JP2013185933A - Neutron-x-ray-laser merging measuring apparatus - Google Patents
Neutron-x-ray-laser merging measuring apparatus Download PDFInfo
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Abstract
Description
本発明は、試料へのレーザー照射と、中性子照射及び検出と、Ｘ線照射及び検出とを、同時又は交互に行うことができる装置に関する。 The present invention relates to an apparatus capable of performing laser irradiation, neutron irradiation and detection, and X-ray irradiation and detection on a sample simultaneously or alternately.
蛋白質をテラレーザーで照射刺激させながら、その際に生じる蛋白質内プロトンの動きを中性子で、さらにその結果もたらされる組織構造変化をX線で計測することで光合成の新しいプロセスモデルの検証を行う新しい蛋白質機構構造モデルの検証が提唱されている（非特許文献１）。しかし、現存する装置では、中性子とX線との同時照射・計測ができないため、中性子照射による蛋白質内プロトンの動向と、組織構造変化とを同時に計測することができず、中性子とX線との照射を個別に行わざるを得ない状況である。 A new protein that verifies a new process model of photosynthesis by measuring the movement of protons in the protein with neutrons and measuring the resulting tissue structure changes with X-rays while irradiating the protein with a tera laser. Verification of the mechanism structure model has been proposed (Non-Patent Document 1). However, the existing equipment cannot simultaneously measure and measure neutrons and X-rays, so it cannot measure the protons in the protein due to neutron irradiation and changes in tissue structure at the same time. Irradiation must be performed individually.
また、機能セラミックスの材料合成をテラヘルツレーザーにより行い、その際の微細組織制御をX線構造解析により行い、高機能素材の開発を行うニーズがある。しかし、同一の試料に対してレーザー照射とX線照射及び検出を同時に行うことができる装置がないため、構造変化とそれにより生じる機能変化との関係を時分割解析することができず、実現できていない。 In addition, there is a need to develop functional materials by synthesizing functional ceramic materials with a terahertz laser and controlling the microstructure by X-ray structural analysis. However, since there is no device that can perform laser irradiation, X-ray irradiation and detection on the same sample at the same time, the relationship between the structural change and the resulting functional change cannot be analyzed in a time-sharing manner. Not.
蛋白質やセラミックス等各種材料の構造変化と機能の関係を解明するため、同一試料内に生じる構造変化情報と機能変化情報とを同時に計測でき、時分割解析等構造変化の追跡や反応機構の実証を可能とするため、同一試料へのレーザー照射、中性子照射及び検出並びにX線照射及び検出を同時又は交互に行うことを可能とする装置を提供することを目的とする。 In order to elucidate the relationship between structural changes and functions of various materials such as proteins and ceramics, structural change information and functional change information generated in the same sample can be measured simultaneously, tracking structural changes such as time-division analysis and demonstrating reaction mechanisms In order to make this possible, an object of the present invention is to provide an apparatus capable of simultaneously or alternately performing laser irradiation, neutron irradiation and detection, and X-ray irradiation and detection on the same sample.
本発明によれば、球体の中心に位置づけられている、被検体を載置する試料台と、当該被検体側面に中性子を照射する中性子源及び中性子導管と、当該被検体により回折された中性子を検出する中性子検出器と、当該被検体側面にX線を照射するX線発生装置及びX線導管と、当該被検体を透過するX線を検出するX線検出器と、当該被検体頂部にレーザーを照射するレーザー源及びレーザー導波管と、X線検出時にX線発生装置及びX線導管並びにX線検出器を当該球体内部に前進させ、X線非検出時にはX線発生装置及びX線導管並びにX線検出器を当該球体から後退させるように作動するX線光源移動用アームと、X線の光軸に沿って当該X線検出器を移動させるX線検出器移動用アームと、を具備し、前記球体の中心と前記中性子源とを結ぶ仮想直線に対して、前記球体の中心と前記X線発生装置とを結ぶ仮想直線が０〜３０度の角度となるように、前記中性子源と前記X線発生装置とは相対的に位置づけられていることを特徴とする、中性子とX線とレーザーとの融合化計測装置が提供される。 According to the present invention, the sample stage on which the subject is placed, which is positioned at the center of the sphere, the neutron source and neutron conduit for irradiating the side surface of the subject with neutrons, and the neutron diffracted by the subject A neutron detector for detection, an X-ray generator and X-ray conduit for irradiating the side surface of the subject with X-rays, an X-ray detector for detecting X-rays transmitted through the subject, and a laser at the top of the subject Source and laser waveguide, and X-ray generator and X-ray conduit and X-ray detector are advanced inside the sphere when X-ray is detected, and X-ray generator and X-ray conduit when X-ray is not detected And an X-ray light source moving arm that operates to retract the X-ray detector from the sphere, and an X-ray detector moving arm that moves the X-ray detector along the optical axis of the X-ray. And a virtual straight line connecting the center of the sphere and the neutron source The neutron source and the X-ray generator are relatively positioned so that a virtual straight line connecting the center of the sphere and the X-ray generator is at an angle of 0 to 30 degrees. An integrated measurement device for neutrons, X-rays and lasers is provided.
