JPH0312320A - Production of boron oxide - Google Patents
Production of boron oxideInfo
- Publication number
- JPH0312320A JPH0312320A JP14563689A JP14563689A JPH0312320A JP H0312320 A JPH0312320 A JP H0312320A JP 14563689 A JP14563689 A JP 14563689A JP 14563689 A JP14563689 A JP 14563689A JP H0312320 A JPH0312320 A JP H0312320A
- Authority
- JP
- Japan
- Prior art keywords
- boron oxide
- nozzle
- oxyhydrogen flame
- cooling
- gas
- 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.)
- Granted
Links
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052810 boron oxide Inorganic materials 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000009833 condensation Methods 0.000 claims abstract description 12
- 230000005494 condensation Effects 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052796 boron Inorganic materials 0.000 claims abstract description 7
- -1 boron halide Chemical class 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 238000009826 distribution Methods 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 239000000112 cooling gas Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 3
- 238000001308 synthesis method Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000002775 capsule Substances 0.000 abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000012808 vapor phase Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 18
- 239000007788 liquid Substances 0.000 description 14
- 238000011084 recovery Methods 0.000 description 12
- 239000007787 solid Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000010453 quartz Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 238000010574 gas phase reaction Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YPSXFMHXRZAGTG-UHFFFAOYSA-N 4-methoxy-2-[2-(5-methoxy-2-nitrosophenyl)ethyl]-1-nitrosobenzene Chemical compound COC1=CC=C(N=O)C(CCC=2C(=CC=C(OC)C=2)N=O)=C1 YPSXFMHXRZAGTG-UHFFFAOYSA-N 0.000 description 1
- 102100021569 Apoptosis regulator Bcl-2 Human genes 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 101000971171 Homo sapiens Apoptosis regulator Bcl-2 Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- YWCYJWYNSHTONE-UHFFFAOYSA-O oxido(oxonio)boron Chemical compound [OH2+][B][O-] YWCYJWYNSHTONE-UHFFFAOYSA-O 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
（発明の産業上利用分野）
本発明は酸化ほう素の製造方法、さらに詳細にはＩｎＰ
、ＧａＡｓ、ＧａＰなどのＩＩＩ −Ｖ族化合物半導体
単結晶の液体カプセル封じ引き上げ法に用いられる高純
度酸化ほう素（８２０３）液体カプセル剤の製造方法に
関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field of the Invention) The present invention relates to a method for producing boron oxide, and more specifically to a method for producing boron oxide.
The present invention relates to a method for producing a high-purity boron oxide (8203) liquid capsule used in a liquid encapsulation pulling method for single crystal III-V compound semiconductors such as GaAs, GaP, etc.
（従来の技術および問題点）
１１１−Ｖ族化合物半導体単結晶の実用的な育成方法と
して従来より第１図に示す液体カプセル封じ引き上げ法
が用いられている。引き上げ法の原理は第１図に示すよ
うに、ルツボ１中に融解した結晶原料２を作り、種結晶
３を液面に接触させて上部低温側にゆっくり引き上げる
ことによって、種結晶３の先端に同じ結晶方位を有する
単結晶４を成長させるものである。しかしＩＩＩ族とＶ
族の２成分元素からなるＩＩＩ −Ｖ族化合物では、Ｐ
、Ａｓなとの■族元素の蒸気圧が高いという特徴がある
。その結果、原料を融点付近に加熱すると■族元素が蒸
発して融液にならず、単結晶を成長させることができな
い、そこで、第１図に示すように、成長容器６内に高圧
の不活性ガスを満たし、不揮発性の液体カプセル剤５で
融液原料を封じて分解を抑えながら単結晶の引き上げを
行なうことが必要である。このカプセル剤の材質として
、
１）低融点高沸点であること、２）比重が小さいこと、
３）透明であること、４坏活性であることが必要であり
、そのため一般にＢ２Ｏ３がカプセル剤として用いられ
る。(Prior Art and Problems) As a practical method for growing 111-V group compound semiconductor single crystals, the liquid encapsulation pulling method shown in FIG. 1 has been used conventionally. As shown in Figure 1, the principle of the pulling method is to create a molten crystal raw material 2 in a crucible 1, bring the seed crystal 3 into contact with the liquid surface, and slowly pull it up to the lower temperature side of the upper part. Single crystals 4 having the same crystal orientation are grown. However, group III and V
In III-V group compounds consisting of binary elements of the group P
, As, and other group elements have a high vapor pressure. As a result, when the raw material is heated to around its melting point, the Group (1) elements evaporate and it does not become a melt, making it impossible to grow a single crystal. Therefore, as shown in FIG. It is necessary to fill the active gas and seal the melt raw material with a non-volatile liquid capsule 5 to suppress decomposition while pulling the single crystal. The materials for this capsule are: 1) low melting point and high boiling point, 2) low specific gravity,
3) It needs to be transparent and have 4-merulent activity, so B2O3 is generally used as a capsule.
