b>. <figref idref="DRAWINGS">FIG. 4</figref> is shown after the step, “Detach the sample membrane from wafer” <b>105</b>.
0041In further detail, still referring to <figref idref="DRAWINGS">FIG. 2</figref> to <figref idref="DRAWINGS">FIG. 4</figref>, the wafer <b>6</b> is loaded into a Focused Ion Beam/Scanning Electron Microscope (FIB/SEM) machine chamber along with the micromanipulator probe <b>3</b> and adhesive <b>4</b> before beginning the process. The micro gripping and manipulation device <b>2</b> is attached to the FIB/SEM machine so that it may manipulate the micromanipulator probe <b>3</b>. The microprobe assembly <b>2</b> must be sufficiently small to capture the sample membrane <b>5</b> typically in sizes of five to fifteen microns long, five to fifteen microns deep and approximately 200 nanometers thick or less, but not subject to these limits. The micromanipulator probe <b>3</b> may vary in size, length, or geometry, but must be usable with typical manipulating devices that are compatible with FIB/SEM machines. The adhesive <b>4</b> may either be preloaded on the micromanipulator probe <b>3</b> prior to insertion into a FIB/SEM machine or a small amount of the adhesive may be placed in the FIB/SEM machine where it is accessible to the micromanipulator probe <b>3</b>.
0042The construction details of the invention as shown in <figref idref="DRAWINGS">FIG. 2</figref> to <figref idref="DRAWINGS">FIG. 4</figref> are that the micromanipulator probe <b>3</b> be made of a metal typically used in the art, such as tungsten, molybdenum, or others. The micromanipulator probe <b>3</b> is cylindrical and tapers to a point where the adhesive <b>4</b> is placed. The adhesive <b>4</b>, in its preferred embodiment would be usable in vacuum chamber environments of a FIB/SEM machine and would also be curable by exposing it to charged electron particles such as particles exerted from a FIB/SEM machine.
0043Referring now to <figref idref="DRAWINGS">FIG. 5-A</figref> to <figref idref="DRAWINGS">FIG. 5-C</figref>, there is shown a sample wafer <b>24</b> attached to a microprobe assembly <b>20</b>, which is held by a micro gripping and manipulation device <b>21</b>, which is near a wafer <b>25</b>. The microprobe assembly <b>20</b> consists of a micromanipulator probe <b>22</b> attached to a spring-loaded locking clip <b>23</b> at its end.
0044In more detail, still referring to <figref idref="DRAWINGS">FIG. 5-A</figref> to <figref idref="DRAWINGS">FIG. 5-C</figref>, the microprobe assembly <b>20</b> attaches the sample membrane <b>24</b> to the micromanipulator probe <b>22</b> using the spring loaded locking clip <b>23</b>. The sample membrane <b>24</b> is held in place by the force applied from the spring loaded locking clip <b>23</b>. The sample membrane <b>24</b> was previously ion milled by FIB from the wafer <b>25</b>. This is an alternate embodiment of the invention.
0045In further detail, still referring to <figref idref="DRAWINGS">FIG. 5-A</figref> to <figref idref="DRAWINGS">FIG. 5-C</figref>, the wafer <b>25</b> is loaded into a Focused Ion Beam/Scanning Electron Microscope (FIB/SEM) machine chamber along with a micromanipulator probe <b>22</b> and spring loaded locking clip <b>23</b> before beginning the process. The micro gripping and manipulation device <b>21</b> is attached to the FIB/SEM machine so that it may manipulate the micromanipulator probe <b>22</b>. The microprobe assembly <b>20</b> must be sufficiently small to capture the sample membrane <b>24</b> typically in sizes of five to fifteen microns long, five to fifteen microns deep, and approximately 200 nanometers thick or less, but not subject to these limits.
0046The micromanipulator probe <b>22</b> may vary in size, length, or geometry, but must be usable with typical manipulating devices that are compatible with FIB/SEM machines. The spring loaded locking clip <b>23</b> is securely attached to the micromanipulator probe <b>22</b> and must apply sufficient force in order to latch and hold onto the sample membrane <b>24</b>.
