JP3762601B2 - Electron microscope sample holder and electron microscope observation method - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
This invention is used in evaluating reaction processes with an electron microscope. Ruden Sample holder for child microscope, and The present invention relates to an electron microscope observation method.
[0002]
[Prior art]
Conventionally, as a method of evaluating a reaction process, there is a method of manufacturing and evaluating a wafer while changing each condition using a semiconductor process apparatus (that is, stop production) with respect to the temperature and gas conditions of each process.
[0003]
In addition, as a method for evaluating a reaction process without using the semiconductor process apparatus, there is a method using an electron microscope (Japanese Patent Laid-Open No. 7-147151). In this method, a special atmosphere is created by supplying gas to a sample pre-exhaust chamber incorporated in the body wall of an electron microscope by a gas introduction mechanism. The sample is heated by the heating holder in this special atmosphere.
[0004]
Moreover, as a reaction process evaluation method using a transmission electron microscope, there is a method described in JP-A-11-54578. In this reaction process evaluation method, the thin piece portion of the sample is simultaneously heated and observed with a transmission electron microscope, and then the bulk portion is thinned and compared with the thin piece portion. In this way, it is examined whether or not the result of simultaneous heating observation in the flake state is consistent with the case of heating in the bulk state. If the results of the comparative observation are different, the result of the simultaneous heating observation is assumed to be a phenomenon specific to the flake state heating.
[0005]
[Problems to be solved by the invention]
However, the conventional reaction process evaluation method has the following problems. First, in the method of evaluating a reaction process using the semiconductor process apparatus, it is not easy to change the temperature setting and gas conditions in order to use an actual semiconductor process apparatus, and many samples are prepared under detailed conditions. There is a problem that it is difficult to do. In addition, in order to evaluate the reaction process by changing the above temperature setting and gas conditions, a wafer for each set temperature and gas condition is required, and a large number of wafers are required, which increases costs. There is also.
[0006]
Next, in the method using an electron microscope disclosed in the above-mentioned Japanese Patent Application Laid-Open No. 7-147151, the sample to be reacted is sliced to a thickness of several tens to several hundreds of nanometers that can be observed with a transmission electron microscope. Yes. For this reason, the results obtained after the reaction, such as a large cross-sectional area with respect to the part where the state change occurs and many parts that are exposed to vacuum or gas atmosphere, are the same as those in the actual wafer state or thick film state. There is a problem that it is difficult to confirm whether the reaction results.
[0007]
Next, in the method using the transmission electron microscope disclosed in the above-mentioned JP-A-11-54578, it is possible to evaluate the state after simultaneous observation with heating. However, when comparison is performed under each temperature condition, it is necessary to interrupt the simultaneous heating observation at each temperature and thin the bulk portion, which is not easy. Moreover, since it is heating in a transmission microscope, it is limited to heating in a vacuum, and there is a problem that heating in a different atmosphere is not possible.
[0008]
Therefore, an object of the present invention is to make it possible to easily change each temperature condition and gas condition on the microscope to faithfully reproduce the reaction in the wafer state. Ruden Sample holder for child microscope, and It is to provide an electron microscope observation method.
[0009]
[Means for Solving the Problems]
In order to achieve the above object, a first invention is an electron microscope sample processing apparatus for processing an electron microscope observation sample, wherein the sample stage of an electron microscope sample holder on which a sample stage is mounted is provided. A sample chamber into which the leading end portion is inserted; an exhaust means for exhausting the sample chamber; a gas supply means for supplying gas into the sample chamber by switching its type and flow rate; and an electron inserted into the sample chamber A sample local heating means for directly and locally heating the location of the sample stage in the sample holder for the microscope, a radiation thermometer for measuring the temperature of the sample stage, and the sample local heating based on the temperature measured by the radiation thermometer Heating temperature control means for controlling the heating temperature by means Power An electron microscope sample holder whose tip is inserted into a sample chamber of a sample processing apparatus for a child microscope, which is provided at a rod-shaped holder body, a sample stage to which a sample is attached and fixed, and one end of the holder body The fitting groove for fitting the sample stage is provided on the other end side opposite to the one end side with respect to the fitting groove in the holder body, and is fitted into the fitting groove. An elastic member that presses and fixes the sample stage against the wall surface on one end side that forms the fitting groove, and is provided on the other end side relative to the fitting groove on the outer peripheral surface of the holder body. When the one end side including the sample stage is inserted into the sample chamber of the sample processing apparatus for the electron microscope, an O-ring that is in close contact with the insertion port of the sample chamber and blocks the internal environment of the sample chamber from the external environment is provided. Preparation And above The one end side of the holder body from the O-ring has a structure that can be inserted into a focused charged particle beam apparatus and mounted. And the whole has a heat-resistant structure It is characterized by being.