X線光源移動用アームには、X線の照射位置を調整するビーム位置調整装置が設けられ、当該ビーム位置調整装置の上にX発生装置は位置づけられていることが好ましい。
球体は、X線光源移動用アーム及びX線検出器移動用アームの作動に連動して開閉する２個の半球体から構成されていることが好ましい。前記２個の半球体は、移動経路となるリニアガイド上に載置されていることがさらに好ましい
本発明の装置において、中性子検出器は、球体の内面に緻密に取り付けられていることが好ましい。
The X-ray light source moving arm is preferably provided with a beam position adjusting device for adjusting the X-ray irradiation position, and the X generator is preferably positioned on the beam position adjusting device.
The sphere is preferably composed of two hemispheres that open and close in conjunction with the operation of the X-ray light source moving arm and the X-ray detector moving arm. More preferably, the two hemispheres are placed on a linear guide serving as a movement path. In the apparatus of the present invention, the neutron detector is preferably closely attached to the inner surface of the sphere.
X線検出器移動用アームと中性子検出器移動用アームとは、試料台を中心として同軸回転する２θアームであり、X線検出器を水平方向に±１５０度以下の範囲で移動可能とし、中性子検出器を中性子導管からの中性子入射ラインに対して上下方向に−１０〜１３５度の範囲で移動可能とすること、X線検出器移動用アームは中性子検出器移動用アームよりも短く、X線検出器が中性子検出器よりも被検体に近い位置に位置づけられること、Ｘ線検出器移動用アーム及び中性子検出器移動用アームの最小移動角は０．００２度／パルスであり、中性子線の発散角度は０．２度であることが好ましい。 The X-ray detector moving arm and the neutron detector moving arm are 2θ arms that rotate coaxially around the sample stage. The X-ray detector can be moved within a range of ± 150 degrees in the horizontal direction. The detector can be moved in the vertical direction within a range of −10 to 135 degrees with respect to the neutron incident line from the neutron conduit, and the X-ray detector moving arm is shorter than the neutron detector moving arm. The detector is positioned closer to the subject than the neutron detector, the minimum movement angle of the X-ray detector moving arm and the neutron detector moving arm is 0.002 degrees / pulse, and neutron beam divergence The angle is preferably 0.2 degrees.
レーザー源は、テラヘルツ光源であることが好ましい。 The laser source is preferably a terahertz light source.
本発明の装置によれば、極低温等極限環境などの所望の環境において、同一試料にレーザーを照射し、中性子とX線を同時に照射・計測すること又は交互に照射し、計測することができる。これによって、構造変化を生じつつ機能発現する蛋白質をはじめとしたさまざまな機能・構造材料の複雑な実現象を観察・解析することが世界に先駆け可能となる。 According to the apparatus of the present invention, in a desired environment such as an extreme environment such as a cryogenic temperature, it is possible to irradiate and measure the same sample, and simultaneously irradiate and measure neutrons and X-rays or alternately irradiate and measure . This makes it possible for the world to observe and analyze complex real phenomena of various functions and structural materials, including proteins that express functions while undergoing structural changes.
以下、図面を参照しながら本発明を具体的に説明するが、本発明はこれらに限定されるものではない。
本発明の中性子・X線・レーザー融合化計測装置の一実施態様を図１及び図２に示す。図１及び図２に示す装置において、球体の中心に位置づけられている、被検体を載置する試料台と、当該被検体に中性子を照射する中性子源及び中性子導管と、当該被検体により回折された中性子を検出する中性子検出器と、当該被検体にX線を照射するX線発生装置及びX線導管と、当該被検体を透過するX線を検出するX線検出器と、当該被検体頂部にレーザーを照射するレーザー源及びレーザー導波管と、X線検出時にX線発生装置及びX線導管並びにX線検出器を当該球体内部に前進させ、X線非検出時にはX線発生装置及びX線導管並びにX線検出器を当該球体から後退させるように作動するX線光源移動用アームと、X線の光軸に沿って当該X線検出器を移動させるX線検出器移動用アームと、を具備し、前記球体の中心と前記中性子源とを結ぶ仮想直線に対して、前記球体の中心と前記X線発生装置とを結ぶ仮想直線が０〜３０度の角度となるように、前記中性子源と前記X線発生装置とは相対的に位置づけられている。
Hereinafter, the present invention will be specifically described with reference to the drawings, but the present invention is not limited thereto.
One embodiment of the neutron / X-ray / laser fusion measuring apparatus of the present invention is shown in FIGS. In the apparatus shown in FIG. 1 and FIG. 2, a sample stage on which a subject is placed, a neutron source and a neutron conduit for irradiating the subject with neutrons, which are positioned at the center of the sphere, and the subject are diffracted by the subject. A neutron detector for detecting neutrons, an X-ray generator and X-ray conduit for irradiating the subject with X-rays, an X-ray detector for detecting X-rays transmitted through the subject, and the top of the subject A laser source and a laser waveguide for irradiating a laser beam, an X-ray generator, an X-ray conduit and an X-ray detector are advanced inside the sphere when X-ray is detected, and an X-ray generator and X when X-ray is not detected An X-ray light source moving arm that operates to retract the X-ray tube and X-ray detector from the sphere, an X-ray detector moving arm that moves the X-ray detector along the optical axis of the X-ray, A virtual straight line connecting the center of the sphere and the neutron source. Respect, as a virtual straight line connecting the center of the sphere and the X-ray generating device is 0 to 30 ° angle, it is positioned relatively to the neutron source and the X-ray generator.
