JP2674506B2 - X-ray diffractometer - Google Patents
X-ray diffractometerInfo
- Publication number
- JP2674506B2 JP2674506B2 JP6116403A JP11640394A JP2674506B2 JP 2674506 B2 JP2674506 B2 JP 2674506B2 JP 6116403 A JP6116403 A JP 6116403A JP 11640394 A JP11640394 A JP 11640394A JP 2674506 B2 JP2674506 B2 JP 2674506B2
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- sample
- ray
- diffraction
- monochromator
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000013078 crystal Substances 0.000 claims description 92
- 238000000034 method Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000008400 supply water Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は結晶学的評価に用いるＸ
線回折装置の改良、改善に関するものである。The present invention relates to X used for crystallographic evaluation.
The present invention relates to improvement and improvement of a line diffraction device.
【０００２】[0002]
【従来の技術】試料結晶である第２結晶と格子面間隔が
ほぼ等しい結晶を第１結晶として用いる二結晶Ｘ線回折
法は、格子歪を回折位置のずれ、反射率の変化として検
出するものである。格子歪に関する信頼性のある情報を
知ることは、極めて重要な問題であり、特に、大面積で
ある材料を取り扱う現在の半導体工業の分野において
は、迅速でかつ非破壊で材料試験を行う必要から、他の
試験法に比較して、非常に有力な試験、評価手段である
として用いられている。2. Description of the Related Art A two-crystal X-ray diffraction method using a crystal having a lattice spacing substantially equal to that of a second crystal, which is a sample crystal, as a first crystal detects a lattice strain as a deviation of a diffraction position and a change of reflectance. Is. Knowing reliable information on lattice strain is a very important issue, especially in the field of the current semiconductor industry dealing with large-area materials, because of the need for rapid and non-destructive material testing. , Is used as a very powerful test and evaluation method compared to other test methods.
【０００３】図２は水平軸型二結晶Ｘ線回折装置を説明
するために用いた回折装置の正面図を模式的に表わした
図面である。Ｘ線源１から出たＸ線ビーム２は第１結晶
４と試料結晶５とで回折してＸ線検出器９で検出され
る。二結晶法では第１結晶４と試料結晶５とに格子面間
隔が等しいものを用いて、第１結晶４とＸ線検出器９と
を固定して試料結晶５を回転中心７の周りで微小角度だ
け回転させて回折パターンを測定する。この回折パター
ンは格子定数の局所的な微小変化や格子面の微小な傾き
に非常に敏感であるため、この回折パターンから試料結
晶の格子歪を評価することが可能である。この測定法で
は、試料結晶５を試料台６に取り付けるときに試料結晶
５に余分な力が加わると試料結晶５に歪が生じ、測定精
度が悪くなるので、試料を無歪で保持することが重要で
ある。そこで従来は、試料結晶を試料台に取り付けるの
に接着力の弱いエレクトロンワックスやマニキュア液を
使用するか、磁石で試料結晶の外周部を支えるようにし
ていた（例えば、特開平３−３９６４３参照）。しかし
ながら、このように試料取り付け法を工夫しても依然と
して試料結晶にはわずかな歪が生じ、測定精度の悪化を
完全には防げていない。FIG. 2 is a diagram schematically showing a front view of a diffracting device used for explaining a horizontal axis type double crystal X-ray diffracting device. The X-ray beam 2 emitted from the X-ray source 1 is diffracted by the first crystal 4 and the sample crystal 5 and detected by the X-ray detector 9. In the two-crystal method, the first crystal 4 and the sample crystal 5 having the same lattice spacing are used, and the first crystal 4 and the X-ray detector 9 are fixed so that the sample crystal 5 is fine around the rotation center 7. Rotate by an angle and measure the diffraction pattern. The diffraction pattern for a very sensitive to small inclination of the local small change and lattice plane of the lattice constant, it is possible to evaluate the lattice strain of the sample crystal from the diffraction pattern. In this measurement method, when the sample crystal 5 is attached to the sample stage 6, when an excessive force is applied to the sample crystal 5, the sample crystal 5 is distorted and the measurement accuracy is deteriorated. Therefore, the sample can be held without distortion. is important. Therefore, conventionally, an electron wax or a nail varnish having a weak adhesive force is used to attach the sample crystal to the sample table, or a magnet is used to support the outer peripheral portion of the sample crystal (see, for example, JP-A-3-39643). . However, even if the sample attachment method is devised in this way, a slight strain still occurs in the sample crystal, and the deterioration of the measurement accuracy cannot be completely prevented.
