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JP6968419B2 - Manufacturing method of wavefront control element - Google Patents
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JP6968419B2 - Manufacturing method of wavefront control element - Google Patents

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JP6968419B2
JP6968419B2 JP2018087478A JP2018087478A JP6968419B2 JP 6968419 B2 JP6968419 B2 JP 6968419B2 JP 2018087478 A JP2018087478 A JP 2018087478A JP 2018087478 A JP2018087478 A JP 2018087478A JP 6968419 B2 JP6968419 B2 JP 6968419B2
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航 矢代
秀実 加藤
大介 北條
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Tohoku University NUC
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Description

本発明は、波面制御素子の製造方法に関する。 The present invention relates to a method for manufacturing a wavefront control element.

X線干渉計や中性子干渉計などでは、X線や中性子線の波面を精密に制御する必要があり、そのために、使用される波面制御素子を高精度で正確な形状に整える必要がある。特に、X線Talbot干渉計や中性子Talbot干渉計では、波面制御素子として回折格子が使用されるが、感度や空間分解能の向上のため、より短周期かつ高精度形状の回折格子が求められている。 In X-ray interferometers and neutron interferometers, it is necessary to precisely control the wavefront of X-rays and neutrons, and for that purpose, it is necessary to arrange the wavefront control element to be used in a highly accurate and accurate shape. In particular, in X-ray Talbot interferometers and neutron Talbot interferometers, diffraction gratings are used as wavefront control elements, but in order to improve sensitivity and spatial resolution, a diffraction grating with a shorter cycle and a higher precision shape is required. ..

従来、X線Talbot干渉計の回折格子として、0.33K/sの昇温速度で過冷却状態にしたPd基の金属ガラス材料に対して転写成形を行うことにより、凹部の深さが約10μm、凹凸の周期が8μmの金属ガラス製の回折格子が、本発明者等により得られている(例えば、非特許文献1参照)。しかし、この方法では、金属ガラス製の回折格子を得るために、成形時の温度を、ガラス遷移温度(T)と結晶化開始温度(Ton)との間の温度に維持する必要があり、粘性率が高い状態で金属ガラス材料を成形しなければならないという問題があった。 Conventionally, as a diffraction grating of an X-ray Talbot interferometer, the depth of the recess is about 10 μm by performing transfer molding on a Pd-based metallic glass material that has been supercooled at a heating rate of 0.33 K / s. A diffraction grating made of metallic glass having a concavo-convex period of 8 μm has been obtained by the present inventors (see, for example, Non-Patent Document 1). However, in this method, in order to obtain a metallic glass diffraction grid, it is necessary to maintain the temperature at the time of molding at a temperature between the glass transition temperature (T g ) and the crystallization start temperature ( Ton). There is a problem that the metallic glass material must be molded in a state of high viscosity.

また、中性子Talbot干渉計の回折格子を得る方法として、Si製の基板格子に、ガドックス(Gd硫酸化物)の粉末を注入して浸透させ、さらに固化させることにより、ガドックス製の回折格子を製造する方法が開発されている(例えば、非特許文献2参照)。しかし、この方法で得られた回折格子は、凹部の深さが500μm、凹凸の周期が477μmであり、数100μmより小さい構造を得るのは困難であるという問題があった。このため、この方法では、中性子Talbot干渉計の回折格子の中でも、凹凸の周期が比較的長いG(Source Grating)の回折格子を製造することはできるが、より周期が短いG(Analyzer Grating)の回折格子を製造することはできない。 Further, as a method of obtaining a diffraction grating of a neutron Talbot interferometer, a diffraction grating made of Gadox is manufactured by injecting a powder of Gadox (Gd sulfate) into a substrate grating made of Si, infiltrating it, and further solidifying it. A method has been developed (see, for example, Non-Patent Document 2). However, the diffraction grating obtained by this method has a problem that it is difficult to obtain a structure smaller than several hundred μm because the depth of the concave portion is 500 μm and the period of the unevenness is 477 μm. Therefore, with this method, it is possible to manufacture a G 0 (Source Grating) diffraction grating having a relatively long uneven period among the diffraction gratings of a neutron Talbot interferometer , but a shorter period G 2 (Analyzer Grating). ) Diffraction grating cannot be manufactured.

また、より短周期の回折格子を得る方法として、Si製の回折格子金型に対して、Gd蒸気を斜め上方から吹き付けて、Si製金型に蒸着させることにより、Gd製の回折格子を製造する方法が開発されている(例えば、非特許文献3参照)。この方法では、凹部の深さが約11μm、凹凸の周期が約4μmであり、中性子Talbot干渉計のGの回折格子に利用可能な、短周期の回折格子が得られているが、形状を精密に制御することができないという問題があった。このため、回折格子の凸部の厚さにムラができてしまい、干渉計の空間分解能が低下する危険性がある。また、1つの回折格子を製造するのに、2日〜1週間程度かかってしまい、製造時間が長いという問題もあった。 Further, as a method of obtaining a diffraction grating having a shorter cycle, a diffraction grating made of Gd is manufactured by spraying Gd steam diagonally from above onto a diffraction grating die made of Si and depositing the diffraction grating on the Si die. A method has been developed (see, for example, Non-Patent Document 3). This method obtains a short-period diffraction grating that has a recess depth of about 11 μm and an uneven period of about 4 μm and can be used as a G 2 diffraction grating for a neutron Talbot interferometer. There was a problem that it could not be controlled precisely. Therefore, there is a risk that the thickness of the convex portion of the diffraction grating will be uneven and the spatial resolution of the interferometer will be reduced. Further, it takes about 2 days to 1 week to manufacture one diffraction grating, and there is also a problem that the manufacturing time is long.

そこで、これらの問題を解決するために、非特許文献1に記載の方法を改良し、過冷却状態の金属ガラス材料を、その金属ガラス材料の過冷却液体の結晶化開始温度(Ton)以上の温度まで加熱して、過冷却液体の結晶化過程が完了するまでの間に、金属ガラス材料を、金属ガラスと結晶相との混相、または、結晶単相を有する成形体に加工する方法が、本発明者等により開発されている(例えば、特許文献1参照)。 Therefore, in order to solve these problems, the method described in Non-Patent Document 1 is improved, and the liquidmetal glass material in the supercooled state is equal to or higher than the crystallization start temperature (Ton) of the supercooled liquid of the supercooled liquidmetal material. By heating to the above temperature and completing the crystallization process of the supercooled liquid, there is a method of processing the metallic glass material into a mixed phase of the metallic glass and the crystalline phase or a molded body having a crystalline single phase. , Developed by the present inventors (see, for example, Patent Document 1).

