JPH0972836A - Method and apparatus for preparation of sample for total-reflection fluorescent x-ray analysis - Google Patents

Abstract

PROBLEM TO BE SOLVED: To simply prepare a sample used for a total-reflection fluorescent X-ray analysis by using a technique in which the surface of a material, to be analyzed, such as a silicone wafer or the like is dissolved by a dissolving liquid. SOLUTION: A material to be analyzed is placed on a material-to-be-analyzed mounting base 2. The material to be analyzed and a dissolving-liquid holding member 3 are faced by keeping a gap. A dissolving liquid which can dissolve the surface of the material to be analyzed is held in the gap. The dissolving- liquid holding member 3 and the material to be analyzed are moved relatively in the plane direction (the direction of A, the direction of B) of the material to be analyzed. The surface component of the material to be analyzed is dissolved by the dissolving liquid. The dissolving-liquid holding member 3 which has held the dissolving liquid is stopped in arbitrary coordinates on the material, to be analyzed, it is pulled up, the dissolving liquid is left on the material to be analyzed in a cohesive state, and dissolving liquid is dried. Thereby, a sample which is used for a total-reflection fluorescent X-ray analysis is prepared.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for preparing a sample to be subjected to total reflection X-ray fluorescence analysis by a method of dissolving the surface of a material to be analyzed such as a silicon wafer with a decomposition solution, and an apparatus used therefor. Regarding

[0002]

2. Description of the Related Art In various technical fields, it is necessary to analyze the surface components of a material to be analyzed with high precision.
Also in the field of electronic materials, trace impurities have a great influence on the characteristics of the electronic materials, and therefore highly sensitive analysis techniques are desired. More specifically, for example, since it is important to know the trace amount of impurities in the surface oxide film of a silicon wafer with respect to oxide film withstand voltage characteristics and the like, high-sensitivity analysis thereof is required.

Conventionally, as a method for detecting a trace amount of impurities in the surface oxide film of a silicon wafer, hydrofluoric acid which does not attack silicon itself but decomposes and dissolves silicon oxide is used as a decomposition liquid. The oxide film on the surface of the silicon wafer is dissolved by the decomposing solution, and this is recovered as an analytical sample, and the metal contained therein is analyzed by an atomic absorption spectrophotometer, IC.
A method of analyzing using a P mass spectrometer or the like is known. Then, as a technique relating to a method for preparing an analytical sample using such a decomposition solution, a technique of dissolving the surface of a silicon wafer by hydrogen fluoride vapor (Japanese Patent Laid-Open No. 60-1406).
No. 20), a method of spraying hydrogen fluoride vapor onto a silicon oxide film (JP-A-62-209335), a method of dissolving and recovering with ultrapure water after decomposition with hydrogen fluoride vapor (JP-A-1-98944). Gazette), the hydrofluoric acid is held between the material to be analyzed (silicon wafer) and the rod-shaped decomposition liquid holding portion, and the material to be analyzed and the decomposition liquid holding portion are moved relatively to each other. There is known a method (Japanese Patent Laid-Open No. 5-203548) for collecting such impurities in the decomposition liquid.

On the other hand, in recent years, a total reflection fluorescent X-ray analysis method has been known as a method for highly sensitively analyzing the surface of the material to be analyzed. In the total reflection X-ray fluorescence analysis method, the material to be analyzed is irradiated with excited X-rays under the condition of total reflection, and the fluorescent X-rays emitted thereby are received above the material to be analyzed and detected by a semiconductor detector. is there. According to this method, the amount of excitation X-rays contained in the detected X-rays can be greatly reduced, and therefore the signal-to-background ratio can be greatly improved, which enables highly sensitive analysis. Further, the excited X-rays that are incident on the material to be analyzed under the condition of total reflection excite only the surface of the material to be analyzed, and thus the obtained fluorescent X-rays are emitted from only the surface of the material to be analyzed. Therefore, the total reflection fluorescence X
The line analysis method enables surface analysis of the material to be analyzed.
Furthermore, according to this method, the analysis is performed for each point (usually, an area of about 1 cm ² ) on the surface of the material to be analyzed, so that the analysis area is scanned over the entire surface of the material to be analyzed for contamination elements. It is also possible to perform mapping.

