JP2012047470A - Sample fixing method, fluorescent x-ray detection method, sample fixture and fluorescent x-ray detection device - Google Patents

Sample fixing method, fluorescent x-ray detection method, sample fixture and fluorescent x-ray detection device Download PDF

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JP2012047470A
JP2012047470A JP2010187104A JP2010187104A JP2012047470A JP 2012047470 A JP2012047470 A JP 2012047470A JP 2010187104 A JP2010187104 A JP 2010187104A JP 2010187104 A JP2010187104 A JP 2010187104A JP 2012047470 A JP2012047470 A JP 2012047470A
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sample
ray
transmission sheet
ray transmission
fluorescent
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Hitomi Ono
ひとみ 大野
Satoshi Goto
智 後藤
Yoshihiro Yokota
佳洋 横田
Shintaro Komatani
慎太郎 駒谷
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Horiba Ltd
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Horiba Ltd
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Abstract

PROBLEM TO BE SOLVED: To provide a sample fixing method capable of fixing a flaky sample flatly without overlap width, a fluorescent X-ray detection method, a sample fixture and a fluorescent X-ray detection device.SOLUTION: An X-ray transmission sheet 14 extended at an opening end of a cylindrical member 11 is fixed by an O-ring (first fitting member) 12, and a flaky sample S is overlappedly arranged on the X-ray transmission sheet 14. Further, an X-ray transmission sheet 15 is overlapped on the sample S and the X-ray transmission sheet 14 to be extended at the opening end of the cylindrical member 11, and fixed by an O-ring (second fitting member) 13. The sample S is sandwiched and fixed between the X-ray transmission sheet 14 and the X-ray transmission sheet 15. The sample S is fixed flatly without overlap width, and there is no support other than the X-ray transmission sheets. An X-ray is transmitted through the X-ray transmission sheet 15 and irradiates the sample S, and a fluorescent X-ray generated by the sample S is detected.

Description

本発明は、蛍光Ｘ線分析を行うために薄片状の試料を固定する方法、蛍光Ｘ線検出方法、薄片状の試料を固定するために用いる試料固定具、及び蛍光Ｘ線検出装置に関する。   The present invention relates to a method for fixing a flaky sample for performing fluorescent X-ray analysis, a fluorescent X-ray detection method, a sample fixture used for fixing a flaky sample, and a fluorescent X-ray detection apparatus.

蛍光Ｘ線分析は、Ｘ線を試料に照射し、試料から発生する蛍光Ｘ線を検出し、蛍光Ｘ線のスペクトルから試料の元素分析を行う手法である。蛍光Ｘ線分析を行う際には、Ｘ線を照射する対象の試料を何らかの方法で固定する必要がある。特許文献１には、薄膜上に液体試料を滴下し、薄膜上で溶媒を蒸発させることにより、液体試料を薄膜上に固定する方法が記載されている。シート状の物体を切り取った試料等の薄片状の試料に対して蛍光Ｘ線分析を行う場合、従来では、アクリル板等の平板上に薄片状の試料を粘着テープで張り付けることにより、薄片状の試料を固定していた。   X-ray fluorescence analysis is a technique for irradiating a sample with X-rays, detecting fluorescent X-rays generated from the sample, and performing elemental analysis of the sample from the spectrum of the fluorescent X-rays. When performing fluorescent X-ray analysis, it is necessary to fix the sample to be irradiated with X-rays by some method. Patent Document 1 describes a method of fixing a liquid sample on the thin film by dropping a liquid sample on the thin film and evaporating the solvent on the thin film. When fluorescent X-ray analysis is performed on a flaky sample such as a sample obtained by cutting a sheet-like object, conventionally, the flaky sample is adhered to a flat plate such as an acrylic plate with an adhesive tape. The sample was fixed.

特開２００５−２９１８２３号公報JP 2005-291823 A

薄片状の試料を固定する従来の方法では、照射されたＸ線を粘着テープが吸収するので、試料中の粘着テープによる止め代の部分の分析ができないという問題がある。また従来の方法では、試料を支持している平板で散乱したＸ線が蛍光Ｘ線と共に検出されるので、蛍光Ｘ線信号のバックグラウンド信号が増加し、蛍光Ｘ線分析の精度が低いという問題がある。更に従来の方法では、薄片状の試料を平坦にして固定することが困難であり、試料の一部が浮き上がった状態で蛍光Ｘ線分析を行うこととなるので、試料の浮き上がりに起因する蛍光Ｘ線強度の変動により、蛍光Ｘ線分析の精度が低くなるという問題があった。   In the conventional method of fixing a flaky sample, the adhesive tape absorbs the irradiated X-rays, so that there is a problem that the portion of the stopper margin in the sample cannot be analyzed. Further, in the conventional method, since X-rays scattered by the flat plate supporting the sample are detected together with the fluorescent X-rays, the background signal of the fluorescent X-ray signal increases and the accuracy of the fluorescent X-ray analysis is low. There is. Further, in the conventional method, it is difficult to flatten and fix a flaky sample, and fluorescent X-ray analysis is performed in a state where a part of the sample is lifted. There was a problem that the accuracy of the fluorescent X-ray analysis was lowered due to the fluctuation of the line intensity.