[0010]
According to the above configuration, the simple operation of simply fitting the sample stage into the fitting groove provided at one end of the rod-shaped holder main body and pressing the sample stage against the wall surface of the fitting groove by an elastic member. Then, the sample stage is mounted on the electron microscope sample holder. Furthermore, the O-ring is brought into close contact with the insertion port of the sample chamber by only one operation of inserting the one end side including the sample stage in the holder body into the sample chamber of the sample processing apparatus for electron microscope. The internal environment is isolated from the external environment. Also, Whole Since it has a heat-resistant structure, it is possible to withstand the heat reaction process by the electron microscope sample processing apparatus. Further, the one end side of the holder body with respect to the O-ring has a structure that can be attached to the focused charged particle beam apparatus, so that the sample after the heating reaction is mounted on the focused charged particle beam apparatus. By mounting, the sample can be thinned to a thickness that can be observed with an electron microscope.
[0011]
Also, above First The sample holder for an electron microscope according to the invention has a sample stage main body having a recess for storing the sample and having heat resistance, and fixing the sample stored in the recess to the sample stage main body and heat resistance. It is desirable to provide a fixing member having the property.
[0012]
According to the above configuration, the sample is attached to the sample stage by a simple operation of storing the sample in the recess of the sample stage main body and fixing the sample to the sample stage main body by the fixing member. Furthermore, since the sample stage main body and the fixing member have heat resistance, the sample stage main body and the fixing member can withstand the heat reaction process performed by the electron microscope sample processing apparatus.
[0013]
Also, above First In the sample holder for an electron microscope according to the present invention, the fixing member for the sample stage is preferably constituted by a plate member for holding the sample and a screw for fixing the plate member to the sample stage main body.
[0014]
According to the above configuration, since the fixing member of the sample stage is configured at a very low cost by the plate member and the screw, even if the sample stage is thermally deformed during the heat reaction process by the electron microscope sample processing apparatus, Cost increase can be suppressed.
[0015]
Also, Second The invention of An electron microscope sample processing apparatus for processing an electron microscope observation sample, a sample chamber in which a tip portion including the sample stage of an electron microscope sample holder equipped with a sample stage is inserted, and the sample Exhaust means for exhausting the chamber, gas supply means for supplying gas into the sample chamber by switching its type and flow rate, and the location of the sample stage in the sample holder for the electron microscope inserted in the sample chamber A sample local heating means for directly heating, a radiation thermometer for measuring the temperature of the sample stage, and a heating temperature control means for controlling the heating temperature by the sample local heating means based on the temperature measured by the radiation thermometer. The A sample holder for an electron microscope having a tip inserted into a sample chamber of a sample processing apparatus for an electron microscope, a holder body having a rod shape, a sample stage to which a sample is attached and fixed, heat resistant and the sample stage A heat-resistant member for holding the sample stage, a fitting groove for fitting the sample stage held by the heat-resistant member, and the one end than the fitting groove in the holder main body. The sample stage, which is provided on the other side opposite to the side and fitted in the fitting groove, is pressed against the wall surface on the one end side forming the fitting groove via the heat-resistant member. The elastic member to be fixed and the one end side including the sample stage provided in the other end side than the fitting groove on the outer peripheral surface of the holder body are inserted into the sample chamber of the sample processing apparatus for the electron microscope. And an O-ring that is in close contact with the insertion port of the sample chamber and blocks the internal environment of the sample chamber from the external environment. And above The one end side of the holder body from the O-ring has a structure that can be inserted into a focused charged particle beam apparatus and mounted. And the whole has a heat-resistant structure It is characterized by being.
[0016]
According to the above configuration, the sample stage held by the heat-resistant member is fitted into the fitting groove provided at one end of the rod-shaped holder main body, and the fitting groove is formed by the elastic member via the heat-resistant member. The sample stage is attached to the sample holder for the electron microscope by a simple operation of pressing and fixing to the wall surface. Furthermore, the O-ring is brought into close contact with the insertion port of the sample chamber by only one operation of inserting the one end side including the sample stage in the holder body into the sample chamber of the sample processing apparatus for electron microscope. The internal environment is isolated from the external environment. Also, Whole Since it has a heat-resistant structure, it is possible to withstand the heat reaction process by the electron microscope sample processing apparatus. Furthermore, since the one end side of the holder body from the O-ring has a structure that can be attached to the focused charged particle beam apparatus, the holder body is mounted on the focused charged particle beam apparatus while the sample after the heating reaction is mounted. Thus, the sample can be thinned to a thickness that can be observed with an electron microscope.