【０００４】このような問題を解決するために、試料面
を水平に保持できる二結晶法回折装置が提供されてい
る。この方式の二結晶法回折装置は図３に示すように、
水平に保たれた試料台６に試料結晶５を自重によって乗
せるだけで保持する部分と、試料表面上の回転中心７を
中心に、Ｘ線管１０と第１結晶４との角度関係を変えな
いように回動する部分、および回折ビーム８を検出する
ために回転中心７を中心にＸ線検出器９を回動する部分
から成っている（例えば、特開平４−１２１６４９参
照）。In order to solve such a problem, a two-crystal method diffracting device which can hold the sample surface horizontally has been provided. As shown in FIG. 3, the double crystal diffractometer of this system is
The angular relationship between the X-ray tube 10 and the first crystal 4 is not changed centering on the rotation center 7 on the surface of the sample and the part where the sample crystal 5 is held by the sample table 6 held horizontally by its own weight. The X-ray detector 9 rotates about the rotation center 7 to detect the diffracted beam 8 (see, for example, Japanese Patent Laid-Open No. 4-121649).
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、上記の
水平軸型二結晶Ｘ線回折装置では、試料を試料台に取り
付けるので試料結晶に歪が生じ易く、測定精度が悪化す
るという欠点がある。また、上記の試料面を水平に保持
できる二結晶法回折装置ではＸ線管１０はかなり大きく
重い上、高電圧ケーブルやターゲット冷却用供給水管が
接続されており、このような物を水平軸によって回動さ
せるには、その調節機構を頑丈にかつ精度よく作らなけ
ればならず、製作費が高くなるのは避けられないという
欠点がある。However, in the above-mentioned horizontal axis type double crystal X-ray diffractometer, since the sample is mounted on the sample stage, the sample crystal is apt to be distorted and the measurement accuracy is deteriorated. Further, in the above-mentioned double-crystal method diffractometer capable of holding the sample surface horizontally, the X-ray tube 10 is considerably large and heavy, and a high voltage cable and a target cooling supply water pipe are connected. In order to rotate, the adjusting mechanism must be made robust and accurate, and the manufacturing cost is inevitable.
【０００６】本発明の目的は、Ｘ線管を動かすことな
く、かつ、試料を無歪で保持できるＸ線回折装置を提供
することにある。An object of the present invention is to provide an X-ray diffractometer capable of holding a sample without strain without moving the X-ray tube.
【０００７】[0007]
【課題を解決するための手段】本発明は、試料結晶であ
る第２結晶と格子面間隔がほぼ等しい第１結晶を有する
水平軸型二結晶Ｘ線回折装置において、Ｘ線源から第１
結晶に至るまでのＸ線経路の途中に第１結晶のほぼ半分
の角度で回折を起こすモノクロメータ結晶を配置して、
Ｘ線源からのＸ線をモノクロメータ結晶、第１結晶、及
び第２結晶で順に回折させるようにしたことを特徴とす
る。モノクロメータ結晶としては、試料結晶と同じ結晶
または異なる結晶を用いることができる。The present invention provides a horizontal-axis double-crystal X-ray diffractometer having a first crystal whose lattice spacing is substantially equal to that of a second crystal which is a sample crystal.
A monochromator crystal that causes diffraction at an angle that is almost half that of the first crystal is placed in the middle of the X-ray path to reach the crystal.