本発明は、斯かる事情に鑑みてなされたものであって、その目的とするところは、薄片状の試料をシートで挟み込むことにより、止め代なしで平坦に試料を固定することができる試料固定方法、蛍光Ｘ線検出方法、試料固定具及び蛍光Ｘ線検出装置を提供することにある。   The present invention has been made in view of such circumstances. The object of the present invention is to fix a sample flatly without a stop margin by sandwiching a flaky sample between sheets. A method, a fluorescent X-ray detection method, a sample fixture, and a fluorescent X-ray detection apparatus are provided.

本発明に係る試料固定方法は、Ｘ線の照射対象となる薄片状の試料を固定する方法において、Ｘ線の通過経路になるべき空間中に、前記試料よりも広い第１のＸ線透過シートを張設し、張設した前記第１のＸ線透過シートに前記試料を重ねて配置し、前記試料よりも広い第２のＸ線透過シートを、前記試料及び前記第１のＸ線透過シートに重ねて張設することにより、前記第１のＸ線透過シート及び前記第２のＸ線透過シートの間に挟まった前記試料を固定することを特徴とする。   The sample fixing method according to the present invention is a method for fixing a flaky sample to be irradiated with X-rays, and is a first X-ray transmission sheet wider than the sample in a space to be an X-ray passing path. And the sample is placed on the stretched first X-ray transmission sheet, and the second X-ray transmission sheet wider than the sample is replaced with the sample and the first X-ray transmission sheet. The sample sandwiched between the first X-ray transmission sheet and the second X-ray transmission sheet is fixed by being overlapped with the first X-ray transmission sheet.

本発明に係る蛍光Ｘ線検出方法は、薄片状の試料へＸ線を照射し、前記試料から発生する蛍光Ｘ線を検出する方法において、Ｘ線の通過経路になるべき空間中に、前記試料よりも広い第１のＸ線透過シートを張設し、張設した前記第１のＸ線透過シートに前記試料を重ねて配置し、前記試料よりも広い第２のＸ線透過シートを、前記試料及び前記第１のＸ線透過シートに重ねて張設することにより、前記第１のＸ線透過シート及び前記第２のＸ線透過シートの間に挟まった前記試料を固定し、前記第２のＸ線透過シートを透過して前記試料へＸ線を照射し、前記試料から発生する蛍光Ｘ線を検出することを特徴とする。   The fluorescent X-ray detection method according to the present invention is a method for irradiating a flaky sample with X-rays to detect the fluorescent X-rays generated from the sample, and the sample is placed in a space to be a path for X-ray passage. A first X-ray transmission sheet wider than the first X-ray transmission sheet, the sample placed on the stretched first X-ray transmission sheet, and a second X-ray transmission sheet wider than the sample, The sample sandwiched between the first X-ray transmission sheet and the second X-ray transmission sheet is fixed by overlapping the sample and the first X-ray transmission sheet, and the second X-ray transmission sheet is fixed. The X-ray transmission sheet is transmitted to the sample, and the sample is irradiated with X-rays to detect fluorescent X-rays generated from the sample.

本発明に係る試料固定具は、Ｘ線の照射対象となる薄片状の試料を固定する試料固定具において、筒状部材と、該筒状部材の開口端に被せられるべき任意の第１のＸ線透過シートの外から前記筒状部材に外嵌すべき第１の嵌合部材と、前記試料を前記第１のＸ線透過シートとの間に挟んで固定すべく前記第１のＸ線透過シートに被せられるべき任意の第２のＸ線透過シートの外から前記筒状部材に外嵌すべき第２の嵌合部材とを備えることを特徴とする。   The sample fixing tool according to the present invention is a sample fixing tool for fixing a flaky sample to be irradiated with X-rays, and a cylindrical member and an arbitrary first X to be put on the opening end of the cylindrical member. The first X-ray transmission so as to sandwich and fix the sample between the first fitting member to be externally fitted to the cylindrical member and the first X-ray transmission sheet from outside the line transmission sheet. And a second fitting member to be fitted on the tubular member from outside an arbitrary second X-ray transmission sheet to be covered with the sheet.

本発明に係る蛍光Ｘ線検出装置は、Ｘ線を照射された試料から発生する蛍光Ｘ線を検出する蛍光Ｘ線検出装置において、本発明の試料固定具と、該試料固定具で固定された薄片状の試料へＸ線を照射する手段と、Ｘ線を照射した前記試料から発生する蛍光Ｘ線を検出する手段とを備えることを特徴とする。   The fluorescent X-ray detection apparatus according to the present invention is a fluorescent X-ray detection apparatus that detects fluorescent X-rays generated from a sample irradiated with X-rays, and is fixed by the sample fixing tool of the present invention and the sample fixing tool. It is characterized by comprising means for irradiating a flaky sample with X-rays and means for detecting fluorescent X-rays generated from the sample irradiated with X-rays.