[0005]

However, when the surface analysis of a silicon wafer is performed by the total reflection fluorescent X-ray analysis method, the analysis sensitivity of contaminant elements is about 10 ¹⁰ atm / cm ² , and thus 500 to 1 point / point. An analysis time of about 1000 seconds is required, which causes a problem that a long analysis time of one day or more is required to analyze the entire surface of a 6-inch silicon wafer.

For this, an atomic absorption spectrophotometer or an ICP
As in the case of surface analysis of a silicon wafer using a mass spectrometer or the like, the surface of the silicon wafer is dissolved with hydrofluoric acid, and the contaminant elements are collected in a hydrofluoric acid solution, and then total reflection fluorescence X It is possible to use it for line analysis. This makes it impossible to map contaminant elements, but it is expected to shorten the analysis time.

However, in the total reflection X-ray fluorescence analysis method, it is necessary to put the analysis sample in a wafer state rather than a solution state. Therefore, after dissolving the surface of the silicon wafer with hydrofluoric acid, the hydrofluoric acid Since the dissolved solution must be dried on the silicon wafer, and static drying is necessary to prevent the droplets from scattering, there arises a problem that this drying requires a long time. For example, when the hydrofluoric acid solution is dried under the condition of naturally drying in the draft, it takes about 12 to 24 hours.

In addition, when the surface of a silicon wafer is dissolved with hydrofluoric acid and the hydrofluoric acid solution is dried on the wafer and analyzed by total reflection fluorescent X-ray analysis, detection by a semiconductor detector is performed. So that the dry matter is located in the area,
It is necessary to dry the hydrofluoric acid solution within a range of a diameter of 10 mm or less so that the coordinates of the drying position can be recognized.

However, in the conventional method of dissolving the surface of the silicon wafer with hydrofluoric acid, the hydrofluoric acid solution is dried on the silicon wafer in such a narrow area and while making its coordinates recognizable. I can't. In particular, when the oxide film on the surface of the silicon wafer is thicker than the film thickness of the natural oxide film (usually 2 to 3 nm), the surface of the silicon wafer becomes hydrophilic and the hydrofluoric acid solution is less likely to aggregate. Difficult to dry in a small area.

Therefore, when the conventional method of dissolving the surface of a silicon wafer with hydrofluoric acid is used to analyze the surface contaminant element of the silicon wafer by using the total reflection X-ray fluorescence analysis method, silicon is used. There are two devices: a device that dissolves the surface of the wafer with hydrofluoric acid, and a device that dries the solution within a narrow range and at a predetermined analysis point so that the solution can be analyzed by total reflection X-ray fluorescence analysis. It is necessary to provide it separately. However, it is not preferable to use such two devices for the preparation of the analysis sample because the analysis operation becomes complicated and new impurities may be mixed.

The present invention is intended to solve the problems of the prior art as described above, and is used for total reflection X-ray fluorescence analysis by a method of dissolving the surface of the material to be analyzed such as a silicon wafer with a decomposition liquid. The purpose is to make it easy to prepare a sample to be provided.

[0012]

The inventor of the present invention holds a decomposition liquid such as hydrofluoric acid between a material to be analyzed such as a silicon wafer and a decomposition liquid holding portion, and When the impurities on the surface of the material to be analyzed are collected in the decomposition liquid by moving the and relative to each other, stop the decomposition liquid holding part at arbitrary coordinates on the analysis material and aggregate the decomposition liquid at the stop position. Let
By drying the aggregated droplets of the decomposition liquid at that position,
The inventors have found that the material to be analyzed can be subjected to total reflection X-ray fluorescence analysis by using the dried portion of the aggregated droplets as a measurement point, and thereby the above-mentioned object can be achieved, and completed the present invention.