It is characterized in that X-rays from the X-ray source are sequentially diffracted by the monochromator crystal, the first crystal, and the second crystal. As the monochromator crystal, the same crystal as the sample crystal or a different crystal can be used.
【０００８】[0008]
【作用】このモノクロメータ結晶を備えることにより、
Ｘ線管を動かすことなく、試料結晶をほぼ水平の状態で
保持することが可能となり、試料結晶を固定することな
く自重によって試料台に置くだけで回折強度曲線を得る
ことができるようになる。[Operation] By providing this monochromator crystal,
The sample crystal can be held in a substantially horizontal state without moving the X-ray tube, and the diffraction intensity curve can be obtained simply by placing the sample crystal on the sample table by its own weight without fixing it.
【０００９】[0009]
【実施例】以下、本発明について図面を用いて説明す
る。図１は本発明の一実施例のＸ線回折装置の断面を模
式的に示した図面である。Ｘ線源１から発生するＸ線ビ
ーム２は、ほぼθB ／２の回折角度で回折を起こすよう
に設計されているモノクロメータ結晶３により水平から
θB の角度だけ上方にはね上げられる。その後Ｘ線ビー
ム２は試料結晶と等しい回折面を持つ第１結晶４により
回折角θB で回折し、試料結晶５に入射する。この時、
試料結晶の回折面を結晶表面とほぼ平行な回折面を選
ぶ。そのように回折面を選べば試料結晶５は、ほぼ水平
に置かれた試料台６に置くだけで回折条件を満足するよ
うにできる。回折強度曲線の角度幅は一般的には０．５
°以内であるので、従来のように試料結晶を固定するこ
となく回折強度曲線が得られる。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to the drawings. FIG. 1 is a drawing schematically showing a cross section of an X-ray diffractometer according to an embodiment of the present invention. The X-ray beam 2 generated from the X-ray source 1 is repelled upward from the horizontal by an angle of θ B by a monochromator crystal 3 designed to cause diffraction at a diffraction angle of approximately θ B / 2. After that, the X-ray beam 2 is diffracted by the first crystal 4 having the same diffraction plane as the sample crystal at the diffraction angle θ B and is incident on the sample crystal 5. At this time,
Select the diffraction plane of the sample crystal that is almost parallel to the crystal surface. If the diffractive surface is selected in this way, the sample crystal 5 can satisfy the diffraction condition only by placing it on the sample table 6 placed substantially horizontally. The angular width of the diffraction intensity curve is generally 0.5
Since it is within °, a diffraction intensity curve can be obtained without fixing the sample crystal unlike the conventional case.
【００１０】以下、一実施例として、厚さ０．４ｍｍ、
直径１００ｍｍの（１１１）表面シリコン単結晶基板に
ついて回折強度曲線を測定する方法を示す。Ｘ線ビーム
としてＣｕＫα1 （波長０．１５４０６ｎｍ）を使用
し、モノクロメータ結晶としてシリコン結晶の２２０反
射を、試料結晶の反射として３３３反射を利用した。こ
の時、シリコン結晶の格子定数として０．５４３１ｎｍ
を使うと、２２０反射の回折角は２３．６５°であり、
３３３反射の回折角は４７．４７°である。この時、２
３．６５°≒（４７．４７°）／２＝２３．７３５°で
あるため、試料結晶を固定することなく試料台に置くだ
けで理想的な回折強度曲線を得ることができた。In the following, as one embodiment, a thickness of 0.4 mm,
A method for measuring a diffraction intensity curve for a (111) surface silicon single crystal substrate having a diameter of 100 mm will be described. CuKα 1 (wavelength 0.15406 nm) was used as the X-ray beam, 220 reflection of the silicon crystal was used as the monochromator crystal, and 333 reflection was used as the reflection of the sample crystal. At this time, the lattice constant of the silicon crystal is 0.5431 nm
Using, the diffraction angle of 220 reflection is 23.65 °,
The diffraction angle of the 333 reflection is 47.47 °. At this time, 2
Since 3.65 ° ≈ (47.47 °) /2=23.735°, an ideal diffraction intensity curve could be obtained simply by placing the sample crystal on the sample stage without fixing it.