本発明においては、空間中に第１のＸ線透過シートを張設し、薄片状の試料を第１のＸ線透過シートに重ねて配置し、第１のＸ線透過シート及び試料に重ねて第２のＸ線透過シートを張設する。薄片状の試料は二枚のＸ線透過シートに挟まれて固定される。粘着テープを用いて試料を固定していた従来の方法と異なり、粘着テープによる止め代が無くなる。またＸ線透過シート以外には試料の支持物が無く、支持物で散乱したＸ線が蛍光Ｘ線と共に検出されることが無くなる。また試料は、張設されて平坦になった二枚のＸ線透過シートに挟まれることにより、平坦な状態で固定される。   In the present invention, the first X-ray transmission sheet is stretched in the space, the flaky sample is placed on the first X-ray transmission sheet, and the first X-ray transmission sheet and the sample are stacked. A second X-ray transmission sheet is stretched. The flaky sample is sandwiched and fixed between two X-ray transmission sheets. Unlike the conventional method in which the sample is fixed using an adhesive tape, there is no need to stop with the adhesive tape. Further, there is no sample support other than the X-ray transmission sheet, and X-rays scattered by the support are not detected together with the fluorescent X-rays. The sample is fixed in a flat state by being sandwiched between two flat X-ray transmission sheets that are stretched and flattened.

本発明にあっては、試料を固定するための止め代が無いので、試料の全域で蛍光Ｘ線分析を行うことが可能となる。また本発明にあっては、試料の支持物で散乱したＸ線が蛍光Ｘ線と共に検出されることが無いので、従来に比べて蛍光Ｘ線信号のバックグラウンド信号が減少し、蛍光Ｘ線分析の精度が向上する。更に、試料の浮き上がりに起因して蛍光Ｘ線強度が変動することが無くなるので、従来に比べて蛍光Ｘ線分析の精度が向上する等、本発明は優れた効果を奏する。   In the present invention, since there is no stop allowance for fixing the sample, it becomes possible to perform fluorescent X-ray analysis over the entire area of the sample. In the present invention, since X-rays scattered by the sample support are not detected together with fluorescent X-rays, the background signal of the fluorescent X-ray signal is reduced compared to the conventional case, and fluorescent X-ray analysis is performed. Improves accuracy. Furthermore, since the fluorescent X-ray intensity does not fluctuate due to the floating of the sample, the present invention has excellent effects such as improved accuracy of fluorescent X-ray analysis as compared with the prior art.

蛍光Ｘ線検出装置の構成を示す模式図である。It is a schematic diagram which shows the structure of a fluorescent X-ray detection apparatus. 中間台及び試料固定具の外観を示す斜視図である。It is a perspective view which shows the external appearance of an intermediate | middle stand and a sample fixing tool. 試料固定具を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using a sample fixing tool. 試料固定具を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using a sample fixing tool. 試料固定具を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using a sample fixing tool. 試料固定具を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using a sample fixing tool. 中間台を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using an intermediate stand. 中間台を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using an intermediate stand. 中間台を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using an intermediate stand. 中間台を用いて薄片状の試料を固定する方法を説明するための説明図である。It is explanatory drawing for demonstrating the method to fix a flaky sample using an intermediate stand.

以下本発明をその実施の形態を示す図面に基づき具体的に説明する。
図１は、蛍光Ｘ線検出装置の構成を示す模式図である。図１に示す蛍光Ｘ線検出装置は、薄片状の試料に対する蛍光Ｘ線分析を行うための構成になっている。蛍光Ｘ線検出装置は、Ｘ線を発生するＸ線源３１と、Ｘ線を照射された試料から発生する蛍光Ｘ線を検出するＸ線検出器３２と、蛍光Ｘ線の検出結果を分析する分析部３３とを備えている。図１中には、Ｘ線源３１から試料へ照射するＸ線と試料から発生する蛍光Ｘ線とを破線矢印で示している。本発明に係る蛍光Ｘ線検出装置では、Ｘ線の照射対象となる試料を載置するための載置台４上に、中間台２１が載置され、薄片状の試料を固定した試料固定具１が中間台２１上に載置される。図１には、中間台２１及び試料固定具１を断面図で示している。 Hereinafter, the present invention will be specifically described with reference to the drawings showing embodiments thereof.
FIG. 1 is a schematic diagram showing a configuration of a fluorescent X-ray detection apparatus. The fluorescent X-ray detection apparatus shown in FIG. 1 is configured to perform fluorescent X-ray analysis on a flaky sample. The X-ray fluorescence detection apparatus analyzes an X-ray source 31 that generates X-rays, an X-ray detector 32 that detects X-ray fluorescence generated from a sample irradiated with X-rays, and a detection result of the X-ray fluorescence. And an analysis unit 33. In FIG. 1, X-rays irradiated from the X-ray source 31 to the sample and fluorescent X-rays generated from the sample are indicated by broken-line arrows. In the fluorescent X-ray detection apparatus according to the present invention, a sample fixture 1 in which an intermediate table 21 is mounted on a mounting table 4 for mounting a sample to be irradiated with X-rays, and a flaky sample is fixed. Is placed on the intermediate stage 21. In FIG. 1, the intermediate stage 21 and the sample fixture 1 are shown in a sectional view.

