JPH052613Y2 - - Google Patents
Info
- Publication number
- JPH052613Y2 JPH052613Y2 JP3750887U JP3750887U JPH052613Y2 JP H052613 Y2 JPH052613 Y2 JP H052613Y2 JP 3750887 U JP3750887 U JP 3750887U JP 3750887 U JP3750887 U JP 3750887U JP H052613 Y2 JPH052613 Y2 JP H052613Y2
- Authority
- JP
- Japan
- Prior art keywords
- inp
- melt
- crucible
- polycrystal
- excess
- 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
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000000155 melt Substances 0.000 claims description 9
- 239000004065 semiconductor Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 3
- 229910021478 group 5 element Inorganic materials 0.000 claims description 3
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 59
- 229910052698 phosphorus Inorganic materials 0.000 description 12
- 239000011574 phosphorus Substances 0.000 description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 239000000565 sealant Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Description
【考案の詳細な説明】
［産業上の利用分野］
本考案は、化合物半導体多結晶育成用坩堝に関
するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a crucible for growing compound semiconductor polycrystals.
［従来の技術］
例えばインジウム・リン（InP）の大結晶を高
圧液体封止方式を用いて育成するような場合は、
高圧引上装置内にセツトされた石英坩堝の中にIn
を入れ、このInを溶融させたIn融液の表面を封止
剤で覆いながら、In融液にリンの蒸気を注入して
反応させてInPの融液を合成し、その後冷却して
InP多結晶を育成する。[Prior art] For example, when growing large crystals of indium phosphide (InP) using a high-pressure liquid sealing method,
In a quartz crucible set in a high-pressure pulling device.
While covering the surface of the In melt with a sealant, phosphorus vapor is injected into the In melt to cause a reaction to synthesize an InP melt, which is then cooled.
Grow InP polycrystals.
更に詳しく述べると、例えば６インチの石英坩
堝を用いた場合、この坩堝にInを2500ｇ、液体封
止剤として酸化ボロン（B2O3）を500ｇ入れ、引
上装置内の圧力をアルゴン（Ar）ガスを用いて
40Kg／cm2とし、装置上方に固形のリンを800ｇ収
容したリン保管部（図示せず）を設ける。このよ
うな条件で坩堝を加熱してIn融液を1100℃に保
ち、このIn融液に上記リン保管部からこのリン保
管部を加熱することにより生じたリンの蒸気を注
入して反応せしめ、InP融液を合成し終えた後、
徐々に降温させてInP多結晶を育成する。 To explain in more detail, for example, when a 6-inch quartz crucible is used, 2500 g of In and 500 g of boron oxide (B 2 O 3 ) as a liquid sealant are placed in the crucible, and the pressure inside the pulling device is changed to argon (Ar). ) using gas
40 kg/cm 2 , and a phosphorus storage section (not shown) containing 800 g of solid phosphorus is provided above the device. The crucible is heated under these conditions to maintain the In melt at 1100°C, and phosphorus vapor generated by heating this phosphorus storage part is injected into the In melt from the above phosphorus storage part to cause a reaction. After completing the synthesis of InP melt,
InP polycrystals are grown by gradually lowering the temperature.
しかしながら、InPの融点でのリンの解離圧が
非常に高いため、InP融液からリンが揮散しやす
く、InP融液の表面を液体封止剤で覆つても、In
とリンの組成比のずれのないInP融液或いはリン
が過剰なInP融液を合成することは困難であり、
通常Inが過剰に含まれたInP融液が合成されてし
まう。 However, since the dissociation pressure of phosphorus at the melting point of InP is very high, phosphorus easily volatilizes from the InP melt, and even if the surface of the InP melt is covered with a liquid sealant, the
It is difficult to synthesize an InP melt with a consistent composition ratio of phosphorus and phosphorus, or an InP melt with an excess of phosphorus.
Usually, an InP melt containing excessive In is synthesized.
上記のようにしてInP多結晶を育成させたとき
のInP融液の合成効率は、InPの多結晶の重量か
ら計算すると98％であり、従つてInP多結晶に２
％の過剰なInが含まれていることになる。 When InP polycrystals are grown as described above, the synthesis efficiency of the InP melt is 98% when calculated from the weight of the InP polycrystals.