[0017]
Also, above Second The sample holder for an electron microscope according to the present invention includes a sample stage body having a recess for housing the sample and having heat resistance, and a lid member having a heat resistance and covering the recess of the sample stage body. The heat-resistant member has a contact surface that simultaneously contacts the end surfaces of the sample stage main body and the lid member, and the contact surface extends in the extending direction of the end surface to When the heat-resistant member is urged by the elastic member, the wall surface of the groove on the contact surface is a lid on the sample stage. It is desirable that the member be in close contact with the sample stage main body.
[0018]
According to the above configuration, when the heat-resistant member sandwiching the sample stage is urged by the elastic member, the lid member of the sample stage is in close contact with the wall surface of the groove on the contact surface of the heat-resistant member. Then, the sample is fixed. Therefore, the sample can be easily attached to the sample stage without using a fixing member or the like. Furthermore, since the sample stage main body and the lid member have heat resistance, the sample stage main body and the lid member can withstand the heat reaction process by the electron microscope sample processing apparatus.
[0019]
Also, above Second In the sample holder for an electron microscope according to the present invention, it is preferable that the lid member of the sample stage has a recess for storing the sample.
[0020]
According to the said structure, the recessed part which accommodates the said sample is provided in both the said sample stage main body and the cover member. Therefore, when the lid member is brought into close contact with the sample stage main body in which the sample is stored, the positions of both do not shift.
[0021]
Also, Third The electron microscope observation method of the invention is the above First Or Second A sample is attached to the sample stage according to the invention, and the sample stage to which the sample is attached is First Or Second The one end side including the sample stage in the sample holder for the electron microscope in which the sample stage is mounted is fitted and mounted in the fitting groove of the electron microscope sample holder of the invention An electron microscope sample processing apparatus for processing an electron microscope observation sample, the sample chamber including the sample stage of the electron microscope sample holder on which the sample stage is mounted, and the above-described sample chamber Exhaust means for exhausting the sample chamber, gas supply means for supplying gas into the sample chamber by switching its type and flow rate, and the location of the sample stage in the electron microscope sample holder inserted in the sample chamber A sample local heating means for directly heating the sample stage, a radiation thermometer for measuring the temperature of the sample stage, and a heating temperature control means for controlling the heating temperature by the sample local heating means based on the temperature measured by the radiation thermometer. Prepared The sample is inserted into a sample chamber in a sample processing apparatus for an electron microscope, the O-ring is brought into close contact with the insertion port of the sample chamber, the sample is heated and reacted under desired gas conditions and desired heating conditions, and after the heating reaction, The sample holder for the electron microscope is taken out from the sample processing apparatus for the electron microscope, and the one end side of the holder body is attached to the converged charged particle beam device with respect to the O-ring, and the sample is converged so that the electron microscope can be observed. Thinned by a charged particle beam, and after the thinning, the electron microscope sample holder is taken out of the focused charged particle beam device and mounted on the electron microscope, and the thinned sample is observed by the electron microscope. It is characterized by doing.
[0022]
According to the above configuration, the bulk sample mounted on the sample holder for the electron microscope is heated and reacted by the sample processing apparatus for the electron microscope, and then thinned by the focused charged particle beam device, and then the sliced. The observed sample is observed with an electron microscope. Thus, by subjecting the sample to heat reaction in the bulk state and then thinning, it is possible to observe the sample in which the heat reaction in the actual wafer state is faithfully reproduced with an electron microscope. Therefore, the reaction process can be evaluated by performing the observation under various heating temperature conditions or by repeatedly performing the observation on the same sample.
[0023]
Moreover, the evaluation under various heating temperature conditions and gas conditions is easily realized by the electron microscope sample processing apparatus. Further, the heat reaction process, the thinning process, and the electron microscope observation are performed on the bulk sample while the sample is mounted on the electron microscope sample holder. Therefore, it is possible to quickly evaluate the reaction process.
