JP3307438B2 - Method for producing cerium-activated gadolinium silicate single crystal - Google Patents
Method for producing cerium-activated gadolinium silicate single crystalInfo
- Publication number
- JP3307438B2 JP3307438B2 JP31327092A JP31327092A JP3307438B2 JP 3307438 B2 JP3307438 B2 JP 3307438B2 JP 31327092 A JP31327092 A JP 31327092A JP 31327092 A JP31327092 A JP 31327092A JP 3307438 B2 JP3307438 B2 JP 3307438B2
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- crystal
- furnace
- growing
- lid
- 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.)
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- Crystals, And After-Treatments Of Crystals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、シンチレータ等の光学
結晶の製造に好適な、セリウム賦活珪酸ガドリニウム単
結晶の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a cerium-activated gadolinium silicate single crystal suitable for producing an optical crystal such as a scintillator.
【０００２】[0002]
【従来の技術】チョクラルスキー法で、良好な真直性を
もち、かつ割れの少ない単結晶を得るために、従来はル
ツボの上部にアフターヒーター等の保温材を設けて単結
晶の育成が行われている（特公昭５８−５０９５６号公
報等）。2. Description of the Related Art In order to obtain a single crystal having good straightness and few cracks by the Czochralski method, a single crystal is conventionally grown by providing a heat insulating material such as an after-heater above a crucible. (JP-B-58-50956, etc.).
【０００３】[0003]
【発明が解決しようとする課題】しかし、ルツボの上部
に保温材を設けると、のぞき窓から育成中の結晶を観察
する際に保温材が邪魔になって観察できない問題があっ
た。本発明は、真直で割れの少ない良質なセリウム賦活
珪酸ガドリニウム単結晶の製造方法を提供することを目
的とする。However, if a heat insulating material is provided on the upper part of the crucible, there is a problem that the heat insulating material hinders observation when observing the growing crystal from the viewing window. The present invention is a high quality cerium activation that is straight and has few cracks.
An object of the present invention is to provide a method for producing a gadolinium silicate single crystal.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、セリウム
賦活珪酸ガドリニウム単結晶の製造方法において、ルツ
ボの上部の保温構造を種々検討した結果、炉の上部に、
単結晶の育成工程中、任意の開閉度に操作できる可動式
の耐火物製の蓋を設け、単結晶の育成工程では耐火物製
の蓋を開放の状態とし、冷却工程では耐火物製の蓋を閉
じれば、真直で円柱状結晶が得られ、割れの発生も著し
く少なくなることを見出し、本発明を完成した。Means for Solving the Problems The present inventors have proposed cerium.
In the production method of the activated gadolinium silicate single crystal, as a result of various studies on the heat insulation structure at the top of the crucible,
During the single crystal growing process, a movable refractory lid that can be operated at any degree of opening and closing is provided.In the single crystal growing process, the refractory lid is opened.In the cooling process, the refractory lid is opened. Closed, a straight columnar crystal was obtained, and the occurrence of cracks was significantly reduced, and the present invention was completed.
【０００５】すなわち、本発明に用いられる炉は、チョ
クラルスキー法による単結晶の製造に最適な炉、すなわ
ち、炉の上部に、単結晶の育成工程中、任意の開閉度に
操作できる可動式の耐火物製の蓋を設けた、単結晶育成
炉である。図１は、本発明に用いられる単結晶育成炉の
一例で、成長させた単結晶を融液から切り離したのち冷
却している場合の育成炉の単結晶育成炉の構成を示して
いる。図１中、１は耐火物製の蓋であり、これは可動式
で、任意の開閉度に操作できる。２は炉本体であり、こ
れはジルコニア等の耐火物から成っている。７はのぞき
窓であり、耐火物製の蓋が開放の状態のとき（単結晶育
成工程）は、のぞき窓から炉内の結晶の育成状態を観察
できる。[0005] That is, the furnace used in the present invention is a movable furnace which can be operated at an arbitrary degree of opening and closing during the single crystal growing process, at the upper part of the furnace, which is optimal for the production of a single crystal by the Czochralski method. This is a single crystal growing furnace provided with a refractory lid. FIG. 1 shows an example of a single crystal growing furnace used in the present invention, in which a grown single crystal is separated from a melt and cooled after cooling. In FIG. 1, reference numeral 1 denotes a refractory lid, which is movable and can be operated to an arbitrary degree of opening and closing. Reference numeral 2 denotes a furnace body, which is made of a refractory such as zirconia. Reference numeral 7 denotes a viewing window. When the refractory lid is in an open state (single crystal growing step), the growth state of crystals in the furnace can be observed from the viewing window.
