JPH01131095A - Crucible for production of single crystal - Google Patents
Crucible for production of single crystalInfo
- Publication number
- JPH01131095A JPH01131095A JP28767187A JP28767187A JPH01131095A JP H01131095 A JPH01131095 A JP H01131095A JP 28767187 A JP28767187 A JP 28767187A JP 28767187 A JP28767187 A JP 28767187A JP H01131095 A JPH01131095 A JP H01131095A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- single crystal
- production
- melting point
- oxide
- 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.)
- Pending
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 19
- 230000008018 melting Effects 0.000 claims abstract description 17
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 11
- 239000000956 alloy Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910018885 Pt—Au Inorganic materials 0.000 claims abstract description 6
- 239000000155 melt Substances 0.000 abstract description 4
- 229910011131 Li2B4O7 Inorganic materials 0.000 abstract 1
- 238000005336 cracking Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
この発明は単結晶製造用るつぼの改良に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> This invention relates to an improvement in a crucible for producing single crystals.
〈従来の技術およびその問題点〉
従来、ＬＬ２Ｂ＋０７やＰｂ １％ ０４などの低融点
酸化物はＰするつほを用いてチョクラルスキー法による
単結晶の育成を行なっている。<Prior art and its problems> Conventionally, single crystals of low melting point oxides such as LL2B+07 and Pb 1% 04 have been grown by the Czochralski method using a P droplet.
しかしながら、−殻内に低融点酸化物は融点付近におい
て高粘性を示すため、Ｐするつぼではるつぼの内壁と溶
融された原料との間に大きな摩擦が生じてしまい、融液
の対流が乱れてしまう。However, since the low melting point oxide in the shell exhibits high viscosity near the melting point, large friction occurs between the inner wall of the crucible and the melted raw material in the P crucible, disrupting the convection of the melt. Put it away.
そのため、るつぼの内径に対して５０％程度の直径の単
結晶しか得られないという欠点を有していた。Therefore, it has the disadvantage that a single crystal having a diameter that is only about 50% of the inner diameter of the crucible can be obtained.
また、るつぼ材としては、 （１）使用温度で融解、軟化しないこと。In addition, as a crucible material, (1) Do not melt or soften at the operating temperature.
（２）雰囲気ガスおよび融液と反応しないこと。(2) Do not react with atmospheric gas or melt.
（３）不純物供給源とならないこと。(3) Not to be a source of impurities.
などの条件を満足する必要がある。It is necessary to satisfy the following conditions.
チョクラルスキー法によって低融点酸化物の単結晶の製
造コストを低下させるためには、大型直径の単結晶を作
成する必要があるが、上記した理由によりるつぼ自体の
内径を大きくするか、またはるつぼの内壁と溶融された
原料との間に摩擦を生じにくくする必要がある。In order to reduce the manufacturing cost of single crystals of low melting point oxides using the Czochralski method, it is necessary to create single crystals with large diameters, but for the reasons mentioned above, it is necessary to increase the inner diameter of the crucible itself or It is necessary to make it difficult for friction to occur between the inner wall of the molten material and the molten raw material.
前者については、るつぼ自体の内径を大きくすると、る
つほのコストが大きくなり、かつ育成装置自体が大きく
なり好ましくない。そのため後者の方法が必要となり、
それに適したるつぼの材質面での検討が望まれていた。Regarding the former, increasing the inner diameter of the crucible itself increases the cost of the crucible and increases the size of the growth apparatus itself, which is not preferable. Therefore, the latter method is necessary,
It was desired to consider the material of the crucible suitable for this purpose.
〈発明の目的〉
この発明はＰｔ−Ａｕ系合金るつぼを用いることによっ
て融点が１４００℃以下の低融酸化物、例えばＬｉ２Ｂ
４Ｏ７やＰｂ ＭＯ０４などの組成物を気泡の混入やク
ラックを生じることなく、るつぼの内径に対して６０％
以上の直径の単結晶をチョクラルスキー法にて供給する
ことのできる単結晶製造用るつぼを提供することを目的
とするものである。<Object of the invention> This invention uses a Pt-Au alloy crucible to produce low-melting oxides with a melting point of 1400°C or less, such as Li2B.
