JP3727532B2 - Thin piece sample processing apparatus and thin piece sample processing method - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a processing apparatus and a processing method for performing surface treatment including chemical treatment on a thin sample used mainly in a transmission electron microscope (TEM).
[0002]
[Prior art]
Conventionally, as a method for chemically treating a thinned sample for a transmission electron microscope sample, as shown in FIG. 1, a method is generally used in which a sample 101 is held by a sharp tweezer 102 and directly immersed in a chemical bath 103. It was the target.
[0003]
In this method, the sample 101 sliced to a predetermined size is fixed to the single-hole mesh 106, and the ends of the single-hole mesh 106 are held by the tweezers 102, while the chemical tank 103, the pure water tank 104, and the organic solvent tank A method in which a predetermined solution treatment is performed in the order of 105 and then placed on the glass plate 107 and dried by blowing air from the dryer 108 from above the sample is often used.
[0004]
JP-A-9-133618 discloses a thin film forming apparatus that is integrated with an ion milling apparatus and sprays a chemical solution for chemical treatment immediately after ion milling. For example, it is said that a thin film sample suitable for high-resolution observation and EDX analysis without an ion damage layer can be produced.
[0005]
On the other hand, Japanese Patent Application Laid-Open No. 60-36676 discloses a plate-like material treatment characterized in that a chemical solution is supplied to a sample from one nozzle while the sample is rotated, and then water is supplied from the nozzle. There is a description of the apparatus, which is said to achieve the uniform and clean etching desired in the semiconductor industry.
[0006]
Further, in Japanese Patent Laid-Open No. 4-215436, a chemical solution is sprayed in a chamber separate from a processing chamber in which a sample is held, and the fog atmosphere is transported to the processing chamber in which the sample is held and reacted. There is a description of a silicon wafer cleaning apparatus characterized by performing water washing in accordance with the above, and according to this, the entire front and back surfaces of the silicon wafer can be cleaned uniformly and with a high degree of cleaning.
[0007]
[Problems to be solved by the invention]
However, a transmission electron microscope sample is usually thinned to a thickness of 0.1 μm or less for electron beam transmission observation, and often breaks during the solution treatment described above. Moreover, in order to prevent breakage, rapid operation cannot be performed during solution processing, and it is difficult to accurately manage the solution processing time. Further, when hydrofluoric acid treatment is performed, a low-quality oxide film is formed on the Si surface due to the influence of light, which may obstruct observation.
[0008]
Further, in the thin film forming apparatus described in Japanese Patent Laid-Open No. 9-133618, in order to perform processing in a vacuum apparatus, it is necessary to take out a sample from the thin film forming apparatus at the time of washing with water, and it is difficult to control the reaction time. . Moreover, it is necessary to perform washing with water while holding the sample with tweezers, which may damage the sample.
[0009]
On the other hand, in the plate-like object processing apparatus described in Japanese Patent Application Laid-Open No. 60-36676, the sample thickness is 0.1 μm or less because the sample is rotated so that the chemical solution is uniformly distributed in the sample. The transmission electron microscope sample that is present may be damaged. In addition, since the chemical solution and the water washing nozzle are shared, it is difficult to shorten the processing time.
[0010]
Furthermore, the silicon wafer cleaning apparatus described in Japanese Patent Laid-Open No. 4-215436 requires a mechanism for generating fog in a separate chamber, and the configuration of the cleaning apparatus becomes complicated. In addition, in order to change the type of chemical solution, it is necessary to sufficiently remove the chemical solution used before in the fog atmosphere chamber and the processing chamber so that the mist mixed with the previously used chemical solution is not generated. The type cannot be changed. Furthermore, since the transmission electron microscope sample is very thin, it is necessary to control the processing time in seconds. However, it takes time because the indoor atmosphere becomes uniform due to the transport of the fog atmosphere. Is difficult to control in seconds.
[0011]
The object of the present invention is to perform surface treatment including chemical treatment in a short time because the reaction time can be controlled in seconds when the sample is processed without damaging the thinned sample. It is to provide a possible flake sample processing apparatus and flake sample processing method.
[0012]
[Means for Solving the Problems]
The present invention has the following configuration.
[0013]
(1) A sample holding mechanism for holding the thin piece sample is provided in a processing chamber for performing surface treatment including chemical treatment with plural kinds of liquids on the thin piece sample, and each of the plural kinds of liquids is provided in the vicinity of the sample. And at least one nozzle, and the liquid is sprayed or ejected from the nozzle toward the sample held by the sample holding mechanism.