[0024]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in detail with reference to the illustrated embodiments. 1 and 2 show a sample preparation procedure using a heating reaction apparatus as the electron microscope sample processing apparatus of the present embodiment. FIG. 3 shows the appearance of the sample stage on which the sample is fixed. FIG. 4 is a plan view and a side view of an electron microscope sample holder on which the sample stage is mounted. FIG. 5 shows the appearance of the heating reaction apparatus. Hereinafter, a procedure for preparing a sample for an electron microscope will be described with reference to FIG. 1 to FIG. 5 by taking silicidation reaction evaluation by thermal reaction of a Ti / Si substrate as an example.
[0025]
First, as shown in FIGS. 1 (a) and 1 (b), a wafer 1 before heat treatment is cut into a size that can be inserted into a transmission electron microscope using a dicing saw (not shown). . Here, the size of the sample 2 is usually W1 = 200 μm, L = 3 mm, W2 = 10 μm to 50 μm, and H = 50 μm to 200 μm. As shown in FIG. 1B, the wafer 1 is sputtered with a Ti film 4 on a Si substrate 3, and further in the same chamber to prevent oxidation of the Ti film 4, evaporation in a vacuum, surface damage, and the like. The TiN film 5 is formed by continuous sputtering. However, in FIGS. 1C to 2G, the expressions of the Ti film 4 and the TiN film 5 are omitted.
[0026]
Next, as shown in FIG. 1C, the sample 2 is attached and fixed to a sample stage 6 as will be described in detail later. The sample stage 6 has a recess 7 cut into a size slightly larger than the planar outer shape of the sample 2. After the sample 2 is stored in the recess 7, the sample 2 is sandwiched between the circular metal plates 8, and the screw 9. Secure with. Normally, the size of the recess 7 is P = 1 mm, Q = 180 μm, and R = 3.1 mm as shown in FIG. In that case, there is a possibility that the sample stage 6, the metal plate 8 and the screw 9 are fused with the sample 2 due to a high temperature reaction and cannot be removed. Therefore, it is preferable to use an inexpensive material such as SUS (stainless steel). Note that the fixing member of the sample 2 is not limited to the metal plate 8 and the screw 9, but the inexpensive metal plate 8 and the screw 9 are desirable for the reasons described above.
[0027]
Next, as shown in FIG. 1 (d), the sample stage 6 is fixed to the tip portion of the electron microscope sample holder 10 using two sample stage fixing jigs 11a and 11b. FIG. 4 (a) shows a plan view of the tip of the electron microscope sample holder 10, while FIG. 4 (b) shows a side view thereof. The sample stage fixing jig 11 is made of quartz or SiC so as not to be fused even at high temperatures. Then, it is mounted in a fitting groove 10 a provided at the tip of the electron microscope sample holder 10, and is biased and fixed to the tip by a spring 12. In this way, the sample stage 6 is attached and fixed to the electron microscope sample holder 10. The front wall surface of the fitting groove 10a has a recess 10b into which the front end portion of the sample stage fixing jig 11a is inserted. On the other hand, a hole 10c for accommodating the rear side of the sample stage fixing jig 11b and the spring 12 is formed in the rear wall surface.
[0028]
Next, as shown in FIG. 2 (e), the tip of the electron microscope sample holder 10 is inserted into the sample chamber 14 of the heating reaction apparatus 13 and sealed. Thus, a predetermined thermal reaction is performed. As shown in FIG. 5, the heating reaction apparatus 13 is schematically configured by a sample chamber 14 and a temperature controller 15 located therebelow. A pipe 16 for evacuation and gas introduction is connected to the sample chamber 14. When the tip of the electron microscope sample holder 10 is inserted, the O-ring 17 blocks the external environment.
[0029]
Thus, when the sample stage 6 is set in the sample chamber 14 of the heating reaction apparatus 13, the inside of the sample chamber 14 is evacuated by an evacuation means (not shown), and desired by a gas supply means (not shown). Are supplied at a desired flow rate. The sample stage 6 is directly heated by IR (infrared) light 19 from the sample local heating device 18 under the control of the temperature controller 15. In this case, the temperature of the sample stage 6 is measured by the radiation thermometer 20. Reference numeral 24 denotes a vacuum gauge.
[0030]
Next, the electron microscope sample holder 10 after the thermal reaction on the sample 2 is completed is introduced into a focused charged particle beam apparatus (not shown), as shown in FIGS. 2 (f) and 2 (g). The surface side of the sample 2 is irradiated with a Ga charged particle ion beam 21 along the side surface. In this way, as shown in the enlarged view of FIG. 2 (g), the surface portion 2a of the sample 2 is sliced into a thickness of 50 nm to 200 nm that can be observed with a transmission electron microscope.
