JPH0422218B2 - - Google Patents
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- Publication number
- JPH0422218B2 JPH0422218B2 JP58201573A JP20157383A JPH0422218B2 JP H0422218 B2 JPH0422218 B2 JP H0422218B2 JP 58201573 A JP58201573 A JP 58201573A JP 20157383 A JP20157383 A JP 20157383A JP H0422218 B2 JPH0422218 B2 JP H0422218B2
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- Prior art keywords
- polycrystalline body
- diffraction
- sample
- optical system
- intensity
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Description
【発明の詳細な説明】
本発明はＸ線あるいは粒子線ビーム（以下これ
を総称してＸ線と言う）を用いて多結晶体の結晶
粒子状態の検出測定装置に関する。更に詳しくは
多結晶体を構成する結晶粒子の形、大きさ、配向
性、充填度、分散状態等の結晶粒子状態を検出測
定する装置に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for detecting and measuring the crystal grain state of a polycrystalline body using X-rays or particle beams (hereinafter collectively referred to as X-rays). More specifically, the present invention relates to an apparatus for detecting and measuring crystal grain states such as shape, size, orientation, filling degree, and dispersion state of crystal grains constituting a polycrystalline body.
多結晶体の結晶粒子の空間的な分布状態、及び
温度、圧力等の変化による動的な状態変化等の情
報は、膜状、板状、柱状等の多結晶体を連続的に
製造する場合、また、膜状、板状、柱状の多結晶
体及び複合材料の検査、結晶構造の同定、構造解
析等に極めて有用である。従来、結晶粒子の形
状、大きさ等を検べる方法としては、光学顕微鏡
法、電子顕微鏡法、ふるい法、沈降法等種々な方
法がある。またその配向性を検べる方法としては
極点図形法、充填度を検べる方法としては比重
法、結晶粒子の分布状態を総合的に検べる方法と
しては粉末デフラクトメータ法がある。 Information on the spatial distribution of crystal grains of polycrystals and dynamic changes in state due to changes in temperature, pressure, etc. is required when continuously manufacturing polycrystals in the form of films, plates, columns, etc. It is also extremely useful for inspecting film-like, plate-like, and columnar polycrystals and composite materials, identifying crystal structures, and analyzing structures. Conventionally, there are various methods for examining the shape, size, etc. of crystal particles, such as optical microscopy, electron microscopy, sieving method, and sedimentation method. A method for examining the orientation is the pole figure method, a method for determining the degree of filling is the specific gravity method, and a method for comprehensively examining the distribution state of crystal particles is the powder defractometer method.
しかし、光学顕微鏡法、電子顕微鏡法、ふるい
法、沈降法においては、適切な分散剤がない場合
は、二次粒子の形・大きさであることが多い。ま
た一次粒子であつても、Ｘ線的形・大きさでない
ことが多い。すなわち、光学的に観測された外観
的粒子の形・大きさと、Ｘ線的に回折された結晶
粒子の形・大きさと異なる。 However, in optical microscopy, electron microscopy, sieving methods, and sedimentation methods, in the absence of an appropriate dispersant, the shape and size of secondary particles are often used. Furthermore, even if they are primary particles, they often do not have the shape and size of an X-ray. In other words, the shape and size of the external grains observed optically are different from the shape and size of the crystal grains diffracted by X-rays.
また極点図形法は多結晶体の組織の研究あるい
は検査上で精密な極点図形を求めるために開発さ
れたものであり、そのために種々の制約がある。
すなわち、多結晶体の結晶粒子の配向性（極点図
形）の角度制度を上げるためには、入射Ｘ線をで
きる限り細める必要があり、発散Ｘ線の場合でも
その縦方向の発散はできる限り抑える必要があ
る。従つて回折線の反射強度は弱く、測定には長
時間を必要とするばかりでなく、弱い反射強度の
回折線の測定は不可能である。また、その使用は
吸収因子の補正をできる限り避け得られる場合、
あるいはその補正を簡単に処理可能な場合に限ら
れていた。しかも、この吸収因子の補正は試料そ
れ自身配向性のない条件で正確に測定する必要が
ある。さらに、極点図形の全角度範囲を測定する
ためには、単結晶デフラクトメータのような複雑
な動きをさせる機構及び計算処理装置を必要と
し、また結晶粒子形・大きさの影響をさけるため
に、その回折線の強度を平均化するための駆動機
構を必要とする。 Furthermore, the pole figure method was developed to obtain precise pole figures for research or inspection of the structure of polycrystalline bodies, and therefore has various limitations.