% of excess In is included.
第４図は合成反応完了後のInP融液の状態を示
す説明図、第５図及び第６図はInP融液を冷却し
てほぼ全体を固化させた状態を示す説明図であ
る。 FIG. 4 is an explanatory diagram showing the state of the InP melt after the synthesis reaction is completed, and FIGS. 5 and 6 are explanatory diagrams showing the state where the InP melt is cooled and almost entirely solidified.
図において１は石英坩堝、２は液体封止剤、３
はInP融液、４はInP融液中に存在する過剰なIn、
５はInPの多結晶を示す。 In the figure, 1 is a quartz crucible, 2 is a liquid sealant, and 3 is a quartz crucible.
is the InP melt, 4 is the excess In present in the InP melt,
5 indicates InP polycrystal.
第４図は比重5.05ｇ／cm3のInP融液３より比重
の大きいIn４の融液（比重7.28ｇ／cm3）が熱対流
によりInP融液３の中に一様に分布している状態
を示しているが、この状態からInP融液３の表面
から一様に冷却すると、第５図及び第６図に示す
ように過剰なInは取込まれることなくInP多結晶
５が析出され、このInP多結晶５は残つたInP融
液３の上に浮んだ状態になる。 Figure 4 shows a state in which In4 melt (specific gravity 7.28 g/cm 3 ), which has a higher specific gravity than InP melt 3 with specific gravity 5.05 g/cm 3 , is uniformly distributed in InP melt 3 due to thermal convection. However, when the surface of the InP melt 3 is uniformly cooled from this state, InP polycrystals 5 are precipitated without taking in excess In, as shown in FIGS. 5 and 6. This InP polycrystal 5 becomes floating on the remaining InP melt 3.
このとき、InP融液３は過剰なIn４の融液を高
濃度に含んだものとなり、第５図に示すように
InP多結晶５の底面が下に凸状になつたり、また
第６図に示すようにInP多結晶５の底面が下に凹
状になる。 At this time, the InP melt 3 contains a high concentration of excess In4 melt, as shown in Figure 5.
The bottom surface of the InP polycrystal 5 becomes convex downward, or the bottom surface of the InP polycrystal 5 becomes concave downward as shown in FIG.
このように、多結晶化が進行してInP融液３に
含まれるIn４の融液が高濃度になると、InP融液
３の融点が著しく降下して過冷却状態となり、
InP多結晶５の最終凝固部は急速に固化してしま
うため、この際排出できなつたIn４を多結晶５内
に取込んでしまう。 As described above, as polycrystalization progresses and the In4 melt contained in the InP melt 3 becomes highly concentrated, the melting point of the InP melt 3 drops significantly and becomes supercooled.
Since the final solidified portion of the InP polycrystal 5 solidifies rapidly, the In4 that could not be discharged at this time is taken into the polycrystal 5.
［考案が解決しようとする問題点］
上述したように、例えばInPの多結晶化を育成
する場合は、坩堝の中でInP融液を合成し、次い
でInP融液を固化して結晶を育成させるのである
が、育成したInP多結晶の縦切断面を観察してみ
ると、第７図に示すように結晶最終凝固部、即ち
坩堝１の底の部分に広範囲にわたつてIn４が含ま
れていることが認められた。[Problems to be solved by the invention] As mentioned above, for example, when growing polycrystalline InP, an InP melt is synthesized in a crucible, and then the InP melt is solidified to grow crystals. However, when observing the longitudinal cross-section of the grown InP polycrystal, it is found that In4 is widely contained in the final solidification area of the crystal, that is, the bottom of crucible 1, as shown in Figure 7. This was recognized.
このようにInPの融液３を合成する場合には、
Inが過剰なInP融液となる場合が多く、そのまま
多結晶を育成すると第７図に示すような広範囲に
In４を含んだ多結晶しか得られないことになる。
この過剰In４を含むInP多結晶から引き上げ法に
よりInP単結晶を成長させようとすると、成長中
の単結晶胴体部の途中から多結晶となり、高品質
の単結晶を得ることはできない。 When synthesizing InP melt 3 in this way,
In many cases, the InP melt contains excess In, and if polycrystals are grown as is, it will spread over a wide area as shown in Figure 7.