[0031]
Next, the electron microscope sample holder 10 is inserted into a transmission electron microscope (not shown), and as shown in FIGS. 2 (f) and 2 (g), electrons are traversed across the thin piece 2a. Pass line 22 through. Thus, the reaction state between the Ti film 4 and the Si substrate 3 at the above heat treatment temperature is observed. Then, the silicidation reaction evaluation by thermal reaction of the Ti / Si substrate at various temperatures can be performed by performing the same procedure as described above for each temperature.
[0032]
Furthermore, it is also possible to compare the progress of the thermal reaction by using the sample 2 subjected to the above-mentioned observation and performing the observation by the same procedure again by changing the position of the thin piece portion 2a.
[0033]
As described above, in this embodiment, when the thermal reaction state of the semiconductor wafer is observed with a transmission electron microscope, the sample 2 in the bulk state is heat-treated by the heating reaction device 13. In this case, the heating reaction apparatus 13 uses an IR light 19 to remove the sample chamber 14 into which various gases are introduced by inserting the sample holder 10 for the electron microscope with the sample 2 mounted thereon, and the sample 2 in the sample chamber 14. And a temperature controller 15 for direct heating. The sample 2 is attached to the sample stage 6 and mounted and fixed in the fitting groove 10a of the sample holder 10 for electron microscope. Then, the heat-treated sample 2 in the bulk state is introduced into the converged charged particle beam apparatus while being mounted on the electron microscope sample holder 10 and thinned to a thickness that allows observation with a transmission electron microscope. Thereafter, the reaction state is observed by being inserted into the transmission electron microscope while being mounted on the electron microscope sample holder 10.
[0034]
Thus, after heat-treating the sample 2 in the bulk state, it can be thinned and observed with a transmission electron microscope. Therefore, it is possible to faithfully reproduce the heating reaction in an actual wafer state, and contribute greatly to the evaluation of the reaction process. Moreover, the atmosphere in the sample chamber 14 of the heating reactor 13 can be easily changed, and evaluation under various heating temperature conditions and gas conditions can be easily realized. Further, the thinning process and the transmission electron microscope observation for the heat-treated sample 2 in the bulk state can be performed with the sample 2 mounted on the electron microscope sample holder 10 as shown in FIG. . Therefore, the thinning process and the transmission electron microscope observation of the sample 2 can be performed quickly, the reaction process condition examination work can be facilitated, and the time required for the process development can be greatly shortened.
[0035]
FIG. 6 is an external view of a sample stage 31 different from the sample stage 6 shown in FIG. FIG. 7 shows a state in which the sample stage 31 is mounted on the electron microscope sample holder 35. This sample stage 31 has a sample stage member 31a having a recess 33 cut into a size slightly larger than the planar outline of the sample 32, and a recess (not shown) similar to the sample stage member 31a, and has the same planar shape. It is comprised from the sample stage member 31b which has. Then, after the sample 32 is accommodated in the recess 33 in the sample stage member 31a, the sample stage member 31b is covered, the sample 2 is accommodated in the recesses of both the sample stage members 31a, 31b, and the tip portion of the sample holder 35 for the electron microscope Are fixed using two sample stage fixing jigs 34a and 34b.
[0036]
The size of the recess 33 is usually P ′ = 1 mm, Q ′ = 90 μm, and R ′ = 3.1 mm. As shown in FIG. 7, the sample stage 31 with the sample 32 sandwiched in the recess 33 is mounted in a fitting groove 35 a provided at the tip of the electron microscope sample holder 35, and is moved to the tip side by a spring 36. It is urged and fixed. In this case, since the sample stage members 31a and 31b are not fixed to each other, V grooves 34c and 34d in the vertical direction are provided on the contact surfaces of the sample stage fixing jigs 34a and 34b with the sample stage 31. Yes. Then, by sandwiching the sample stage 31 using the elastic force of the spring 36 between the two V grooves 34c and 34d facing each other, the sample stage members 31a and 31b are brought into close contact with each other to fix the sample 32. At this time, since the sample 32 is accommodated in the recesses of the sample stage members 31a and 31b, the positions of the sample stage members 31a and 31b are not shifted.
[0037]
If this sample stage 31 is used, it is not necessary to fix the sample 2 with the screw 9 as in the case of the sample stage 6 shown in FIG. Therefore, the loading / unloading operation of the sample 32 is facilitated, and the reaction process can be evaluated more rapidly.