In other words, in order to improve the angular accuracy of the crystal grain orientation (pole figure) of a polycrystal, it is necessary to narrow the incident X-rays as much as possible, and even in the case of divergent X-rays, the vertical divergence must be suppressed as much as possible. There is a need. Therefore, the reflection intensity of the diffraction line is weak, and not only does measurement require a long time, but also it is impossible to measure a diffraction line with a weak reflection intensity. In addition, its use can be avoided as much as possible from correction of absorption factors,
Otherwise, it was limited to cases where the correction could be easily processed. Furthermore, correction of this absorption factor requires accurate measurement under conditions where the sample itself has no orientation. Furthermore, in order to measure the entire angular range of the polar figure, a complicated movement mechanism such as a single-crystal defractometer and a calculation processing device are required, and in order to avoid the influence of crystal grain shape and size, , requires a driving mechanism to average the intensity of the diffraction lines.
従つて、多結晶体を連続的に製造する際、結晶
粒子の状態を同時に測定したり、あるいは多結晶
体の連続的な検査等には従来の極点図形法を適用
することは不可能である。 Therefore, when polycrystals are continuously produced, it is impossible to simultaneously measure the state of crystal grains or to apply the conventional pole figure method to continuous inspection of polycrystals. .
従来の粉末デフラクトメータ法は、試料の回転
角θに対して回折線の検出器を２倍の回転角2θで
相対的に同時に回転させ、2θに対する回折線の強
度の変化を測定する方法である。この粉末デフラ
クトメータ法はこれによる回折線の強度には多結
晶体の結晶粒子分布状態のすべてが反映してく
る。従つて結晶構造が既知たるいは推定される多
結晶体試料以外の結晶粒子の分布状態の情報を分
離することが困難で、また分離された情報を推定
するには膨大な計算処理を必要とする。また、そ
の回折線の半価幅から求められる結晶粒子の大き
さの範囲は凡そ200Å〜1μｍであり、それ以上の
結晶粒子の大きさは求められない。 The conventional powder defractometer method is a method in which the diffraction line detector is simultaneously rotated at twice the rotation angle 2θ relative to the rotation angle θ of the sample, and the change in the intensity of the diffraction line with respect to 2θ is measured. be. In this powder defractometer method, the intensity of the diffraction line reflects all the crystal grain distribution states of the polycrystalline body. Therefore, it is difficult to separate information on the distribution state of crystal particles in samples other than polycrystalline samples whose crystal structures are known or estimated, and estimating the separated information requires extensive computational processing. do. Further, the range of the crystal grain size determined from the half width of the diffraction line is approximately 200 Å to 1 μm, and a larger crystal grain size cannot be determined.
本発明の目的は前記のような従来法における各
種の欠点を取除き、集中法の長所、すなわち、回
折線を集中させることにより強い反射強度を得る
ようにして、測定時間の短縮の弱い反射強度の回
折線の測定を可能にし、また、多結晶体材料を破
壊することなく、それを相対的に回転、移動させ
ることにより、結晶粒子の回転及び移動方向に対
する分布状態及びその他結晶粒子の状態を分離し
て正確に検出測定し得られる検出測定装置を提供
するにある。 The purpose of the present invention is to eliminate the various drawbacks of the conventional methods as described above, and to utilize the advantages of the concentration method, that is, to obtain a strong reflection intensity by concentrating the diffraction lines, thereby reducing the measurement time and reducing the weak reflection intensity. Also, by relatively rotating and moving the polycrystalline material without destroying it, it is possible to measure the distribution state of the crystal grains in the direction of rotation and movement, as well as other states of the crystal grains. The object of the present invention is to provide a detection and measurement device that can perform separate and accurate detection and measurement.