[0014]
In this configuration, a sample holding mechanism that holds a thin sample in the processing chamber is provided, and tips of a plurality of nozzles are directed so that the surface treatment can be performed on the sample held in the sample holding mechanism. Therefore, the surface treatment with multiple types of liquids is performed without moving the sample, and the treatment time can be controlled with high precision because it is possible to instantly switch between chemicals, pure cleaning, etc., and damage to the sample due to movement is prevented. Is done. In addition, by spraying or spraying only one type of liquid for each nozzle, mixing of different types of liquid is prevented, and cleaning of the nozzle each time the liquid is sprayed or sprayed becomes unnecessary, thereby shortening the work time. Figured.
[0015]
(2) The processing chamber includes a light source unit that irradiates a sample with light from a specific light source, and a light shielding wall that blocks light other than the light from the specific light source.
[0016]
In this configuration, since the sample is irradiated with light from a light source that promotes the surface treatment and light unnecessary for the surface treatment is blocked, the influence of the light in the surface treatment is controlled.
[0017]
(3) the processing chamber you comprising the exhaust mechanism for exhaust individually for each liquid used in the surface treatment.
[0018]
In this configuration, since the gas mixture generated by the plurality of types of liquids used for the surface treatment is eliminated, the thin sample processing apparatus is safely operated.
[0019]
(4) The processing chamber individually includes a plurality of waste liquid tanks that individually store waste liquids generated by spraying or jetting liquid from the nozzles supplied to the sample, and each of these waste liquid tanks and the processing chamber. And a plurality of waste liquid paths communicating with each other.
[0020]
In this configuration, the waste liquid generated by spraying or jetting the liquid from the nozzle is individually stored for each waste liquid, so there is no danger of mixing different types of waste liquids to cause a chemical reaction, and the treatment of these waste liquids is not possible. Easy to do.
[0021]
(5) The processing chamber includes a blower mechanism that supplies hot air or cold air to the sample, and blows air to the sample at a predetermined timing.
[0022]
In this configuration, since the sample surface is instantaneously dried by the surface treatment using the nozzle, the time required for a series of surface treatments can be shortened and the sample can be prevented from being damaged.
[0023]
(6) The sample holding portion of the sample holding mechanism is formed of a conductive material and a chemical resistant material covering the conductive material, and a desired voltage is applied to the conductive material from a power source provided outside the processing chamber. Features.
[0024]
In this configuration, a voltage is applied to the thin piece sample subjected to the surface treatment from a power source provided outside the processing chamber via a sample holding mechanism, so that the electrical and chemical processes such as electrolytic etching are performed. Treatment by reaction is easily performed. In addition, since the surface of the sample holder is made of a chemical resistant material, deterioration of the conductivity function and the holding function of the sample holder due to corrosion caused by the liquid used for the surface treatment is prevented.
[0025]
(7) The sample holding mechanism can be inserted into and removed from the processing chamber through an insertion port provided in the processing chamber, and the insertion port includes a sample holding mechanism, an insertion port, and a chemical resistant sealing material. The present invention is characterized in that a leakage prevention mechanism for preventing leakage of liquid from the joint portion is provided.
[0026]
In this configuration, there is provided a leakage prevention mechanism for preventing leakage of liquid from the joint between the sample holding mechanism and the insertion port when the sample holding mechanism is inserted or removed at the insertion port provided in the processing chamber. Therefore, leakage of dangerous liquid from the thin sample processing apparatus is prevented, and the sample holding mechanism can be inserted or removed safely.
[0027]
(8) The processing chamber includes an inert gas supply nozzle that fills the processing chamber with an inert gas.
[0028]
In this configuration, since the nitrogen supply nozzle is provided to make the inside of the processing chamber a nitrogen atmosphere in which the sample is hardly oxidized, oxidation of the sample surface after the surface treatment is prevented.
[0029]
(9) A surface treatment step including chemical treatment for spraying or jetting liquid on the thin piece sample held in the treatment chamber, a drying step for blowing air to the thin piece sample from the blower mechanism, A series of processes including exhaust and drain processes for exhausting and draining gases and liquids are repeatedly performed on each of a plurality of types of liquids, and the surface treatment process irradiates light from a light source as necessary. An irradiation step to be performed; and a voltage application step of applying a voltage from a power source through a sample holding mechanism.