That is, according to the present invention, the material to be analyzed and the decomposition liquid holding member are opposed to each other with a gap, and the decomposition liquid capable of dissolving the surface of the material to be analyzed is held in the gap, and the decomposition liquid is held. The holding member and the material to be analyzed are relatively moved in the plane direction of the material to be analyzed to dissolve the surface components of the material to be analyzed into a decomposition liquid, and a decomposition liquid holding member holding the decomposition liquid is optionally provided on the material to be analyzed. The sample is prepared for use in total reflection fluorescent X-ray analysis by stopping and pulling up the solution at the coordinates to allow the solution to remain in an aggregated state on the material to be analyzed, and then drying the solution. A sample preparation method for total internal reflection X-ray fluorescence analysis is provided.

Further, the present invention is an apparatus for carrying out such a method, which is an analytical material mounting base for mounting the analytical material, and the analytical material mounted on the analytical material mounting table. A decomposition liquid holding member for holding a decomposition liquid capable of dissolving the surface of the analysis material, and the analysis material and the decomposition liquid holding member mounted on the analysis material mounting table are relatively moved in the plane direction of the analysis material. Planar direction moving means, decomposition liquid holding member stopping means for stopping the decomposition liquid holding member at arbitrary coordinates on the analyzed material, pulling up the decomposition liquid holding member above the analyzed material placed on the analyzed material mounting table, Holding member pulling means for causing the decomposed liquid to remain in the agglomerated state on the analyzed material, and the decomposed liquid remaining on the analyzed material placed on the analyzed material mounting table in the agglomerated state Total reflection fluorescent X-ray having a drying means for drying Providing 析用 sample preparation device.

When the method of the present invention is carried out using the apparatus of the present invention, first, the material to be analyzed is placed on the material mounting table for the material to be analyzed,
The decomposition liquid is dropped at a predetermined position on the material to be analyzed, a decomposition liquid holding member is arranged thereon, and the decomposition liquid is held in a gap between the material to be analyzed and the decomposition liquid holding member. Alternatively, a decomposing liquid holding member is arranged at a predetermined position on the material to be analyzed, and the decomposing liquid is put in a gap between the two. Next, the analysis-direction material and the decomposition liquid holding member are relatively moved in the plane direction of the analysis material by the plane direction moving means, thereby moving the decomposition solution held on the analysis material along a predetermined locus, Next, the decomposition liquid holding member stopping means stops the movement of the decomposition liquid at a predetermined position on the material to be analyzed. As a result, the surface component of the material to be analyzed on the trajectory of the decomposition liquid is dissolved in the decomposition liquid and is collected in the decomposition liquid. Next, the decomposition liquid holding member holding the decomposition liquid on the material to be analyzed is pulled up above the material to be analyzed by the decomposition liquid holding member pulling means. Then, the decomposed liquid remains in an aggregated state on the analyzed material. In the present invention, the decomposed liquid in the agglomerated state is dried in situ by a drying means. Therefore, the material to be analyzed thus obtained is such that the dissolved substance of the surface component of the material to be analyzed is collected at the aggregation / drying site of the decomposition liquid. In the present invention, the aggregation / drying site of this decomposition liquid can be set at a predetermined position on the material to be analyzed. Therefore, it becomes possible to analyze the material to be analyzed by total reflection fluorescent X-ray analysis using this portion as an analysis point.

Further, at this aggregation / drying site, the surface components dissolved in the decomposition liquid are concentrated more than the original surface of the material to be analyzed. Therefore, the time required for the analysis can be shortened to an extremely short time as compared with the case where the surface of the material to be analyzed is directly analyzed by total reflection X-ray fluorescence analysis without dissolving the surface components in the decomposition liquid. Become. For example,
The surface analysis of the entire surface of the silicon wafer, which has conventionally been required all day and night, can be performed in about 1.5 hours.

Furthermore, it is possible to map the surface components of the material to be analyzed by appropriately controlling the path of the decomposed liquid on the material to be analyzed and using the aggregation / drying site for each path as the analysis point. .

[0018]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be specifically described below with reference to the drawings. In each drawing, the same reference numerals represent the same or equivalent constituent elements.