しかしながら、第１図から明らかなように、Ｂ２Ｏ３カ
プセル剤とルツボは融液原料と直接に接触しているため
に、その純度、材質はＩＩＩ−Ｖ族化合物半導体単結晶
の純度に大きく影響する。このうち、ルツボは近年にお
いて気相成長法によるｐＢＮルツボなどの開発により結
晶純度に影響しない高純度な材料が使えるようになった
。一方、Ｂ２Ｏ３カプセル剤はこれまでホウ砂などの天
然原料を精製して得る方法が一般的に用いられているが
、この方法ではＢ２Ｏ３の純度を上げるには限界があっ
た。また、ハロゲン化ほう素と酸素との気相反応により
高純度Ｂ２Ｏ３を得る方法が試みられているが、次のよ
うな問題点があった。However, as is clear from FIG. 1, since the B2O3 capsule and the crucible are in direct contact with the melt raw material, their purity and material greatly affect the purity of the III-V compound semiconductor single crystal. Among these, in recent years, the development of pBN crucibles using vapor phase growth methods has made it possible to use high-purity materials that do not affect crystal purity. On the other hand, B2O3 capsules have generally been obtained by purifying natural raw materials such as borax, but this method has limitations in increasing the purity of B2O3. Furthermore, attempts have been made to obtain high purity B2O3 through a gas phase reaction between boron halide and oxygen, but these methods have had the following problems.
ハロゲン化ほう素と酸素との気相反応によりＢ２Ｏ３を
合成するには、−例として次の気相反応が用いられる。To synthesize B2O3 by gas phase reaction of boron halide and oxygen, the following gas phase reaction is used as an example.
４８Ｃ１３＋６８２−１−３０２→２Ｂ２０３＋１２Ｈ
Ｃ１この反応は、酸水素炎中にＢＣｌ３のガス（室温で
気体）を吹き込むことによって行なわれる。48C13+682-1-302→2B203+12H
C1 This reaction is carried out by blowing BCl3 gas (a gas at room temperature) into an oxyhydrogen flame.
生成物としてＢ２Ｏ３の他にＨＣＩができるが、製造容
器に排気装置を接続しておけば気体成分であるＨＣＩは
排気されて固相のＢ２Ｏ３とは分離できる。この反応の
原料となるＢＣ’１３（室温）、Ｎ２．０２の各ガス成
分は高純度化が容易なため、生成物の８２０３の高純度
化は容易である。HCI is produced in addition to B2O3 as a product, but if an exhaust device is connected to the production container, the gaseous HCI can be exhausted and separated from the solid phase B2O3. Since the gas components BC'13 (room temperature) and N2.02, which are raw materials for this reaction, can be easily purified, the product 8203 can be easily purified.
この方法を用いた従来の装置構成を第２図に示す、８は
酸水素炎バーナーで三重ノズル構造である。The configuration of a conventional device using this method is shown in FIG. 2, where 8 is an oxyhydrogen flame burner with a triple nozzle structure.
