JPH09169589A - Production of single crystal and apparatus for production therefor - Google Patents
Production of single crystal and apparatus for production thereforInfo
- Publication number
- JPH09169589A JPH09169589A JP34689995A JP34689995A JPH09169589A JP H09169589 A JPH09169589 A JP H09169589A JP 34689995 A JP34689995 A JP 34689995A JP 34689995 A JP34689995 A JP 34689995A JP H09169589 A JPH09169589 A JP H09169589A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- partition
- single crystal
- partition body
- plates
- 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
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、るつぼ内に少なくとも
１枚の仕切板からなる仕切体を設置することによって、
その仕切体内の空間に板状の単結晶を製造するための製
造方法とその製造装置に関する。BACKGROUND OF THE INVENTION The present invention provides a partition body comprising at least one partition plate in a crucible.
The present invention relates to a manufacturing method and a manufacturing apparatus for manufacturing a plate-shaped single crystal in the space inside the partition.
【０００２】[0002]
【従来の技術】従来より、金属や酸化物あるいは半導体
の単結晶を製造する方法としては、原料融液中に種結晶
（シード）を入れ、この種結晶についた単結晶を回転さ
せながら引き上げるチョクラルスキー法や、筒状の縦型
あるいは横型ボートの中に原料を入れて融液化した後に
その融液の温度をボート下部から下げて行き、ボート内
に結晶を成長させるボート法の他、水平あるいは垂直ブ
リッジマン法や、ＶＧＦあるいはＨＧＦ法といわれる垂
直および水平グラジエントフリーズ法が知られている。2. Description of the Related Art Conventionally, as a method for producing a single crystal of a metal, an oxide, or a semiconductor, a seed crystal is placed in a raw material melt, and a single crystal attached to the seed crystal is rotated and pulled up. In addition to the Larsky method, the boat method of putting raw materials in a cylindrical vertical or horizontal boat and melting it and then lowering the temperature of the melt from the bottom of the boat to grow crystals in the boat, Alternatively, the vertical Bridgman method and the vertical and horizontal gradient freeze methods called VGF or HGF method are known.
【０００３】これらの製造法によって得られた単結晶体
はいずれもそのるつぼ径に沿ったバルク単結晶体がほと
んどであり、得られた単結晶体をスライスすることによ
って所望の厚みの板状体とするのが通常の手法であっ
た。Most of the single crystal bodies obtained by these production methods are bulk single crystal bodies along the diameter of the crucible, and a plate-like body having a desired thickness is obtained by slicing the obtained single crystal body. Was the usual method.
【０００４】[0004]
【発明が解決しようとする課題】上述のように、従来法
では、得られたバルク単結晶体から所望形状の板材をス
ライスしていたため、その工程にある程度の所要時間を
必要とし、その上、対象物によっては例えばＧａＡｓの
ような有害な半導体等の残滓の発生が避けられないとい
う欠点があった。As described above, according to the conventional method, a plate material having a desired shape is sliced from the obtained bulk single crystal body, so that the process requires a certain amount of time, and further, Depending on the object, there is a drawback that the generation of residues of harmful semiconductors such as GaAs cannot be avoided.
【０００５】本発明は、従来法に代わって、原料から直
接目的形状の板状の単結晶を製造できる新規な製造方法
及びそのための製造装置の開発を目的とするものであ
る。An object of the present invention is to develop a novel manufacturing method and a manufacturing apparatus therefor capable of directly manufacturing a plate-shaped single crystal having a desired shape from raw materials instead of the conventional method.
【０００６】[0006]
【課題を解決するための手段】本発明者等はかかる課題
を解決するために鋭意研究したところ、従来法で使用さ
れるるつぼ内に特定形状の仕切体を設置することによっ
て所望の厚みを有する単結晶体を得ることができること
を見出し、本発明を提供すことができた。Means for Solving the Problems The inventors of the present invention have conducted extensive studies to solve the above problems, and found that a desired shape can be obtained by installing a partition of a specific shape in the crucible used in the conventional method. It was found that a single crystal body can be obtained, and the present invention can be provided.
【０００７】すなわち本発明の第１は、るつぼ内に少な
くとも１枚の仕切板からなる仕切体を設け、該仕切体内
の空間において板状の単結晶を製造することを特徴とす
る単結晶の製造方法である。That is, the first aspect of the present invention is the production of a single crystal characterized in that a partition body comprising at least one partition plate is provided in the crucible and a plate-shaped single crystal is produced in the space inside the partition body. Is the way.