本発明の要旨は多結晶体に発散するＸ線あるい
は粒子線の線束を照射して、多結晶体からの回折
線の中で受光スリツトに集束する線束のみを検出
する光学系において、この光学系をブラツグ条件
を満たす位置に固定し、この光学系と多結晶体と
を相対的に回転、回転振動、並進及び三次元的に
移動させることによつて得られる回折線の強度及
びその変化を空間的、方位的及び時間的に検出
し、測定して、多結晶体中に含まれる結晶粒の大
きさ、方位及び充填率の分布状態を解析し得るよ
うに構成したことを特徴とする多結晶体の結晶粒
子状態の検出測定装置にある。 The gist of the present invention is to provide an optical system that irradiates a polycrystal with a divergent beam of X-rays or particle beams and detects only the beam of diffraction rays from the polycrystal that is focused on a light receiving slit. is fixed at a position that satisfies the bragg condition, and the intensity of the diffraction lines obtained by rotating, rotationally vibrating, translating, and three-dimensionally moving this optical system and the polycrystalline body relative to each other is calculated spatially. A polycrystal, characterized in that the polycrystal is configured to be able to detect and measure the size, orientation, and filling rate of crystal grains contained in the polycrystal body by detecting and measuring the target, orientation, and time. It is a device for detecting and measuring the state of crystal particles in the body.
本発明の装置を図面を基いて説明する。 The apparatus of the present invention will be explained based on the drawings.
第１図及び第２図は本発明の装置の概要図あ
り、第１図ａは反射法、ｃは透過法である。ａ，
ｃにおいては、検出器３は検出する結晶粒子に特
有のブラツグ反射条件の位置2θBに設け、多結晶
体材料１（以下試料と略記する。）を回転α及び
移動ｘさせて、これに対する回折線の強度の変化
を測定する。ｂはａの特殊の場合で、従来の粉末
デフラクトメータを用い、ブラツグ角2θBに設け、
試料１の回転方向としてデフラクトメータの回転
方向すなわち、θ回転する反射法である。 1 and 2 are schematic diagrams of the apparatus of the present invention, in which FIG. 1a shows a reflection method and FIG. 1c shows a transmission method. a,
In c, the detector 3 is installed at a position 2θ B with Bragg reflection conditions specific to the crystal grain to be detected, and the polycrystalline material 1 (hereinafter abbreviated as the sample) is rotated α and moved x to detect the diffraction for this. Measure the change in intensity of the line. b is a special case of a, using a conventional powder defractometer, installed at Bragg angle 2θ B ,
This is a reflection method in which the rotation direction of the sample 1 is the rotation direction of the defractometer, that is, θ rotation.
試料１の回転軸として、第２図に示すように、
Ａ軸及びＣ軸を互に直交するように、試料表面に
取り、この表面の法線方向にＢ軸を取る。また入
射Ｘ線の中心線と回折Ｘ線の中心線を含む面（以
下光線面と言う）内に、入射Ｘ線の中心線と回折
Ｘ線の中心線のなす角の２等分線をＸ線、これに
直交する軸をＹ軸とし、光線面の法線方向をＺ軸
とする。 As the rotation axis of sample 1, as shown in Fig. 2,
The A-axis and the C-axis are taken on the sample surface so that they are perpendicular to each other, and the B-axis is taken in the normal direction of this surface. In addition, in a plane containing the center line of the incident X-ray and the center line of the diffracted X-ray (hereinafter referred to as the ray plane), a bisector of the angle formed by the center line of the incident X-ray and the center line of the diffracted The axis perpendicular to this line is the Y axis, and the normal direction to the light beam plane is the Z axis.