【０００６】本発明は、セリウム賦活珪酸ガドリニウム
単結晶の製造方法を提供する。すなわち、炉内で原料を
加熱して融液とし、その融液に種結晶の下端を接触さ
せ、種結晶を引き上げながら結晶を成長させる育成工
程、及び成長させた単結晶を融液から切り離したのち冷
却する冷却工程、を経るチョクラルスキー法によるセリ
ウム賦活珪酸ガドリニウム単結晶の製造方法において、
炉の上部に単結晶の育成工程中、任意の開閉度に操作で
きる可動式の蓋を設け、育成工程では耐火物製の蓋を開
放の状態とし、冷却工程では一部もしくは全過程でその
蓋を閉じて行う単結晶の製造方法である。The present invention provides a gadolinium silicate activated with cerium.
Provided is a method for producing a single crystal . That is, the raw material is heated in a furnace to form a melt, the lower end of the seed crystal is brought into contact with the melt, a growing step of growing the crystal while pulling up the seed crystal, and separating the grown single crystal from the melt. Seri by the Czochralski method to go through the cooling step of cooling later, the
In a method for producing a gallium-activated gadolinium silicate single crystal,
At the top of the furnace, a movable lid that can be operated at any degree of opening and closing during the single crystal growth process is provided.The refractory lid is opened during the growth process, and the lid is partially or wholly used during the cooling process. Is a method for producing a single crystal by closing the process.
【０００７】本発明で製造することのできる単結晶とし
ては、Ｇｄ 2-x Ｃｅ x ＳｉＯ 5 等の、チョクラルスキー法
で育成できるセリウム賦活珪酸ガドリニウム単結晶が挙
げられる。A single crystal which can be produced by the present invention
Te is such Gd 2-x Ce x SiO 5 , include cerium-activated gadolinium silicate single crystal can be grown by the Czochralski method.
【０００８】[0008]
【実施例】本発明を実施例により、更に具体的に説明す
る。EXAMPLES The present invention will be described more specifically with reference to examples.
【０００９】実施例１ 図１に示したような、炉（ジルコニア耐火物）の上部に
可動式の耐火蓋（アルミナ耐火物）を設けた単結晶育成
炉を用い、チョクラルスキー法で単結晶を製造した。直
径５０ｍｍのＩｒ製ルツボに、原料のセリウム賦活珪酸
ガドリニウム（Ｇｄ1.995Ｃｅ0.005ＳｉＯ5）をとっ
た。可動式の耐火蓋を開けた状態で、先ず、育成炉内に
予め３リットル／分の速さで窒素ガスを供給した。窒素
ガスを供給した状態のまま、ルツボ内の原料が溶融する
温度（珪酸ガドリニウムの融点は１，９５０℃）まで加
熱源の高周波電力を上げた。融液に種結晶を接触させ、
この状態で上昇速度１〜５ｍｍ／ｈ及び回転速度１０〜
５０ｒｐｍで種結晶を引き上げた。結晶を融液から切り
離す前に、耐火蓋をゆっくり閉じ、結晶を融液から切り
離し、窒素ガス雰囲気中、５０℃／ｈの冷却速度で室温
まで冷却した。その後、結晶を取り出した。結晶は、割
れのない、約２５ｍｍ（直径）×８０ｍｍ（長さ）の円
柱状の良質な単結晶であった。Example 1 A single crystal growing furnace having a movable refractory lid (alumina refractory) provided above a furnace (zirconia refractory) as shown in FIG. 1 was used, and a single crystal was grown by the Czochralski method. Was manufactured. A raw material cerium-activated gadolinium silicate (Gd 1.995 Ce 0.005 SiO 5 ) was placed in an Ir crucible having a diameter of 50 mm. With the movable refractory lid open, nitrogen gas was first supplied into the growing furnace at a rate of 3 liters / minute in advance. While the nitrogen gas was supplied, the high-frequency power of the heating source was increased to a temperature at which the raw material in the crucible was melted (the melting point of gadolinium silicate was 1,950 ° C.). The seed crystal is brought into contact with the melt,
In this state, the rising speed is 1 to 5 mm / h and the rotation speed is 10 to 10.
The seed crystal was pulled up at 50 rpm. Before separating the crystal from the melt, the refractory lid was slowly closed, and the crystal was separated from the melt and cooled to room temperature in a nitrogen gas atmosphere at a cooling rate of 50 ° C./h. Thereafter, the crystal was taken out. The crystal was a columnar high-quality single crystal of about 25 mm (diameter) x 80 mm (length) without cracks.
【００１０】比較例 炉（ジルコニア耐火物）の上部に可動式の耐火物製の蓋
がない点を除き、図１に示した単結晶育成炉と同様の炉
を用い、実施例１と同様にして、チョクラルスキー法で
単結晶を製造した。得られた結晶は、肩部から中央部に
かけて割れが多数観察された。Comparative Example A furnace similar to the single crystal growing furnace shown in FIG. 1 was used, except that a movable refractory lid was not provided on the upper part of the furnace (zirconia refractory). In the same manner as in Example 1, a single crystal was produced by the Czochralski method . In the obtained crystal, many cracks were observed from the shoulder to the center.