本実施形態において、測定時に、中性子導管、X線導管、レーザー導波管、中性子検出器及びX線検出器は、試料台を中心とする球体内部の所定位置に位置づけられる。すなわち、レーザー導波管、中性子導管及びX線導管は、試料台上の被検体に対してそれぞれ干渉しないようにレーザー、中性子及びX線を同時に照射できる位置にあり、中性子検出器は、被検体から反射する中性子を受け取ることができる球体内面の位置にあり、X線検出器は被検体を透過するX線を受け取ることができるX線導管と同軸上の対称位置にある。中性子検出とX線検出とを同時に行うためには後述するように、被検体と中性子検出器とX線検出器との位置関係が重要になり、X線発生装置及びX線検出器は中性子検出器と干渉しない範囲に設けられる。例えば、中性子検出器が図１中A-B上を計測移動中にX線検出器がこの円内にある場合には、両者が干渉を起こす。そのため、図１においては、円弧ＡＢ（2θ＝１６０度）の位置に中性子検出器が設けられ、円弧ＡＢを除いた扇形部分にＸ線発生装置及び中性子導管が設けられる。球体の大きさは、半径30cm以上1500cm以下が好ましい。 In this embodiment, at the time of measurement, the neutron conduit, the X-ray conduit, the laser waveguide, the neutron detector, and the X-ray detector are positioned at predetermined positions inside the sphere centering on the sample stage. That is, the laser waveguide, the neutron conduit, and the X-ray conduit are at positions where laser, neutron, and X-rays can be irradiated simultaneously so as not to interfere with the subject on the sample stage. The X-ray detector is located on the inner surface of the sphere where the neutrons reflected from the X-ray can be received, and the X-ray detector is positioned coaxially and symmetrically with the X-ray conduit capable of receiving the X-rays transmitted through the subject. In order to perform neutron detection and X-ray detection simultaneously, as will be described later, the positional relationship between the subject, the neutron detector, and the X-ray detector is important, and the X-ray generator and X-ray detector can detect neutrons. Provided in a range not interfering with the vessel. For example, when the X-ray detector is in this circle while the neutron detector is measuring and moving on A-B in FIG. Therefore, in FIG. 1, a neutron detector is provided at the position of the arc AB (2θ = 160 degrees), and an X-ray generator and a neutron conduit are provided in the fan-shaped portion excluding the arc AB. The size of the sphere is preferably a radius of 30 cm to 1500 cm.
試料台としては、φ軸回転と被検体のセンタリングができる直交３軸の並進が可能なカッパー型ゴニオメータ、４軸回折計などを好適に用いることができる。
被検体の位置決めに用いるCCD付顕微望遠鏡は、図１のA点の上方及びB点の下方の2カ所に90度の角度で設置し、モニター観測する。あるいは、X線の通る穴をあけた鏡を用いて、後述するX線ビーム合わせに用いるダイレクトビームと同じ方向から観測してもよい。
As the sample stage, a copper-type goniometer, a four-axis diffractometer or the like capable of three-axis translation capable of rotating the φ axis and centering the subject can be suitably used.
The microscopic telescope with CCD used for positioning the subject is installed at two positions above the A point and below the B point in FIG. Or you may observe from the same direction as the direct beam used for the X-ray beam alignment mentioned later using the mirror which opened the hole which X-ray passes.
中性子源は、波長領域０．７〜８Åを実現できる大強度陽子加速器J-PARC（茨城県東海村）を用いるが、これに限定されるものではなく、例えば、冷中性子源や熱外中性子源を用いることもできる。中性子線のビーム合わせを行うため、中性子が通る位置をレーザー光線で可視化するため、中性子導管に中性子専用ビームトンネル（真空あるいはヘリウムパス）を設けることが好ましい。中性子源は固定されているため、中性子線のビーム合わせ用に、球体を載置するベースに、水平面内回転、上下方向調整、上下左右並行移動機構を設け、たとえば液体界面反射率を計測する場合には被検体平面への入射角を±0.0001〜0.2度の範囲に調整することができる。 The neutron source uses a high-intensity proton accelerator J-PARC (Tokai Village, Ibaraki Prefecture) that can realize a wavelength region of 0.7 to 8 mm, but is not limited to this. For example, a cold neutron source or an epithermal neutron source Can also be used. In order to perform neutron beam alignment, it is preferable to provide a neutron dedicated beam tunnel (vacuum or helium path) in the neutron conduit in order to visualize the position through which the neutron passes with a laser beam. Since the neutron source is fixed, the base on which the sphere is mounted is equipped with a horizontal plane rotation, vertical adjustment, vertical and horizontal translation mechanism for neutron beam alignment, for example, when measuring liquid interface reflectivity The angle of incidence on the object plane can be adjusted to a range of ± 0.0001 to 0.2 degrees.