This means that only polycrystals containing In4 can be obtained.
If an attempt is made to grow an InP single crystal from this InP polycrystal containing excess In4 by a pulling method, the polycrystalline becomes polycrystalline from the middle of the growing single crystal body, making it impossible to obtain a high-quality single crystal.
よつて、高品質のInP単結晶を得るためには、
過剰Inを含まない高品質の多結晶が必要であり、
多結晶底部に残留した過剰Inを除去する必要があ
る。この過剰Inの除去は、研削機等を用いて行わ
れるが、この除去作業を多結晶の広範囲部分につ
いて行うには、かなりの労力と時間とを必要とす
る。 Therefore, in order to obtain a high quality InP single crystal,
A high quality polycrystal without excess In is required,
It is necessary to remove excess In remaining at the bottom of the polycrystal. This excess In is removed using a grinder or the like, but it requires considerable effort and time to perform this removal over a wide area of the polycrystal.
研削後の多結晶の重量を測定すると研削前に比
べて約30％以上減少していることが認められてい
るが、これはIn４を含んでいる部分が広範囲に亘
つているためで、このように過剰In４の多結晶へ
の取込みは歩留りを低下させる大きな要因とな
る。 When measuring the weight of the polycrystal after grinding, it has been found that the weight has decreased by more than 30% compared to before grinding, but this is because the area containing In4 is spread over a wide area. The incorporation of excess In4 into the polycrystal is a major factor in reducing yield.
本考案の目的は、化合物半導体多結晶育成用時
に歩留りを大幅に向上する化合物半導体多結晶育
成用坩堝を提供することにある。 An object of the present invention is to provide a crucible for growing compound semiconductor polycrystals that greatly improves the yield when growing compound semiconductor polycrystals.
［問題点を解決するための手段］
本考案の要旨は、収容させた族元素の融液に
Ｖ族元素の蒸気を反応させて合成した前記族元
素及びＶ族元素からなる化合物半導体の融液を冷
却固化して多結晶を育成するための化合物半導体
多結晶育成用坩堝において、該坩堝の底部に、前
記族元素の過剰分を高濃度に含む前記融液が固
化されるポケツト部が設けられていることにあ
り、これによつて族元素の過剰分を容易に除去
できるようにして歩留りを向上させ目的の達成を
計つたものである。[Means for Solving the Problems] The gist of the present invention is to provide a melt of a compound semiconductor composed of a group element and a group V element, which is synthesized by reacting a vapor of a group V element to a contained melt of a group element. In a compound semiconductor polycrystal growth crucible for growing polycrystals by cooling and solidifying the crucible, a pocket portion is provided at the bottom of the crucible in which the melt containing a high concentration of an excess of the group element is solidified. By this, the excess of group elements can be easily removed to improve the yield and achieve the purpose.
［作用］
高圧チヤンバ内に収納された坩堝内の封止剤で
覆われた例えばInPの融液からInPの多結晶を育
成させる場合には、合成させたInP融液のInとＰ
の組成比がずれてInが過剰となり、固化したInP
多結晶の底部に過剰Inが取込まれてしまうという
現象を生ずる。そこで本考案では、坩堝の底部に
ポケツト部を設けて、このポケツト内で過剰Inを
高濃度に含む融液を固化させるようにし、このポ
ケツト内で固化した多結晶を研削するだけで高品
質のInP結晶が得られる。従つて、従来のように
結晶の底面を広範囲で研削する必要がなくなり、
作業効率を向上させ、過大な研削を軽減して歩留
を向上させることができる。[Operation] When growing polycrystals of InP from, for example, an InP melt covered with a sealant in a crucible housed in a high-pressure chamber, In and P of the synthesized InP melt are grown.
The composition ratio of InP deviates, resulting in excess In and solidified InP.
A phenomenon occurs in which excess In is incorporated into the bottom of the polycrystal. Therefore, in the present invention, a pocket is provided at the bottom of the crucible, and the melt containing a high concentration of excess In is solidified within this pocket, and high-quality polycrystals can be obtained by simply grinding the polycrystal that has solidified within this pocket. InP crystal is obtained. Therefore, it is no longer necessary to grind the bottom surface of the crystal over a wide area as in the past.