図２は、中間台２１及び試料固定具１の外観を示す斜視図である。中間台２１は、両端が開口した角筒の形状に形成されている。中間台２１は、蛍光Ｘ線検出装置の載置台４上に載置され、その上に試料固定具１が載置されるように使用される。中間台２１は、試料固定具１で固定される試料の載置台４からの高さを調整するためのものである。試料の載置台４からの高さを大きくするために、複数の中間台２１が重ねて使用されることもある。また試料の載置台４からの高さを小さくするために、中間台２１を使用せずに試料固定具１が直接に載置台４上に載置されることもある。中間台２１の形状は、円筒状等の他の筒状形状であってもよい。   FIG. 2 is a perspective view showing the external appearance of the intermediate stage 21 and the sample fixture 1. The intermediate stage 21 is formed in a rectangular tube shape having both ends opened. The intermediate table 21 is mounted on the mounting table 4 of the fluorescent X-ray detection apparatus, and is used so that the sample fixture 1 is mounted thereon. The intermediate table 21 is for adjusting the height of the sample fixed by the sample fixing tool 1 from the mounting table 4. In order to increase the height of the sample from the mounting table 4, a plurality of intermediate tables 21 may be used in an overlapping manner. Further, in order to reduce the height of the sample from the mounting table 4, the sample fixture 1 may be directly mounted on the mounting table 4 without using the intermediate table 21. The shape of the intermediate stage 21 may be another cylindrical shape such as a cylindrical shape.

試料固定具１は、筒状部材１１と、筒状部材１１に二枚のＸ線透過シートを夫々に固定するためのオーリング（第１の嵌合部材）１２及びオーリング（第２の嵌合部材）１３とを含んでなる。筒状部材１１は、両端が開口した円筒の形状に形成されており、一端は開口端であり、他端にはフランジ部が形成されている。なお、筒状部材１１の形状はフランジ部を有さない形状であってもよい。筒状部材１１の内部の空間は、試料へ照射するＸ線の通過経路上にあるべき空間であり、試料固定具１を蛍光Ｘ線検出装置の所定の位置に配置することにより、筒状部材１１内の空間はＸ線の通過経路上に位置することとなる。オーリング１２は、筒状部材１１に被せた第１のＸ線透過シートを固定するために筒状部材１１の側面に外嵌される。またオーリング１３は、第１のＸ線透過シートに被せた第２のＸ線透過シートを固定するために筒状部材１１の側面に外嵌される。なお、筒状部材１１の形状は、オーリング１２及びオーリング１３を位置決めするための溝を側面に形成してある形状であってもよい。薄片状の試料Ｓは、後述するように、二枚のＸ線透過シートに挟まれて筒状部材１１の開口端の位置に固定される。   The sample fixture 1 includes a cylindrical member 11, an O-ring (first fitting member) 12 and an O-ring (second fitting) for fixing the two X-ray transmission sheets to the cylindrical member 11, respectively. Joint member) 13. The cylindrical member 11 is formed in a cylindrical shape with both ends open, one end is an open end, and the other end is formed with a flange portion. The shape of the cylindrical member 11 may be a shape that does not have a flange portion. The space inside the cylindrical member 11 is a space that should be on the passage of X-rays irradiated onto the sample, and the cylindrical member is arranged by placing the sample fixture 1 at a predetermined position of the fluorescent X-ray detection device. The space in 11 is located on the X-ray passage route. The O-ring 12 is fitted on the side surface of the tubular member 11 in order to fix the first X-ray transmissive sheet placed on the tubular member 11. The O-ring 13 is externally fitted to the side surface of the cylindrical member 11 in order to fix the second X-ray transmissive sheet placed on the first X-ray transmissive sheet. The cylindrical member 11 may have a shape in which a groove for positioning the O-ring 12 and the O-ring 13 is formed on the side surface. As will be described later, the flaky sample S is sandwiched between two X-ray transmission sheets and fixed to the position of the opening end of the tubular member 11.