なお、本発明の場合、多結晶体の回転軸として
は、任意に取ることができるが、Ａ軸をＺ軸、Ｂ
軸をＸ軸、あるいはＣ軸をＹ軸にとると、装置上
及び解析上容易で便利である。特に回転させなが
ら結晶成長させる多結晶膜の製造の場合、回転軸
としてＢ軸をとり、Ｘ軸と一致させると、装置と
しては端的に言えばＸ線源と検出装置のみがあれ
ばよい。そして本発明におけるα回転（任意軸）
及びｘ移動（試料面内の任意方向）の速さは、回
折Ｘ線の強度の変化に追従できる速さである。ま
た多結晶体試料を厚さ方向への微動（Δt）、ある
いは受光スリツト系を微動（Δ2θ）することによ
り、厚さ方向の結晶粒子分布状態を検出すること
ができる。 In the case of the present invention, the rotation axis of the polycrystalline body can be arbitrarily selected, but the A-axis may be the Z-axis, the B-axis may be
Setting the axis as the X axis or the C axis as the Y axis is easy and convenient for equipment and analysis. In particular, in the case of manufacturing a polycrystalline film in which crystals are grown while rotating, if the B-axis is used as the rotation axis and is aligned with the X-axis, simply speaking, only an X-ray source and a detection device are required as equipment. And α rotation (arbitrary axis) in the present invention
The speed of x movement (in any direction within the sample plane) is such that it can follow changes in the intensity of the diffracted X-rays. Furthermore, by slightly moving the polycrystalline sample in the thickness direction (Δt) or by slightly moving the light receiving slit system (Δ2θ), the state of crystal grain distribution in the thickness direction can be detected.
本発明の装置を使用して各種原料を検出測定し
た試験結果を次に示す。 Test results obtained by detecting and measuring various raw materials using the apparatus of the present invention are shown below.
試験例 １
市販の20μｍのSi粉末のθ回転及び平行移動に
よる回折線の強度変化を示すと第３図ａ及び第３
図ｂの通りであつた。試料中の結晶粒子分布状態
は第３図ｃの通りであつた。回折線の強度変化の
図より、この試料には20μｍの結晶粒子の中に比
較的大きい90μｍ以下の結晶粒子が所々に存在し
ていることがわかる。Test Example 1 Figures 3a and 3 show the intensity changes of diffraction lines due to θ rotation and parallel movement of commercially available 20 μm Si powder.
It was as shown in Figure b. The crystal grain distribution state in the sample was as shown in FIG. 3c. From the diagram of the intensity change of the diffraction line, it can be seen that relatively large crystal particles of 90 μm or less are present in some places among the 20 μm crystal grains in this sample.
第３図ａは粒度20μｍのSiの111回折線の強度の
任意の場所における方位変化を示している。この
回折曲線の中で比較的大きな振れ或いはピークは
試料中に含まれる粒度90μｍのSi結晶粒子に起因
することが同試料のSEM（走査型電子顕微鏡）像
から判断することができる。そして、そのピーク
の角度からその結晶粒子の反射面１１１の試料表
面からの偏りの角度εはε＝θ−θBとして見積も
ることができる。更に、微細な粉末による平均の
回折曲線は測定条件と回折角のみに依存し、試料
によらないので、その予想される回折曲線からの
測定された平均回折曲線の異常は充填率の方位異
常と判断することができる。その系統的な方位異
常は試料の選択配向であり、その角度依存性を算
出することができる。 Figure 3a shows the change in orientation of the intensity of the 111 diffraction line of Si with a particle size of 20 μm at any location. It can be determined from the SEM (scanning electron microscope) image of the sample that the relatively large deviation or peak in this diffraction curve is caused by Si crystal particles with a particle size of 90 μm contained in the sample. Then, from the angle of the peak, the angle ε of the deviation of the reflecting surface 111 of the crystal particle from the sample surface can be estimated as ε=θ−θ B. Furthermore, since the average diffraction curve for fine powders depends only on the measurement conditions and diffraction angles, and not on the sample, anomalies in the measured average diffraction curve from its expected diffraction curve are likely to be an azimuthal anomaly in the filling factor. can be judged. The systematic orientation anomaly is the preferred orientation of the sample, and its angular dependence can be calculated.