[0038]
In the embodiment shown in FIGS. 6 and 7, a recess is also provided on the side of the sample stage member 31b constituting the sample stage 31 so that the positions of the sample stage members 31a and 31b do not shift. Yes. However, the present invention is not limited to this. Even if the stage member 31b is formed in a flat plate shape so as to function as a lid, a simple engaging portion for alignment is provided on the contact surfaces of both stage members. I do not care.
[0039]
【The invention's effect】
As is clear from the above, the first invention Power of Sample holder for microscope Is the electric A sample holder for an electron microscope inserted into a sample chamber of a sample processing apparatus for a child microscope, and has a fitting groove for fitting the sample stage at one end of a rod-shaped holder body, and the fitting is performed by an elastic member. Since the prepared sample stage is pressed against the wall surface of the fitting groove and fixed, the sample stage can be mounted on the electron microscope sample holder with a simple operation. Further, when the one end side of the holder body is inserted into the sample chamber of the sample processing apparatus for an electron microscope, the O-ring comes into close contact with the insertion port of the sample chamber, so that the internal environment of the sample chamber can be easily controlled. Can be isolated from the external environment. Also, Whole Since it has a heat resistant structure, it can withstand the heat reaction treatment by the sample processing apparatus for electron microscope. Furthermore, the one end side of the holder body from the O-ring has a structure that can be mounted on the focused charged particle beam apparatus, so that the sample after the heating reaction is mounted on the focused charged particle beam apparatus. Then, the sample can be thinned to a thickness that can be observed with an electron microscope.
[0040]
Also, above First The sample holder for an electron microscope according to the invention has a sample stage main body having a recess for storing the sample and having heat resistance, and fixing the sample stored in the recess to the sample stage main body and heat resistance. If the fixing member having the property is provided, the sample can be easily attached to the sample stage by the fixing member. Furthermore, since this sample stage has heat resistance, it can also withstand the heat reaction process by the electron microscope sample processing apparatus.
[0041]
Also, above First According to the electron microscope sample holder of the invention, if the fixing member for the sample stage is constituted by a plate member for holding the sample and a screw for fixing the plate member to the sample stage main body, the fixing member is very Can be configured at low cost. Therefore, even if heat deformation occurs during the heat reaction process by the electron microscope sample processing apparatus, it is possible to suppress an increase in cost.
[0042]
Also, Second Sample holder for electron microscope of the invention Is the electric A sample holder for an electron microscope inserted into a sample chamber of a sample processing apparatus for a child microscope, and has a fitting groove for fitting the sample stage sandwiched between heat-resistant members at one end of a holder body that forms a rod shape, Since the sample stage fitted by the elastic member is pressed against the wall surface of the fitting groove via the heat-resistant member and fixed, the sample stage can be attached to the sample holder for the electron microscope with a simple operation. it can. Further, when the one end side of the holder body is inserted into the sample chamber of the sample processing apparatus for an electron microscope, the O-ring comes into close contact with the insertion port of the sample chamber, so that the internal environment of the sample chamber can be easily controlled. Can be isolated from the external environment. Also, Whole Since it has a heat resistant structure, it can withstand the heat reaction treatment by the sample processing apparatus for electron microscope. Further, the one end side of the holder body with respect to the O-ring has a structure that can also be attached to the focused charged particle beam apparatus. The sample can be mounted and thinned to a thickness that allows observation with an electron microscope.
[0043]
Also, above Second The sample holder for an electron microscope according to the present invention includes a sample stage body having a recess for housing the sample and having heat resistance, and a lid member having a heat resistance and covering the recess of the sample stage body. The heat-resistant member is provided with a groove having a cross-sectional shape that opens toward the opening side on a contact surface of the heat-resistant member that simultaneously contacts the end surfaces of the sample stage main body and the lid member. If the lid member is brought into close contact with the sample stage body on the wall surface of the groove on the contact surface when biased by the member, the sample can be easily attached to the sample stage without using a fixing member or the like. Can do. Furthermore, since this sample stage has heat resistance, it can also withstand the heat reaction process by the sample processing apparatus for an electron microscope.
[0044]
Also, above Second In the sample holder for an electron microscope according to the invention, when the lid member of the sample stage has a concave portion in which the sample is accommodated, the lid member is in close contact with the sample stage main body in which the sample is accommodated. , It is possible to prevent the positions of both from shifting.