Compositions such as 4O7 and Pb MO04 are mixed at 60% of the inner diameter of the crucible without creating bubbles or cracks.
It is an object of the present invention to provide a crucible for producing single crystals that can supply single crystals having the above diameters by the Czochralski method.
〈問題点を解決するための手段〉
この発明は上記した問題点を解消するためになされたも
のであって、その要旨とするところはチョクラルスキー
法によって低融点酸化物の単結晶を作製する際に使用す
るＰｔ−Ａｕ系合金製るつぼにおいて、その材質をＰｔ
’−Ａｕ系合金中のＡｕの原子百分率が１〜３０％の範
囲であるるつぼとすることによってるつぼの内壁と溶融
された原料との間に摩擦が生じにくくなり、るつぼの内
径に対して６０％以上の直径の低融点酸化物の単結晶が
得られることを見出したのである。<Means for solving the problems> This invention was made to solve the above problems, and its gist is to produce a single crystal of a low melting point oxide by the Czochralski method. In the Pt-Au alloy crucible used for this purpose, the material is Pt.
By using a crucible in which the atomic percentage of Au in the Au-based alloy is in the range of 1 to 30%, friction is less likely to occur between the inner wall of the crucible and the molten raw material, and They found that it is possible to obtain a single crystal of a low melting point oxide with a diameter of 50% or more.
〈作用〉
この発明におけるＰｔ −Ａｕ系合金るつぼにおいてＡ
ｕの原子百分率を１〜３０％と限定するのは、１％より
小さいと、るつぼの内径に対して６０％以上の直径の低
融点酸化物の単結晶を育成した場合、クラックが生じて
好ましくない。<Function> In the Pt-Au alloy crucible according to the present invention, A
It is preferable to limit the atomic percentage of u to 1 to 30% because if it is smaller than 1%, cracks will occur when a single crystal of a low melting point oxide with a diameter of 60% or more of the inner diameter of the crucible is grown. do not have.
またＡｕの原子百分率が３０％より大きいと、Ｐｔ −
Ａｕ系合金の融点が１４００°Ｃより低くなり、使用中
にるつぼが変形してしまい、るつぼの耐用期間が短くな
り好ましくない。Moreover, when the atomic percentage of Au is greater than 30%, Pt −
The melting point of the Au-based alloy becomes lower than 1400°C, which is undesirable because the crucible deforms during use and the service life of the crucible is shortened.
〈実施例〉 以下、この発明を実施例により詳細に説明づ−る。<Example> Hereinafter, this invention will be explained in detail with reference to Examples.
実施例１
ＰｔとＡｕとを第１表に示す原子百分率になるＪ：うに
空気中でアーク溶融により合金を合成した。Example 1 An alloy containing Pt and Au having the atomic percentages shown in Table 1 was synthesized by arc melting in air.
その後、この合金を用いて１１００°Ｃの熱間加工によ
り第１図にその形状を示すような高さ６０ｍｍ、内径６
０ｍｍ５外径６２１１＋ＩＩ＋の円筒形るつぼ１に成形
したのち冷却し、弗化水素水によって表面処理を行なっ
てこの発明のるつぼを得た。Thereafter, this alloy was hot worked at 1100°C to form a shape with a height of 60 mm and an inner diameter of 6 as shown in Figure 1.
After molding into a cylindrical crucible 1 with an outer diameter of 0 mm5 and an outer diameter of 6211+II+, it was cooled and surface treated with hydrogen fluoride water to obtain a crucible of the present invention.
次に、このるつぼにし、３４０７原料を３５０９充填し
たのち、高周波誘導加熱により原料を９３０℃で融解し
、その後ＬＬＪ＋０７種子結晶を融液に接触させ、引上
速度１．０〜２．０ ｍｍ／ｈｒ 、引上軸回転数を１
０〜３０ｒｐｍで単結晶を育成した。Next, this crucible was filled with 3509 of the 3407 raw material, and then the raw material was melted at 930°C by high-frequency induction heating, and then the LLJ+07 seed crystal was brought into contact with the melt, and the pulling rate was 1.0 to 2.0 mm/ hr, the number of rotations of the pulling shaft is 1
Single crystals were grown at 0-30 rpm.