以下、本発明の試料固定具１を用いて試料Ｓを固定する方法を説明する。図３〜図６は、試料固定具１を用いて薄片状の試料Ｓを固定する方法を説明するための説明図である。まず、図３に示す如く、筒状部材１１の開口端を塞ぐように、Ｘ線透過シート（第１のＸ線透過シート）１４を筒状部材１１に被せる。Ｘ線透過シートは、マイラー膜等、Ｘ線が透過しやすい材料をシート状に形成したものである。本実施の形態においては、透明なＸ線透過シートを用いた例を示している。またＸ線透過シート１４の広さは、筒状部材１１の開口端よりも広くしておく。次に、Ｘ線透過シート１４を間に挟んでオーリング１２を筒状部材１１の側面に外嵌させるように、Ｘ線透過シート１４で塞がれた開口端からオーリング１２を押し込む。オーリング１２を押し込む際には、Ｘ線透過シート１４を外側向けに引っ張る。オーリング１２を筒状部材１１に外嵌させた後では、図４に示すように、オーリング１２は、Ｘ線透過シート１４の外からＸ線透過シート１４を挟んで筒状部材１１に外嵌する。またＸ線透過シート１４は、筒状部材１１の開口端を塞いで張設される。次に、図４に示すように、Ｘ線透過シート１４の開口端を塞いだ部分の上に薄片状の試料Ｓを載置する。薄片状の試料Ｓは、筒状部材１１の開口端よりも小さいサイズに形成されている。試料Ｓを載置する際には、試料Ｓの一面がＸ線透過シート１４に密着するようにする。なお、試料ＳをＸ線透過シート１４に載置する際に、Ｘ線源３１からのＸ線が適切に照射される位置に試料Ｓが配置されるように試料Ｓの位置決めを行うための用具を用いて試料Ｓを載置してもよい。   Hereinafter, a method for fixing the sample S using the sample fixing tool 1 of the present invention will be described. 3-6 is explanatory drawing for demonstrating the method to fix the flaky sample S using the sample fixing tool 1. FIG. First, as shown in FIG. 3, an X-ray transmission sheet (first X-ray transmission sheet) 14 is placed on the cylindrical member 11 so as to close the opening end of the cylindrical member 11. The X-ray transmission sheet is a sheet-like material that easily transmits X-rays, such as a Mylar film. In the present embodiment, an example using a transparent X-ray transmission sheet is shown. Further, the width of the X-ray transmission sheet 14 is set wider than the opening end of the cylindrical member 11. Next, the O-ring 12 is pushed in from the opening end closed by the X-ray transmitting sheet 14 so that the O-ring 12 is fitted on the side surface of the cylindrical member 11 with the X-ray transmitting sheet 14 interposed therebetween. When the O-ring 12 is pushed in, the X-ray transmission sheet 14 is pulled outward. After the O-ring 12 is fitted on the cylindrical member 11, as shown in FIG. 4, the O-ring 12 is externally attached to the cylindrical member 11 with the X-ray transmitting sheet 14 sandwiched from outside the X-ray transmitting sheet 14. Fit. The X-ray transmission sheet 14 is stretched by closing the opening end of the tubular member 11. Next, as shown in FIG. 4, the flaky sample S is placed on the portion where the open end of the X-ray transmission sheet 14 is closed. The flaky sample S is formed in a size smaller than the opening end of the cylindrical member 11. When the sample S is placed, one surface of the sample S is brought into close contact with the X-ray transmission sheet 14. It should be noted that when the sample S is placed on the X-ray transmission sheet 14, a tool for positioning the sample S so that the sample S is disposed at a position where X-rays from the X-ray source 31 are appropriately irradiated. The sample S may be mounted using

次に、図５に示すように、Ｘ線透過シート１４及び試料Ｓの上にＸ線透過シート（第２のＸ線透過シート）１５を被せる。Ｘ線透過シート１５の広さは、筒状部材１１の開口端よりも広くしておく。次に、Ｘ線透過シート１４及びＸ線透過シート１５を間に挟んでオーリング１３を筒状部材１１の側面に外嵌させるように、Ｘ線透過シート１４及びＸ線透過シート１５で覆われた開口端からオーリング１３を押し込む。オーリング１３を押し込む際には、Ｘ線透過シート１５を外側向けに引っ張る。オーリング１３を筒状部材１１に外嵌させた後では、図６に示すように、オーリング１３は、Ｘ線透過シート１５の外からＸ線透過シート１４及びＸ線透過シート１５を挟んで筒状部材１１に外嵌する。またＸ線透過シート１５は、Ｘ線透過シート１４及び試料Ｓに重なって張設される。薄片状の試料Ｓは、筒状部材１１の開口端に張設されたＸ線透過シート１４及びＸ線透過シート１５に挟まれて、筒状部材１１の開口端の位置に固定される。また試料Ｓは、張設されたＸ線透過シート１４及びＸ線透過シート１５に挟まれることにより、平坦な状態で固定される。   Next, as shown in FIG. 5, an X-ray transmission sheet (second X-ray transmission sheet) 15 is placed on the X-ray transmission sheet 14 and the sample S. The width of the X-ray transmission sheet 15 is set wider than the opening end of the tubular member 11. Next, the O-ring 13 is covered with the X-ray transmission sheet 14 and the X-ray transmission sheet 15 so that the O-ring 13 is fitted on the side surface of the cylindrical member 11 with the X-ray transmission sheet 14 and the X-ray transmission sheet 15 interposed therebetween. The O-ring 13 is pushed in from the opened end. When the O-ring 13 is pushed in, the X-ray transmission sheet 15 is pulled outward. After the O-ring 13 is fitted on the cylindrical member 11, the O-ring 13 sandwiches the X-ray transmissive sheet 14 and the X-ray transmissive sheet 15 from the outside of the X-ray transmissive sheet 15 as shown in FIG. 6. It fits around the cylindrical member 11. The X-ray transmission sheet 15 is stretched so as to overlap the X-ray transmission sheet 14 and the sample S. The flaky sample S is sandwiched between the X-ray transmission sheet 14 and the X-ray transmission sheet 15 stretched around the opening end of the cylindrical member 11 and fixed at the position of the opening end of the cylindrical member 11. The sample S is fixed in a flat state by being sandwiched between the stretched X-ray transmission sheet 14 and the X-ray transmission sheet 15.