It is possible to improve work efficiency, reduce excessive grinding, and improve yield.
［実施例］ 以下、本考案の一実施例を図により説明する。[Example] Hereinafter, one embodiment of the present invention will be described with reference to the drawings.
第１図は本考案の化合物半導体多結晶育成用坩
堝の一実施例の縦断面図を示す。 FIG. 1 shows a longitudinal sectional view of an embodiment of a crucible for growing compound semiconductor polycrystals according to the present invention.
図において６は坩堝を示し、７はその底部に設
けられたポケツト部を示す。なお、図において、
第４図〜第６図に示してある融液３、封止剤２に
ついては図示を省略してあるが、多結晶を育成す
る場合は従来と同様に高圧液体封止方式を用いて
育成する。なお、本実施例の坩堝６は、第５図に
示すような析出する多結晶５の底部が下に凸状と
なり、過剰In４を高濃度に含むInPが坩堝底部の
周辺部に残る場合に効果がある。 In the figure, 6 indicates a crucible, and 7 indicates a pocket provided at the bottom thereof. In addition, in the figure,
Although illustrations of the melt 3 and sealant 2 shown in Figures 4 to 6 are omitted, when growing polycrystals, they are grown using a high-pressure liquid sealing method as in the past. . The crucible 6 of this example is effective when the bottom of the precipitated polycrystal 5 is convex downward as shown in FIG. 5, and InP containing a high concentration of excess In4 remains in the periphery of the bottom of the crucible. There is.
本実施例の坩堝を用いてInP多結晶を育成させ
たところ、InP多結晶の合成効率は従来と同様に
98％であつたが、多結晶の縦断面を観察すると第
２図に示すように過剰In４はポケツト部７に集中
していることが確認された。このポケツト部７の
多結晶部分を研削することにより、過剰In４は完
全に除去され、高品質のInP多結晶を簡単に得る
ことができた。 When InP polycrystals were grown using the crucible of this example, the synthesis efficiency of InP polycrystals was the same as before.
However, when the longitudinal section of the polycrystal was observed, it was confirmed that the excess In4 was concentrated in the pocket portion 7, as shown in FIG. By grinding the polycrystalline portion of the pocket portion 7, the excess In4 was completely removed and a high quality InP polycrystal could be easily obtained.
研削後の多結晶の重量を求めたところ、研削前
の重量の90％であり、損失を10％に抑えることが
できた。従来の損失は30％以上であり、これに比
べて大幅に歩留りを向上させることができた。 The weight of the polycrystal after grinding was determined to be 90% of the weight before grinding, and the loss could be kept to 10%. The conventional loss was more than 30%, and compared to this, we were able to significantly improve the yield.
又、上記のポケツト部７の多結晶の研削は極め
て容易に行うことができるので研削作業効率を大
幅に改善することができた。 Further, since the polycrystal of the pocket portion 7 can be ground very easily, the efficiency of the grinding operation can be greatly improved.
第３図は本考案の他の実施例を示すもので、坩
堝６の底部中央部ポケツト部８を設けた場合であ
る。本実施例の坩堝６は、第６図に示すような析
出する多結晶５の底部が下に凹状となり、過剰In
４を高濃度に含むInPが坩堝底部の中央部に残る
場合に効果がある。従つて、過剰In４を高濃度に
含むInP融液はポケツト部８内で固化し、多結晶
を取出した後、このポケツト部８内の多結晶を研
削することにより高品質の多結晶を容易に得るこ
とができる。 FIG. 3 shows another embodiment of the present invention, in which a pocket 8 is provided at the center of the bottom of the crucible 6. In the crucible 6 of this example, the bottom of the precipitated polycrystal 5 is concave downward as shown in FIG.
This is effective when InP containing a high concentration of 4 remains in the center of the bottom of the crucible. Therefore, the InP melt containing a high concentration of excess In4 solidifies in the pocket part 8, and after taking out the polycrystal, the polycrystal in the pocket part 8 is ground to easily produce high-quality polycrystals. Obtainable.