【０００８】本発明の第２は、結晶製造るつぼと、その
周りに配置された加熱領域変動可能なヒーターとを主要
部とする結晶製造装置において、上記るつぼ内に縦状ま
たは横状の少なくとも１枚の仕切板からなる仕切体を設
置してあることを特徴とする単結晶の製造装置に関す
る。A second aspect of the present invention is a crystal production apparatus, which comprises a crystal production crucible and a heater disposed around the crystal production crucible as a variable heating region, wherein at least one vertical or horizontal shape is provided in the crucible. The present invention relates to an apparatus for producing a single crystal, characterized in that a partition body composed of a plurality of partition plates is installed.
【０００９】[0009]
【作用】本発明法の単結晶育成手段としては、従来公知
のＶＧＦ法や垂直または水平ブリッジマン法を用いるこ
とができる。装置内部に設けるるつぼとしては、低伝導
性のビトロカーボン（日本カーボン社製ガラス質カーボ
ン材の商品名）やグラファイトからなるるつぼを用い、
該るつぼ内に同材質の板状仕切、少なくとも１枚の仕切
板からなる仕切体を縦状または横状に装入する。As the single crystal growing means of the method of the present invention, the conventionally known VGF method or the vertical or horizontal Bridgman method can be used. As the crucible provided inside the device, a crucible made of graphite with low conductivity (trade name of vitreous carbon material manufactured by Nippon Carbon Co., Ltd.) or graphite is used.
Into the crucible, a plate-shaped partition made of the same material and a partition body composed of at least one partition plate are loaded vertically or horizontally.
【００１０】この場合、仕切板は１枚以上あればよく、
この仕切板の間隔を実施例１においては１．５mmの幅と
したが、これは目的とする任意の厚みに調節すればよ
い。また、縦型の仕切体は、断面がＵ字形の仕切板を複
数枚重ねて最後に平板を重ねた積層構造となっており、
この積層体がるつぼ内部に設置されている。In this case, one or more partition plates are enough,
In the first embodiment, the interval between the partition plates is set to 1.5 mm, but it may be adjusted to any desired thickness. Further, the vertical partition body has a laminated structure in which a plurality of partition plates having a U-shaped cross section are stacked, and finally flat plates are stacked,
This laminated body is installed inside the crucible.
【００１１】また他の仕切体の形態として実施例４に示
すように、仕切板をるつぼ内に平行状に配置し、るつぼ
上部から融解金属を結晶連絡ノズルを通して、各仕切板
によって得られた円板状の空間に融液が充填される構造
となっている。As another embodiment of the partition body, as shown in Example 4, the partition plates are arranged in parallel in the crucible, and the molten metal is passed from the upper part of the crucible through the crystal connecting nozzle to obtain a circle obtained by each partition plate. The plate-like space is filled with the melt.
【００１２】この仕切体を用いることによって、原料で
ある銅、亜鉛、錫、ビスマスの金属や、ＧａＡｓ、Ｉｎ
Ａｓ等の化合物半導体を融解して得た融液を仕切板の間
隙に流し込み、底部はシードに接合するようにした。By using this partition, metals such as copper, zinc, tin and bismuth as raw materials, GaAs and In
A melt obtained by melting a compound semiconductor such as As was poured into the gap of the partition plate so that the bottom portion was joined to the seed.
【００１３】以下、図面を参照して本発明法並びに本発
明装置を詳細に説明するが、本発明の範囲はこれらに限
定されるものでない。Hereinafter, the method of the present invention and the apparatus of the present invention will be described in detail with reference to the drawings, but the scope of the present invention is not limited thereto.
【００１４】[0014]
【実施例１】図１に本発明で使用する装置の一例の概略
を示す。１は原料、２はるつぼ、３はシード、４は封止
材、５は縦状仕切体、６は上部ヒーター、７は中央部ヒ
ーター、８は下部ヒーター、９は水冷ジャケット、１０
は断熱材をそれぞれ表わす。該装置内に設けられたグラ
ファイト製るつぼ２の中に、３枚のＵ字形仕切り板と１
枚の平板を積層して構成した縦状仕切体５（図２に断面
を示す）を縦状に挿入した後、るつぼ２内に金属原料１
として６Ｎ高純度銅１００ｇを入れ、縦状仕切体５上部
の原料１を１１５０℃で融解すると共に、該仕切板５下
部とシード３の共通部分の温度を１０８３℃となるよう
に調整した。[Embodiment 1] FIG. 1 schematically shows an example of an apparatus used in the present invention. 1 is a raw material, 2 is a crucible, 3 is a seed, 4 is a sealing material, 5 is a vertical partition, 6 is an upper heater, 7 is a central heater, 8 is a lower heater, 9 is a water cooling jacket, 10
Represents heat insulating materials. In a graphite crucible 2 provided in the apparatus, three U-shaped partition plates and 1
After vertically inserting a vertical partition 5 (a cross section is shown in FIG. 2) configured by laminating a plurality of flat plates, the metal raw material 1 is placed in the crucible 2.