[0045]
Also, Third The method for observing an electron microscope of the present invention is the one end side including the sample stage in the sample holder for the electron microscope, in which the sample is attached to the sample stage and fitted in the fitting groove of the sample holder for the electron microscope. Is inserted into the sample chamber of the sample processing apparatus for the electron microscope, the O-ring is brought into close contact with the insertion port of the sample chamber, and the sample is heated and reacted under a desired gas condition and a desired heating condition. The one end side including the sample stage in the sample holder is attached to a focused charged particle beam apparatus, and the sample is thinned by a focused charged particle beam so that the electron microscope can be observed. The thinned sample is attached to the sample and observed with an electron microscope. The heating reaction in real wafer state is faithfully reproduced sample can be electron microscopy. Therefore, the reaction process can be evaluated by performing the observation under various heating temperature conditions or by repeatedly performing the observation on the same sample.
[0046]
In addition, the above-described electron microscope sample processing apparatus can easily realize evaluation under various heating temperature conditions and gas conditions without using an actual semiconductor process apparatus. Furthermore, the heat reaction process, the thinning process, and the electron microscope observation can be performed on the bulk sample while the sample is mounted on the same electron microscope sample holder. Therefore, the sample after the thermal reaction treatment can be quickly observed with the electron microscope, and the reaction process can be quickly evaluated.
[0047]
That is, according to the present invention, the time required for developing a semiconductor manufacturing process can be greatly reduced.
[Brief description of the drawings]
FIG. 1 is a diagram showing a sample preparation procedure using a heating reaction apparatus as a sample processing apparatus for an electron microscope of the present invention.
FIG. 2 is a diagram showing a sample preparation procedure following FIG. 1;
FIG. 3 is a diagram showing an appearance of a sample stage on which a sample is fixed.
FIGS. 4A and 4B are a plan view and a side view of a sample holder for an electron microscope according to the present invention. FIGS.
FIG. 5 is a view showing an appearance of a heating reaction apparatus in FIG.
6 is a diagram showing an appearance of a sample stage different from FIG. 3. FIG.
7 is a view showing a state in which the sample stage shown in FIG. 6 is mounted on a sample holder for an electron microscope.
[Explanation of symbols]
2, 32 ... sample, 2a ... thin piece,
6,31 ... Sample stage 7,33 ... Recess,
8 ... Metal plate, 9 ... Screw
10, 35 ... Sample holder for electron microscope, 11, 34 ... Sample stage fixing jig,
13 ... Heating reaction device, 14 ... Sample chamber,
15 ... temperature controller, 16 ... piping,
18 ... Local sample heating device, 19 ... IR light,
21 ... Ga charged particle ion beam, 22 ... electron beam,
31a, 31b ... Sample stage members.

Claims (7)

An electron microscope sample processing apparatus for processing a sample for electron microscope observation,
A sample chamber into which a tip portion including the sample stage of the sample holder for an electron microscope equipped with the sample stage is inserted;
Exhaust means for exhausting the sample chamber;
Gas supply means for supplying gas in the sample chamber by switching its type and flow rate;
A sample local heating means for directly directly heating the location of the sample stage in the sample holder for the electron microscope inserted in the sample chamber;
A radiation thermometer for measuring the temperature of the sample stage;
Based on the temperature measured by the radiation thermometer, the sample for electron microscope tip into the sample chamber of the child microscope sample processing apparatus electrodeposition having heating temperature control means for controlling the heating temperature by the sample local heating means is inserted A holder,
A holder body having a rod shape;
A sample stage on which the sample is mounted and fixed;
Provided at one end of the holder body, and a fitting groove for fitting the sample stage;
The one end that forms the fitting groove on the sample stage that is provided on the other end side opposite to the one end side with respect to the fitting groove in the holder main body and is fitted in the fitting groove. An elastic member that is pressed against and fixed to the side wall;
When the one end side including the sample stage is inserted into the sample chamber of the sample processing apparatus for an electron microscope, provided on the other end side than the fitting groove on the outer peripheral surface of the holder body, the sample chamber An O-ring that is in close contact with the insertion port of the sample chamber and blocks the internal environment of the sample chamber from the external environment;
With
The one end side than the O-ring in the holder body has a structure that can be inserted into a converged charged particle beam apparatus and mounted.
The whole has a heat-resistant structure
A sample holder for an electron microscope . Te sample holder odor for electron microscope according to claim 1,
The sample stage is
A sample stage body having a recess for storing the sample, and having heat resistance,
A fixing member that fixes the sample stored in the recess to the sample stage body and has heat resistance.