0047The construction details of the invention as shown in <figref idref="DRAWINGS">FIG. 5-A</figref> to <figref idref="DRAWINGS">FIG. 5-C</figref> are that the micromanipulator probe <b>22</b> be made of a metal typically used in the art, such as tungsten, molybdenum, or others. The spring loaded locking clip <b>23</b> is made of a metal typically used in the art, such that the metal is pliable as to exert a force suitable to hold the sample membrane <b>24</b> without inflicting damage to the sample membrane <b>24</b>. The spring loaded locking clip <b>23</b> may vary in shape, size, and geometry as long as it can deliver the same function.
0048Referring now to <figref idref="DRAWINGS">FIG. 6</figref> to <figref idref="DRAWINGS">FIG. 8</figref>, there is shown a sample membrane <b>5</b> attached to a microprobe assembly <b>1</b> held by a micro gripping and manipulation device <b>2</b> and attached to a grid adhesive <b>7</b> which is attached to a modified TEM mesh support grid <b>8</b>. The microprobe assembly <b>1</b> consists of a micromanipulator probe <b>3</b> and an adhesive <b>4</b> at the end.
0049In more detail, still referring to <figref idref="DRAWINGS">FIG. 6</figref> to <figref idref="DRAWINGS">FIG. 8</figref>, the microprobe assembly <b>1</b> with the sample membrane <b>5</b> attached by the adhesive <b>4</b> is moved by the micro gripping and manipulation device <b>2</b> to the modified TEM mesh support grid <b>8</b>. The microprobe assembly <b>1</b> is then bonded by the grid adhesive <b>7</b> to the TEM mesh support grid <b>8</b> in such a way that the attached sample membrane <b>5</b> will be in a hollow viewing window of the modified TEM mesh support grid <b>8</b>. When the grid adhesive <b>7</b> is sufficiently cured so that the microprobe assembly <b>1</b> is bonded to the modified TEM mesh support grid <b>8</b>, the micro gripping and manipulation device <b>2</b> releases the microprobe assembly <b>1</b>. In reference to the flowchart <b>100</b> shown in <figref idref="DRAWINGS">FIG. 1</figref>, <figref idref="DRAWINGS">FIG. 6</figref> and <figref idref="DRAWINGS">FIG. 7</figref> is shown after the following steps; “Move microprobe assembly with attached sample membrane to a TEM support grid” <b>106</b>; “Secure microprobe assembly with attached sample membrane to a TEM support grid” <b>107</b>. <figref idref="DRAWINGS">FIG. 8</figref> is shown after the step, “Release microprobe assembly from micro gripping and manipulation device” <b>108</b>.
0050In further detail, still referring to <figref idref="DRAWINGS">FIG. 6</figref> to <figref idref="DRAWINGS">FIG. 8</figref>, the modified TEM mesh support grid is placed in a FIB/SEM chamber before beginning the process as shown in the flowchart of <figref idref="DRAWINGS">FIG. 1</figref>. The grid adhesive <b>7</b> would be preloaded onto the modified TEM mesh grid <b>8</b> or a small amount of the grid adhesive <b>7</b> may be placed in the FIB/SEM machine where it is accessible to the microprobe assembly <b>1</b>. The modified TEM mesh support grid <b>8</b> is built with hollow viewing windows where the sample membrane <b>5</b> may be viewed later by a TEM or similar machine.
0051The construction details of the invention as shown in <figref idref="DRAWINGS">FIG. 6</figref> to <figref idref="DRAWINGS">FIG. 8</figref> are that the grid adhesive <b>7</b> would be curable either inside or outside the vacuum chamber of a FIB/SEM machine. The grid adhesive <b>7</b> must also be able to sufficiently secure the microprobe assembly <b>1</b> to the modified TEM mesh support grid <b>8</b>. A modified TEM mesh support grid <b>8</b> is a standard 3 millimeter mesh support grid, typically made of metals used in the art, such as copper, molybdenum or others with mesh of viewing windows incorporated into its structure. It would typically be approximately 20-50 microns thick and circular or semicircular with a typical diameter of 3 millimeters. It has been modified by cutting a portion of the mesh support grid off to expose the viewing windows at the edge of the cut.