As a raw material, 100 g of 6N high-purity copper was added, and the raw material 1 on the upper part of the vertical partition 5 was melted at 1150 ° C., and the temperature of the common part of the lower part of the partition plate 5 and the seed 3 was adjusted to 1083 ° C.
【００１５】次いで５０℃／hrの割合でるつぼ全体を徐
冷して、縦状仕切体５内部の空隙に図３（仕切板は図示
せず）に示すような１．５mm厚×１０mm幅×５０mm長の
単結晶銅板３枚を同時に製造し、るつぼ外でシード３の
共通部（多結晶部）を切断して所望の単結晶銅板を得
た。Next, the entire crucible is gradually cooled at a rate of 50 ° C./hr, and the space inside the vertical partition 5 is filled with 1.5 mm thickness × 10 mm width × 1.5 mm thickness × 10 mm width as shown in FIG. 3 (partition plate is not shown). Three 50 mm long single crystal copper plates were simultaneously manufactured, and the common part (polycrystalline part) of the seed 3 was cut outside the crucible to obtain a desired single crystal copper plate.
【００１６】[0016]
【実施例２】実施例１と同様に、るつぼ２内に原料１と
して６Ｎ（９９．９９９９％）高純度銅１００ｇを入
れ、縦状仕切体５上部の原料１を１１５０℃で融解する
と共に、仕切体５下部を１０８３℃に調整した。Example 2 As in Example 1, 100 g of 6N (99.9999%) high-purity copper was placed as a raw material 1 in the crucible 2 and the raw material 1 above the vertical partition 5 was melted at 1150 ° C. The lower part of the partition 5 was adjusted to 1083 ° C.
【００１７】次いで６０mm／hrの速度でるつぼを下方に
引き下げて冷却し、該仕切体５内部の空隙に１．５mm厚
×１０mm幅×５０mm長の単結晶銅板３枚を同時に製造
し、実施例１と同様にシード３の共通部（多結晶部）を
切断して所望の単結晶銅板を得た。Then, the crucible was pulled down at a speed of 60 mm / hr to cool it, and three 1.5 mm thick × 10 mm wide × 50 mm long single crystal copper plates were simultaneously produced in the voids inside the partition body 5. A common portion (polycrystalline portion) of the seed 3 was cut in the same manner as in 1 to obtain a desired single crystal copper plate.
【００１８】[0018]
【実施例３】実施例１におけるグラファイト製るつぼに
代えて、より低伝導率を示すビトロカーボン製るつぼを
作成して装置内に設置し、るつぼ２内に原料１として５
０ｇのＧａＡｓ（純度６Ｎ）と１０ｇのＢ2 Ｏ3 （封止
材４）を装入した後、常圧より１kg／cm2 高い圧力のＡ
ｒ雰囲気内で、縦状仕切体５上部を１２８０℃、該仕切
体５下部を１２３８℃となるように調整した。Example 3 In place of the graphite crucible used in Example 1, a Vitrocarbon crucible having a lower conductivity was prepared and placed in the apparatus, and the crucible 2 was charged with 5 as raw material 1.
After charging 0 g of GaAs (purity 6N) and 10 g of B 2 O 3 (sealing material 4), A at a pressure of 1 kg / cm 2 higher than the normal pressure was applied.
In the r atmosphere, the upper part of the vertical partition 5 was adjusted to 1280 ° C, and the lower part of the partition 5 was adjusted to 1238 ° C.
【００１９】次いで１０℃／hrの割合でるつぼ全体を徐
冷し、縦状仕切体５の空隙に１．５mm厚×１０mm幅×５
０mm長の単結晶ＧａＡｓ板３枚を同時に製造し、実施例
１と同様にシード３の共通部（多結晶部）を切断して所
望の単結晶ＧａＡｓ板を得た。Next, the entire crucible is gradually cooled at a rate of 10 ° C./hr, and the space in the vertical partition 5 is 1.5 mm thick × 10 mm width × 5.
Three 0 mm-long single crystal GaAs plates were simultaneously manufactured, and the common part (polycrystalline part) of the seed 3 was cut in the same manner as in Example 1 to obtain a desired single crystal GaAs plate.
【００２０】[0020]
【実施例４】図４に示すように、横方向に互いに平行な
複数枚の仕切板からなる横状仕切体１３を配置した原料
ホルダー１１を、実施例１で用いた結晶装置に装入して
結晶化を図った。この場合、金属原料１として６Ｎ高純
度銅１００ｇを入れ、横状仕切板１３上部の原料１を１
１５０℃で融解するとともに、該仕切板１３下部とシー
ド３との空間部の温度を１０８３℃となるように調整し
た。[Embodiment 4] As shown in FIG. 4, a raw material holder 11 in which a horizontal partition body 13 composed of a plurality of partition plates parallel to each other in the lateral direction is arranged is placed in the crystallizing apparatus used in Embodiment 1. Was crystallized. In this case, 100 g of 6N high-purity copper was added as the metal raw material 1, and the raw material 1 above the horizontal partition plate 13 was
While melting at 150 ° C, the temperature of the space between the lower part of the partition plate 13 and the seed 3 was adjusted to 1083 ° C.