A sample holder for an electron microscope, comprising: The sample holder for an electron microscope according to claim 2,
Fixing member of the sample stage is a plate member for holding the specimen, the specimen holder for electron microscope, characterized in Oh Rukoto the screws to secure the plate member to the sample stage body. An electron microscope sample processing apparatus for processing a sample for electron microscope observation,
A sample chamber into which a tip portion including the sample stage of the sample holder for an electron microscope equipped with the sample stage is inserted;
Exhaust means for exhausting the sample chamber;
Gas supply means for supplying gas in the sample chamber by switching its type and flow rate;
A sample local heating means for directly directly heating the location of the sample stage in the sample holder for the electron microscope inserted in the sample chamber;
A radiation thermometer for measuring the temperature of the sample stage;
A heating temperature control means for controlling the heating temperature by the sample local heating means based on the temperature measured by the radiation thermometer.
It met sample holder for electron microscope which tip is inserted into the sample chamber of the electron microscope sample processing apparatus having a,
A holder body having a rod shape;
A sample stage on which the sample is mounted and fixed;
A heat-resistant member having heat resistance and sandwiching the sample stage;
A fitting groove that is provided at one end of the holder body and fits the sample stage sandwiched between the heat-resistant members;
The sample stage, which is provided on the other end side opposite to the one end side than the fitting groove in the holder main body and is fitted in the fitting groove, is inserted into the fitting stage via the heat-resistant member. An elastic member that is pressed against and fixed to the wall surface on the one end side to form a groove;
When the one end side including the sample stage is inserted into the sample chamber of the sample processing apparatus for an electron microscope, provided on the other end side than the fitting groove on the outer peripheral surface of the holder body, the sample chamber An O-ring that is in close contact with the insertion port of the sample chamber and blocks the internal environment of the sample chamber from the external environment;
With
The one end side than the O-ring in the holder body has a structure that can be inserted into a converged charged particle beam apparatus and mounted.
Whole sample holder for electron microscope, characterized that you have had a thermostructural. Te sample holder odor for electron microscope according to claim 4,
The sample stage includes a heat-resistant sample stage body having a recess for housing the sample, and a heat-resistant lid member that covers the recess of the sample stage body,
The heat-resistant member has a contact surface that simultaneously contacts the end surfaces of the sample stage main body and the lid member. The heat-resistant member extends in the extending direction of the end surface and opens toward the end surface side. Provided with a groove having a cross-sectional shape,
An electron microscope characterized in that when the heat-resistant member is urged by the elastic member, the lid member of the sample stage is brought into close contact with the sample stage main body on the wall surface of the groove on the contact surface Sample holder. In the electron microscope sample holder according to claim 5,
The lid member of said sample stage, the sample holder for electron microscope, characterized in that it have a recess for housing the sample. A sample is attached to the sample stage according to any one of claims 1 to 6,
The sample stage to which the sample is attached is fitted and mounted in the fitting groove of the electron microscope sample holder according to claim 1 or claim 4,
An electron microscope sample processing apparatus for processing the one end side including the sample stage in an electron microscope sample holder on which the sample stage is mounted on a sample for electron microscope observation,
A sample chamber into which a tip portion including the sample stage of the sample holder for an electron microscope equipped with the sample stage is inserted;
Exhaust means for exhausting the sample chamber;
Gas supply means for supplying gas in the sample chamber by switching its type and flow rate;
A sample local heating means for directly directly heating the location of the sample stage in the sample holder for the electron microscope inserted in the sample chamber;
A radiation thermometer for measuring the temperature of the sample stage;
A heating temperature control means for controlling the heating temperature by the sample local heating means based on the temperature measured by the radiation thermometer.
Inserted into a sample chamber in a sample processing apparatus for an electron microscope, and the O-ring is brought into close contact with the insertion port of the sample chamber, and the sample is heated and reacted under desired gas conditions and desired heating conditions,
After the heating reaction, the electron microscope sample holder is taken out from the electron microscope sample processing apparatus, and the one end side of the holder main body is attached to the converged charged particle beam apparatus with respect to the O-ring. Thinned by a focused charged particle beam so that it can be observed,
After the thinning process, the electron microscope sample holder is taken out from the focused charged particle beam apparatus and attached to the electron microscope, and the thinned sample is observed with the electron microscope. Electron microscope observation method .

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