中性子検出器は、TOF（時間差による波長決定）用の２次元検出器、たとえばPILATUS−２Mを用いることができる。
X線発生装置は、小型で高輝度X線発生を可能とする装置、たとえば高輝度Ｘ線発生装置 MicroMax007HF（リガク製）、この字型高輝度X線発生装置（特許文献１〜３参照）を好ましく用いることができる。X線源としては、MoKα（λ＝0.711Å）、CuKα（λ＝1.542Å）を用いることができるが、MoKαがより好ましい。
As the neutron detector, a two-dimensional detector for TOF (determining wavelength by time difference), for example, PILATUS-2M can be used.
The X-ray generator is a small device capable of generating high-intensity X-rays, such as a high-intensity X-ray generator MicroMax007HF (manufactured by Rigaku), and this character-type high-intensity X-ray generator (see Patent Documents 1 to 3). It can be preferably used. As the X-ray source, MoKα (λ = 0.711Å) and CuKα (λ = 1.542Å) can be used, but MoKα is more preferable.
X線発生装置はシャッター、４象限スリットなどの基本的に必須な要素を具備し、X線光源台座の上に載置されている。X線光源台座の上には、必要に応じて、ミラー、光学素子、モノクロメータ、多層膜コリメータなどの光学系も載置することができる。例えば、電子線エネルギーが１００〜１２０keVに達するコの字型回転体陰極X線発生装置を用いる場合には、倍音カット用のミラーを載置することが好ましい。集光による高輝度化を達成するためには三角ベント型のモノクロメータ、平行性を向上させるためにはチャンネルカット型のモノクロメータを載置することができる。多層膜収束コリメータを用いるときはコリメータの焦点と被検体位置とが一致するようにX線光源台座を前方に移動させる。このときの最小移動距離は0.1mm／パルス程度が好ましい。X線光源台座は、X線光源移動用アームの上に載置されている。X線光源台座とX線光源移動用アームとの間には、X線光源台座を被検体に近づける前進と被検体から遠ざける後退とを可能にする前後移動用台座と、X線の照射方向を前後及び上下左右に１〜５μm／パルスで調整することができるビーム位置調整装置が設けられている。光軸合わせは、被検体位置に取り付けるピンホール、コリメータ取付台にX線を可視化するためのレーザーや金属金具を用いて、X線検出器にてピンホール通過後のダイレクトビームを検知することにより行うその後の測定中にビーム位置が変動したときは、コリメータと被検体との間にダイレクトビームを通して、X線検出器にて検出し、その情報を基にビーム位置調整装置にフィードバックし、自動的にX線ビーム位置を調整する。 The X-ray generator has basically essential elements such as a shutter and a quadrant slit, and is placed on an X-ray light source base. On the X-ray light source base, an optical system such as a mirror, an optical element, a monochromator, and a multilayer film collimator can be mounted as necessary. For example, when using a U-shaped rotating body cathode X-ray generator in which the electron beam energy reaches 100 to 120 keV, it is preferable to place a mirror for overtone cut. In order to achieve high brightness by condensing, a triangular vent type monochromator can be mounted, and in order to improve parallelism, a channel cut type monochromator can be mounted. When the multilayer film converging collimator is used, the X-ray light source base is moved forward so that the focus of the collimator coincides with the subject position. The minimum moving distance at this time is preferably about 0.1 mm / pulse. The X-ray light source pedestal is placed on the X-ray light source moving arm. Between the X-ray light source pedestal and the X-ray light source moving arm, a back-and-forth movement pedestal that enables the X-ray light source pedestal to move forward and backward from the subject, and the X-ray irradiation direction A beam position adjusting device that can be adjusted at 1 to 5 μm / pulse in front and rear, and up and down, left and right is provided. Optical axis alignment is achieved by detecting the direct beam after passing through the pinhole with an X-ray detector using a pinhole attached to the subject position, a laser or metal fitting for visualizing X-rays on the collimator mounting base. When the beam position fluctuates during the subsequent measurement, it is detected by the X-ray detector through the direct beam between the collimator and the subject and fed back to the beam position adjustment device based on that information. Adjust the X-ray beam position.
本装置において用いるX線検出器は、２次元X線検出器を好ましく用いることができる。たとえば、パルス計数型のX線画像検出器であるPilatus-2M（pixel apparatus for the SLS）を好適に用いることができる。X線検出器は、X線検出器移動用アーム上に載置されていて、測定時には球体内の測定位置まで前進し、非測定時には球体外の後退位置まで後退する。 As the X-ray detector used in this apparatus, a two-dimensional X-ray detector can be preferably used. For example, Pilatus-2M (pixel apparatus for the SLS), which is a pulse counting type X-ray image detector, can be suitably used. The X-ray detector is placed on the X-ray detector moving arm, and moves forward to the measurement position inside the sphere when measuring, and moves back to the retracted position outside the sphere when not measuring.
レーザー源として、テラヘルツ光源を用いることが好ましい。テラヘルツ光源としては、たとえば、テラヘルツ光波長×出力が７８GHz〜１．０１６THz×１０W〜２．３kWであることが好適である。レーザーは、被検体に照射できるように、球体外部に設けたレーザー源からレーザー導波管を介して導入する。レーザー導波管は、図１のA点とB点との間に位置づけ、被検体の上方空間から下方に向けてレーザーを照射する。 A terahertz light source is preferably used as the laser source. As the terahertz light source, for example, it is preferable that the terahertz light wavelength × output is 78 GHz to 1.016 THz × 10 W to 2.3 kW. The laser is introduced via a laser waveguide from a laser source provided outside the sphere so that the subject can be irradiated. The laser waveguide is positioned between point A and point B in FIG. 1, and irradiates the laser downward from the space above the subject.