【００２１】次いで５０℃/hr の割合で原料ホルダー１
１全体を徐冷して、横状仕切体１３内部の円板状空隙に
φ２０mm、厚さ１．５mmの単結晶銅板６枚を同時に製造
し、ホルダー外でシード３との共通部（多結晶部）を切
断して所望の単結晶板を得た。Next, the raw material holder 1 at a rate of 50 ° C./hr.
1 The whole 1 is gradually cooled, and 6 single crystal copper plates with a diameter of 20 mm and a thickness of 1.5 mm are simultaneously manufactured in the disk-shaped void inside the horizontal partition 13, and outside the holder, the common part with the seed 3 (polycrystalline) (Part) was cut to obtain a desired single crystal plate.
【００２２】[0022]
【発明の効果】上述のように本発明によって得られた単
結晶板は、仕切体内部で板状となるため、従来法のよう
にバルク結晶体をスライスして所望形状にするという工
程は不要となり、本発明が操業上コストダウンに寄与す
る効果は大である。As described above, since the single crystal plate obtained by the present invention has a plate shape inside the partition body, the step of slicing the bulk crystal body into a desired shape unlike the conventional method is unnecessary. Therefore, the effect of the present invention that contributes to cost reduction in operation is great.
【図１】本発明装置の断面を示す概略図である。FIG. 1 is a schematic view showing a cross section of a device of the present invention.
【図２】本発明装置のるつぼ内に設置された縦状仕切体
の断面図である。FIG. 2 is a sectional view of a vertical partition installed in the crucible of the device of the present invention.
【図３】本発明装置のるつぼの透視図である。FIG. 3 is a perspective view of the crucible of the device of the present invention.
【図４】本発明装置のるつぼ内に設置される横状仕切体
を示す透過斜視図である。FIG. 4 is a transparent perspective view showing a horizontal partition body installed in the crucible of the device of the present invention.
１ 原料 ２ るつぼ ３ シード ４ 封止材 ５ 縦状仕切体 ６ 上部ヒーター ７ 中央部ヒーター ８ 下部ヒーター ９ 水冷ジャケット １０ 断熱材 １１ 原料ホルダー １２ 結晶連絡ノズル １３ 横状仕切体 １４ シード容器 1 Raw Material 2 Crucible 3 Seed 4 Sealing Material 5 Vertical Partition 6 Upper Heater 7 Central Heater 8 Lower Heater 9 Water Cooling Jacket 10 Heat Insulation Material 11 Raw Material Holder 12 Crystal Connecting Nozzle 13 Horizontal Partition 14 Seed Container
Claims (2)
なる仕切体を設け、該仕切体内の空間において板状の単
結晶を製造することを特徴とする単結晶の製造方法。1. A method for producing a single crystal, characterized in that a partition body comprising at least one partition plate is provided in a crucible, and a plate-shaped single crystal is produced in a space inside the partition body.
た加熱領域変動可能なヒーターとを主要部とする結晶製
造装置において、上記るつぼ内に縦状または横状の少な
くとも１枚の仕切板からなる仕切体を設置してあること
を特徴とする単結晶の製造装置。2. A crystal production apparatus comprising a crystal production crucible and a heater disposed around the crystal production crucible as a variable part, wherein at least one vertical or horizontal partition plate is provided in the crucible. An apparatus for producing a single crystal, characterized in that a partition body is installed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34689995A JP3640454B2 (en) | 1995-10-17 | 1995-12-13 | Single crystal manufacturing method |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7-293590 | 1995-10-17 | ||
| JP29359095 | 1995-10-17 | ||
| JP34689995A JP3640454B2 (en) | 1995-10-17 | 1995-12-13 | Single crystal manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09169589A true JPH09169589A (en) | 1997-06-30 |
| JP3640454B2 JP3640454B2 (en) | 2005-04-20 |
Family
ID=26559480
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34689995A Expired - Fee Related JP3640454B2 (en) | 1995-10-17 | 1995-12-13 | Single crystal manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3640454B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0947610A3 (en) * | 1998-03-31 | 2002-01-23 | Ngk Insulators, Ltd. | A single crystal-manufacturing equipment and a method for manufacturing the same |
-
1995
- 1995-12-13 JP JP34689995A patent/JP3640454B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0947610A3 (en) * | 1998-03-31 | 2002-01-23 | Ngk Insulators, Ltd. | A single crystal-manufacturing equipment and a method for manufacturing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3640454B2 (en) | 2005-04-20 |
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