FIG. 1 is a basic configuration diagram of an apparatus 1 of the present invention for analyzing various thin films (including a natural oxide film) on the surface of a silicon wafer and trace amounts of impurities in the wafer surface layer. The apparatus 1 shown in FIG. 1 includes an analyte mounting base 2 for mounting a silicon wafer as an analyte, a decomposition liquid holding member 3,
A plane direction moving means 4 for moving the decomposition liquid holding member 3 with respect to the silicon wafer placed on the analyzed material placing table 2 in the plane direction (generally diametrical direction) of the silicon wafer indicated by an arrow A in the figure,
The position detecting unit 5 (5-1, 5-2) functioning as a decomposing liquid holding member stopping means for stopping the decomposing liquid holding member 3 holding the decomposing liquid at arbitrary coordinates of the silicon wafer, and the decomposing liquid holding member 3 are made of silicon. A pneumatic cylinder 6 that functions as a means for pulling up the decomposition liquid holding member above the wafer, and a drying means (not shown) for drying the decomposition liquid condensed on the silicon wafer mounted on the analyte mounting base 2. ) Is basically composed of.

Here, the analyte mounting base 2 is constructed so that a silicon wafer can be fixed. For this purpose, a vacuum chuck may be provided on the analyte mounting table 2,
Since an orientation flat is usually formed on a silicon wafer, as shown in FIG. 2, the analyte mounting base 2 is preferably shaped to engage with the silicon wafer on which the orientation flat is formed. As a result, the positional relationship between the analyzed material mounting table 2 and the analyzed material can always be the same.

Further, the material mounting base 2 is rotated by the driving means 7 provided therebelow as indicated by an arrow B in the figure. As a result, on the silicon wafer placed on the analyte mounting base 2, the silicon wafer and the decomposition liquid holding member 3
It is possible to move the decomposed liquid held between and in the circumferential direction of the silicon wafer.

The decomposing liquid holding member 3 is a silicon wafer placed on the analyte mounting base 2 and the decomposing liquid holding member 3, and hydrofluoric acid or a mixed acid of hydrofluoric acid and nitric acid. It holds the droplets of the decomposition liquid of the silicon wafer. In this case, the droplet amount of the decomposition liquid is 50 to
It is preferably about 100 μl. Therefore, the decomposition liquid holding member 3 is about 0.5 to 3 mm between the decomposition liquid holding member 3 and the silicon wafer mounted on the analyzed material mounting base 2 so as to hold such a droplet amount when holding the decomposition liquid. It is preferable to provide them so that there is an interval.

The shape of the decomposition liquid holding member 3 is such that the decomposition liquid is held between the decomposition liquid holding member 3 and the silicon wafer placed on the analyte mounting base 2, and the decomposition liquid is held on the silicon wafer. Although it is not particularly limited as long as it can be moved by, the fine protrusion 3a is preferably provided at the central portion of the bottom surface of the decomposition liquid holding member 3 facing the silicon wafer S, as shown in FIG. Thereby, when the decomposition liquid holding member 3 is pulled up above the silicon wafer S, the center of the droplets of the decomposition liquid L that are aggregated and remain on the silicon wafer S are
Due to the surface tension of the droplet, it comes to the position of the minute protrusion 3a regardless of the size of the droplet. Therefore, in combination with the action of the position detection unit 5, it becomes possible to accurately leave the aggregated droplets of the decomposition liquid at a predetermined position on the silicon wafer.

The decomposition liquid holding member 3 is made of a material having acid resistance such as hydrofluoric acid or a mixed acid of hydrofluoric acid and nitric acid, water repellency, and high material purity. Therefore, it is preferable to use polytetrafluoroethylene.

In the apparatus 1 of FIG. 1, the plane direction moving means 4 includes an arm 4a for supporting the decomposed liquid holding member 3 and a joint 4.
b, a shaft 4c, and a cam mechanism 4d. As a result, the decomposition liquid holding member 3 moves in the plane direction (generally the diameter direction) of the silicon wafer indicated by the arrow A in the figure.