試料Ｓが試料固定具１で固定された後は、図１に示すように、中間台２１上に試料固定具１が載置される。図１に示す状態で、Ｘ線源３１からＸ線が照射される。Ｘ線源３１からのＸ線は、Ｘ線透過シート１５を透過して試料Ｓへ照射される。試料Ｓで発生した蛍光Ｘ線は、Ｘ線透過シート１５を透過し、Ｘ線検出器３２で検出される。分析部３３は、Ｘ線検出器３２での蛍光Ｘ線の検出結果に基づき、試料Ｓに含まれる元素の定量分析等の蛍光Ｘ線分析を行う。なお、図１〜図６に示した例では、本発明における嵌合部材としてオーリングを用いた例を示したが、嵌合部材は、樹脂製又は金属製のリング等、オーリング以外の形態であってもよい。   After the sample S is fixed by the sample fixture 1, the sample fixture 1 is placed on the intermediate stage 21, as shown in FIG. In the state shown in FIG. 1, X-rays are emitted from the X-ray source 31. X-rays from the X-ray source 31 pass through the X-ray transmission sheet 15 and are irradiated to the sample S. The fluorescent X-ray generated in the sample S passes through the X-ray transmission sheet 15 and is detected by the X-ray detector 32. The analysis unit 33 performs fluorescent X-ray analysis such as quantitative analysis of elements contained in the sample S based on the detection result of fluorescent X-rays by the X-ray detector 32. In the example shown in FIGS. 1 to 6, an example in which an O-ring is used as a fitting member in the present invention is shown. However, the fitting member has a form other than an O-ring, such as a resin or metal ring. It may be.

また、図１〜図６に示した例では、試料固定具１を用いて薄片状の試料Ｓを固定する方法を示しているが、本発明の試料固定方法では、試料固定具１を用いずに薄片状の試料Ｓを固定することも可能である。例えば、中間台２１を用いて試料Ｓを固定することも可能である。図７〜図１０は、中間台２１を用いて薄片状の試料Ｓを固定する方法を説明するための説明図である。まず、図７に示すように、中間台２１の開口部にＸ線透過シート１４を被せる。Ｘ線透過シート１４の広さは、中間台２１の開口部よりも大きくしておく。次に、Ｘ線透過シート１４を外側向けに引っ張りながらＸ線透過シート１４の端を中間台２１の側面に粘着テープで固定する。Ｘ線透過シート１４を固定した後では、図８に示すように、Ｘ線透過シート１４は、中間台２１の開口部を塞いで張設される。次に、図８に示すように、Ｘ線透過シート１４の開口部を塞いだ部分の上に薄片状の試料Ｓを載置する。試料Ｓを載置する際には、試料Ｓの一面がＸ線透過シート１４に密着するようにする。   Moreover, although the method shown in FIGS. 1-6 has shown the method of fixing the flaky sample S using the sample fixing tool 1, in the sample fixing method of this invention, the sample fixing tool 1 is not used. It is also possible to fix the flaky sample S to the surface. For example, it is possible to fix the sample S using the intermediate stage 21. 7-10 is explanatory drawing for demonstrating the method to fix the flaky sample S using the intermediate stand 21. FIG. First, as shown in FIG. 7, the X-ray transmission sheet 14 is put on the opening of the intermediate table 21. The width of the X-ray transmission sheet 14 is set larger than the opening of the intermediate table 21. Next, the end of the X-ray transmission sheet 14 is fixed to the side surface of the intermediate table 21 with an adhesive tape while pulling the X-ray transmission sheet 14 outward. After fixing the X-ray transmission sheet 14, the X-ray transmission sheet 14 is stretched by closing the opening of the intermediate table 21 as shown in FIG. 8. Next, as shown in FIG. 8, the flaky sample S is placed on the portion where the opening of the X-ray transmission sheet 14 is closed. When the sample S is placed, one surface of the sample S is brought into close contact with the X-ray transmission sheet 14.