【００１１】これまでは、モノクロメータ結晶と試料結
晶が同じ種類の結晶についてのみ記載してきたが、本発
明はモノクロメータ結晶と試料結晶が異なる場合にも有
効である。その場合の一実施例を以下に示す。試料結晶
としては（００１）表面のシリコン単結晶基板を、モノ
クロメータ結晶としては立法晶の炭化珪素（ＳｉＣ：格
子定数０．４３５９７ｎｍ）を使用した。Ｘ線ビームと
してはＣｕＫα1 を使用し、モノクロメータ結晶は１１
１反射（反射角：１７．８２°）を、試料結晶の反射と
しては００４反射（反射角：３４．５６°）を使用し
た。この場合も、試料結晶を限定することなく試料台に
置くだけで理想的な回折強度曲線を得ることができた。Up to now, the monochromator crystal and the sample crystal have been described only for the same type of crystal, but the present invention is also effective when the monochromator crystal and the sample crystal are different. An example in that case is shown below. A (001) surface silicon single crystal substrate was used as a sample crystal, and cubic silicon carbide (SiC: lattice constant 0.43597 nm) was used as a monochromator crystal. CuKα 1 is used as the X-ray beam, and the monochromator crystal is 11
One reflection (reflection angle: 17.82 °) was used, and 004 reflection (reflection angle: 34.56 °) was used as the reflection of the sample crystal. Also in this case, the ideal diffraction intensity curve could be obtained by placing the sample crystal on the sample stage without limitation.
【００１２】なお、上述した実施例ではシリコン単結晶
の（１１１）表面と（００１）表面のものを試料結晶と
して用いたが、表面は（０１１）、（５１１）等どんな
面でもよく、またシリコン以外のＧａＡＳ、ＩｎＰ、Ｃ
ｄＴｅ、ＬｉＮｂＯ3 等の他の単結晶基板についても、
モノクロメータ結晶との組合せを変えるだけで適用でき
る。In the above-mentioned embodiments, the (111) surface and the (001) surface of the silicon single crystal were used as the sample crystal, but the surface may be any surface such as (011) and (511). Other than GaAS, InP, C
For other single crystal substrates such as dTe and LiNbO 3 ,
It can be applied only by changing the combination with the monochromator crystal.
【００１３】また、上述の実施例は二結晶法Ｘ線回折装
置にこの発明を適用したものであるが、この発明は二結
晶法Ｘ線回折顕微装置に適用しても効果的である。Although the present invention is applied to the two-crystal method X-ray diffraction apparatus in the above-mentioned embodiment, the present invention is also effective when applied to the two-crystal method X-ray diffraction microscope apparatus.
【００１４】[0014]
【発明の効果】以下の如く、本発明は、Ｘ線源から第１
結晶に至るまでの経路にモノクロメータ結晶を配設し、
試料結晶を水平状態に保持できるようにしたので、二結
晶Ｘ線回折測定の改良、改善が達成され、大口径材料、
薄い材料の試験、評価等に与える効果は大きく、その経
済的効果は大きい。As described below, the present invention provides a first X-ray source.
Arrange a monochromator crystal in the route to the crystal,
Since the sample crystal can be held in the horizontal state, the improvement and improvement of the double crystal X-ray diffraction measurement can be achieved.
It has a great effect on the testing and evaluation of thin materials, and its economic effect is great.
【図１】本発明の一実施例におけるＸ線回折装置の正面
図の模式図である。FIG. 1 is a schematic diagram of a front view of an X-ray diffraction apparatus according to an embodiment of the present invention.
【図２】従来のＸ線回折装置の正面図の模式図である。FIG. 2 is a schematic diagram of a front view of a conventional X-ray diffractometer.
【図３】従来の試料水平型Ｘ線回折装置の正面図の模式
図である。FIG. 3 is a schematic view of a front view of a conventional sample horizontal X-ray diffractometer.