また、マイクロ鋳造法(microcasting)を改良して、Si製の回折格子金型(テンプレート)に、溶融したBi、Au−Sn系合金またはPb系合金を流し込むことにより、数μm〜数10μmの構造を有する、高アスペクト比のX線干渉計の回折格子を製造する方法も開発されている(例えば、非特許文献4〜6参照)。また、X線リソグラフィーと電気鋳造とを用いて、Si基板の上に金メッキを施した、数μm程度の構造を有する高アスペクト比のX線干渉計の回折格子を製造する方法も開発されている(例えば、非特許文献7参照)。 Further, by improving the microcasting method and pouring a molten Bi, Au-Sn-based alloy or a Pb-based alloy into a diffraction grating mold (template) made of Si, a structure of several μm to several tens of μm is formed. A method for manufacturing a diffraction grating of an X-ray interferometer having a high aspect ratio has also been developed (see, for example, Non-Patent Documents 4 to 6). Further, a method of manufacturing a diffraction grating of a high aspect ratio X-ray interferometer having a structure of about several μm, which is gold-plated on a Si substrate by using X-ray lithography and electroforming, has also been developed. (See, for example, Non-Patent Document 7).

Wataru Yashiro, Daiji Noda, Tadashi Hattori, Kouichi Hayashi, Atsushi Momose, and Hidemi Kato, “A metallic glass grating for X-ray grating interferometers fabricated by imprinting”, Applied Physics Express, 2014, 7, 032501Wataru Yashiro, Daiji Noda, Tadashi Hattori, Kouichi Hayashi, Atsushi Momose, and Hidemi Kato, “A metallic glass grating for X-ray grating interferometers plotted by imprinting”, Applied Physics Express, 2014, 7, 032501 J. Kim, et al., “Fabrication and characterization of the source grating for visibility improvement of neutron phase imaging with gratings”, Rev. Sci. Instrum., 2013, 84, 063705J. Kim, et al., “Fabrication and characterization of the source grating for visibility improvement of neutron phase imaging with gratings”, Rev. Sci. Instrum., 2013, 84, 063705 C. Grunzweig, et al., “Design, fabrication, and characterization of diffraction gratings for neutron phase contrast imaging”, Rev. Sci. Instrum., 2008, 79, 053703C. Grunzweig, et al., “Design, fabrication, and characterization of diffraction gratings for neutron phase contrast imaging”, Rev. Sci. Instrum., 2008, 79, 053703 Yaohu Lei, et al., “Improvement of filling bismuth for x-ray absorption gratings through the enhancement of wettability”, J. Micromech. Microeng., 2016, 26, 065011Yaohu Lei, et al., “Improvement of filling bismuth for x-ray absorption gratings through the enhancement of wettability”, J. Micromech. Microeng., 2016, 26, 065011 L. Romano, et al., “High aspect ratio metal microcasting by hot embossing for X-ray optics fabrication”, Microelectronic Engineering, 2017, 176, p.6-10L. Romano, et al., “High aspect ratio metal microcasting by hot embossing for X-ray optics fabrication”, Microelectronic Engineering, 2017, 176, p.6-10 L. Romano, et al., “Hot embossing of Au- and Pb-based alloys for x-ray grating fabrication”, J. Vac. Sci. Technol. B, 2017, Vol.35, No.6, 06G302L. Romano, et al., “Hot embossing of Au- and Pb-based alloys for x-ray grating fabrication”, J. Vac. Sci. Technol. B, 2017, Vol.35, No.6, 06G302 株式会社ASICON、「製品とサービス;カールスルーエ技術研究所・IMT Talbot-Lau干渉計向け回折格子(Gratings for X-ray Talbot-Lau Interferometry)」、[online]、[平成30年4月25日検索]、インターネット〈URL: http://www.asicon-tokyo.com/imt04.php〉ASICON Co., Ltd., "Products and Services; Gratings for X-ray Talbot-Lau Interferometry", [online], [Search on April 25, 2018] , Internet <URL: http://www.asicon-tokyo.com/imt04.php>

国際公開WO2016/208517号International release WO2016 / 208517

特許文献1に記載の方法によれば、結晶化開始温度(Ton)以上まで加熱することにより、粘性が低い状態で金属ガラス材料を成形体に加工することができるため、成形時に、形状をより精密に制御することができる。このため、数10μm〜数100nmの小さい構造を有する中性子Talbot干渉計やX線Talbot干渉計のGの回折格子などを製造することができる。また、金属ガラス材料が過冷却状態を含有する間に成形を行うため、必然的に製造時間も短縮される。しかし、製造時に、金属ガラス材料の温度管理を精密に行う必要があり、そのためのコストがかかってしまうという課題があった。 According to the method described in Patent Document 1, by heating to a crystallization start temperature (Ton ) or higher, a metallic glass material can be processed into a molded product in a state of low viscosity, so that the shape can be changed at the time of molding. It can be controlled more precisely. Therefore, it is possible to manufacture a G 2 diffraction grating of a neutron Talbot interferometer or an X-ray Talbot interferometer having a small structure of several tens of μm to several hundred nm. Further, since the molding is performed while the metallic glass material contains the supercooled state, the manufacturing time is inevitably shortened. However, there is a problem that it is necessary to precisely control the temperature of the metallic glass material at the time of manufacturing, which increases the cost.

また、非特許文献4〜6に記載の方法も、数μm〜数10μmの構造を有し、高アスペクト比の波面制御素子を製造することができるが、マイクロ鋳造を行う際の温度や圧力を精密に管理する必要があるため、やはり製造時のコストが高くなるという課題があった。また、非特許文献7に記載の方法も、数μm程度の構造を有し、高アスペクト比の波面制御素子を製造することができるが、製造条件の精密な管理が必要となり、やはり製造時のコストが高くなるという課題があった。 Further, the methods described in Non-Patent Documents 4 to 6 also have a structure of several μm to several tens of μm, and can manufacture a wave surface control element having a high aspect ratio. Since it is necessary to manage it precisely, there is also a problem that the manufacturing cost is high. Further, the method described in Non-Patent Document 7 also has a structure of about several μm and can manufacture a wavefront control element having a high aspect ratio, but it requires precise control of manufacturing conditions, and is also at the time of manufacturing. There was a problem that the cost was high.

本発明は、このような課題に着目してなされたもので、より低いコストで、数10μm以下の構造を有する波面制御素子を製造することができる、波面制御素子の製造方法を提供することを目的とする。 The present invention has been made by paying attention to such a problem, and provides a method for manufacturing a wavefront control element capable of manufacturing a wavefront control element having a structure of several tens of μm or less at a lower cost. The purpose.

上記目的を達成するために、本発明に係る波面制御素子の製造方法は、周期的に凹凸を有する型を用い、金属元素を含む材料粒子を、遠心充填により前記型の凹部に充填して波面制御素子を製造することを特徴とする。 In order to achieve the above object, the method for manufacturing a wavefront control element according to the present invention uses a mold having irregularities periodically, and material particles containing a metal element are filled in the concave portions of the mold by centrifugal filling to fill the concave portions of the mold. It is characterized by manufacturing a control element.