【００１１】[0011]
【発明の効果】本発明の製造方法により、割れの少ない
良質なセリウム賦活珪酸ガドリニウム単結晶を歩留りよ
く製造できる。The production method of the present invention, a crack less quality cerium-activated gadolinium silicate single crystal can manufactured with good yield.
【図１】炉の上部に可動式の耐火物製の蓋を設けた、本
発明に用いられる単結晶育成炉の構成を示す模式図であ
る。FIG. 1 shows a book with a movable refractory lid at the top of the furnace.
FIG. 1 is a schematic diagram showing a configuration of a single crystal growing furnace used in the present invention .
１： 可動式の耐火物製の蓋 ２： 炉本体 ３： ルツボ ４： 電気誘導コイル ５： チャンバー ６： 重量計 ７： のぞき窓 ８： 種結晶 ９： 成長した単結晶 １０： 原料融液1: Movable refractory lid 2: Furnace body 3: Crucible 4: Electric induction coil 5: Chamber 6: Weight scale 7: Viewing window 8: Seed crystal 9: Grown single crystal 10: Raw material melt
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭58−130192（ＪＰ，Ａ) 特開 昭63−222090（ＪＰ，Ａ) 特開 平４−321600（ＪＰ，Ａ) 特開 平４−228492（ＪＰ，Ａ) 特開 昭60−122793（ＪＰ，Ａ) 特開 昭58−41797（ＪＰ，Ａ) 実開 平２−17563（ＪＰ，Ｕ) (58)調査した分野(Int.Cl.7，ＤＢ名) C30B 1/00 - 35/00 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-58-130192 (JP, A) JP-A-63-222090 (JP, A) JP-A-4-321600 (JP, A) JP-A-4-321600 228492 (JP, A) JP-A-60-122793 (JP, A) JP-A-58-41797 (JP, A) JP-A-2-17563 (JP, U) (58) Fields investigated (Int. Cl. 7 , DB name) C30B 1/00-35/00
Claims (1)
その融液に種結晶の下端を接触させ、種結晶を引き上げ
ながら結晶を成長させる育成工程；及び（２）成長させ
た単結晶を融液から切り離したのち冷却する冷却工程；
を経るチョクラルスキー法による、セリウムで賦活した
珪酸ガドリニウム単結晶の製造方法において、 炉の上部に、単結晶の育成工程中、任意の開閉度に操作
できる可動式の、耐火物製の蓋を設け、育成工程ではそ
の蓋を開放の状態として結晶の育成状態を観察し、冷却
工程では一部もしくは全過程でその蓋を閉じることを特
徴とする、単結晶の製造方法。(1) heating a raw material in a furnace to form a melt;
A growing step of bringing the lower end of the seed crystal into contact with the melt and growing the crystal while pulling up the seed crystal; and (2) a cooling step of separating the grown single crystal from the melt and then cooling;
Cerium activated by Czochralski method
In the method for producing a gadolinium silicate single crystal, a movable, refractory lid that can be operated at any degree of opening and closing during the single crystal growing step is provided at the upper part of the furnace, and the lid is opened in the growing step. A method for producing a single crystal, comprising observing a growing state of a crystal and closing a lid in a part or all of a cooling step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31327092A JP3307438B2 (en) | 1992-11-24 | 1992-11-24 | Method for producing cerium-activated gadolinium silicate single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31327092A JP3307438B2 (en) | 1992-11-24 | 1992-11-24 | Method for producing cerium-activated gadolinium silicate single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06157187A JPH06157187A (en) | 1994-06-03 |
| JP3307438B2 true JP3307438B2 (en) | 2002-07-24 |
Family
ID=18039192
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31327092A Expired - Fee Related JP3307438B2 (en) | 1992-11-24 | 1992-11-24 | Method for producing cerium-activated gadolinium silicate single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3307438B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190114642A (en) * | 2018-03-30 | 2019-10-10 | 주식회사 엘지화학 | Single crystal growth device and single crystal growth method of using the same |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100320586B1 (en) * | 1999-10-21 | 2002-01-18 | 정세영 | apparatus for single crystal growing using high pressure |
| JP4203647B2 (en) * | 2002-06-13 | 2009-01-07 | 株式会社日立製作所 | Single crystal manufacturing apparatus and manufacturing method thereof |
| KR102466502B1 (en) * | 2018-03-30 | 2022-11-10 | 주식회사 엘지화학 | Single crystal growth device and single crystal growth method of using the same |
| KR102493182B1 (en) * | 2019-03-12 | 2023-01-27 | 주식회사 엘지화학 | Single crystal growth apparatus and single crystal growth method of using the same |
-
1992
- 1992-11-24 JP JP31327092A patent/JP3307438B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190114642A (en) * | 2018-03-30 | 2019-10-10 | 주식회사 엘지화학 | Single crystal growth device and single crystal growth method of using the same |
| KR102475322B1 (en) * | 2018-03-30 | 2022-12-06 | 주식회사 엘지화학 | Single crystal growth device and single crystal growth method of using the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06157187A (en) | 1994-06-03 |
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