次に、図９に示すように、Ｘ線透過シート１４及び試料Ｓの上にＸ線透過シート１５を被せる。次に、Ｘ線透過シート１５を外側向けに引っ張りながらＸ線透過シート１５の端を中間台２１の側面に粘着テープで固定する。Ｘ線透過シート１５を固定した後では、図１０に示すように、Ｘ線透過シート１５は、Ｘ線透過シート１４及び試料Ｓに密着して張設される。薄片状の試料Ｓは、中間台２１の開口部に張設されたＸ線透過シート１４及びＸ線透過シート１５に挟まれて、中間台２１の開口部の位置に固定される。図１０における上方向からＸ線を照射することにより、Ｘ線透過シート１５を透過してＸ線が試料Ｓに照射され、蛍光Ｘ線分析が行われる。なお、中間台２１を用いずとも、薄片状の試料Ｓを間に挟んだＸ線透過シート１４及びＸ線透過シート１５を空間中に張設することにより、本発明の試料固定方法を実行することは可能である。   Next, as shown in FIG. 9, the X-ray transmission sheet 15 is placed on the X-ray transmission sheet 14 and the sample S. Next, the end of the X-ray transmission sheet 15 is fixed to the side surface of the intermediate table 21 with an adhesive tape while pulling the X-ray transmission sheet 15 outward. After fixing the X-ray transmission sheet 15, the X-ray transmission sheet 15 is stretched in close contact with the X-ray transmission sheet 14 and the sample S as shown in FIG. The flaky sample S is sandwiched between the X-ray transmission sheet 14 and the X-ray transmission sheet 15 stretched on the opening of the intermediate table 21 and fixed at the position of the opening of the intermediate table 21. By irradiating X-rays from above in FIG. 10, X-rays are transmitted through the X-ray transmission sheet 15 and irradiated to the sample S, and fluorescent X-ray analysis is performed. Even if the intermediate stage 21 is not used, the sample fixing method of the present invention is executed by stretching the X-ray transmission sheet 14 and the X-ray transmission sheet 15 sandwiching the flaky sample S in the space. It is possible.

以上詳述した如く、本発明においては、薄片状の試料Ｓは、空間中に張設されたＸ線透過シート１４及びＸ線透過シート１５に挟まれて固定される。薄片状の試料Ｓの両面は、張設されたＸ線透過シート１４及びＸ線透過シート１５の夫々に密着しており、試料Ｓは容易に移動しないように固定される。粘着テープを用いて試料Ｓを固定していた従来の方法と異なり、粘着テープによる止め代がないので、試料Ｓの全域で蛍光Ｘ線分析を行うことが可能となる。また本発明においては、Ｘ線透過シート以外には試料Ｓを支持するアクリル板等の支持物が無く、蛍光Ｘ線を検出する際にはＸ線透過シートを透過してＸ線を試料Ｓへ照射する。このため、Ｘ線透過シート以外の支持物で散乱したＸ線が蛍光Ｘ線と共に検出されることが無くなり、従来に比べて蛍光Ｘ線信号のバックグラウンド信号が減少し、蛍光Ｘ線分析の精度が向上する。また本発明においては、薄片状の試料Ｓは、張設されて平坦になったＸ線透過シート１４及びＸ線透過シート１５に挟まれることにより、一部が浮き上がることなく平坦な状態で固定される。このため、試料Ｓの浮き上がりに起因して蛍光Ｘ線強度が変動することが無くなるので、従来に比べて蛍光Ｘ線分析の精度が向上する。   As described above in detail, in the present invention, the flaky sample S is sandwiched and fixed between the X-ray transmission sheet 14 and the X-ray transmission sheet 15 stretched in the space. Both surfaces of the flaky sample S are in close contact with the stretched X-ray transmission sheet 14 and the X-ray transmission sheet 15, and the sample S is fixed so as not to move easily. Unlike the conventional method in which the sample S is fixed using an adhesive tape, there is no stop allowance with the adhesive tape, so that the fluorescent X-ray analysis can be performed on the entire area of the sample S. In the present invention, there is no support such as an acrylic plate that supports the sample S other than the X-ray transmission sheet. When detecting fluorescent X-rays, the X-rays are transmitted to the sample S through the X-ray transmission sheet. Irradiate. For this reason, the X-rays scattered by the support other than the X-ray transmission sheet are not detected together with the fluorescent X-rays, the background signal of the fluorescent X-ray signal is reduced compared to the conventional case, and the accuracy of the fluorescent X-ray analysis is reduced. Will improve. In the present invention, the flaky sample S is fixed in a flat state without being lifted up by being sandwiched between the X-ray transmissive sheet 14 and the X-ray transmissive sheet 15 that are stretched and flattened. The For this reason, since the fluorescent X-ray intensity does not fluctuate due to the floating of the sample S, the accuracy of the fluorescent X-ray analysis is improved as compared with the conventional case.