中央のノズルはＢＣｌ３＋８２ガス用で、外側の二重の
ノズルはＮ２およびｏ２ガス用である。The middle nozzle is for BCl3+82 gas and the outer double nozzle is for N2 and O2 gas.
中央ノズルには液体１２（ＢＣｌ３）の入ったバブラー
１３を介してＢＣｌ３＋Ｈ２の混合ガスを供給している
。前記液体１２は氷の入った冷却容器１４によって冷却
されている。A mixed gas of BCl3+H2 is supplied to the central nozzle via a bubbler 13 containing liquid 12 (BCl3). The liquid 12 is cooled by a cooling container 14 containing ice.
Ｎ２、Ｎ２および０２の各ガスはバブラー導入管または
各ノズルに供給している。Each of the N2, N2 and 02 gases is supplied to the bubbler introduction pipe or each nozzle.
１０は８２０３回収容器である。Ｂ２Ｏ３を生成するた
めには、まず、各ノズルよりＮ２、Ｑ２、Ｎ２ガスを出
し点火して酸水素炎９を発生させる１次いで、バルブ１
５をバブラー１３側に切り替え、Ｎ２ガスを液体ＢＣｌ
３１２中を通してＢＣｌ３＋Ｈ２ガスを発生させ、中央
ノズルより９の酸水素炎中に、ＢＣｌ３を放出する。こ
の結果、微粉末ガス状のＢ２Ｏ３が生成し、さらに容器
１０の低温部で凝縮して数ｍｍ角から数ｃｍ角の板状の
Ｂ２Ｏ３固形物１１となる。しかし、第２図の構成では
、回収容器１０外へのＢ２Ｏ３の飛散が多く、また、酸
水素炎９と回収容器１０の距離が大きく取れないことに
より、Ｂ２Ｏ３の容器１０への凝縮が起きにくいので、
原料に対するＢ２Ｏ３の回収率が２０％程度と低く実用
にならないという問題があった。10 is an 8203 collection container. In order to generate B2O3, first, N2, Q2, and N2 gases are emitted from each nozzle and ignited to generate an oxyhydrogen flame 9.Then, the valve 1 is
5 to the bubbler 13 side, and change the N2 gas to liquid BCl.
312 to generate BCl3+H2 gas, and discharge the BCl3 from the central nozzle into the oxyhydrogen flame 9. As a result, B2O3 in the form of a fine powder gas is generated, which is further condensed in the low-temperature part of the container 10 to form a plate-shaped B2O3 solid substance 11 of several mm square to several cm square. However, in the configuration shown in FIG. 2, there is a large amount of B2O3 scattering outside the recovery container 10, and because the distance between the oxyhydrogen flame 9 and the recovery container 10 cannot be large, condensation of B2O3 into the container 10 is difficult to occur. So,
There was a problem that the recovery rate of B2O3 based on the raw material was as low as about 20%, making it impractical.
以上の理由により、高純度のＩＩＩ−Ｖ族化合物半導体
単結晶を得るために高純度Ｂ２Ｏ３カプセル剤の実用的
な製造方法が必要であった。For the above reasons, a practical method for producing high-purity B2O3 capsules was needed in order to obtain high-purity III-V group compound semiconductor single crystals.
本発明は、上述の問題点に鑑みなされたものであり、ハ
ロゲン化ほう素の酸水素炎中の酸化反応による高純度Ｂ
２Ｏ３カプセル剤の実用的な製造方法を提供することに
ある。The present invention was made in view of the above-mentioned problems, and is made by producing high-purity B by an oxidation reaction of boron halide in an oxyhydrogen flame.
The object of the present invention is to provide a practical method for producing 2O3 capsules.