また、第３図ｂはε＝０の場合の粒度20μｍの
Siの111回折線の強度の結晶粒子の大きさと充填
率の異常の一次元分布を示している。この激しい
振れの中で、鋭いピークは大きな結晶粒子の存在
を、谷は不存在を示している。 In addition, Fig. 3b shows the particle size of 20 μm when ε=0.
The 111 diffraction line intensity of Si shows a one-dimensional distribution of anomalies in crystal grain size and filling factor. In this violent swing, sharp peaks indicate the presence of large crystal grains, and valleys indicate their absence.
試験例 ２
マダガスカル産の２mmφ以下の鱗片状グラフア
イトのθ回転及び平行移動による回折線の強度変
化を示すと、第４図ａ及び第４図ｂの通りであつ
た。試料中の結晶粒子の分布状態は第４図ｃの通
りであつた。第４図ｂは選択配向の一次元的異常
を示している。この鋭いピークはマダガスカル産
グラフアイト試料中の大きな結晶粒子に起因して
いる。回折線の強度変化の図より、この試料中の
結晶粒子の厚さは1000Å以下で、湾曲しているこ
とがわかる。また配向性は試料表面に平行に分布
し、その分布函数を（１−Cε2）-1と仮定する（但
し、ε＝θ−θBである。）とＣは0.047であること
がわかる。Test Example 2 Figures 4a and 4b show changes in the intensity of diffraction lines due to θ rotation and parallel movement of scale-like graphite with a diameter of 2 mm or less from Madagascar. The distribution of crystal particles in the sample was as shown in FIG. 4c. Figure 4b shows a one-dimensional anomaly in preferred orientation. This sharp peak is due to large crystal grains in the graphite sample from Madagascar. The diagram of the intensity change of the diffraction line shows that the crystal grains in this sample have a thickness of less than 1000 Å and are curved. Further, the orientation is distributed parallel to the sample surface, and assuming that the distribution function is (1-Cε 2 ) -1 (where ε=θ-θ B ), it is found that C is 0.047.
なお、走査角度範囲±εを小さくして、試験例
１の第３図ａおよび試験例２の第４図ｂに示すよ
うなε走査法（θ走査法）を繰り返すことによつ
て、時間的および温度・圧力・雰囲気依存性を
“その場観察”することができる。 In addition, by decreasing the scanning angle range ±ε and repeating the ε scanning method (θ scanning method) as shown in FIG. 3a of Test Example 1 and FIG. 4B of Test Example 2, the temporal In addition, temperature, pressure, and atmosphere dependence can be observed “on the spot.”
また、上記試験例では、一次元分布像のみを示
したが、吸収係数の大きい試料では、それを二次
元的に移動すれば、その試料表面の二次元分布が
得られ、吸収係数の小さい試料では、それを三次
元的に移動すれば、空間的な分布が得られる。 In addition, in the above test example, only a one-dimensional distribution image was shown, but for a sample with a large absorption coefficient, if you move it two-dimensionally, you can obtain a two-dimensional distribution image on the sample surface. Now, if we move it three-dimensionally, we can obtain a spatial distribution.
このように、この方法による回折線の強度の異
常から、結晶粒子の充填状態の異常は容易に観察
することが可能であり、かつ、その原因の追及は
容易であるので、この方法は、単に粉末Ｘ線回折
計の試料の評価のみならず、一般の多結晶体を充
填状態の評価に使用できる。しかし、この方法の
みでは、上記回折線の異常から結晶粒子の大きさ
と充填率の異常を定量化することは困難であるの
で、試験例１、試験例２において光学顕微鏡像又
はSEM像と比較したように、光学顕微鏡、透過
型電子顕微鏡、走査型電子顕微鏡（SEM）、粒度
測定装置、篩、比重計等の他の方法と併用するこ
とにより、可能であり、容易である。 In this way, abnormalities in the packing state of crystal grains can be easily observed from abnormalities in the intensity of diffraction lines obtained by this method, and it is easy to investigate the cause. In addition to evaluating samples using a powder X-ray diffractometer, general polycrystals can be used to evaluate the filling state. However, using this method alone, it is difficult to quantify the abnormalities in crystal grain size and filling rate from the above-mentioned abnormalities in the diffraction lines, so in Test Examples 1 and 2, comparisons with optical microscope images or SEM images This is possible and easy by using in conjunction with other methods such as an optical microscope, transmission electron microscope, scanning electron microscope (SEM), particle size measuring device, sieve, hydrometer, etc.