その他、必要に応じて、低温窒素吹き付け装置（−２００℃）や低温ヘリウム吹き付け装置などの低温吹き付け装置、ｐＨジャンプ用器具、加熱装置、磁場発生装置、高圧印加装置などを図１のA点とB点との間に配置してもよい。「ｐＨジャンプ」とはタンパク質結晶を観察する手法であり、観察対象となるタンパク質結晶の構造解析を液体窒素温度で凍ったまま行い、その後活性化して化学反応を起こさせるために温度を相転移温度以下（-30〜-50℃）まで昇温させ、霧吹きなどで緩衝液（有機溶媒、たとえば酢酸と酢酸ナトリウムとの混合物）を吹きかけ、微妙なｐＨ調整を行って反応を促進させ、再び液体窒素温度まで凍結して結晶構造の変化を観察する工程を繰り返し行い、反応プロセス全体を明らかにする手法である。 In addition, a low-temperature spraying device such as a low-temperature nitrogen spraying device (−200 ° C.) or a low-temperature helium spraying device, a pH jumping instrument, a heating device, a magnetic field generator, a high-pressure application device, etc. You may arrange | position between B points. “PH jump” is a technique for observing protein crystals. The structural analysis of the protein crystals to be observed is frozen at liquid nitrogen temperature, and then the temperature is set to the phase transition temperature to activate and cause a chemical reaction. The temperature is raised to the following (-30 to -50 ° C), sprayed with a buffer solution (organic solvent, for example, a mixture of acetic acid and sodium acetate) by spraying, etc., finely adjusted the pH to promote the reaction, and again with liquid nitrogen This is a technique for clarifying the entire reaction process by repeating the process of freezing to temperature and observing changes in crystal structure.
本装置では、中性子検出とX線検出とを同時に行うために、互いに干渉することのないように、中性子検出器の内側に、中性子検出器の死角をできるだけ小さくするように２次元X線検出器を配置し、且つ２次元X線検出器と中性子検出器との距離をできるだけ短くする配置をとる。たとえば、X線検出器としてSPring-8で使用されているPilatus-2Mを用い、試料台としてカッパー型ゴニオメータを用い、２次元中性子検出器を球体内面に緻密に配置する場合を例にして説明する。図５に示すように、Pilatus-M2の受光面の寸法は254mm×289mmであり、受光面の中心Oから被検体Sまでの距離（OS）を200mmとする。受光面の長辺側中点をA、受光面の短辺側中点をB、長辺と短辺との交点をCとすると、角度∠ASO（２θ１）は200tanθ１＝254/2から２θ１＝32.4度、角度∠BSO（２θ２）＝35.8度、角度∠CSO（２θ３）＝43.9度となる。X線源としてCuKα（1.542Å）を用いる場合の分解能に換算すると、それぞれ2.76Å、2.51Å、2.06Åとなり、MoKα（0.711Å）を用いる場合の分解能に換算すると、それぞれ1.27Å、1.16Å、0.95Åとなる。よって、X線源としてはMoKα（0.711Å）を用いることが好ましい。中性子線の死角は試料と検出器間距離が200mmだと極めて大きい。さらに、検出器Pilatus-2Mの大きさは受光面の周りに70mmほどの枠があるため、例えば淵を加えた（A、B、C）に相当する∠A’SO＝44.57度、∠B’SO＝47.0度、∠C’SO=55.3度になる。そこで中性子検出器用の枠にX線用検出器を出し入れする穴をあけると穴の大きさは約390mm×430mm以上となり、これを角度で換算すると∠A’’SO=23.5度、∠B’’SO=25.5度の死角が生じることになる。そのため、Pilatusの長軸方向を縦に、短軸を横に配置することにより、中性子線の死角を2度ほど少なくできる。単純なゴニオメータを使用するため、被検体とX線検出器間距離を50mm以下にできる。それにより、無機物や低分子結晶など、格子定数の小さな結晶に対しては50mmでも反射が分離できる。逆に格子定数の極めて大きい結晶に対して200mmでは不足の場合があることから、測定間距離は50mmから1000mmまで任意の位置で計測できる。 In this equipment, in order to perform neutron detection and X-ray detection at the same time, a two-dimensional X-ray detector is installed inside the neutron detector so as to make the dead angle of the neutron detector as small as possible so as not to interfere with each other. And the arrangement which makes the distance between the two-dimensional X-ray detector and the neutron detector as short as possible. For example, a case where Pilatus-2M used in SPring-8 is used as an X-ray detector, a copper goniometer is used as a sample stage, and a two-dimensional neutron detector is densely arranged on the inner surface of a sphere will be described as an example. . As shown in FIG. 5, the dimension of the light receiving surface of Pilatus-M2 is 254 mm × 289 mm, and the distance (OS) from the center O of the light receiving surface to the subject S is 200 mm. Assuming that the long-side midpoint of the light-receiving surface is A, the short-side midpoint of the light-receiving surface is B, and the intersection of the long and short sides is C, the angle SOASO (2θ 1 ) is 2θ from 200 tan θ1 = 254/2 1 = 32.4 degrees, angle ∠BSO (2θ 2 ) = 35.8 degrees, and angle ∠CSO (2θ 3 ) = 43.9 degrees. When converted to the resolution when CuKα (1.542 mm) is used as the X-ray source, they are 2.76 mm, 2.51 mm, and 2.06 mm, respectively, and when converted to the resolution when MoKα (0.711 mm) is used, they are 1.27 mm and 1.16 mm, respectively. 