（問題点を解決するための手段）
上記問題点を解決するため、本発明による二酸化ほう素
の製造方法は、ハロゲン化ほう素、酸素、水素および窒
素の高純度ガスを原料とし、それらを酸水素炎中で反応
させ、生成した酸化ほう素を低温部に凝縮せしめる気相
合成法において、ｌ）冷却ガス吹き出し用の孔を設けた
四重ノズルを用いる工程、
２）酸化ほう素の飛散を防ぐ覆いを設ける工程、３）酸
水素炎と酸化ほう素凝縮部間の温度分布を制御するため
に、両者間の距離の調整と凝縮部の冷却を行なう工程、
４）酸化ほう素の成長を制御するための回転移動機構を
設ける工程、
の少なくとも一つの工程を含むことを特徴としている。(Means for Solving the Problems) In order to solve the above problems, the method for producing boron dioxide according to the present invention uses high purity gases of boron halide, oxygen, hydrogen and nitrogen as raw materials, and uses them as acid In a gas phase synthesis method in which boron oxide is reacted in a hydrogen flame and the generated boron oxide is condensed in a low-temperature part, 1) a step using a quadruple nozzle with holes for blowing out cooling gas; 2) a step to prevent the scattering of boron oxide. 3) A process of adjusting the distance between the oxyhydrogen flame and the boron oxide condensation part and cooling the condensation part in order to control the temperature distribution between the oxyhydrogen flame and the boron oxide condensation part; 4) A process of cooling the condensation part of the oxyhydrogen flame and the boron oxide condensation part; It is characterized by including at least one step of providing a rotational movement mechanism for control.
ハロゲン化ほう素の酸水素炎中の酸化反応による高純度
８２０３の製造方法において四重ノズルを用いることな
どにより微粉末ガス状のＢ２Ｏ３の飛散を防ぐと同時に
冷却効果を高めることができるので、Ｂ２Ｏ３の回収を
効率良く行なうことができる。さらに温度分布の調整に
より８２０３の高温部での生成と低温部での凝縮が制御
できるので、Ｂ２Ｏ３の固体を連続成長させて形状制御
しロッド状の固形物を得ることができる。In the production method of high-purity 8203 by the oxidation reaction of boron halide in an oxyhydrogen flame, by using a quadruple nozzle, etc., it is possible to prevent the scattering of B2O3 in the form of fine powder gas and at the same time increase the cooling effect. can be efficiently collected. Further, by adjusting the temperature distribution, the generation of 8203 in the high temperature part and the condensation in the low temperature part can be controlled, so that the solid B2O3 can be grown continuously and its shape can be controlled to obtain a rod-shaped solid.
（実施例１）
第３図に本発明の実施例１を示す、１６は酸水素炎バー
ナーで四重ノズル構造である。中央のノズル（ＢＣ１３
＋Ｈ２ガス用）はｐＢＮ製で、外側の三重のノズル（Ｎ
２および０２ガス用）は石英製のものを用いた。中央の
ノズルをｐＢＮ製にした理由は、石英製にした場合のＳ
ｉの混入を防ぐためである。中央ノズルには、氷の入っ
た冷却容器１４によって冷却されたＢＣｌ３１２の入っ
たバブラー１３を介してＢＣｌ３＋８２の混合ガスを供
給している。 Ｎ２、Ｎ２およびｏ２の各ガスは純化器
を通して第３図のようにバブラー導入管または各ノズル
に供給している。(Example 1) FIG. 3 shows Example 1 of the present invention. Reference numeral 16 denotes an oxyhydrogen flame burner having a quadruple nozzle structure. Center nozzle (BC13
+H2 gas) is made of pBN, and the outer triple nozzle (N
2 and 02 gases) were made of quartz. The reason why the center nozzle was made of pBN is that the S
This is to prevent i from being mixed in. A mixed gas of BCl3+82 is supplied to the central nozzle via a bubbler 13 containing BCl312 cooled by a cooling container 14 containing ice. Each of the N2, N2 and O2 gases is supplied to the bubbler introduction pipe or each nozzle through a purifier as shown in FIG.
１０はｐＢＮ製のＢ２Ｏ３回収容器で水冷機構１７によ
り冷却されている。10 is a B2O3 recovery container made of pBN and is cooled by a water cooling mechanism 17.