以上のように、本発明の装置によると、多結晶
体の結晶粒子の大きさ、形態は勿論、連続的にそ
の分布状態等を正確に検出し得られる優れた効果
を奏し得られる。 As described above, according to the apparatus of the present invention, it is possible to achieve the excellent effect of accurately detecting not only the size and form of crystal grains of a polycrystalline body but also their distribution state continuously.
第１図及び第２図は本発明装置の概要図で、第
１図ａは反射法、第１図ｂは第１図ａの変形、第
１図ｃは透過法の図、第２図は多結晶体試料の回
転・移動説明図、第３図及び第４図は本発明装置
の使用による各試料の試験結果図で、それぞれ、
ａ，ｂはθ回転及び平行移動による回折線の強度
変化図、ｃは結晶粒子の分布図を示す。
１：多結晶体材料、２：Ｘ線源、３：検出器、
４，５：発散スリツト及び受光スリツト、６：ソ
ーラスリツト。
Figures 1 and 2 are schematic diagrams of the apparatus of the present invention, where Figure 1a is a reflection method, Figure 1b is a modification of Figure 1a, Figure 1c is a transmission method, and Figure 2 is a diagram of a transmission method. Explanatory diagrams of rotation and movement of polycrystalline samples, Figures 3 and 4 are diagrams of test results of each sample using the device of the present invention, respectively.
a and b show intensity changes of diffraction lines due to θ rotation and translation, and c shows a distribution chart of crystal particles. 1: polycrystalline material, 2: X-ray source, 3: detector,
4, 5: Divergent slit and light receiving slit, 6: Solar slit.
Claims (1)
束を照射して、多結晶体からの回折線の中で受光
スリツトに集束する線束のみを検出する光学系に
おいて、この光学系をブラツグ条件を満たす位置
に固定し、この光学系と多結晶体とを相対的に回
転、回転振動、並進及び三次元的に移動させるこ
とによつて得られる回折線の強度及びその変化を
空間的、方位的及び時間的に検出し、測定して、
多結晶体中に含まれる結晶粒の大きさ、方位及び
充填率の分布状態を解析し得るように構成したこ
とを特徴とする多結晶体の結晶粒子状態の検出測
定装置。1. In an optical system that irradiates a polycrystal with a divergent X-ray or particle beam and detects only the diffraction rays from the polycrystal that are focused on the receiving slit, this optical system is set under bragging conditions. The intensity of the diffraction lines obtained by fixing the optical system and the polycrystalline body at a position where the polycrystalline body satisfies the requirements, and moving the optical system and the polycrystalline body relative to each other in rotation, rotational vibration, translation, and three dimensions is measured spatially and azimuthally. and temporally detecting and measuring,
1. A detection and measurement device for the state of crystal grains in a polycrystalline body, characterized in that it is configured to analyze the distribution state of the size, orientation, and filling rate of crystal grains contained in the polycrystalline body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58201573A JPS6093335A (en) | 1983-10-27 | 1983-10-27 | Detection and measurement device for crystal grain state of polycrystalline material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58201573A JPS6093335A (en) | 1983-10-27 | 1983-10-27 | Detection and measurement device for crystal grain state of polycrystalline material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6093335A JPS6093335A (en) | 1985-05-25 |
| JPH0422218B2 true JPH0422218B2 (en) | 1992-04-16 |
Family
ID=16443297
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58201573A Granted JPS6093335A (en) | 1983-10-27 | 1983-10-27 | Detection and measurement device for crystal grain state of polycrystalline material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6093335A (en) |
Cited By (2)
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|---|---|---|---|---|
