JP4478792B2 - Back-mounted X-ray detection method - Google Patents
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- JP4478792B2 JP4478792B2 JP2003320847A JP2003320847A JP4478792B2 JP 4478792 B2 JP4478792 B2 JP 4478792B2 JP 2003320847 A JP2003320847 A JP 2003320847A JP 2003320847 A JP2003320847 A JP 2003320847A JP 4478792 B2 JP4478792 B2 JP 4478792B2
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本発明は、Ｘ線測定技術に関し、特に、元素固有の特性Ｘ線を効率よく検出する方法に関するものである。 The present invention relates to an X-ray measurement technique, and more particularly to a method for efficiently detecting characteristic X-rays specific to an element.
試料をＸ線、電子線、イオンビームなどの一次ビームで衝撃して、その際に試料から発生する各元素固有の特性Ｘ線を検出する方法は、生物学、医学、歯学、材料科学、地質学、地球科学から犯罪捜査など非常に幅広い分野で利用されている。例えば、特性Ｘ線を分光することにより元素分析を行う方法などが知られている。 A method for detecting characteristic X-rays specific to each element generated from a specimen by bombarding the specimen with a primary beam such as an X-ray, an electron beam, or an ion beam is used in biology, medicine, dentistry, material science, geology It is used in a very wide range of fields such as science, earth science, and criminal investigation. For example, a method of performing elemental analysis by spectroscopic analysis of characteristic X-rays is known.
特性Ｘ線を分光する際には、Ｘ線検出器は従来、一次ビームが入射する試料面を基準としてビーム光源と同じ側に設置され、ビーム光源からみて試料前面から発せられる特性Ｘ線を測定する方式が採用されてきた。しかしながら、一次ビームの入射を妨害しないように検出器を設置する必要があるため、この方式では、幾何学的な制約から検出器を試料に近づけることができず、試料を臨む角度は制限されてしまう。 When spectrally analyzing characteristic X-rays, X-ray detectors are conventionally installed on the same side as the beam light source with respect to the sample surface on which the primary beam is incident, and measure characteristic X-rays emitted from the front of the sample as seen from the beam light source. Has been adopted. However, because it is necessary to install a detector so as not to interfere with the incidence of the primary beam, this method cannot bring the detector closer to the sample due to geometrical restrictions, and the angle at which the sample faces is limited. End up.
したがって、本発明は、試料の前方、すなわち、一次ビームが入射する試料面を基準としてビーム光源と同じ側にＸ線検出器を設置する従来の特性Ｘ線検出法と比較して、検出器と試料の位置関係の制限が少なく、格段に効率よくＸ線検出を行うことができる方法を提供することを課題とする。 Therefore, the present invention provides a detector in comparison with a conventional characteristic X-ray detection method in which an X-ray detector is installed in front of the sample, that is, on the same side as the beam light source with respect to the sample surface on which the primary beam is incident. It is an object of the present invention to provide a method capable of performing X-ray detection extremely efficiently with few restrictions on the positional relationship of the sample.
上記課題を解決するため、本発明は、ビーム光源を基準として光軸延長上に配置された試料の背面にＸ線検出器を配置する方式により特性Ｘ線検出を行う方法を課題解決手段とする。 In order to solve the above problems, the present invention provides a method for solving characteristic X-rays by a method in which an X-ray detector is arranged on the back surface of a sample arranged on an optical axis extension with a beam light source as a reference. .
要するに、本発明は、イオンビームの一次ビームの衝撃により、試料から発生する特性Ｘ線を検出する方法であって、ビーム光源を基準として光軸延長上に配置された試料の背面にＸ線検出器を配置し、ビーム光源を基準として該検出器のビームの光軸延長上を含む前面に、入射一次ビームの該Ｘ線検出素子への透過を防ぐダンパー材を設置することを特徴とする方法である。
In summary, the present invention is, by impact of the primary beam of Lee Onbimu, a method of detecting the characteristic X-rays generated from the sample, the X-ray detector on the back of the sample placed on the optical axis on an extension of the beam source as a reference And a damper material for preventing transmission of the incident primary beam to the X-ray detection element on the front surface including the extension of the optical axis of the beam of the detector with reference to the beam light source. It is.