In addition, in the apparatus 1 of FIG. 1, the position detection unit 5
Is a detection unit 5-1 that regulates the movement of the decomposition liquid holding member 3 in the direction of arrow A in the figure, and a detection unit 5-2 that regulates the rotational movement of the analyte mounting table 2 in the direction of arrow B in the diagram. Has become. Of these, the detection unit 5-1 that regulates the movement of the decomposed liquid holding member 3 in the direction of the arrow A stops the decomposed liquid holding member 3 at predetermined coordinates on the material to be analyzed. As for this concrete configuration,
A stopper that can move in the direction of arrow C in the drawing can be provided so that the moving range of the cam mechanism 4d can be limited to a predetermined range.

On the other hand, the detection unit 5-2 which regulates the rotational movement of the analyte mounting base 2 in the direction of the arrow B is, for example, a reflection plate attached to the peripheral edge of the back surface 2b of the analyte mounting base 2 at a predetermined interval. And a detection means for irradiating the peripheral portion of the back surface 2b of the analyzed material mounting table and receiving the reflected light from the peripheral portion, and the detection signal from the detection section 5-2 is used for the analyzed material mounting table. 2 is fed back to the driving means 7 for rotating.

By providing the position detector in this way, for example, as shown in FIG. 4, the decomposed liquid is aggregated at the center point P1 of the material S to be analyzed or at fixed points P2 to P6 on a straight line in the radial direction. It becomes possible.

Further, in this case, the decomposing liquid to be aggregated at the fixed points P2 to P6 can be set to move on an arc having a predetermined center angle θ of the radius r. For example,
The decomposition liquid that agglomerates at the fixed points P2 to P6 moves in an arc shape having a central angle θ = 180 ° on the side opposite to the orientation flat, and it can be assumed that contaminant elements on the surface of the silicon wafer are collected during that time.

By thus aggregating the decomposed solution at multiple points on the silicon wafer and controlling the movement loci thereof appropriately, the distribution of contaminant elements on the silicon wafer can be determined by the conventional total reflection X-ray fluorescence analysis method. It becomes possible to analyze according to the mapping in.

In the apparatus 1 shown in FIG. 1, the pneumatic cylinder 6 provided as a means for pulling up the decomposed liquid holding member controls the position of the decomposed liquid holding member 3 in the vertical direction, and the moving speed in the vertical direction. Control. As the pneumatic cylinder 6, for example, the one having the configuration shown in FIG. 5 can be used. The pneumatic cylinder of FIG. 5 has upper and lower internal spaces 6x, 6
An ordinary two-way valve 8 is used as a valve that communicates with y.
Needle valves 8x, 8y in addition to p, 8q, 8r, 8s
Is provided. Due to the action of the needle valves 8x and 8y, the vertical movement of the pneumatic cylinder 6 is, for example, 0.
Since the control is performed at a slow speed of about 5 to 1 mm / sec, it is possible to prevent the decomposition liquid on the silicon wafer from splashing when the decomposition liquid holding member 3 is pulled up. Therefore, it is possible to improve the positional accuracy when the decomposed liquid is aggregated at a predetermined position on the silicon wafer.

The drying means for drying the decomposed liquid condensed on the silicon wafer is not particularly limited, and for example, as shown in FIG. 6, a heater plate 9 is provided immediately below the analyte mounting base 2. be able to. As the heater plate 9, for example, one having an electric heater and a temperature sensor inside can be provided. As a result, the silicon wafer S mounted on the analyzed material mounting table 2 is
It is possible to rapidly dry the droplets of the decomposition liquid aggregated on the top.

In addition to the above, as the drying means, an exhaust means for incorporating the analyte mounting base 2 in a sealed chamber and exhausting the inside of the chamber may be provided to further reduce the vapor pressure of the decomposition solution in the chamber. A gas replacement means for replacing with dry nitrogen or the like may be provided. Further, a heating lamp for irradiating the decomposition liquid condensed on the analysis material from above the analysis material may be provided, or a magnetron for heating the decomposition solution by microwave may be provided.