[0030]
In this configuration, a control unit that efficiently performs a series of processes including the surface treatment process, the drying process, and the exhaust / drain process is provided. If necessary, an irradiation process and a voltage application process are provided. Are controlled to be added to the series of steps, the surface treatment of the thin sample can be performed efficiently in a short time.
[0031]
DETAILED DESCRIPTION OF THE INVENTION
The present invention will be described below with reference to the drawings.
[0032]
FIG. 2A is a front view of the thin piece sample processing apparatus 20 of the present invention, and FIG. 2B is a top view of the processing apparatus. The inner wall of the processing apparatus is covered with a material that can withstand an acidic solution and an alkaline solution, such as polytetrafluoroethylene. At this time, in consideration of the influence of unnecessary light on the etching process of the sample, if a sufficient light shielding property cannot be obtained with only the inner wall, a light shielding outer wall is provided separately.
[0033]
A sample holder insertion port 14 is provided on any of the inner walls described above, and the sample holder 11 for fixing the single-hole mesh 10 holding the sample 9 is inserted and removed from the sample holder insertion port 14. Is possible. In this embodiment, the sample holder 11 serves as a sample holding mechanism.
[0034]
If the position of the sample 9 in a state in which the sample holder 11 is completely inserted into the thin piece sample processing apparatus 20 is referred to as a sample processing position A for convenience, the sample processing position A is located at substantially the center of the processing chamber 30. ing.
[0035]
A plurality of nozzles for performing surface treatment including chemical treatment protrude from the wall surface of the processing chamber 30, and their tips are arranged so as to face the sample processing position A in the vicinity of the sample 9. ing. These nozzles are provided so that nozzles for performing surface treatment including the same kind of chemical treatment are located on both sides of the sample 9.
[0036]
First, among these nozzles, an air nozzle 3 that blows warm air or cold air to the sample 9 in order to dry the sample 9 is positioned obliquely above the sample 9. In FIG. 2 (b), nozzles 1b, 1d, 1f, and 2b are provided counterclockwise from the air nozzle 3 around the sample 9, respectively, on the opposite side of the sample 9 with respect to them. Nozzles 1a, 1c, 1e and 2a are provided.
[0037]
Of these nozzles, the nozzle 1b and the nozzle 1a on the opposite side spray the M dash liquid described later, and the nozzle 1d and the nozzle 1c on the opposite side spray the hydrofluoric acid described later. In the present embodiment, the nozzle 1f and the opposite side 1e are not used, but these nozzles are also used depending on the type of surface treatment performed on the sample 9. The number of nozzles is not limited to that of the present embodiment, and more nozzles may be used depending on the use of the thin piece sample to be processed.
[0038]
The nozzles 2a and 2b are nozzles for injecting pure water for rinsing the sample surface, thereby washing away the liquid sprayed on the surface of the sample 9.
[0039]
On the other hand, although not near the sample 9, a nitrogen nozzle 4 is provided on the inner wall of the processing chamber 30 to keep the inside of the sample chamber 30 in a nitrogen atmosphere in which the sample 9 is less likely to be oxidized. Similarly, on the inner wall of the processing chamber 30, an alkali exhaust port 5a is provided with an acid exhaust port 5b and an organic exhaust port 5c used when an organic solvent is used.
[0040]
In addition, in order to guide the liquid supplied to the sample 9 to the waste liquid path 6 on the bottom surface of the processing chamber 30, an inclination is provided toward the center of the bottom surface. The route 6 is led.
[0041]
Further, the sample chamber 30 is provided with waste liquid paths 6a, 6b, and 6c that communicate with the waste liquid path 6 and a waste liquid tank (not shown) that individually stores different waste liquids.
[0042]
Valves 15a to 15c are provided at the entrances of the respective waste liquid paths 6a to 6c, and the opening and closing of the valves 15a to 15c is controlled according to the liquid supplied to the sample 9 by a control unit (not shown). Thus, the same kind of waste liquid is accommodated in each waste liquid tank.
[0043]
Further, a light source unit 8 for irradiating light from a specific light source 7 is provided almost directly above the sample processing position A, and light from a specific light source that promotes surface treatment of the sample from here toward the sample 9. Is irradiated.