８２０３の生成方法は第２図の説明と同様である。同時
に生成したＨＣＩガスは容器１０後方に置いた排気装置
により回収しな。The method of generating 8203 is the same as that described in FIG. The HCI gas generated at the same time is collected by an exhaust device placed at the rear of the container 10.
本発明では、四重ノズルを用いることによって、最外郭
ノズルよりＮ２ガスを放射状に吹き出せる構造に特徴が
ある。これにより、高温のガス状のＢ２Ｏ３の冷却効果
を上げ、さらにＢ２Ｏ３の容器外への飛散を防げるので
、回収率を大幅に高めることができる。実施例１では、
原料ＢＣｌ３に対してＢ換算で４０％のＢ２Ｏ３を回収
することができた。さらに、実施例１では最外郭のノズ
ルからのＮ２ガスを冷却媒体を通して出すか、または液
体Ｎ２ガスに交換すれば高温Ｂ２Ｏ３の冷却効率が上が
るのでＢ２Ｏ３の回収率を４０％以上に高めることが可
能であった。The present invention is characterized by a structure in which N2 gas can be radially blown out from the outermost nozzle by using quadruple nozzles. This increases the cooling effect of the high-temperature gaseous B2O3 and prevents the B2O3 from scattering outside the container, making it possible to significantly increase the recovery rate. In Example 1,
It was possible to recover 40% B2O3 in terms of B based on the raw material BCl3. Furthermore, in Example 1, if the N2 gas from the outermost nozzle is discharged through a cooling medium or replaced with liquid N2 gas, the cooling efficiency of high-temperature B2O3 will increase, making it possible to increase the recovery rate of B2O3 to over 40%. Met.
（実施例２）
第４図は実施例２の説明図であって、Ｂ２Ｏ３の回収率
をさらに高めるための改善方法である。(Example 2) FIG. 4 is an explanatory diagram of Example 2, which is an improvement method for further increasing the recovery rate of B2O3.
Ｂ２Ｏ３の回収率を高めるためには、高温で生成したＢ
２Ｏ３を効果的に冷却すると同時に容器１０外への飛散
を防ぐことが重要である。In order to increase the recovery rate of B2O3, it is necessary to
It is important to effectively cool the 2O3 and at the same time prevent it from scattering outside the container 10.
実施例２は基本構成は実施例１と同じであるが、導管構
造の石英容器１８を用い、ａ）８２０３の外部への飛散
を防ぐ効果と、ｂ）回収容器ＩＯへ８２０３を導く効果
によりＢ２Ｏ３の回収率を７０％以上に高めることがで
きた。さらに、覆い構造にすることにより有害なＨＣＩ
ガスを外部に漏れることなく排気することができる。一
方、第４図のような導管１８を用いると酸水素炎９と回
収容器１０の距離を変えてもガス状のＢ２Ｏ３は確実に
回収容器に導かれるので、以下の効果が生じる。Embodiment 2 has the same basic configuration as Embodiment 1, but uses a quartz container 18 with a conduit structure, which has the effect of a) preventing the scattering of 8203 to the outside, and b) the effect of guiding 8203 to the recovery container IO. We were able to increase the recovery rate to over 70%. Furthermore, the cover structure prevents harmful HCI.
Gas can be exhausted without leaking to the outside. On the other hand, when a conduit 18 as shown in FIG. 4 is used, gaseous B2O3 is reliably guided to the recovery container even if the distance between the oxyhydrogen flame 9 and the recovery container 10 is changed, so that the following effects are produced.
すなわち、この距離を調整して温度分布を最適化すると
８２０３の高温部での生成と低温部での凝縮が制御可能
となり、容器ＩＯ内に８２０３の大きな固形物ができる
。すなわち、８２０３を連続成長させることができる。That is, by adjusting this distance and optimizing the temperature distribution, it is possible to control the generation of 8203 in the high temperature part and the condensation in the low temperature part, and a large solid substance of 8203 is created in the container IO. In other words, 8203 can be grown continuously.