The apparatus 1 shown in FIG. 1 is used as follows. That is, first, the silicon wafer S is placed on the analyte mounting base 2.
The decomposing liquid holding member 3 is placed at a predetermined position on the silicon wafer S with a gap from the silicon wafer S, and the decomposing liquid is supplied to the gap using a micropipette or the like. Alternatively, after placing the silicon wafer S on the analyzed material placing table 2, the decomposing solution is dropped at a predetermined position on the silicon wafer S by using a micropipette or the like, and the decomposing solution holding member 3 is arranged thereon. The decomposition liquid is held in the gap between the silicon wafer S and the decomposition liquid holding member 3. Next, the decomposing liquid holding member 3 is moved so that the decomposing liquid takes a predetermined locus on the silicon wafer S, and the driving means 7 is driven. Then, the movement of the decomposition liquid holding member 3 and the driving by the driving means 7 are stopped at a predetermined aggregation position on the silicon wafer S, the decomposition liquid holding member 3 is pulled up, and the decomposition liquid is aggregated and left at that position. Then, the decomposition liquid is dried by a drying means. The silicon wafer thus obtained can be subjected to total reflection fluorescent X-ray analysis with the aggregation / drying region of the decomposed liquid as an analysis point.

The apparatus of the present invention can take various modes other than the apparatus 1 shown in the apparatus of FIG. For example, FIG.
As shown in FIG.
0, and a lid 11 for sealing the silicon wafer S placed on the analyte mounting base 2 can be provided. Hydrofluoric acid or the like is put into the liquid reservoir 10, the silicon wafer S is placed on the analyte mounting base 2, sealed with the lid 11, and heated by the heater plate 9 if necessary, by vapor of hydrofluoric acid or the like. The surface oxide film of the silicon wafer S can be decomposed in the vapor phase. Therefore, even if it is difficult to agglomerate the decomposing solution at one point because the surface oxide film of the silicon wafer S is thick, it is possible to agglomerate the decomposing solution at a point by vapor-decomposing the surface oxide film in advance. It becomes possible and the method of the present invention can be applied.

Further, while holding the decomposition liquid between the decomposition liquid holding member and the silicon wafer, the droplets of the decomposition liquid are moved on the surface of the silicon wafer to collect the pollutant element in the decomposition liquid. The decomposition solution holding member may move in the direction perpendicular to the plane of the silicon wafer. This allows
Even if bubbles are generated in the decomposition liquid while moving the droplets of the decomposition liquid on the surface of the silicon wafer, the bubbles can be removed, and the dissolution action of the decomposition liquid on the surface of the silicon wafer is constantly maintained. It becomes possible to do.

The material to be analyzed is not limited to the silicon wafer. Various analytes can be prepared as samples for total reflection fluorescent X-ray analysis by changing the type of decomposition solution.

[0038]

【Example】

Example A silicon wafer (5 inches) was prepared as a sample for total reflection fluorescent X-ray analysis using the apparatus 1 shown in FIG. 1 and surface analysis was performed. In this case, 100 μl of a mixed acid of hydrofluoric acid and hydrogen peroxide was used as the decomposition liquid, and
As described above, the surface component of the silicon wafer on the locus was collected, and the surface component of the silicon wafer was collected and dried by heating (170 ° C., 90 min) with a heater just below the silicon wafer mounting table to dry.

The measurement conditions for the total reflection X-ray fluorescence analysis were set as follows.

X-ray source: voltage 30 KV, current 200 mA,
Target Tungsten Measurement time: 500 sec X-ray glancing angle: 0.12 degrees This result is shown in FIG.

Comparative Example A total reflection X-ray fluorescence analysis was carried out in the same manner as in the above example except that a silicon wafer was directly used as an analysis sample without collecting surface components of the silicon wafer with a decomposition solution. The result is shown in FIG.

By comparing the analysis results of these Examples and Comparative Examples, the impurity elements on the surface of the silicon wafer appear as large peaks in the Examples, so that the method of the present invention improves the analysis accuracy and analysis efficiency. It turns out that it can be improved.

[0043]

According to the present invention, it is possible to easily prepare a sample to be subjected to total reflection X-ray fluorescence analysis by using a method of dissolving the surface of a material to be analyzed such as a silicon wafer with a decomposition liquid. Further, by using the sample prepared according to the present invention, it is possible to greatly improve the analysis efficiency when the surface analysis of the material to be analyzed such as the silicon wafer is performed by the total reflection X-ray fluorescence analysis.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram of an apparatus of the present invention.