0.95cm. Therefore, it is preferable to use MoKα (0.711 mm) as the X-ray source. The dead angle of the neutron beam is extremely large when the distance between the sample and the detector is 200 mm. Furthermore, since the size of the detector Pilatus-2M has a frame of about 70 mm around the light receiving surface, for example, ∠A'SO = 44.57 degrees, ∠B 'corresponding to (A, B, C) with 加 え added SO = 47.0 degrees and ∠C'SO = 55.3 degrees. Therefore, when a hole for inserting and removing the X-ray detector is drilled in the frame for the neutron detector, the size of the hole becomes about 390 mm x 430 mm or more, and this is converted into an angle ∠A''SO = 23.5 degrees, ∠B '' SO = 25.5 degrees blind spot will occur. Therefore, the dead angle of the neutron beam can be reduced by about 2 degrees by arranging the long axis direction of Pilatus vertically and the short axis horizontally. Since a simple goniometer is used, the distance between the subject and the X-ray detector can be reduced to 50 mm or less. As a result, reflections can be separated even at 50 mm for crystals with a small lattice constant, such as inorganic substances and low-molecular crystals. Conversely, 200 mm may be insufficient for crystals with extremely large lattice constants, so the distance between measurements can be measured at any position from 50 mm to 1000 mm.
図３及び４は、X線源及びX線検出器を球体の内部又は外部に位置づける機構を説明する。図３に示すように、球体は、リニアガイド上に載置されている２個の半球体からなり、X線源及びX線検出器を出し入れする際に開放することができる構成である。X線源及びX線検出器は、図３において、実線で示す測定位置と、点線で示す待機位置との間で前後移動可能である。Ｘ線検出器を球体の内部に入れるためには、先ず、球弧A-Cを頑丈なリニアガイド上を移動させ点線で示した球弧a-c 迄移動し、同様に球弧B-Dをb-dまで移動させる。その結果開いたc-dの隙間からＸ線検出器を球体内に移動する事が可能になる。被検体の交換や、保守などは上記2箇の球弧が開いた状態で行う。測定位置と待機位置に対応するX線検出器と中性子検出器との位置関係を図４に示す。図４上は、X線源及びX線検出器が球体の外部にある待機位置であり、中性子計測のみを行うことができる。図４下は、X線源及びX線検出器が球体の内部にある測定位置であり、X線検出と中性子検出とを同時に行うことができる。 3 and 4 illustrate a mechanism for positioning the X-ray source and X-ray detector inside or outside the sphere. As shown in FIG. 3, the sphere is composed of two hemispheres placed on a linear guide and can be opened when the X-ray source and the X-ray detector are taken in and out. In FIG. 3, the X-ray source and the X-ray detector can move back and forth between a measurement position indicated by a solid line and a standby position indicated by a dotted line. In order to put the X-ray detector inside the sphere, first, the spherical arc A-C is moved on the sturdy linear guide to move to the spherical arc a-c shown by the dotted line, and similarly the spherical arc B-D is moved to b-d. As a result, the X-ray detector can be moved into the sphere from the open c-d gap. The exchange and maintenance of the subject are performed with the two ball arcs open. FIG. 4 shows the positional relationship between the X-ray detector and the neutron detector corresponding to the measurement position and the standby position. 4 is a standby position where the X-ray source and the X-ray detector are outside the sphere, and only neutron measurement can be performed. The lower part of FIG. 4 shows a measurement position where the X-ray source and the X-ray detector are inside the sphere, and X-ray detection and neutron detection can be performed simultaneously.
図５及び６は、本発明の別の実施態様を示す。図１〜図３に示す装置と同じ構成については説明を割愛し、異なる構成のみ説明する。
図５及び６に示す実施態様において、X線検出器移動用アームと中性子検出器移動用アームとは、試料台を中心として同軸回転する２θアームであり、水平方向は±１５０度以下、上下方向は中性子入射ラインに対して−１０〜１３５度の範囲で移動可能であり、X線検出器移動用アームは中性子検出器移動用アームよりも短く、X線検出器が中性子検出器よりも被検体に近い位置に位置づけられ、Ｘ線及び中性子線の最小移動角は０．００２度／パルスであり、中性子線の発散角度は０．２度である。つまり、中性子線発散角度０．２度の範囲内で、中性子ビーム（パルス波）を１パルスあたり０．００２度移動させることで十分な精度のデータを採取できる。
Figures 5 and 6 illustrate another embodiment of the present invention. The description of the same configuration as the apparatus shown in FIGS. 1 to 3 will be omitted, and only a different configuration will be described.