本発明に係る波面制御素子の製造方法は、遠心充填により、材料粒子を型の凹部に、比較的高い充填率で充填することができる。このため、数10μm以下の構造を有する型と、その型の凹部に挿入可能な材料粒子とを用いることにより、数10μm以下の構造を有する波面制御素子を製造することができる。また、製造時に、精密な温度や圧力の管理が不要であり、精密な温度や圧力の管理が必要なものと比較して、より低いコストで波面制御素子を製造することができる。 In the method for manufacturing a wavefront control element according to the present invention, material particles can be filled in the recesses of a mold with a relatively high filling rate by centrifugal filling. Therefore, by using a mold having a structure of several tens of μm or less and material particles that can be inserted into the recesses of the mold, a wavefront control element having a structure of several tens of μm or less can be manufactured. In addition, precise temperature and pressure control is not required at the time of manufacture, and the wavefront control element can be manufactured at a lower cost than those requiring precise temperature and pressure control.

本発明に係る波面制御素子の製造方法は、型により、形状を精密に制御して、波面制御素子を製造することができる。このため、アスペクト比が高い波面制御素子を製造することもできる。型は、周期的に凹凸を有していれば、製造する波面制御素子の用途に応じていかなるものであってもよく、例えば、凹部および凸部が1方向に連続的に伸び、それに直交する方向に凹凸が繰り返し現れるものや、凹凸が直交する2方向に繰り返し現れるものであってもよい。 In the method for manufacturing a wavefront control element according to the present invention, the shape can be precisely controlled by a mold to manufacture a wavefront control element. Therefore, it is also possible to manufacture a wavefront control element having a high aspect ratio. The mold may be anything as long as it has irregularities periodically, depending on the application of the wavefront control element to be manufactured. For example, the concave portions and the convex portions are continuously extended in one direction and orthogonal to the concave portions and the convex portions. The unevenness may appear repeatedly in the direction, or the unevenness may appear repeatedly in two directions orthogonal to each other.

本発明に係る波面制御素子の製造方法は、40000rpm以上の回転数で前記遠心充填を行うことが好ましい。この場合、凹部への材料粒子の充填率を高めることができる。また、より短時間で波面制御素子を製造することができる。回転数を大きくすることにより、よりアスペクト比が高い波面制御素子を精度良く製造することができる。 In the method for manufacturing a wavefront control element according to the present invention, it is preferable to perform the centrifugal filling at a rotation speed of 40,000 rpm or more. In this case, the filling rate of the material particles in the recesses can be increased. In addition, the wavefront control element can be manufactured in a shorter time. By increasing the rotation speed, it is possible to accurately manufacture a wavefront control element having a higher aspect ratio.

本発明に係る波面制御素子の製造方法で、前記型は、前記凹部の深さが10μm以上1000μm以下、前記凹凸の周期が100nm以上100μm以下であり、前記材料粒子は、直径が5nm以上10μm以下であり、前記凹部に充填可能な大きさを有することが好ましい。この場合、中性子Talbot干渉計やX線Talbot干渉計のGの回折格子などの、アスペクト比が高く、より小さい構造を有する波面制御素子を製造することができる。 In the method for manufacturing a wavefront control element according to the present invention, in the mold, the depth of the recess is 10 μm or more and 1000 μm or less, the period of the unevenness is 100 nm or more and 100 μm or less, and the material particles have a diameter of 5 nm or more and 10 μm or less. It is preferable that the concave portion has a size that can be filled. In this case, it is possible to manufacture a wavefront control element having a high aspect ratio and a smaller structure, such as a neutron Talbot interferometer and a G 2 diffraction grating of an X-ray Talbot interferometer.

本発明に係る波面制御素子の製造方法は、前記遠心充填の後、焼結を行ってもよく、前記材料粒子の融点以上の温度で熱処理を行ってもよい。焼結を行う場合、材料粒子同士が結合するため、緻密な波面制御素子を製造することができる。また、材料粒子の融点以上の温度で熱処理を行う場合、材料粒子が軟化または融解するため、凹部の形状に合わせて流動し、形状精度を高めることができる。軟化または融解した材料粒子の表面張力や、材料粒子と型との間の付着力などにより、材料粒子が流動しにくい場合には、材料粒子が凹部に充填されるよう、材料粒子に圧力を加えてもよい。 In the method for manufacturing a wavefront control element according to the present invention, sintering may be performed after the centrifugal filling, or heat treatment may be performed at a temperature equal to or higher than the melting point of the material particles. When sintering is performed, the material particles are bonded to each other, so that a precise wavefront control element can be manufactured. Further, when the heat treatment is performed at a temperature equal to or higher than the melting point of the material particles, the material particles soften or melt, so that the material particles flow according to the shape of the concave portion, and the shape accuracy can be improved. If the material particles are difficult to flow due to the surface tension of the softened or melted material particles or the adhesive force between the material particles and the mold, pressure is applied to the material particles so that the material particles are filled in the recesses. You may.

本発明に係る波面制御素子の製造方法で、製造される波面制御素子は、例えば、中性子線干渉計もしくはX線干渉計の回折格子や、中性子Talbot干渉計もしくはX線Talbot干渉計のGの回折格子である。前記波面制御素子が、中性子線干渉計の回折格子または中性子Talbot干渉計のGの回折格子である場合には、前記材料粒子は、Gdを含む合金粒子、または、主成分としてGdを含む金属酸化物粒子から成ることが好ましい。これらの場合、Gdが、他の元素と比べて、熱中性子を良く吸収するため、中性子線干渉計や中性子Talbot干渉計の回折格子として最適である。 The wavefront control element manufactured by the method for manufacturing a wavefront control element according to the present invention is, for example, the diffraction grating of a neutron beam interferometer or an X-ray interferometer, or the G 2 of a neutron Talbot interferometer or an X-ray Talbot interferometer. It is a diffraction grating. When the wavefront control element is a diffraction grating of a neutron beam interferometer or a G 2 diffraction grating of a neutron Talbot interferometer, the material particles are alloy particles containing Gd or a metal containing Gd as a main component. It is preferably composed of oxide particles. In these cases, Gd absorbs thermal neutrons better than other elements, and is therefore most suitable as a diffraction grating for a neutron beam interferometer or a neutron Talbot interferometer.