0052Referring now to <figref idref="DRAWINGS">FIG. 9-A</figref>, there is shown a modified TEM mesh support grid <b>32</b> attached to a group of microprobe assemblies <b>30</b> which are each individually attached to a sample membrane <b>31</b>.
0053In more detail, still referring to <figref idref="DRAWINGS">FIG. 9-A</figref>, the modified TEM mesh support grid <b>32</b> has been processed with multiple sample membranes <b>31</b> from their attached microprobes assemblies <b>30</b>. The method in the flowchart shown in <figref idref="DRAWINGS">FIG. 1</figref> is repeated until the desired number of sample membranes <b>31</b> are placed onto the modified TEM mesh support grid <b>32</b>. In reference to the flowchart <b>100</b> shown in <figref idref="DRAWINGS">FIG. 1</figref>, <figref idref="DRAWINGS">FIG. 9-A</figref> is shown after the following step, “Repeat Process?” <b>109</b>, has occurred multiple times. The step “Repeat Process?” <b>109</b>, repeats the method starting at the step, “Place microprobe assembly in micro gripping and manipulation device” <b>102</b>. When the process no longer needs to be repeated, then the last step, “Remove TEM support grid from FIB/SEM for examination” <b>110</b>, would follow.
0054Referring now to the invention shown in <figref idref="DRAWINGS">FIG. 9-B</figref>, there is shown a micro gripping and manipulation device <b>40</b> near a group of micromanipulator probes <b>41</b> that are attached to a temporary bonding agent <b>42</b>, which is attached to a modified TEM slotted support grid <b>43</b>.
0055In more detail, still referring to <figref idref="DRAWINGS">FIG. 9-B</figref>, the micro gripping and manipulation device <b>40</b> may detach the micromanipulator probe <b>41</b> and use the previously described method as shown in the flowchart in <figref idref="DRAWINGS">FIG. 1</figref>. After the method described is completed, the micromanipulator probe <b>41</b> may be returned to the modified TEM slotted support grid <b>43</b>. The temporary bonding agent <b>42</b> may allow for the micromanipulator probe <b>41</b> to detach and reattach to the modified TEM slotted grid <b>43</b>. This is an alternate embodiment of the invention.
0056In further detail, still referring to <figref idref="DRAWINGS">FIG. 9-B</figref>, the modified TEM slotted support grid <b>43</b> with the temporary bonding agent <b>42</b> is placed in a FIB/SEM machine chamber before beginning the process as shown in the flowchart of <figref idref="DRAWINGS">FIG. 1</figref>. The temporary bonding agent <b>42</b> allows the micromanipulator probe <b>41</b> to bond to the modified TEM slotted grid <b>43</b>. The micro gripping and manipulation device <b>40</b> may grab the micromanipulator probe <b>41</b> and pull it from the modified TEM slotted grid <b>43</b>. The micro gripping and manipulation device <b>40</b> may also move a micromanipulator probe <b>41</b> to the modified TEM slotted grid <b>43</b> where contact with the temporary bonding agent <b>42</b> will allow the pieces to bond.
0057The construction details of the invention as shown in <figref idref="DRAWINGS">FIG. 9-B</figref> are that the temporary bonding agent <b>42</b> to be strong enough to securely hold a micromanipulator probe <b>41</b> but weak enough to detach the micromanipulator probe <b>41</b> from it without damage to the micromanipulator probe <b>41</b> when force is applied by the micro gripping and manipulation device <b>40</b>. The temporary bonding agent <b>42</b> may also be able to reattach a micromanipulator probe <b>41</b> to the modified TEM slotted support grid <b>43</b> by contact and force applied without damage to the micromanipulator probe <b>41</b>.