この方法により得られた８２０３固形物は大きな塊とな
るので後処理が容易であり、表面積は物理的に小さくな
るので水分および不純物の混入を少なくすることができ
た。Since the 8203 solid obtained by this method forms large lumps, post-processing is easy, and the surface area becomes physically small, so contamination with water and impurities can be reduced.
（実施例３）
第５図は実施例３の説明図である。実施例３は実施例２
を８２０３の固形物成長法として発展させたものである
。１９は四重ノズルであるが、最外郭の石英壁は導管構
造となっている。２０はリング状に並んだ石英パイプで
液体窒素または冷却したＮ２ガスを吹き出し、ガス状の
８２０３を冷却するのに用いる。２１は回転移動機構と
連結している金属円板とロッドから成り、Ｂ２Ｏ３固形
物の成長速度に合わせて矢印の方向に移動させる。実施
例３では、酸水素炎９と円板２１面との距離を調整し、
ノズル（石英パイプ）２０より吹き出す窒素の吹き出し
量を制御することによりＢ２Ｏ３固形物１１を円柱状に
連続成長させることができた。すなわち、実施例３では
高純度Ｂ２Ｏ３が高効率に得られるだけでなく、Ｂ２Ｏ
３固形物１１の形状制御を行なうことができた。この方
法を用いれば、円柱状の８２０３１１を輪切りにするだ
けで、結晶成長用のルツボ形状に合わせたＢ２Ｏ３カプ
セル剤として用いることができる。(Example 3) FIG. 5 is an explanatory diagram of Example 3. Example 3 is Example 2
8203 was developed as a solid growth method. No. 19 is a quadruple nozzle, but the outermost quartz wall has a conduit structure. 20 is a quartz pipe arranged in a ring shape and is used to blow out liquid nitrogen or cooled N2 gas to cool the gaseous 8203. Reference numeral 21 consists of a metal disk and a rod connected to a rotational movement mechanism, which is moved in the direction of the arrow in accordance with the growth rate of the B2O3 solids. In Example 3, the distance between the oxyhydrogen flame 9 and the surface of the disk 21 was adjusted,
By controlling the amount of nitrogen blown out from the nozzle (quartz pipe) 20, it was possible to continuously grow the B2O3 solid material 11 in a cylindrical shape. In other words, in Example 3, not only high purity B2O3 can be obtained with high efficiency, but also B2O
3. The shape of the solid material 11 could be controlled. By using this method, simply by cutting cylindrical 820311 into rings, it can be used as a B2O3 capsule that matches the shape of a crucible for crystal growth.
（発明の効果）
以上説明したように、本発明によれば高純度Ｂ２Ｏ３カ
プセル剤を大量に製造することができる。したがって、
これまで高純度酸化ほう素液体カプセル剤が使用できな
かった化合物半導体単結晶引き上げ法に適用すれば、高
純度結晶が育成できるので新しい電子光学的デバイスの
実現に役立てることができる。(Effects of the Invention) As explained above, according to the present invention, high purity B2O3 capsules can be produced in large quantities. therefore,
If applied to a method for pulling compound semiconductor single crystals, for which high-purity boron oxide liquid capsules could not be used until now, high-purity crystals can be grown, making it useful for the realization of new electro-optical devices.