その結果は第２表に示した。The results are shown in Table 2.
なお、＊印はこの発明の請求範囲外である。Note that *marks are outside the scope of the claims of this invention.
第 １ 表
くるつぼ材質の組成比）
第 ２ 表
（注）＊印のＮ０１１はＬｉＪ４０ｖ原料を融解してい
る途中でるつぼが変形してしまい、単結晶が育成できな
かった。Table 1 Composition ratio of crucible material) Table 2 (Note) For N011 marked with *, the crucible was deformed while melting the LiJ40v raw material, and a single crystal could not be grown.
実施例２
実施例１で作製したるつほにＰｂ ＭＯＯノ、原料を１
０００ｇ充填した後、高周波誘導加熱により原料を１０
８０℃で融解し、その後Ｐｂ Ｎｏ Ｏ４種子結晶を融
液に接触させ、引上速度２．５〜３．０ ｍｍ／ｈｒ
、引上軸回転数、３２〜４５ｒｐｎの条件で単結晶を育
成した。その結果は第３表に示した。Example 2 Pb MOO was added to the rutsuho produced in Example 1, and 1 part of the raw material was added.
After filling 000g, the raw material was heated to 10% by high-frequency induction heating.
Melt at 80°C, then bring Pb No O4 seed crystals into contact with the melt, and pull up at a pulling rate of 2.5 to 3.0 mm/hr.
Single crystals were grown under conditions of a pulling shaft rotation speed of 32 to 45 rpm. The results are shown in Table 3.
第 ３ ｓ
（注）＊印の試料Ｎｏ、１１はＰｂ ＭＯＯ４原料を融
解している途中でるつぼが変形してしまい、単結晶が育
成できなかった。3rd s (Note) For sample No. 11 marked with *, the crucible was deformed during melting of the Pb MOO4 raw material, and a single crystal could not be grown.
〈発明の効果〉
以上説明したように、この発明は組成中のんの原子百分
率が１〜３０％の範囲内である汽−へ〇合金系るつぼと
したことによって、このるつぼを用いてチョクラルスキ
ー法にて融点が１４００℃以下の低融点酸化物の単結晶
を製造すると、気泡の混入やクラックが生ずることなく
、るつぼの内径に対して６０％以上の直径を有する単結
晶を得ることができるのである。<Effects of the Invention> As explained above, the present invention provides a steam alloy crucible in which the atomic percentage of nitrogen in the composition is within the range of 1 to 30%. When producing a single crystal of a low melting point oxide with a melting point of 1400°C or less using the ski method, it is possible to obtain a single crystal with a diameter of 60% or more of the inner diameter of the crucible without the inclusion of bubbles or cracks. It can be done.
第１図は、この発明で得られたるつぼの斜視図である。 １は円筒形るつぼである。 FIG. 1 is a perspective view of a crucible obtained by the present invention. 1 is a cylindrical crucible.
Claims (1)
低融点酸化物を製造する際に使用するＰｔ−Ａｕ系合金
るつぼにおいて、Ａｕの原子百分率が１〜３０％の範囲
にあることを特徴とする単結晶製造用るつぼ。A Pt-Au alloy crucible used for producing a low melting point oxide having a melting point of 1400°C or less by the Czochralski method, characterized in that the atomic percentage of Au is in the range of 1 to 30%. Crucible for producing single crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28767187A JPH01131095A (en) | 1987-11-13 | 1987-11-13 | Crucible for production of single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28767187A JPH01131095A (en) | 1987-11-13 | 1987-11-13 | Crucible for production of single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01131095A true JPH01131095A (en) | 1989-05-23 |
Family
ID=17720212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28767187A Pending JPH01131095A (en) | 1987-11-13 | 1987-11-13 | Crucible for production of single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01131095A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624781A (en) * | 2016-01-14 | 2016-06-01 | 福建福晶科技股份有限公司 | Lithium tetraborate crystal preparation method and growth device |
-
1987
- 1987-11-13 JP JP28767187A patent/JPH01131095A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624781A (en) * | 2016-01-14 | 2016-06-01 | 福建福晶科技股份有限公司 | Lithium tetraborate crystal preparation method and growth device |
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