In the embodiment shown in FIGS. 5 and 6, the X-ray detector moving arm and the neutron detector moving arm are 2θ arms that rotate coaxially around the sample stage, the horizontal direction is ± 150 degrees or less, and the vertical direction Can move within the range of -10 to 135 degrees with respect to the neutron incident line, the X-ray detector moving arm is shorter than the neutron detector moving arm, and the X-ray detector is more subject than the neutron detector. The minimum movement angle of X-rays and neutrons is 0.002 degrees / pulse, and the divergence angle of neutrons is 0.2 degrees. That is, sufficiently accurate data can be collected by moving the neutron beam (pulse wave) by 0.002 degrees per pulse within the range of the neutron beam divergence angle of 0.2 degrees.
本実施態様において、試料台は、大型の試料を載置できる大型４軸型回折計を用いることが好ましい。本発明において用いることができる大型４軸回折計としては、φ軸並進距離20mm、φ軸が垂直の場合の耐荷重1kgとすることが好ましい。大型４軸回折計を用いる場合には、すべての反射を１平面内（χ＝０）で測定可能であるが、X線検出器移動用アーム及び中性子検出器移動用アームは、χサークル付の固定長とすることが好ましい。χサークル用リングの半径は20cｍ〜30cmが好ましい。X線検出器及び中性子検出器は、χサークル上を−１０度〜１３５度の範囲で移動可能である。χサークルを設けることにより、液体試料あるいは試料が重くてφ軸を斜めにできない場合にも計測が可能となる。特に単色X線の万歳型測定にはχサークルが不可欠となる。また、トポグラフィーなど画像撮影の場合には、晶帯軸の回転では常に反射条件を満たしているが同一反射でも見る方向により画像が変化する場合があり、χサークルを設けることで画像の変化を修正することができる。 In this embodiment, the sample stage is preferably a large 4-axis diffractometer that can mount a large sample. The large 4-axis diffractometer that can be used in the present invention preferably has a φ axis translation distance of 20 mm and a load resistance of 1 kg when the φ axis is vertical. When a large 4-axis diffractometer is used, all reflections can be measured in one plane (χ = 0), but the X-ray detector moving arm and neutron detector moving arm are equipped with χ circles. A fixed length is preferred. The radius of the ring for χ circle is preferably 20 cm to 30 cm. The X-ray detector and the neutron detector can move in the range of −10 degrees to 135 degrees on the χ circle. By providing the χ circle, measurement is possible even when the liquid sample or the sample is heavy and the φ axis cannot be inclined. In particular, χ circle is indispensable for the measurement of monochromatic X-rays. In the case of imaging such as topography, rotation of the zone axis always satisfies the reflection condition, but the image may change depending on the viewing direction even with the same reflection. It can be corrected.
本実施態様には、４軸回折計のω軸に並進機構を付加し、被検体の移動と検出器のχ軸に沿った動きを連動させて、ラングカメラ（Lang Camera）の機能を持たせることもできる。検出器を取り付けるχサークルの半径を300ｍｍとするとΔχ＝2度に対してフィルムの移動距離は10.5ｍｍであり、並進との差は厚さ方向（回折Ｘ線の進行方向）で0.37mm、長さ方向（移動方向）でcos２度が0.9994mmとなり、誤差は無視できる。 In this embodiment, a translation mechanism is added to the ω-axis of the 4-axis diffractometer, and the movement of the subject and the movement along the χ-axis of the detector are linked to provide the function of a Lang Camera. You can also. If the radius of the χ circle to which the detector is attached is 300 mm, the moving distance of the film is 10.5 mm for Δχ = 2 degrees, and the difference from translation is 0.37 mm in the thickness direction (diffracted X-ray traveling direction), which is long. In the vertical direction (moving direction), cos 2 degrees becomes 0.9994mm, and the error can be ignored.
本発明の装置は、試料へのレーザー照射と、中性子照射及び検出と、Ｘ線照射及び検出とを、同時又は交互に行うことができることから、各種分野での構造変化と機能解析に有用である。たとえば、蛋白質をテラレーザーで照射刺激させながら、その際に生じる蛋白質内プロトンの動きを中性子で、さらにその結果もたらされる組織構造変化をX線で同時計測することで光合成の新しいプロセスモデルの検証を行う蛋白質機構構造モデルの検証に使用することが期待できる。また、機能セラミックスの材料合成をテラヘルツレーザーにより行い、その際の微細組織制御をX線構造解析により行う、高機能素材の開発にも使用することが期待できる。さらに、計測機器の取り換えにより、単結晶からの反射データ計測の他、界面反射率計測、小角散乱計測、トポグラフ等、非破壊検査、ラジオグラフなど広範囲な計測が本体装置だけで実現することが期待できる。さらに、各量子ビームを高輝度化し、装置をコンパクト化することにより量子ビーム発生源を小型化して全体装置の空間負担を軽減し、工業利用化装置としても将来において転用することが期待できる。 Since the apparatus of the present invention can perform laser irradiation, neutron irradiation and detection, and X-ray irradiation and detection on a sample simultaneously or alternately, it is useful for structural changes and functional analysis in various fields. . For example, while irradiating a protein with a tera laser, the movement of protons in the protein is detected with neutrons, and the resulting tissue structure changes are simultaneously measured with X-rays to verify a new process model for photosynthesis. It can be expected to be used to verify the structural model of protein mechanism. In addition, it can be expected to be used for the development of highly functional materials, in which functional ceramic materials are synthesized using a terahertz laser and the microstructure is controlled by X-ray structural analysis. In addition to the measurement of reflection data from single crystals, a wide range of measurements such as non-destructive inspection and radiographs, such as interface reflectance measurement, small angle scattering measurement, topography, etc., can be realized with the main unit only by replacing measurement equipment. it can. Further, by increasing the brightness of each quantum beam and downsizing the apparatus, the quantum beam generation source can be downsized to reduce the space burden on the entire apparatus, and it can be expected to be used as an industrial utilization apparatus in the future.