0058The modified TEM slotted support grid <b>43</b> is a typical TEM slotted support grid used in the art. It is approximately 3 millimeters in diameter with a slotted hole in the middle. It is made of typical metals used in the art, such as copper, molybdenum or others. The TEM slotted support grid is modified by cutting a portion away from the grid so that the cut is roughly parallel with the long axis of the hollow slot. The extent of cut is variable, but leaves the hollow slot of the slotted TEM grid intact.
0059Referring now to <b>9</b>-C, there is shown a micro gripping and manipulation device <b>50</b> near a micromanipulator probe <b>51</b> which is attached to a temporary bonding agent <b>52</b>, which is attached to a modified TEM slotted support grid <b>53</b>.
0060In more detail, still referring to <figref idref="DRAWINGS">FIG. 9-C</figref>, the micro gripping and manipulation device <b>50</b> may manipulate the micromanipulator probe <b>51</b> and use the previously described method shown in the flowchart of <figref idref="DRAWINGS">FIG. 1</figref>. After the method described is completed, the micromanipulator probe may be returned to the modified TEM slotted support grid <b>53</b>. The temporary bonding agent <b>52</b> may allow for the micromanipulator probe <b>51</b> to detach and reattach to the modified TEM slotted support grid <b>53</b>. This is an alternate embodiment of the invention.
0061In further detail, still referring to <figref idref="DRAWINGS">FIG. 9-C</figref>, the modified TEM slotted support grid <b>53</b> with the temporary bonding agent <b>52</b> is placed in a FIB/SEM machine chamber before beginning the process as shown in the flowchart of <figref idref="DRAWINGS">FIG. 1</figref>. The temporary bonding agent <b>52</b> allows a micromanipulator probe <b>51</b> to bond to the modified TEM slotted support grid <b>53</b>. The micro gripping and manipulation device <b>50</b> may grab the micromanipulator probe <b>51</b> and pull it from the modified TEM slotted support grid <b>53</b>. The micro gripping and manipulation device <b>50</b> may also move a micromanipulator probe <b>51</b> to the modified TEM slotted support grid <b>53</b> where contact with the temporary bonding agent <b>52</b> will allow the pieces to bond.
0062The construction details of the invention as shown in <figref idref="DRAWINGS">FIG. 9-C</figref> are that the temporary bonding agent <b>52</b> be strong enough to securely attach a micromanipulator probe <b>51</b> but weak enough to be able to detach the micromanipulator probe <b>51</b> from it without damage to micromanipulator probe <b>51</b> when force is applied by the micro gripping and manipulation device <b>50</b>. The temporary bonding agent <b>52</b> will also be used to reattach the micromanipulator probe <b>51</b> to the modified TEM slotted support grid <b>53</b> by contact and force applied without damage to the micromanipulator probe <b>51</b>. The modified TEM slotted support grid <b>53</b> is based on a typical TEM slotted support grid used in the art or a close variation of it. It is approximately 3 millimeters in diameter with a slotted hole in the middle. It is made of typical metals used in the art, such as copper, molybdenum or others. A TEM slotted support grid is modified by cutting a portion away from the grid so that it is roughly parallel with the long axis of the slot. The extent of the cut is variable, but leaves the slotted portion of the grid intact. The micromanipulator probe <b>51</b> is flat and made of a metal typically used in the art, such as copper, molybdenum or others.
0063Referring now to <figref idref="DRAWINGS">FIGS. 10-A</figref> and <b>10</b>-B, there is shown a micro gripping and manipulation device <b>63</b> near a micromanipulator probe <b>60</b> which is attached to a spring loaded locking clip <b>61</b>, which is attached to a modified TEM slotted support grid <b>62</b>.
0064In more detail, still referring to <figref idref="DRAWINGS">FIG. 10-A</figref> and <figref idref="DRAWINGS">FIG. 10-B</figref>, the micro gripping and manipulation device <b>63</b> may manipulate the micromanipulator probe <b>60</b> and use the previously described method shown in the flowchart of <figref idref="DRAWINGS">FIG. 1</figref>. After the method described is completed, the micromanipulator probe <b>60</b> may be returned to the modified TEM slotted support grid <b>62</b>. The spring loaded locking clip <b>61</b> may allow for the micromanipulator probe <b>60</b> to detach and reattach to the modified TEM slotted support grid <b>62</b>. This is an alternate embodiment of the invention.