また、前記波面制御素子が、X線干渉計の回折格子またはX線Talbot干渉計のGの回折格子である場合には、前記材料粒子は、Pt、Au、Ta、W、Re、PbもしくはBiから成る金属粒子、主成分としてPt、Au、Ta、W、Re、PbもしくはBiを有する合金粒子、または、主成分としてPt、Au、Ta、W、Re、PbもしくはBiの酸化物を有する金属酸化物粒子から成ることが好ましい。この場合、Pt、Au、Ta、W、Re、Pb、Biが、他の元素と比べて、X線を良く吸収するため、X線干渉計やX線Talbot干渉計の回折格子として最適である。 When the wave surface control element is a diffraction grating of an X-ray interferometer or a G 2 diffraction grating of an X-ray Talbot interferometer, the material particles are Pt, Au, Ta, W, Re, Pb or It has a metal particle composed of Bi, an alloy particle having Pt, Au, Ta, W, Re, Pb or Bi as a main component, or an oxide of Pt, Au, Ta, W, Re, Pb or Bi as a main component. It is preferably composed of metal oxide particles. In this case, Pt, Au, Ta, W, Re, Pb, and Bi absorb X-rays better than other elements, so that they are most suitable as diffraction gratings for X-ray interferometers and X-ray Talbot interferometers. ..

また、前記材料粒子は、Gd基、Sm基、Eu基、Dy基、Pt基、Au基、Pd基またはNi基の金属ガラス粒子から成っていてもよい。Gd基、Sm基、Eu基、Dy基の金属ガラス粒子の場合には、製造される波面制御素子は、中性子線干渉計や中性子Talbot干渉計の回折格子として最適であり、Pt基、Au基、Pd基、Ni基の金属ガラス粒子の場合には、製造される波面制御素子は、X線干渉計やX線Talbot干渉計の回折格子として最適である。この場合、材料粒子が金属ガラス粒子から成るため、遠心充填の後、特許文献1に記載のような、過冷却液体状態を利用した転写成形などの成形を行うことにより、隣り合う凸部と凹部との間隔がnmオーダーの回折格子を製造することができる。 Further, the material particles may be composed of Gd group, Sm group, Eu group, Dy group, Pt group, Au group, Pd group or Ni group metallic glass particles. In the case of Gd group, Sm group, Eu group, and Dy group metal glass particles, the wavefront control element to be manufactured is most suitable as a diffraction grating for a neutron beam interferometer or a neutron Talbot interferometer, and has a Pt group or Au group. In the case of Pd-based and Ni-based metal glass particles, the manufactured wavefront control element is most suitable as a diffraction grating of an X-ray interferometer or an X-ray Talbot interferometer. In this case, since the material particles are made of metallic glass particles, adjacent convex portions and concave portions are formed by performing molding such as transfer molding using a supercooled liquid state as described in Patent Document 1 after centrifugation. A diffraction grating having a distance from and on the order of nm can be manufactured.

本発明に係る波面制御素子の製造方法は、前記遠心充填の後、前記材料粒子が充填された前記凹部を覆うよう金属ガラスリボンを敷設し、熱処理を行ってもよい。この場合、材料粒子の焼結可能温度と、金属ガラスリボンのガラス遷移温度とを同等にしておくことで、焼結などの熱処理により、材料粒子および金属ガラスリボンを同時に緻密化することができる。また、熱処理の際に、材料粒子が凹部に充填されるよう、金属ガラスリボンの上から材料粒子に圧力を加えてもよい。これにより、形状精度を高めることができる。 In the method for manufacturing a wavefront control element according to the present invention, after the centrifugal filling, a metallic glass ribbon may be laid so as to cover the recesses filled with the material particles, and heat treatment may be performed. In this case, by keeping the sinterable temperature of the material particles equal to the glass transition temperature of the metallic glass ribbon, the material particles and the metallic glass ribbon can be densified at the same time by a heat treatment such as sintering. Further, during the heat treatment, pressure may be applied to the material particles from above the metallic glass ribbon so that the material particles are filled in the recesses. This makes it possible to improve the shape accuracy.

この金属ガラスリボンを利用する場合、波面制御素子が、X線干渉計やX線Talbot干渉計の回折格子のとき、例えば、材料粒子を純金ナノ粒子とし、金属ガラスリボンを、純金ナノ粒子の融点と同等のガラス遷移温度(Tg)を有し、平均原子番号が大きい組成の金属ガラス製としてもよい。また、波面制御素子が、中性子線干渉計や中性子線Talbot干渉計の回折格子のとき、例えば、材料粒子をGdを含む合金粒子とし、金属ガラスリボンを、その合金粒子の融点と同等のガラス遷移温度(Tg)を有し、平均原子番号が大きい組成のGd基の金属ガラス製としてもよい。 When this metal glass ribbon is used, when the wave surface control element is a diffraction lattice of an X-ray interferometer or an X-ray Talbot interferometer, for example, the material particles are pure gold nanoparticles and the metal glass ribbon is the melting point of the pure gold nanoparticles. It may be made of metal glass having a glass transition temperature (Tg) equivalent to that of the above and having a composition having a large average atomic number. Further, when the wave surface control element is a diffraction lattice of a neutron beam interferometer or a neutron beam Talbot interferometer, for example, the material particles are alloy particles containing Gd, and the metal glass ribbon is a glass transition equivalent to the melting point of the alloy particles. It may be made of Gd-based metal glass having a temperature (Tg) and a composition having a large average atomic number.

また、この金属ガラスリボンを利用する場合、材料粒子が金属ガラス粒子から成り、材料粒子および金属ガラスリボンが、金属ガラスと結晶相との混相または結晶単相となるよう熱処理を行ってもよい。この場合、材料粒子同士が結合すると共に、金属ガラスリボンと一体化するため、緻密で、金属ガラスの組成と同じ組成を有する合金から成る波面制御素子を製造することができる。 Further, when this metallic glass ribbon is used, heat treatment may be performed so that the metallic particles are made of metallic glass particles and the metallic particles and the metallic glass ribbon are in a mixed phase or a crystalline single phase of the metallic glass and the crystalline phase. In this case, since the material particles are bonded to each other and integrated with the metallic glass ribbon, it is possible to manufacture a wavefront control element made of an alloy having the same composition as that of the metallic glass, which is dense.

本発明によれば、より低いコストで、数10μm以下の構造を有する波面制御素子を製造することができる、波面制御素子の製造方法を提供することができる。 According to the present invention, it is possible to provide a method for manufacturing a wavefront control element, which can manufacture a wavefront control element having a structure of several tens of μm or less at a lower cost.