なお、上記各実施例ではポケツト部が半円筒形
の場合について述べたが、これは任意の形状、寸
法に選定することができ、要はポケツト部を、過
剰Inを高濃度に含むInP融液が全て固化できる大
きさ又はそれよりも若干大きいものにすればよ
い。 In each of the above embodiments, the case where the pocket part is semi-cylindrical is described, but this can be selected to have any shape and dimensions.In short, the pocket part is made of InP melt containing a high concentration of excess In. The size may be such that all of the particles can be solidified, or slightly larger than that.
［考案の効果］
以上に説明した如く、本考案によれば、坩堝の
底部にポケツト部を設け、多結晶の育成時に過剰
に存在する族元素を含む融液をこのポケツト部
内で固化させるようにしたことにより、ポケツト
部内で固化した多結晶部分のみを研削するだけで
高品質の多結晶を得ることができるようになり、
研削作業能率及び歩留まりを大幅に向上させるこ
とができる、という顕著な効果を奏する。[Effect of the invention] As explained above, according to the invention, a pocket is provided at the bottom of the crucible, and the melt containing group elements present in excess during polycrystal growth is solidified within the pocket. By doing this, it is now possible to obtain high-quality polycrystals by simply grinding only the polycrystalline parts that have solidified inside the pocket.
This has the remarkable effect of significantly improving grinding efficiency and yield.
第１図は本考案の化合物半導体多結晶育成用坩
堝の一実施例を示す縦断面図、第２図は本考案の
坩堝を使用して育成したInP多結晶の縦切断面を
示す縦断面図、第３図は他の実施例を示す縦断面
図、第４図は合成反応完了後のInP融液の状態を
示す説明図、第５図及び第６図はInP融液を冷却
してほぼ全体を固化させた状態を示す説明図、第
７図は従来の坩堝を使用して育成したInP多結晶
の縦切断面を示す縦断面図である。
１，６……坩堝、２……封止剤、３……InP融
液、４……過剰In、５……InP多結晶、７，８…
…ポケツト部。
FIG. 1 is a vertical cross-sectional view showing an embodiment of the compound semiconductor polycrystal growth crucible of the present invention, and FIG. 2 is a vertical cross-sectional view showing a vertical cross-section of an InP polycrystal grown using the crucible of the present invention. , FIG. 3 is a longitudinal cross-sectional view showing another example, FIG. 4 is an explanatory diagram showing the state of the InP melt after the synthesis reaction is completed, and FIGS. 5 and 6 are approximately the same after cooling the InP melt. An explanatory view showing the entire solidified state, and FIG. 7 is a vertical cross-sectional view showing a vertical cross section of an InP polycrystal grown using a conventional crucible. 1, 6... Crucible, 2... Sealing agent, 3... InP melt, 4... Excess In, 5... InP polycrystal, 7, 8...
...Pocket section.
Claims (1)
反応させて合成した前記族及びＶ族元素からな
る化合物半導体の融液を冷却固化して多結晶を育
成するための化合物半導体多結晶育成用坩堝にお
いて、該坩堝の底部に、前記族元素の過剰分を
高濃度に含む前記融液が固化されるポケツト部が
設けられていることを特徴とする化合物半導体多
結晶育成用坩堝。 A crucible for growing compound semiconductor polycrystals, which is used to grow polycrystals by cooling and solidifying a melt of a compound semiconductor composed of Group and V elements, the melt being synthesized by reacting a melt of a Group element contained therein with vapor of a Group V element, characterized in that a pocket portion is provided at the bottom of the crucible, in which the melt containing a high concentration of an excess of the Group element is solidified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3750887U JPH052613Y2 (en) | 1987-03-13 | 1987-03-13 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3750887U JPH052613Y2 (en) | 1987-03-13 | 1987-03-13 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63145867U JPS63145867U (en) | 1988-09-27 |
| JPH052613Y2 true JPH052613Y2 (en) | 1993-01-22 |
Family
ID=30848898
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3750887U Expired - Lifetime JPH052613Y2 (en) | 1987-03-13 | 1987-03-13 |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH052613Y2 (en) |
-
1987
- 1987-03-13 JP JP3750887U patent/JPH052613Y2/ja not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63145867U (en) | 1988-09-27 |
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