本発明のＸ線検出方法によれば、従来の方法に比べて検出効率が大幅に向上することから、その波及効果は非常に大きいと思われる。 According to the X-ray detection method of the present invention, the detection efficiency is greatly improved as compared with the conventional method, so that the ripple effect seems to be very large.
本発明は、イオンビームの一次ビームの衝撃により、試料から発生する特性Ｘ線を検出する方法であって、ビーム光源を基準として光軸延長上に配置された試料の背面にＸ線検出器を配置し、ビーム光源を基準として該検出器のビームの光軸延長上を含む前面に、入射一次ビームの該Ｘ線検出素子への透過を防ぐダンパー材（ビームダンパー）を設置することを特徴とする方法である。本発明のＸ線検出方法の一実施態様を図１に示す。 The present invention, by the impact of the primary beam of Lee Onbimu, a method of detecting the characteristic X-rays generated from the sample, the X-ray detector on the back of the sample disposed on the optical axis extending the beam light source as a reference And a damper material (beam damper) that prevents transmission of the incident primary beam to the X-ray detection element is disposed on the front surface including the extension of the optical axis of the beam of the detector with reference to the beam light source. It is a method to do. One embodiment of the X-ray detection method of the present invention is shown in FIG.
検出器から試料を見込む角度を最大にするためには、一次ビームを妨害することのない試料背面に検出器を設置すればよい。この場合、一次ビームを止めるビームダンパーを検出器前面に取り付けなければならない。このビームダンパーを可能限り小さくかつ薄くして、試料と検出器の間に設置することで、試料から発生する低エネルギーから高エネルギーまでの特性Ｘ線を効率よく検出することが可能になる。 In order to maximize the angle at which the sample is viewed from the detector, the detector may be installed on the back of the sample without interfering with the primary beam. In this case, a beam damper for stopping the primary beam must be attached to the front surface of the detector. By making this beam damper as small and thin as possible and installing it between the sample and the detector, it becomes possible to efficiently detect characteristic X-rays generated from the sample from low energy to high energy.
本発明においてＸ線検出器は、当技術分野において既知のいずれか適するものを使用することができる。ビームダンパーは、入射一次ビームのＸ線検出素子への透過を防ぐ材質のものであればよい。二次Ｘ線の発生を防ぐため、炭素などの軽元素で構成され、不純物が少ないことを要する。本発明においては、例えば、グラッシーカーボンを使用することができる。低いエネルギーの特性Ｘ線の遮蔽を避けるため、Ｘ線検出素子より面積が小さいことが好ましいが、測定対象のＸ線のエネルギーがダンパー材を透過できるほど高い場合には、検出素子より大きくてもよい。ビームダンパーの厚さは一次ビームの種類とエネルギーに依存して選択することができる。電子・イオンなど物質中での飛程（その物質を透過できる距離）が短い場合は、厚さは数百ミクロンでよく、透過力の強いＸ線の場合は、そのエネルギーに依存して数ミリ程度の厚さを要する。 In the present invention, any suitable X-ray detector known in the art can be used. The beam damper may be made of a material that prevents the transmission of the incident primary beam to the X-ray detection element. In order to prevent the generation of secondary X-rays, it is necessary to be composed of light elements such as carbon and have few impurities. In the present invention, for example, glassy carbon can be used. In order to avoid shielding of low energy characteristic X-rays, it is preferable that the area is smaller than the X-ray detection element, but if the energy of the X-ray to be measured is high enough to pass through the damper material, it may be larger than the detection element. Good. The thickness of the beam damper can be selected depending on the type and energy of the primary beam. Thickness may be several hundred microns when the range (distance that can pass through the substance) in materials such as electrons and ions is short, and several millimeters depending on the energy of X-rays with strong penetrating power. It needs a certain thickness.
以下、本発明を実施例により詳細に説明するが、本発明はこの実施例により限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited by this Example.
本発明のＸ線検出方法を用いて特性Ｘ線検出評価を行った。評価は、従来法である検出器を試料の前方に配置する方式と比較して行った。
使用した測定系の配置図を図１及び図２に示す。図１は、本発明のＸ線検出方法であり、図２は、従来技術のＸ線検出方法を示す図である。
Characteristic X-ray detection evaluation was performed using the X-ray detection method of the present invention. The evaluation was performed in comparison with a conventional method in which a detector is arranged in front of the sample.