本発明の実施の形態の波面制御素子の製造方法の、(a)容器に、型および粒子分散液を入れた状態、(b)遠心充填を行っている状態を示す正面図である。It is a front view which shows the state which (a) the state which put the mold and the particle dispersion liquid in a container, and (b) the state which is performing the centrifugal filling of the manufacturing method of the wavefront control element of embodiment of this invention. 本発明の実施の形態の波面制御素子の製造方法の、金粒子を用いて遠心充填を行った後の型の断面の(a)走査型電子顕微鏡(SEM)写真、(b) (a)の凹部を拡大したSEM写真である。Of the method for manufacturing a wave surface control element according to the embodiment of the present invention, (a) scanning electron microscope (SEM) photograph, (b) (a) of the cross section of the mold after centrifugal filling using gold particles. It is an SEM photograph which enlarged the concave part. 本発明の実施の形態の波面制御素子の製造方法により製造された波面制御素子の、(a)正面側から照射した単色X線の透過光を、裏面側から撮影したSEM写真、(b) (a)中の線に沿った透過率の測定結果を示すグラフである。An SEM photograph of (a) the transmitted light of monochromatic X-rays irradiated from the front side of the wavefront control element manufactured by the method for manufacturing the wavefront control element according to the embodiment of the present invention, taken from the back side, (b) (b). a) It is a graph which shows the measurement result of the transmittance along the line in a). 本発明の実施の形態の波面制御素子の製造方法の、Pt粒子を用いて遠心充填を行った後の型の断面の走査型電子顕微鏡(SEM)写真である。It is a scanning electron microscope (SEM) photograph of the cross section of the mold after centrifugal filling using Pt particles of the method of manufacturing the wave surface control element of the embodiment of this invention. 本発明の実施の形態の波面制御素子の製造方法の、酸化ガドリニウム粒子を用いて遠心充填を行った後の型の断面の走査型電子顕微鏡(SEM)写真である。It is a scanning electron microscope (SEM) photograph of the cross section of the mold after centrifugal filling using gadolinium oxide particles of the method of manufacturing the wave surface control element of the embodiment of this invention.

以下、図面に基づいて、本発明の実施の形態について説明する。
図1乃至図5は、本発明の実施の形態の波面制御素子の製造方法を示している。
本発明の実施の形態の波面制御素子の製造方法は、波面制御素子を製造するために、まず、図1(a)に示すように、周期的に凹凸を有する型11を、凹部の開口側を上にして、容器12の底に配置する。
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
1 to 5 show a method for manufacturing a wavefront control element according to an embodiment of the present invention.
In the method of manufacturing the wavefront control element according to the embodiment of the present invention, in order to manufacture the wavefront control element, first, as shown in FIG. 1A, a mold 11 having periodic irregularities is placed on the opening side of the recess. Is placed on the bottom of the container 12 with the face up.

型11は、製造する波面制御素子の凹部の深さや凹凸の周期が所望のサイズになるよう形成されている。具体的な一例では、型11は、凹部の深さが、10μm以上300μm以下、凹凸の周期が、100nm以上100μm以下である。また、型11の製造方法としては、例えば、Deep RIE(深堀エッチング)、異方性エッチング、X線リソグラフィ、陽極酸化ポーラスアルミナ、3Dプリンティングなどの方法を利用することができる。型11は、後で実施する遠心充填で破壊されない素材であれば、シリコンなど、いかなる素材で形成されていてもよい。 The mold 11 is formed so that the depth of the concave portion and the period of the unevenness of the wavefront control element to be manufactured have a desired size. As a specific example, in the mold 11, the depth of the concave portion is 10 μm or more and 300 μm or less, and the period of the unevenness is 100 nm or more and 100 μm or less. Further, as a method for manufacturing the mold 11, for example, a method such as Deep RIE (deep digging etching), anisotropic etching, X-ray lithography, anodized porous alumina, and 3D printing can be used. The mold 11 may be made of any material such as silicon as long as it is a material that is not destroyed by the centrifugal filling performed later.

また、型11は、周期的に凹凸を有していれば、製造する波面制御素子の用途に応じていかなるものであってもよく、例えば、凹部および凸部が1方向に連続的に伸び、それに直交する方向に凹凸が繰り返し現れるものや、凹凸が直交する2方向に繰り返し現れるものであってもよい。 Further, the mold 11 may be of any shape as long as it has irregularities periodically, depending on the application of the wavefront control element to be manufactured. For example, the concave portions and the convex portions are continuously extended in one direction. The unevenness may appear repeatedly in the direction orthogonal to it, or the unevenness may appear repeatedly in two directions orthogonal to it.

次に、型11を配置した容器12の中に、水中に金属元素を含む材料粒子を分散させた粒子分散液13を入れる。材料粒子は、型11の凹部に充填可能な大きさを有している。具体的な一例では、材料粒子は、直径が5nm以上10μm以下である。材料粒子は、例えば、波面制御素子として、中性子線干渉計の回折格子または中性子Talbot干渉計のGの回折格子を製造する場合には、熱中性子を良く吸収するGdを含む合金粒子、または、主成分としてGdを含む金属酸化物粒子から成ることが好ましい。 Next, the particle dispersion liquid 13 in which the material particles containing the metal element are dispersed in water is placed in the container 12 in which the mold 11 is arranged. The material particles have a size that can be filled in the recesses of the mold 11. In a specific example, the material particles have a diameter of 5 nm or more and 10 μm or less. The material particles are, for example, alloy particles containing Gd that absorbs thermal neutrons well, or alloy particles in the case of manufacturing a diffraction grating of a neutron beam interferometer or a G 2 diffraction grating of a neutron Talbot interferometer as a wave surface control element. It is preferably composed of metal oxide particles containing Gd as a main component.

また、材料粒子は、波面制御素子として、X線干渉計の回折格子またはX線Talbot干渉計のGの回折格子を製造する場合には、X線を良く吸収するPt、Au、Ta、W、Re、PbもしくはBiから成る金属粒子、主成分としてPt、Au、Ta、W、Re、PbもしくはBiを有する合金粒子、主成分としてPt、Au、Ta、W、Re、PbもしくはBiの酸化物を有する金属酸化物粒子、または、Pt基、Au基、Pd基、Ni基の金属ガラス粒子から成ることが好ましい。 Further, when the material particles are used as a wave surface control element to manufacture a diffraction grid of an X-ray interferometer or a G 2 diffraction grid of an X-ray alloy Talbot interferometer, Pt, Au, Ta, W that absorb X-rays well. , Re, Pb or Bi metal particles, alloy particles having Pt, Au, Ta, W, Re, Pb or Bi as main components, oxidation of Pt, Au, Ta, W, Re, Pb or Bi as main components It is preferably composed of metal oxide particles having a substance, or metal glass particles having a Pt group, an Au group, a Pd group, or a Ni group.