0065In further detail, still referring to <figref idref="DRAWINGS">FIG. 10-A</figref> and <figref idref="DRAWINGS">FIG. 10-B</figref>, the modified TEM slotted support grid <b>62</b> with the spring loaded locking clip <b>61</b> is placed in a FIB/SEM machine chamber before the process begins as described in the flowchart of <figref idref="DRAWINGS">FIG. 1</figref>. The spring loaded locking clip <b>61</b> allows a micromanipulator probe <b>60</b> to attach to the modified TEM slotted support grid <b>62</b>. The micro gripping and manipulation device <b>63</b> may grab the micromanipulator probe <b>60</b> and pull it from the modified TEM slotted support grid <b>62</b>. The micro gripping and manipulation device <b>63</b> may also move a micromanipulator probe <b>60</b> to the modified TEM slotted support grid <b>62</b> where contact and applied force with the spring loaded locking clip <b>61</b> will allow the micromanipulator probe <b>60</b> to attach to the modified TEM slotted support grid <b>62</b>.
0066The construction details of the invention as shown in <figref idref="DRAWINGS">FIG. 10-A</figref> and <figref idref="DRAWINGS">FIG. 10-B</figref> are that the spring loaded locking clip <b>61</b> is strong enough to hold a micromanipulator probe <b>60</b> but weak enough to be able to detach the micromanipulator probe <b>60</b> from it without damage to the micromanipulator probe <b>60</b> when force is applied by the micro gripping and manipulation device <b>63</b>. The spring loaded locking clip <b>61</b> must also be able to reattach a micromanipulator probe <b>60</b> to a modified TEM slotted support grid <b>62</b> by contact and force applied without damage to the micromanipulator probe <b>60</b>. The spring loaded locking clip <b>6</b> may vary in shape, size, and geometry as long as it can deliver the same function.
0067The modified TEM slotted support grid <b>62</b> is a typical TEM support slotted grid used in the art or a close variation of it. It is typically approximately 3 millimeters in diameter with a slotted hole in the middle. It is made of typical metals used in the art, such as copper, molybdenum or others. The modified TEM slotted support grid <b>62</b> is modified by cutting a portion away from the grid so that it is roughly parallel with the long axis of the slot. The extent of cut is variable, but leaves the slotted portion of the support grid intact.
0068The advantages include, without limitation, that it allows for multiple sample membranes to be placed on a single TEM support grid for viewing by a TEM or similar machine. The method further avoids the need for assisted metal weld deposition and its inherent metal sputtering on and around the area of interest for microscopy. The method further allows for SEM only type of machines to continue the lift-out process, thereby freeing the more expensive FIB/SEM machine from the downtime of the in-situ lift-out attachment process.
0069While the foregoing written description of the invention enables one of ordinary skill to make and use what is considered presently to be the best mode thereof, those of ordinary skill will understand and appreciate the existence of variations, combinations, and equivalents of the specific embodiment, method, and examples herein. The invention should therefore not be limited by the above described embodiment, method, and examples, but by all embodiments and methods within the scope and spirit of the invention.
0070Accordingly, it is to be understood that the embodiments of the invention herein described are merely illustrative of the application of the principles of the invention. Reference herein to details of the illustrated embodiments is not intended to limit the scope of the claims, which themselves recite those features regarded as essential to the invention.
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Numbers
- Publication
- 20120119084
- Application
- 13050561
Titles
- English
- Method and Apparatus for Rapid Preparation of Multiple Specimens for Transmission Electron Microscopy
Patent term adjustment
- A delay
- +40 daysthe office missed an examination deadline
- Net adjustment
- 40 days
Classification
- CPC, 5
- H01J37/20
- G01N1/286
- G01N23/2202
- H01J2237/208
- H01J2237/31745
- IPC, 2
- G21K5 08
- G01N23 00