Claims (7)
当該被検体側面に中性子を照射する中性子源及び中性子導管と、
当該被検体により回折された中性子を検出する中性子検出器と、
当該被検体側面にX線を照射するX線発生装置及びX線導管と、
当該被検体を透過するX線を検出するX線検出器と、
当該被検体頂部にレーザーを照射するレーザー源及びレーザー導波管と、
X線検出時にX線発生装置及びX線導管並びにX線検出器を当該球体内部に前進させ、X線非検出時にはX線発生装置及びX線導管並びにX線検出器を当該球体から後退させるように作動するX線光源移動用アームと、X線の光軸に沿って当該X線検出器を移動させるX線検出器移動用アームと、を具備し、
前記球体の中心と前記中性子源とを結ぶ仮想直線に対して、前記球体の中心と前記X線発生装置とを結ぶ仮想直線が０〜３０度の角度となるように、前記中性子源と前記X線発生装置とは相対的に位置づけられていることを特徴とする、
中性子とX線とレーザーとの融合化計測装置。 A sample stage on which the subject is placed, positioned at the center of the sphere,
A neutron source and a neutron conduit for irradiating the side surface of the subject with neutrons;
A neutron detector for detecting neutrons diffracted by the subject;
An X-ray generator and X-ray conduit for irradiating the subject side surface with X-rays;
An X-ray detector that detects X-rays transmitted through the subject;
A laser source and a laser waveguide for irradiating the top of the subject with laser; and
The X-ray generator, X-ray conduit, and X-ray detector are advanced inside the sphere when X-ray is detected, and the X-ray generator, X-ray conduit, and X-ray detector are retracted from the sphere when X-ray is not detected. An X-ray light source moving arm that operates on, and an X-ray detector moving arm that moves the X-ray detector along the optical axis of the X-ray,
The neutron source and the X so that the virtual line connecting the center of the sphere and the X-ray generator is at an angle of 0 to 30 degrees with respect to the virtual line connecting the center of the sphere and the neutron source. It is characterized by being positioned relative to the line generator,
Neutron, X-ray and laser integrated measurement device.
前記X線検出器移動用アームは、前記中性子検出器移動用アームよりも短く、X線検出器が中性子検出器よりも被検体に近い位置に位置づけられ、
Ｘ線検出器移動用アーム及び中性子検出器移動用アームの最小移動角は０．００２度／パルスであり、中性子線の発散角度は０．２度であることを特徴とする、請求項１又は２に記載の装置。 The X-ray detector moving arm and the neutron detector moving arm are 2θ arms that rotate coaxially around the sample stage, and can move the X-ray detector in a range of ± 150 degrees or less in the horizontal direction. The neutron detector is movable in the range of −10 to 135 degrees in the vertical direction with respect to the neutron incident line from the neutron conduit,
The X-ray detector moving arm is shorter than the neutron detector moving arm, the X-ray detector is positioned closer to the subject than the neutron detector,
The minimum moving angle of the X-ray detector moving arm and the neutron detector moving arm is 0.002 degrees / pulse, and the divergence angle of the neutron beam is 0.2 degrees. 2. The apparatus according to 2.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950236A (en) * | 2017-05-17 | 2017-07-14 | 中国工程物理研究院核物理与化学研究所 | A kind of device for the quick localizing sample position of neutron small angle scattering spectrometer |
| CN109596646A (en) * | 2018-12-30 | 2019-04-09 | 东莞材料基因高等理工研究院 | A kind of in situ X-ray diffraction CT imaging device for Neutron diffractometer |
| CN111693553A (en) * | 2019-03-12 | 2020-09-22 | Fei 公司 | Method and system for ribbon axis alignment |
| WO2021035765A1 (en) * | 2019-08-26 | 2021-03-04 | 中国科学院地质与地球物理研究所 | Method for neutron imaging during triaxial mechanical test of sediment of natural gas hydrate |
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2012
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950236A (en) * | 2017-05-17 | 2017-07-14 | 中国工程物理研究院核物理与化学研究所 | A kind of device for the quick localizing sample position of neutron small angle scattering spectrometer |
| CN109596646A (en) * | 2018-12-30 | 2019-04-09 | 东莞材料基因高等理工研究院 | A kind of in situ X-ray diffraction CT imaging device for Neutron diffractometer |
| CN111693553A (en) * | 2019-03-12 | 2020-09-22 | Fei 公司 | Method and system for ribbon axis alignment |
| WO2021035765A1 (en) * | 2019-08-26 | 2021-03-04 | 中国科学院地质与地球物理研究所 | Method for neutron imaging during triaxial mechanical test of sediment of natural gas hydrate |
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