The layout of the measurement system used is shown in FIGS. FIG. 1 shows an X-ray detection method according to the present invention, and FIG. 2 shows a conventional X-ray detection method.
図１において、Ｘ線検出器の外径はφ30mm、素子の有効面積は100mm2である。検出器前面（試料側）からその内部の素子までの距離は4mm、試料から検出器までの距離は2.5mmである。ビームダンパーは、直径φ2mm、厚さ0.5mmのグラッシーカーボン（密度1.519g/cm3）を使用した。したがって、試料から検出器素子までの距離は6.5mmで、試料を臨む全体の立体角は1.54sr、ビームダンパーにより影になる部分の立体角は0.66srとなる。Ｘ線の検出効率の評価に際しては、ビームダンパーによるＸ線の吸収を考慮して行った。 In FIG. 1, the outer diameter of the X-ray detector is φ30 mm, and the effective area of the element is 100 mm 2 . The distance from the detector front (sample side) to the internal element is 4 mm, and the distance from the sample to the detector is 2.5 mm. As the beam damper, glassy carbon (density 1.519 g / cm 3 ) having a diameter of 2 mm and a thickness of 0.5 mm was used. Therefore, the distance from the sample to the detector element is 6.5 mm, the entire solid angle facing the sample is 1.54 sr, and the solid angle of the portion shaded by the beam damper is 0.66 sr. The X-ray detection efficiency was evaluated in consideration of X-ray absorption by the beam damper.
図２において、Ｘ線検出器は図１と同様であり、一次ビーム光軸に対して45°の角度で、ビーム光軸を妨害しないように検出器をビーム光軸から2mm離すとすると、試料から検出器素子までの距離は21.8mmで、試料を臨む立体角は0.2srとなる。 In FIG. 2, the X-ray detector is the same as in FIG. 1, and if the detector is separated by 2 mm from the beam optical axis at an angle of 45 ° with respect to the primary beam optical axis so as not to disturb the beam optical axis, The distance from the detector to the detector element is 21.8 mm, and the solid angle facing the sample is 0.2 sr.
透過率はＸ線のエネルギーにより異なることから、評価は、カルシウムの特性Ｘ線（3.69keV）と銅の特性Ｘ線（8.04keV）について行った。カルシウムの場合、ビームダンパーでのＸ線の透過率は2.6％であるから、従来法と比較して（0.66×0.026＋0.88）／0.2≒4.4倍効率が高くなった。また、銅の場合は、ビームダンパーでのＸ線の透過率は73％であり、従来法と比較して（0.66×0.73＋0.88）／0.2≒6.8倍高効率となった。 Since the transmittance varies depending on the energy of the X-ray, the evaluation was performed on the characteristic X-ray of calcium (3.69 keV) and the characteristic X-ray of copper (8.04 keV). In the case of calcium, the X-ray transmittance of the beam damper is 2.6%, so the efficiency is (0.66 × 0.026 + 0.88) /0.2≈4.4 times that of the conventional method. In the case of copper, the X-ray transmittance of the beam damper is 73%, which is (0.66 × 0.73 + 0.88) /0.2≈6.8 times higher efficiency than the conventional method.
本実施例では、およそ4〜7倍効率よく特性Ｘ線を検出することが可能であり、従来の５分の１程度の時間で元素分析を行うことが可能になる。したがって、本発明は、特に、測定に長時間を要する元素の二次元分布測定を行う面分析に有効である。また、一次ビームの照射量を５分の１に低減可能であることから、試料の照射損傷を防ぐことができ、元素分析における感度・精度が格段に向上する。 In this embodiment, characteristic X-rays can be detected approximately 4 to 7 times more efficiently, and elemental analysis can be performed in about 1/5 of the conventional time. Therefore, the present invention is particularly effective for surface analysis for performing two-dimensional distribution measurement of elements that require a long time for measurement. In addition, since the irradiation amount of the primary beam can be reduced to 1/5, it is possible to prevent the irradiation damage of the sample, and the sensitivity and accuracy in the elemental analysis are remarkably improved.
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