FIG. 2 is a perspective view of an analyte mounting table.

FIG. 3 is a cross-sectional explanatory view of a decomposition liquid holding member.

FIG. 4 is an explanatory diagram of a trajectory of a decomposition liquid on a material to be analyzed and an aggregation / drying position.

FIG. 5 is an explanatory diagram of a pneumatic cylinder.

FIG. 6 is an explanatory diagram of a heater plate provided immediately below an analysis material mounting table.

FIG. 7 is a cross-sectional view of another aspect of the analyte mounting base.

FIG. 8 is an explanatory diagram of the trajectory of the decomposition liquid on the material to be analyzed and the aggregation / drying position in the example.

FIG. 9 is a chart of total reflection X-ray fluorescence analysis of an example.

FIG. 10 is a chart of a total reflection X-ray fluorescence analysis of a comparative example.

[Explanation of symbols]

 1 Sample preparation device for total reflection X-ray fluorescence analysis 2 Analytical material mounting table 3 Decomposition liquid holding member 4 Plane direction moving means 5, 5-1 and 5-2 Position detection unit 6 Pneumatic cylinder 9 Heater plate 10 Liquid reservoir 11 Lid S Analyte

Front page continuation (72) Inventor Masahisa Enomoto 6-735 Kita-Shinagawa, Shinagawa-ku, Tokyo Sony Corporation

Claims (8)

[Claims] 1. A material to be analyzed and a decomposition liquid holding member are opposed to each other with a gap, and a decomposition liquid capable of dissolving the surface of the material to be analyzed is held in the gap, and the decomposition liquid holding member and the member to be decomposed. Dissolve the surface component of the analysis material in the decomposition liquid by relatively moving the analysis material in the plane direction of the analysis material,
By stopping the decomposition liquid holding member holding the decomposition liquid at any coordinate on the material to be analyzed and pulling it up, the decomposition liquid remains in the aggregated state on the material to be analyzed, and then the decomposition liquid is dried. A method for preparing a sample for total reflection fluorescent X-ray analysis, which comprises preparing a sample for total reflection X-ray fluorescence analysis. 2. The method for preparing a sample for total reflection fluorescent X-ray analysis according to claim 1, wherein the decomposition liquid left in the aggregated state on the material to be analyzed is dried by heating with a heater. 3. The decomposed liquid holding member having a projection at the center of the surface facing the material to be analyzed is used.
Or the method for preparing a sample for total reflection fluorescent X-ray analysis according to item 2. 4. The method for preparing a sample for total internal reflection fluorescent X-ray analysis according to claim 1, wherein the decomposition liquid holding member is pulled up by a pneumatic cylinder. 5. A sample preparation apparatus for total internal reflection fluorescent X-ray analysis for carrying out the method according to claim 1, wherein the analysis material mounting table for mounting the analysis material and the analysis material mounting table are mounted. The decomposed liquid holding member for holding the decomposed liquid capable of dissolving the surface of the analyzed material on the placed analyzed material, the analyzed material and the decomposed liquid holding member mounted on the analyzed material mounting table Plane direction moving means for relative movement in the plane direction of the analytical material, decomposing liquid holding member stopping means for stopping the decomposing liquid holding member at arbitrary coordinates on the analyzed material, and of the analyzed material placed on the analyzed material mounting table A decomposition liquid holding member pulling means for pulling up the decomposition liquid holding member upward and leaving the decomposition liquid in an aggregated state on the material to be analyzed,
And a drying means for drying the decomposition liquid remaining in an agglomerated state on the analyzed material placed on the analyzed material placing table. 6. The apparatus according to claim 5, wherein a heater plate is provided as a drying means immediately below the analyte mounting base. 7. The apparatus according to claim 5, wherein the decomposition liquid holding member has a protrusion at the center of the surface facing the material to be analyzed. 8. The apparatus according to claim 5, further comprising a pneumatic cylinder as the means for pulling up the decomposition liquid holding member.