容器12に粒子分散液13を入れた後、容器12に蓋12aをして密封し、図1(b)に示すように、型11が配置された容器12の底が、回転中心に対して外側になるようにして、遠心充填を行う。具体的な一例では、遠心充填の回転数は、40000rpm以上である。これにより、型11の凹部に材料粒子が充填され、波面制御素子を製造することができる。なお、型11の凹部からはみ出た材料粒子は、除去されることが好ましい。この場合、例えば、Arミリング、反応性ドライエッチング、ウェットエッチング、研磨などにより、容易に除去することができる。 After the particle dispersion liquid 13 is put in the container 12, the container 12 is sealed with a lid 12a, and as shown in FIG. 1 (b), the bottom of the container 12 in which the mold 11 is arranged is with respect to the center of rotation. Centrifugal filling is performed so that it is on the outside. In a specific example, the rotation speed of centrifugal filling is 40,000 rpm or more. As a result, the recesses of the mold 11 are filled with the material particles, and the wavefront control element can be manufactured. It is preferable that the material particles protruding from the recesses of the mold 11 are removed. In this case, it can be easily removed by, for example, Ar milling, reactive dry etching, wet etching, polishing, or the like.

次に、作用について説明する。
本発明の実施の形態の波面制御素子の製造方法は、遠心充填により、材料粒子を型11の凹部に、比較的高い充填率で充填することができる。このため、型11のサイズに応じて、例えば、数100μm〜数10μm以下の厚さを有する中性子線干渉計やX線干渉計の回折格子などの波面制御素子を製造することができる。また、製造時に、精密な温度や圧力の管理が不要であり、精密な温度や圧力の管理が必要なものと比較して、より低いコストで波面制御素子を製造することができる。
Next, the action will be described.
In the method for manufacturing a wavefront control element according to the embodiment of the present invention, material particles can be filled in the recesses of the mold 11 with a relatively high filling rate by centrifugal filling. Therefore, depending on the size of the mold 11, for example, a wavefront control element such as a diffraction grating of a neutron beam interferometer or an X-ray interferometer having a thickness of several hundred μm to several tens of μm or less can be manufactured. In addition, precise temperature and pressure control is not required at the time of manufacture, and the wavefront control element can be manufactured at a lower cost than those requiring precise temperature and pressure control.

本発明の実施の形態の波面制御素子の製造方法は、型11により、形状を精密に制御して、波面制御素子を製造することができる。このため、アスペクト比が高い波面制御素子を製造することもできる。このように、本発明の実施の形態の波面制御素子の製造方法によれば、100nm程度のサイズの波面制御素子を製造することも可能であり、中性子Talbot干渉計やX線Talbot干渉計のGの回折格子などの、アスペクト比が高く、より小さい構造を有する波面制御素子を製造することができる。 In the method for manufacturing a wavefront control element according to the embodiment of the present invention, the shape can be precisely controlled by the mold 11 to manufacture the wavefront control element. Therefore, it is also possible to manufacture a wavefront control element having a high aspect ratio. As described above, according to the method for manufacturing a wavefront control element according to the embodiment of the present invention, it is possible to manufacture a wavefront control element having a size of about 100 nm, and G of a neutron Talbot interferometer or an X-ray Talbot interferometer. It is possible to manufacture a wavefront control element having a high aspect ratio and a smaller structure, such as a diffraction grating of 2.

本発明の実施の形態の波面制御素子の製造方法は、40000rpm以上の回転数で遠心充填を行うことにより、凹部への材料粒子の充填率を高めることができる。また、より短時間で波面制御素子を製造することができる。回転数を大きくすることにより、よりアスペクト比が高い波面制御素子を精度良く製造することができる。 In the method for manufacturing a wavefront control element according to the embodiment of the present invention, the filling rate of material particles in the recesses can be increased by performing centrifugal filling at a rotation speed of 40,000 rpm or more. In addition, the wavefront control element can be manufactured in a shorter time. By increasing the rotation speed, it is possible to accurately manufacture a wavefront control element having a higher aspect ratio.

なお、本発明の実施の形態の波面制御素子の製造方法は、遠心充填の後、焼結を行ってもよく、材料粒子の融点以上の温度で熱処理を行ってもよい。焼結を行う場合、材料粒子同士が結合するため、緻密な波面制御素子を製造することができる。また、材料粒子の融点以上の温度で熱処理を行う場合、材料粒子が軟化または融解するため、凹部の形状に合わせて流動するため、形状精度を高めることができる。軟化または融解した材料粒子の表面張力や、材料粒子と型との間の付着力などにより、材料粒子が流動しにくい場合には、材料粒子が凹部に充填されるよう、材料粒子に圧力を加えてもよい。 In the method for manufacturing the wavefront control element according to the embodiment of the present invention, sintering may be performed after centrifugal filling, or heat treatment may be performed at a temperature equal to or higher than the melting point of the material particles. When sintering is performed, the material particles are bonded to each other, so that a precise wavefront control element can be manufactured. Further, when the heat treatment is performed at a temperature equal to or higher than the melting point of the material particles, the material particles soften or melt and flow according to the shape of the concave portion, so that the shape accuracy can be improved. If the material particles are difficult to flow due to the surface tension of the softened or melted material particles or the adhesive force between the material particles and the mold, pressure is applied to the material particles so that the material particles are filled in the recesses. You may.

また、本発明の実施の形態の波面制御素子の製造方法は、遠心充填の後、材料粒子が充填された凹部を覆うよう金属ガラスリボンを敷設し、熱処理を行ってもよい。この場合、材料粒子の焼結可能温度と、金属ガラスリボンのガラス遷移温度とを同等にしておくことで、焼結などの熱処理により、材料粒子および金属ガラスリボンを同時に緻密化することができる。また、熱処理の際に、材料粒子が凹部に充填されるよう、金属ガラスリボンの上から材料粒子に圧力を加えてもよい。これにより、形状精度を高めることができる。 Further, in the method for manufacturing the wavefront control element according to the embodiment of the present invention, after centrifugal filling, a metallic glass ribbon may be laid so as to cover the recesses filled with the material particles, and heat treatment may be performed. In this case, by keeping the sinterable temperature of the material particles equal to the glass transition temperature of the metallic glass ribbon, the material particles and the metallic glass ribbon can be densified at the same time by a heat treatment such as sintering. Further, during the heat treatment, pressure may be applied to the material particles from above the metallic glass ribbon so that the material particles are filled in the recesses. This makes it possible to improve the shape accuracy.

また、材料粒子が金属ガラス粒子から成り、金属ガラスリボンを利用する場合、材料粒子および金属ガラスリボンが、金属ガラスと結晶相との混相または結晶単相となるよう熱処理を行ってもよい。この場合、材料粒子同士が結合すると共に、金属ガラスリボンと一体化するため、緻密で、金属ガラスの組成と同じ組成を有する合金から成る波面制御素子を製造することができる。 Further, when the material particles are made of metallic glass particles and a metallic glass ribbon is used, heat treatment may be performed so that the metallic particles and the metallic glass ribbon have a mixed phase of metallic glass and a crystalline phase or a single crystalline phase. In this case, since the material particles are bonded to each other and integrated with the metallic glass ribbon, it is possible to manufacture a wavefront control element made of an alloy having the same composition as that of the metallic glass, which is dense.