[0044]
Here, as a surface treatment method, if the objective is simply to make the sample 9 thin, the surface treatment may be performed using only an acidic solution. An acidic solution is used for the purpose of forming a step in the oxide film of the sample 9, and an alkaline solution is used for the purpose of forming a step in the silicon substrate that is not the oxide film but the sample body. Must be used. Therefore, it is necessary to use both an acidic solution and an alkaline solution for the surface treatment, but the sample is treated by having an exhaust port, a waste liquid path, and a valve corresponding to each of the acidic solution and the alkaline solution. This can be performed in one processing apparatus.
[0045]
Usually, the sample used for TEM etc. is very thin and easily damaged. When a dedicated device is used for each of the surface treatment with an acidic solution and the surface treatment with an alkaline solution, the alkaline solution is removed from the device dedicated to the treatment with an acidic solution. However, according to the present invention, it is possible to prevent such damage.
[0046]
In addition, by configuring the device to block light from the surroundings and irradiate light from a specific light source, the surface treatment speed can be adjusted by light, preventing reaction due to the influence of ambient light, Or it becomes possible to perform only the reaction by the light of a desired wavelength with good controllability.
[0047]
Next, operation | movement of the thin piece sample processing apparatus 20 of this invention is demonstrated. Here, FIG. 3 is a diagram showing the configuration of the sample holder.
[0048]
A peripheral portion of the single-hole mesh 10 holding the sample 9 processed into a shape capable of TEM observation is inserted into the sample holder 11 and fixed. This sample holder 11 is made of a core member 12 made of a conductive metal material inside, and the outside has no water absorption, such as polytetrafluoroethylene having chemical resistance, heat resistance, and solvent resistance. It is covered with a covering member 13.
[0049]
A portion where the single-hole mesh 10 holding the sample 9 is fixed is provided with a cut portion in the covering member 13, and when the single-hole mesh 10 is pushed in, the sample 9 is fitted into the covering member 13. Further, a through hole is formed in the covering member 13, and a fastener 16 is fitted from the surface of the covering member 13 into a hole provided in the single hole mesh 10 in advance in order to fix the sample 9. At this time, since the single-hole mesh 10 and the core member 12 are in contact with each other, the voltage applied to the core member 12 is also applied to the sample 9 through the single-hole mesh 10.
[0050]
Therefore, a potential can be applied to the sample 9 by applying a voltage to the conductive core member 12, and the etching rate of the sample 9 can be adjusted by adjusting this potential as necessary.
[0051]
Actually, when operating the thin piece sample processing apparatus 20, the sample holder 11 to which the sample 9 is fixed is inserted from the sample holder insertion port 14 of the processing chamber 30, and the sample 9 is disposed at the sample processing position A. The sample holder 11 is fixed.
[0052]
And in order to prevent the oxidation of the surface of the sample 9 after an etching process, the inside of the process chamber 30 is made into nitrogen atmosphere with the nitrogen nozzle 4. FIG. At this time, a mixed solution called an M dash solution is usually used as a chemical solution for etching the diffusion portion.
[0053]
A general composition ratio of the M dash liquid is HNO ₃ : HF: CH ₃ COOH: AgNO ₃ = 26: 6: 172: 1. The M dash solution has a high etching rate, and this M dash solution is used. When a thin TEM sample whose observation target is 0.1 μm or less is processed, time management in units of seconds is required. In this embodiment, the M dash liquid is sprayed from the chemical liquid nozzles 1a and 1b for about 10 seconds.
[0054]
After spraying with the M dash liquid on the sample 9, pure water is injected from the pure water nozzle 2 in order to sufficiently remove the M dash liquid remaining on the sample 9.
[0055]
At this time, in the processing apparatus of the present invention, by directly spraying the chemical solution in the vicinity of the sample 9, surface treatment can be performed by instantaneously changing the surface to be used to a chemical solution atmosphere, and by spraying pure water, it contributes to the surface treatment. Since the surface treatment can be stopped by washing away the liquid, the reaction time can be controlled in seconds.
[0056]
In addition, since the sample 9 can be held vertically while the surface treatment is being performed, the surface of the sample 9 can be removed without being immersed in an organic solvent for the purpose of water replacement drying. It can be dried sufficiently.
[0057]
Further, regarding the drying of the sample 9, the surface of the sample 9 can be further efficiently dried by blowing air from the air nozzle 3.
[0058]
Since this processing apparatus has a plurality of chemical liquid nozzles, it is possible to continuously perform different types of chemical liquid processing. For example, when a step is generated in the Si oxide film following the surface treatment with the M dash solution, 5% diluted hydrofluoric acid is sprayed from the chemical nozzles 1c and 1d for 10 seconds, and then pure water is sprayed from the pure water nozzle 2. By sufficiently removing hydrofluoric acid and blowing air from the air nozzle 3 to sufficiently dry the sample surface, different surface treatments can be continuously performed in the same processing chamber.