第１図は液体カプセル封じ引き上げ法の原理を説明した
説明図、第２図は従来の方法を説明した説明図、第３図
は本発明による第一の実施例の説明図、第４図は本発明
による第二の実施例の説明図、第５図は本発明による第
三の実施例の説明図である。
１・・・ルツボ、２・・・融液（融解した単結晶原料）
、３・・・種結晶、４・・・単結晶、５・・・液体カプ
セル、６・・・高圧結晶成長容器、７・・・軸シール、
８・・・三重ノズル、９・・・酸水素炎、１０・・・回
収容器、１１・・・Ｂ２Ｏ２固形物、１２・・・ＢＣｌ
２（液体）、１３・・・バブラー、１４・・・氷水使用
の冷却容器、１５・・・バルブ、１６・・・四重ノズル
、１７・・・水冷機構、１８・・・石英容器、１９・・
・導管付き四重ノズル、２０・・・石英パイプ、２１・
・・回転移動機構付き回転基板台。
第１図FIG. 1 is an explanatory diagram explaining the principle of the liquid capsule sealing and pulling method, FIG. 2 is an explanatory diagram explaining the conventional method, FIG. 3 is an explanatory diagram of the first embodiment of the present invention, and FIG. FIG. 5 is an explanatory diagram of a second embodiment according to the present invention, and FIG. 5 is an explanatory diagram of a third embodiment according to the present invention. 1... Crucible, 2... Melt (melted single crystal raw material)
, 3... Seed crystal, 4... Single crystal, 5... Liquid capsule, 6... High pressure crystal growth container, 7... Shaft seal,
8... Triple nozzle, 9... Oxygen hydrogen flame, 10... Collection container, 11... B2O2 solids, 12... BCl
2 (Liquid), 13... Bubbler, 14... Cooling container using ice water, 15... Valve, 16... Quadruple nozzle, 17... Water cooling mechanism, 18... Quartz container, 19・・・
・Quadruple nozzle with conduit, 20...Quartz pipe, 21・
...Rotating board stand with rotation movement mechanism. Figure 1
Claims (1)
度ガスを原料とし、それらを酸水素炎中で反応させ、生
成した酸化ほう素を低温部に凝縮せしめる気相合成法に
おいて、 １）冷却ガス吹き出し用の孔を設けた四重ノズルを用い
る工程、 ２）酸化ほう素の飛散を防ぐ覆いを設ける工程、 ３）酸水素炎と酸化ほう素凝縮部間の温度分布を制御す
るために、両者間の距離の調整と凝縮部の冷却を行なう
工程、 ４）酸化ほう素の成長を制御するための回転移動機構を
設ける工程、 の少なくとも一工程を含むことを特徴とする酸化ほう素
の製造方法。(1) In a gas phase synthesis method that uses high-purity gases such as boron halides, oxygen, hydrogen, and nitrogen as raw materials, reacts them in an oxyhydrogen flame, and condenses the generated boron oxide in a low-temperature part. A process using a quadruple nozzle with holes for blowing out cooling gas, 2) A process to provide a cover to prevent boron oxide from scattering, 3) To control the temperature distribution between the oxyhydrogen flame and the boron oxide condensation section. , adjusting the distance between the two and cooling the condensing part; 4) providing a rotational movement mechanism for controlling the growth of boron oxide. Production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14563689A JP2883955B2 (en) | 1989-06-08 | 1989-06-08 | Method for producing boron oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14563689A JP2883955B2 (en) | 1989-06-08 | 1989-06-08 | Method for producing boron oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0312320A true JPH0312320A (en) | 1991-01-21 |
| JP2883955B2 JP2883955B2 (en) | 1999-04-19 |
Family
ID=15389595
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14563689A Expired - Fee Related JP2883955B2 (en) | 1989-06-08 | 1989-06-08 | Method for producing boron oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2883955B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110217803A (en) * | 2019-06-28 | 2019-09-10 | 广东先导先进材料股份有限公司 | A kind of system and method preparing long brilliant grade primary oxidation boron |
-
1989
- 1989-06-08 JP JP14563689A patent/JP2883955B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110217803A (en) * | 2019-06-28 | 2019-09-10 | 广东先导先进材料股份有限公司 | A kind of system and method preparing long brilliant grade primary oxidation boron |
| CN110217803B (en) * | 2019-06-28 | 2024-02-13 | 广东先导微电子科技有限公司 | System and method for preparing primary boron oxide with long crystal grade |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2883955B2 (en) | 1999-04-19 |
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