１ Ｘ線源 ２ Ｘ線ビーム ３ モノクロメータ結晶 ４ 第１結晶 ５ 試料結晶 ６ 試料台 ７ 回転中心 ８ 回折ビーム ９ Ｘ線検出器 １０ Ｘ線管 １１ ２θ設定用レール 1 X-ray source 2 X-ray beam 3 Monochromator crystal 4 First crystal 5 Sample crystal 6 Sample stage 7 Rotation center 8 Diffraction beam 9 X-ray detector 10 X-ray tube 11 2 θ Setting rail
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平４−121649（ＪＰ，Ａ) 特開 平３−95446（ＪＰ，Ａ) 特開 平４−329347（ＪＰ，Ａ) 特開 平４−110646（ＪＰ，Ａ) 特開 平５−180789（ＪＰ，Ａ) 特開 平４−125444（ＪＰ，Ａ) 特開 平５−52775（ＪＰ，Ａ) 特公 平４−59582（ＪＰ，Ｂ２) 1992年10月10日理学電気株式会社発行 「理学電気ジャーナル第23巻第２号通巻 58号」第70−74頁 ─────────────────────────────────────────────────── --- Continuation of the front page (56) References JP-A-4-121649 (JP, A) JP-A-3-95446 (JP, A) JP-A-4-329347 (JP, A) JP-A-4- 110646 (JP, A) JP 5-180789 (JP, A) JP 4-125444 (JP, A) JP 5-52775 (JP, A) JP 4-59582 (JP, B2) October 10, 1992 Published by Rigaku Denki Co., Ltd. “Rigaku Denki Journal, Vol. 23, No. 2, Vol. 58,” pages 70-74
Claims (1)
ほぼ等しい第１結晶を有する試料水平型二結晶Ｘ線回折
装置において、Ｘ線源から第１結晶に至るまでのＸ線経
路の途中に第１結晶のほぼ半分の角度で回折を起こすモ
ノクロメータ結晶を配置して、Ｘ線源からのＸ線をモノ
クロメータ結晶、第１結晶、及び第２結晶で順に回折さ
せるようにしたことを特徴とするＸ線回折装置。1. A horizontal sample two-crystal X-ray diffractometer having a first crystal having a lattice spacing substantially equal to that of a second crystal, which is a sample crystal, of an X-ray path from an X-ray source to the first crystal. A monochromator crystal that causes diffraction at an angle approximately half that of the first crystal is arranged on the way, and X-rays from the X-ray source are sequentially diffracted by the monochromator crystal, the first crystal, and the second crystal. An X-ray diffractometer characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6116403A JP2674506B2 (en) | 1994-05-30 | 1994-05-30 | X-ray diffractometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6116403A JP2674506B2 (en) | 1994-05-30 | 1994-05-30 | X-ray diffractometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07318517A JPH07318517A (en) | 1995-12-08 |
| JP2674506B2 true JP2674506B2 (en) | 1997-11-12 |
Family
ID=14686192
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6116403A Expired - Lifetime JP2674506B2 (en) | 1994-05-30 | 1994-05-30 | X-ray diffractometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2674506B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2881264B1 (en) * | 2005-01-21 | 2007-06-01 | Commissariat Energie Atomique | X-RAY OR NEUTRON MONOCHROMATOR |
| KR20070002726A (en) * | 2005-06-30 | 2007-01-05 | 주식회사 에이엘티 | Apparatus for measuring the direction of crystallization and the measuring method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04121649A (en) * | 1990-09-13 | 1992-04-22 | Rigaku Corp | Sample horizontal type two-crystal x-ray diffraction apparatus |
-
1994
- 1994-05-30 JP JP6116403A patent/JP2674506B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| １９９２年１０月１０日理学電気株式会社発行「理学電気ジャーナル第２３巻第２号通巻５８号」第７０−７４頁 |
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| Publication number | Publication date |
|---|---|
| JPH07318517A (en) | 1995-12-08 |
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