| WO2013150758A1 (en) * | 2012-04-04 | 2013-10-10 | 信越化学工業株式会社 | Method for evaluating degree of crystal orientation in polycrystalline silicon, selection method for polycrystalline silicon rods, and production method for single-crystal silicon |
| WO2013190829A1 (en) * | 2012-06-18 | 2013-12-27 | 信越化学工業株式会社 | Polycrystalline silicon crystal orientation degree evaluation method, polycrystalline silicon rod selection method, polycrystalline silicon rod, polycrystalline silicon ingot, and polycrystalline silicon fabrication method |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63139238A (en) * | 1986-12-01 | 1988-06-11 | Natl Inst For Res In Inorg Mater | Simple one-dimensional scanning X-ray diffraction microscope |
| JPS63139298A (en) * | 1986-12-01 | 1988-06-11 | 科学技術庁無機材質研究所長 | Simple one-dimensional scanning X-ray diffraction microscope with monochromator |
| JPH0727080B2 (en) * | 1986-12-02 | 1995-03-29 | 科学技術庁無機材質研究所長 | One-dimensional scanning X-ray diffraction microscope |
| JPH04164239A (en) * | 1990-10-26 | 1992-06-09 | Natl Inst For Res In Inorg Mater | Powder x-ray diffraction meter |
| JP2904055B2 (en) * | 1995-05-30 | 1999-06-14 | 株式会社島津製作所 | X-ray diffractometer |
| NL1009012C2 (en) | 1998-04-28 | 1999-10-29 | Stichting Tech Wetenschapp | Method for determining cell parameters of a crystal structure by diffraction. |
| CN100485373C (en) * | 2004-07-14 | 2009-05-06 | 西南技术工程研究所 | Short wave length X-ray diffraction measuring device and method |
| JP5903900B2 (en) * | 2012-01-16 | 2016-04-13 | 住友金属鉱山株式会社 | Particle abundance ratio calculation method and particle crystal size calculation method |
| JP5923463B2 (en) * | 2013-06-26 | 2016-05-24 | 信越化学工業株式会社 | Method for evaluating crystal grain size distribution of polycrystalline silicon, method for selecting polycrystalline silicon rod, polycrystalline silicon rod, polycrystalline silicon lump, and method for producing single crystalline silicon |
| EP2818851B1 (en) * | 2013-06-26 | 2023-07-26 | Malvern Panalytical B.V. | Diffraction Imaging |
-
1983
- 1983-10-27 JP JP58201573A patent/JPS6093335A/en active Granted
Cited By (4)
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|---|---|---|---|---|
| WO2013150758A1 (en) * | 2012-04-04 | 2013-10-10 | 信越化学工業株式会社 | Method for evaluating degree of crystal orientation in polycrystalline silicon, selection method for polycrystalline silicon rods, and production method for single-crystal silicon |
| WO2013190829A1 (en) * | 2012-06-18 | 2013-12-27 | 信越化学工業株式会社 | Polycrystalline silicon crystal orientation degree evaluation method, polycrystalline silicon rod selection method, polycrystalline silicon rod, polycrystalline silicon ingot, and polycrystalline silicon fabrication method |
| CN104395740A (en) * | 2012-06-18 | 2015-03-04 | 信越化学工业株式会社 | Polycrystalline silicon crystal orientation evaluation method, polycrystalline silicon rod selection method, polycrystalline silicon rod, polycrystalline silicon block, and single crystal silicon manufacturing method |
| US9274069B2 (en) | 2012-06-18 | 2016-03-01 | Shin-Etsu Chemical Co., Ltd. | Method for evaluating degree of crystalline orientation of polycrystalline silicon, method for selecting polycrystalline silicon rod, polycrystalline silicon rod, polycrystalline silicon ingot, and method for manufacturing monocrystalline silicon |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6093335A (en) | 1985-05-25 |
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