本発明の実施の形態の波面制御素子の製造方法により、波面制御素子の製造を行った。型11は、10mm角のシリコン製の薄板の表面の、8mm角の領域に、Deep RIEにより、周期的な凹凸を形成したものを使用した。型11は、凹凸の周期が30μm、凹部の幅が20μm、凹部の深さが80μmである。また、粒子分散液13は、6mlの水に、材料粒子14として、直径1.5μmの球状の金(Au)粒子を0.1g入れたものを使用した。また、遠心充填を、周囲の温度を4℃にして、40000rpmの回転数で1時間行った。 The wavefront control element was manufactured by the method for manufacturing the wavefront control element according to the embodiment of the present invention. As the mold 11, a 10 mm square silicon thin plate having periodic irregularities formed in an 8 mm square region by Deep RIE was used. The mold 11 has a concave-convex period of 30 μm, a concave portion width of 20 μm, and a concave portion depth of 80 μm. Further, as the particle dispersion liquid 13, 0.1 g of spherical gold (Au) particles having a diameter of 1.5 μm was used as the material particles 14 in 6 ml of water. Centrifugal filling was performed at an ambient temperature of 4 ° C. and a rotation speed of 40,000 rpm for 1 hour.

遠心充填後の型11の断面の走査型電子顕微鏡(SEM)写真を、図2に示す。図2に示すように、凹部11aに材料粒子14が充填されており、数10μm程度の構造を有する波面制御素子が製造されていることが確認された。なお、製造された波面制御素子は、シリコン製の型11を取り付けたまま、図2に示す状態で、X線干渉計の回折格子として使用することができる。 A scanning electron microscope (SEM) photograph of the cross section of the mold 11 after centrifugation is shown in FIG. As shown in FIG. 2, it was confirmed that the recess 11a is filled with the material particles 14 and that a wavefront control element having a structure of about several tens of μm is manufactured. The manufactured wavefront control element can be used as a diffraction grating of an X-ray interferometer in the state shown in FIG. 2 with the silicon mold 11 attached.

また、33.3keVの単色X線を用い、図2(a)に示す波面制御素子の透過率を測定した。このとき、非対称Bragg反射によって水平方向のビームサイズを拡大することにより、10μmよりも十分に高い空間分解能で測定を行った。波面制御素子の表面側、すなわち型11の凸部の先端側から照射したX線の透過光を、波面制御素子の裏面側から撮影した走査型電子顕微鏡(SEM)写真を、図3(a)に示す。また、図3(a)中の線(図中の上縁付近の横方向に伸びる線)に沿った透過率を求め、図3(b)に示す。 Further, the transmittance of the wavefront control element shown in FIG. 2A was measured using a monochromatic X-ray of 33.3 keV. At this time, by expanding the beam size in the horizontal direction by asymmetric Bragg reflection, the measurement was performed with a spatial resolution sufficiently higher than 10 μm. FIG. 3A is a scanning electron microscope (SEM) photograph of the transmitted light of X-rays emitted from the front surface side of the wavefront control element, that is, the tip end side of the convex portion of the mold 11, taken from the back surface side of the wavefront control element. Shown in. Further, the transmittance along the line in FIG. 3 (a) (the line extending in the lateral direction near the upper edge in the figure) is obtained and shown in FIG. 3 (b).

図3(a)に示すように、波面制御素子の凹凸に対応して、透過光の明暗の縞模様が明瞭に確認された。すなわち、Siが厚くなっている型11の凸部が、X線を多く透過して明るくなっており、材料粒子14が充填されている型11の凹部11aが、X線が透過しにくく、暗くなっていることが確認された。また、図3(b)の透過率の値から、型11の凹部11aへの材料粒子14の体積充填率が75%以上であり、ほぼ最密充填されていることが確認された。 As shown in FIG. 3A, the bright and dark striped pattern of the transmitted light was clearly confirmed corresponding to the unevenness of the wavefront control element. That is, the convex portion of the mold 11 in which Si is thick is brightened by transmitting a large amount of X-rays, and the concave portion 11a of the mold 11 filled with the material particles 14 is difficult to transmit X-rays and is dark. It was confirmed that it was. Further, from the transmittance value in FIG. 3B, it was confirmed that the volume filling rate of the material particles 14 into the recess 11a of the mold 11 was 75% or more, and the packing was almost close-packed.

本発明の実施の形態の波面制御素子の製造方法により、波面制御素子の製造を行った。型11は、10mm角のシリコン製の薄板の表面の、8mm角の領域に、Deep RIEにより、周期的な凹凸を形成したものを使用した。型11は、凹凸の周期が9μm、凹部の幅が平均4.5μm、凹部の深さが約45μmである。また、粒子分散液13は、6mlの水に、材料粒子14として、直径100nmの球状のPt粒子を0.1g入れたものを使用した。また、遠心充填を、周囲の温度を4℃にして、40000rpmの回転数で1時間行った。 The wavefront control element was manufactured by the method for manufacturing the wavefront control element according to the embodiment of the present invention. As the mold 11, a 10 mm square silicon thin plate having periodic irregularities formed in an 8 mm square region by Deep RIE was used. The mold 11 has a concave-convex period of 9 μm, a concave portion width of 4.5 μm on average, and a concave portion depth of about 45 μm. Further, as the particle dispersion liquid 13, 0.1 g of spherical Pt particles having a diameter of 100 nm was used as the material particles 14 in 6 ml of water. Centrifugal filling was performed at an ambient temperature of 4 ° C. and a rotation speed of 40,000 rpm for 1 hour.

遠心充填後の型11の断面の走査型電子顕微鏡(SEM)写真を、図4に示す。図4に示すように、断面を作製したときに材料粒子14が多少こぼれているが、凹部11aに材料粒子14が充填されており、数μm程度の構造を有する波面制御素子が製造されていることが確認された。製造された波面制御素子は、例えば、X線Talbot干渉計のGの回折格子として使用することができる。 A scanning electron microscope (SEM) photograph of the cross section of the mold 11 after centrifugation is shown in FIG. As shown in FIG. 4, the material particles 14 are slightly spilled when the cross section is produced, but the recesses 11a are filled with the material particles 14, and a wavefront control element having a structure of about several μm is manufactured. It was confirmed that. The manufactured wavefront control element can be used, for example, as a G 2 diffraction grating of an X-ray Talbot interferometer.