[0059]
When treatment with an organic solvent is required, there is a risk of explosion when an acidic solution is mixed with the organic solvent, and thus treatment in the same treatment apparatus is often dangerous. Further, there are cases where surface treatment with a liquid of a kind greater than the number of nozzles provided in the processing chamber 30 is necessary.
[0060]
In such a case, since the sample holder 11 can be removed from the sample holder insertion port 14 of the processing chamber 30 in this case, another processing device having the same configuration as that of the present invention is prepared separately, and the organic solvent is removed. You may make it use when using. Thus, after removing the sample 9 from the sample holder 11 and re-fixing it to the sample holder 11 again, the sample holder 11 is replaced with another processing apparatus prepared in advance, and then the organic solvent is discharged from the nozzle in the same manner as described above. The surface treatment of the sample 9 can be continued.
[0061]
The insertion port 14 of the present invention is processed with a seal member for preventing liquid leakage in the above replacement operation.
[0062]
As described above, after the thin piece sample is processed, the sample holder 11 is extracted from the processing apparatus, and the sample and the single-hole mesh 10 can be used as a sample for TEM observation in the present embodiment, for example. .
[0063]
【The invention's effect】
As described above, according to the present invention,
(1) A sample holding mechanism for holding a thin sample in the processing chamber is provided, and tips of a plurality of nozzles are directed so that the surface treatment can be performed on the sample held in the sample holding mechanism. Therefore, surface treatment with multiple types of liquids is possible without moving the sample, and it is possible to instantly switch between chemicals and pure cleaning, enabling highly controllable processing in seconds, and moving samples. Can be prevented from being damaged. Also, by spraying or spraying only one type of liquid for each nozzle, it is possible to prevent mixing of different types of liquids, eliminating the need for cleaning the nozzles every time the liquid is sprayed or sprayed, and shortening the work time. Can be achieved.
[0064]
(2) Since the sample is irradiated with light from a light source that promotes the surface treatment and light unnecessary for the surface treatment is blocked, the influence of light in the surface treatment can be controlled.
[0065]
(3) Since there is no gas mixing caused by a plurality of types of liquids used for the surface treatment, the thin sample processing apparatus can be operated safely.
[0066]
(4) Since the waste liquid generated by spraying or jetting the liquid from the nozzle is individually stored for each waste liquid, it is possible to eliminate the risk of mixing different types of waste liquid and causing a chemical reaction. can it is easy to row.
[0067]
(5) Since the sample surface by the surface treatment by the nozzle is instantly dried, the time required for a series of surface treatments can be shortened and the sample can be prevented from being damaged.
[0068]
(6) Since a voltage is applied to the thin sample subjected to the surface treatment through a sample holding mechanism from a power source provided outside the processing chamber, it is based on an electro-chemical reaction such as electrolytic etching. Processing can be performed easily. Further, since the surface of the sample holder is made of a chemical resistant material, it is possible to prevent deterioration of the conductivity function and the holding function of the sample holder due to corrosion caused by the liquid used for the surface treatment. .
[0069]
(7) Since the sample holding mechanism is equipped with a leakage prevention mechanism for preventing leakage of liquid from the joint between the sample holding mechanism and the insertion port when the sample holding mechanism is inserted or removed at the insertion port provided in the processing chamber. Further, leakage of dangerous liquid from the thin sample processing apparatus can be prevented, and the sample holding mechanism can be inserted or removed safely.
[0070]
(8) Since the nitrogen supply nozzle that makes the inside of the processing chamber a nitrogen atmosphere in which the sample is not easily oxidized is provided, oxidation of the sample surface after the surface treatment can be prevented.
[0071]
(9) A control unit that efficiently performs a series of processes including the surface treatment process, the drying process, and the exhaust / drain process is provided, and if necessary, an irradiation process and a voltage application process are performed. Since the control is performed so as to be added to the series of steps, the surface treatment of the thin sample can be performed efficiently in a short time.
[0072]
By using the thin sample processing apparatus of the present invention, it is possible to produce a sample with high reproducibility by a series of operations without damaging the sample.
[0073]
In addition, it is possible to observe the boundary position of the multilayer structure portion having the same main component and the diffusion shape of ion implantation with high resolution, which are difficult to observe with the conventional sample preparation method.