１ 試料固定具
１１ 筒状部材
１２、１３ オーリング（嵌合部材）
１４、１５ Ｘ線透過シート
２１ 中間台
３１ Ｘ線源
３２ Ｘ線検出器
Ｓ 試料 1 Sample fixture 11 Tubular member 12, 13 O-ring (fitting member)
14, 15 X-ray transmission sheet 21 Intermediate stand 31 X-ray source 32 X-ray detector S Sample

Claims (4)

Ｘ線の照射対象となる薄片状の試料を固定する方法において、
Ｘ線の通過経路になるべき空間中に、前記試料よりも広い第１のＸ線透過シートを張設し、
張設した前記第１のＸ線透過シートに前記試料を重ねて配置し、
前記試料よりも広い第２のＸ線透過シートを、前記試料及び前記第１のＸ線透過シートに重ねて張設することにより、前記第１のＸ線透過シート及び前記第２のＸ線透過シートの間に挟まった前記試料を固定すること
を特徴とする試料固定方法。 In a method for fixing a flaky sample to be irradiated with X-rays,
A first X-ray transmission sheet wider than the sample is stretched in a space to be an X-ray passage path,
Placing the sample on the stretched first X-ray transmission sheet,
A second X-ray transmissive sheet wider than the sample is stretched over the sample and the first X-ray transmissive sheet, and the first X-ray transmissive sheet and the second X-ray transmissive sheet are stretched. A sample fixing method comprising fixing the sample sandwiched between sheets. 薄片状の試料へＸ線を照射し、前記試料から発生する蛍光Ｘ線を検出する方法において、
Ｘ線の通過経路になるべき空間中に、前記試料よりも広い第１のＸ線透過シートを張設し、
張設した前記第１のＸ線透過シートに前記試料を重ねて配置し、
前記試料よりも広い第２のＸ線透過シートを、前記試料及び前記第１のＸ線透過シートに重ねて張設することにより、前記第１のＸ線透過シート及び前記第２のＸ線透過シートの間に挟まった前記試料を固定し、
前記第２のＸ線透過シートを透過して前記試料へＸ線を照射し、
前記試料から発生する蛍光Ｘ線を検出すること
を特徴とする蛍光Ｘ線検出方法。 In a method of irradiating a flaky sample with X-rays and detecting fluorescent X-rays generated from the sample,
A first X-ray transmission sheet wider than the sample is stretched in a space to be an X-ray passage path,
Placing the sample on the stretched first X-ray transmission sheet,
A second X-ray transmissive sheet wider than the sample is stretched over the sample and the first X-ray transmissive sheet, and the first X-ray transmissive sheet and the second X-ray transmissive sheet are stretched. Fix the sample sandwiched between sheets,
Irradiating the sample with X-rays through the second X-ray transmission sheet,
A fluorescent X-ray detection method comprising detecting fluorescent X-rays generated from the sample. Ｘ線の照射対象となる薄片状の試料を固定する試料固定具において、
筒状部材と、
該筒状部材の開口端に被せられるべき任意の第１のＸ線透過シートの外から前記筒状部材に外嵌すべき第１の嵌合部材と、
前記試料を前記第１のＸ線透過シートとの間に挟んで固定すべく前記第１のＸ線透過シートに被せられるべき任意の第２のＸ線透過シートの外から前記筒状部材に外嵌すべき第２の嵌合部材と
を備えることを特徴とする試料固定具。 In a sample fixture for fixing a flaky sample to be irradiated with X-rays,
A tubular member;
A first fitting member to be externally fitted to the cylindrical member from the outside of an arbitrary first X-ray transmission sheet to be put on the opening end of the cylindrical member;
The sample is placed outside the second X-ray transmission sheet to be covered with the first X-ray transmission sheet to be fixed between the first X-ray transmission sheet and the cylindrical member. A sample fixture, comprising: a second fitting member to be fitted. Ｘ線を照射された試料から発生する蛍光Ｘ線を検出する蛍光Ｘ線検出装置において、
請求項３に記載の試料固定具と、
該試料固定具で固定された薄片状の試料へＸ線を照射する手段と、
Ｘ線を照射した前記試料から発生する蛍光Ｘ線を検出する手段と
を備えることを特徴とする蛍光Ｘ線検出装置。 In a fluorescent X-ray detection apparatus for detecting fluorescent X-rays generated from a sample irradiated with X-rays,
A sample fixture according to claim 3;
Means for irradiating the flaky sample fixed with the sample fixture with X-rays;
And a means for detecting fluorescent X-rays generated from the sample irradiated with X-rays.
JP2010187104A 2010-08-24 2010-08-24 Sample fixing method, fluorescent x-ray detection method, sample fixture and fluorescent x-ray detection device Pending JP2012047470A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105181726A (en) * 2015-10-19 2015-12-23 四川新先达测控技术有限公司 Transmission-type X fluorescent device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105181726A (en) * 2015-10-19 2015-12-23 四川新先达测控技术有限公司 Transmission-type X fluorescent device

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