本発明の実施の形態の波面制御素子の製造方法により、波面制御素子の製造を行った。型11は、10mm角のシリコン製の薄板の表面の、8mm角の領域に、Deep RIEにより、周期的な凹凸を形成したものを使用した。型11は、凹凸の周期が9μm、凹部の幅が平均4.5μm、凹部の深さが約45μmである。また、粒子分散液13は、6mlの水またはエタノールに、材料粒子14として、直径2μm以下の球状の酸化ガドリニウム粒子を0.1g入れたものを使用した。また、遠心充填を、周囲の温度を4℃にして、50000rpmの回転数で1時間行った。 The wavefront control element was manufactured by the method for manufacturing the wavefront control element according to the embodiment of the present invention. As the mold 11, a 10 mm square silicon thin plate having periodic irregularities formed in an 8 mm square region by Deep RIE was used. The mold 11 has a concave-convex period of 9 μm, a concave portion width of 4.5 μm on average, and a concave portion depth of about 45 μm. Further, as the particle dispersion liquid 13, 0.1 g of spherical gadolinium oxide particles having a diameter of 2 μm or less was used as the material particles 14 in 6 ml of water or ethanol. Centrifugal filling was performed at an ambient temperature of 4 ° C. and a rotation speed of 50,000 rpm for 1 hour.

遠心充填後の型11の断面の走査型電子顕微鏡(SEM)写真を、図5に示す。図5に示すように、断面を作製したときに材料粒子14が多少こぼれているが、凹部11aに材料粒子14が充填されており、数μm程度の構造を有する波面制御素子が製造されていることが確認された。製造された波面制御素子は、例えば、中性子Talbot干渉計のGの回折格子として使用することができる。 A scanning electron microscope (SEM) photograph of the cross section of the mold 11 after centrifugation is shown in FIG. As shown in FIG. 5, the material particles 14 are spilled to some extent when the cross section is produced, but the recesses 11a are filled with the material particles 14, and a wavefront control element having a structure of about several μm is manufactured. It was confirmed that. The manufactured wavefront control element can be used, for example, as a G 2 diffraction grating of a neutron Talbot interferometer.

11 型
11a 凹部
12 容器
12a 蓋
13 粒子分散液
14 材料粒子
11 type 11a recess 12 container 12a lid 13 particle dispersion 14 material particles

Claims (9)

周期的に凹凸を有する型を用い、金属元素を含む材料粒子を、遠心充填により前記型の凹部に充填して波面制御素子を製造することを特徴とする波面制御素子の製造方法。 A method for manufacturing a wavefront control element, which comprises using a mold having irregularities periodically and filling the recesses of the mold with material particles containing a metal element by centrifugal filling to manufacture a wavefront control element. 40000rpm以上の回転数で前記遠心充填を行うことを特徴とする請求項1記載の波面制御素子の製造方法。 The method for manufacturing a wavefront control element according to claim 1, wherein the centrifugal filling is performed at a rotation speed of 40,000 rpm or more. 前記型は、前記凹部の深さが10μm以上1000μm以下、前記凹凸の周期が100nm以上100μm以下であり、
前記材料粒子は、直径が5nm以上10μm以下であり、前記凹部に充填可能な大きさを有することを
特徴とする請求項1または2記載の波面制御素子の製造方法。
In the mold, the depth of the concave portion is 10 μm or more and 1000 μm or less, and the period of the unevenness is 100 nm or more and 100 μm or less.
The method for manufacturing a wavefront control element according to claim 1 or 2, wherein the material particles have a diameter of 5 nm or more and 10 μm or less and have a size capable of filling the recesses.
前記遠心充填の後、焼結を行うことを特徴とする請求項1乃至3のいずれか1項に記載の波面制御素子の製造方法。 The method for manufacturing a wavefront control element according to any one of claims 1 to 3, wherein sintering is performed after the centrifugal filling. 前記遠心充填の後、前記材料粒子の融点以上の温度で熱処理を行うことを特徴とする請求項1乃至3のいずれか1項に記載の波面制御素子の製造方法。 The method for manufacturing a wavefront control element according to any one of claims 1 to 3, wherein the heat treatment is performed at a temperature equal to or higher than the melting point of the material particles after the centrifugal filling. 前記材料粒子は、Gdを含む合金粒子、または、主成分としてGdを含む金属酸化物粒子から成り、
前記波面制御素子は、中性子線干渉計の回折格子または中性子Talbot干渉計のGの回折格子であることを
特徴とする請求項1乃至5のいずれか1項に記載の波面制御素子の製造方法。
The material particles are composed of alloy particles containing Gd or metal oxide particles containing Gd as a main component.
The wavefront control element, the manufacturing method of the wavefront control device according to any one of claims 1 to 5, characterized in that a diffraction grating G 2 of the diffraction grating or neutron Talbot interferometer neutron interferometer ..
前記材料粒子は、Pt、Au、Ta、W、Re、PbもしくはBiから成る金属粒子、主成分としてPt、Au、Ta、W、Re、PbもしくはBiを有する合金粒子、または、主成分としてPt、Au、Ta、W、Re、PbもしくはBiの酸化物を有する金属酸化物粒子から成り、
前記波面制御素子は、X線干渉計の回折格子またはX線Talbot干渉計のGの回折格子であることを
特徴とする請求項1乃至5のいずれか1項に記載の波面制御素子の製造方法。
The material particles are metal particles composed of Pt, Au, Ta, W, Re, Pb or Bi, alloy particles having Pt, Au, Ta, W, Re, Pb or Bi as main components, or Pt as main components. , Au, Ta, W, Re, Pb or Bi, composed of metal oxide particles having oxides.
The wavefront control element, the manufacture of the wavefront control device according to any one of claims 1 to 5, characterized in that a diffraction grating G 2 of the diffraction grating or X-ray Talbot interferometer X-ray interferometer Method.
前記材料粒子は、Gd基、Sm基、Eu基、Dy基、Pt基、Au基、Pd基またはNi基の金属ガラス粒子から成り、
前記波面制御素子は、中性子線干渉計もしくはX線干渉計の回折格子、または、中性子Talbot干渉計もしくはX線Talbot干渉計のGの回折格子であることを
特徴とする請求項1乃至5のいずれか1項に記載の波面制御素子の製造方法。
The material particles are composed of Gd group, Sm group, Eu group, Dy group, Pt group, Au group, Pd group or Ni group metallic glass particles.
The wavefront control element is a diffraction grating of a neutron beam interferometer or an X-ray interferometer, or a G 2 diffraction grating of a neutron Talbot interferometer or an X-ray Talbot interferometer. The method for manufacturing a wavefront control element according to any one item.
前記遠心充填の後、前記材料粒子が充填された前記凹部を覆うよう金属ガラスリボンを敷設し、熱処理を行うことを特徴とする請求項1乃至8のいずれか1項に記載の波面制御素子の製造方法。


The wavefront control element according to any one of claims 1 to 8, wherein a metallic glass ribbon is laid so as to cover the recess filled with the material particles after the centrifugal filling, and heat treatment is performed. Production method.


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