[0074]
Furthermore, after the treatment with acid, it is possible to efficiently perform continuous treatment such as washing the sample and further carrying out treatment with alkali.
[0075]
Therefore, it is possible to control the reaction time in seconds when processing the sample without damaging the thinned sample, and it is possible to perform surface treatment including chemical treatment in a short time because the reaction time can be controlled in seconds. A processing apparatus and a flake sample processing method can be provided.
[Brief description of the drawings]
FIG. 1 is a view showing a conventional thin piece sample processing method;
FIG. 2 is a diagram showing a configuration of a thin piece sample processing apparatus of the present invention.
FIG. 3 is a diagram showing a configuration of a sample holder of the present invention.
[Explanation of symbols]
1 (1a to 1f) -chemical nozzle 2-pure water nozzle 3-air nozzle 4-nitrogen nozzle 5 (5a-5b) -exhaust port 6 (6a-6b) -waste liquid port 7-light source 8-window 9-sample 10- Single-hole mesh 11-Sample holder 12-Core member 13-Coating member 14-Sample holder insertion port 15 (15a-15c) -Valve 16-Fastener 20-Flame sample processing apparatus 30-Processing chamber

Claims (9)

A sample holding mechanism for holding the thin piece sample is provided in a processing chamber for performing surface treatment including chemical treatment with a plurality of types of liquid on the thin piece sample, and at least one for each of the plurality of types of liquid is provided in the vicinity of the sample. Providing one nozzle, spraying or jetting the liquid from the nozzle toward the sample held in the sample holding mechanism ; and
The thin sample processing apparatus according to claim 1, wherein the processing chamber is provided with an exhaust mechanism for individually exhausting each liquid used for the surface treatment . A sample holding mechanism for holding the thin piece sample is provided in a processing chamber for performing surface treatment including chemical treatment with a plurality of types of liquid on the thin piece sample, and at least one for each of the plurality of types of liquid is provided in the vicinity of the sample. Providing one nozzle, spraying or jetting the liquid from the nozzle toward the sample held in the sample holding mechanism ; and
The processing chamber includes a plurality of waste liquid tanks for individually storing waste liquids generated by spraying or jetting the liquid supplied from the nozzle to the sample for each waste liquid, and a plurality of these waste liquid tanks individually communicating with the processing chamber. And a waste liquid path . The said processing chamber is provided with the light source part which irradiates the light of a specific light source to a sample, and the light-shielding wall which interrupts light other than the light of this specific light source, The Claim 1 or 2 characterized by the above-mentioned. Thin piece sample processing equipment. The said processing chamber is equipped with the ventilation mechanism which supplies a warm air or a cold wind with respect to a sample, and ventilates with a predetermined timing with respect to a sample. Thin piece sample processing equipment. The sample holding portion of the sample holding mechanism is formed of a conductive material and a chemical-resistant material covering the conductive material, and a desired voltage is applied to the conductive material from a power source provided outside the processing chamber. The thin piece sample processing apparatus according to claim 1. The sample holding mechanism can be inserted into and removed from the processing chamber through an insertion port provided in the processing chamber, and the insertion port is joined to the sample holding mechanism and the insertion port by a chemical-resistant sealing material. The thin sample processing apparatus according to any one of claims 1 to 5, further comprising a leakage prevention mechanism for preventing leakage of liquid from the apparatus. The thin sample processing apparatus according to claim 1, wherein the processing chamber includes an inert gas supply nozzle that fills the processing chamber with an inert gas. A surface treatment step including a chemical treatment for spraying or spraying a liquid on the thin sample held in the treatment chamber;
A drying step of blowing air from the air blowing mechanism to the thin piece sample;
A series of processes including exhaust and drain processes for exhausting and draining gas and liquid in the processing chamber are repeatedly performed for each of a plurality of types of liquids ,
The thin sample processing method, wherein the evacuation / drainage step includes a step of individually evacuating each liquid by an evacuation mechanism provided in the processing chamber . The processing chamber includes a plurality of waste liquid tanks that individually store waste liquids generated by spraying or jetting liquid supplied from the nozzles to the sample for each waste liquid, and a plurality of these waste liquid tanks that individually communicate with the processing chamber. A waste liquid path, and
  9. The thin piece sample processing method according to claim 8, wherein the exhausting / draining step includes a step of individually performing a waste liquid treatment for each liquid by the waste liquid tank and the waste liquid path.

Images