CN103866390B - A kind of gallium phosphide polycrystal body mixes zinc method - Google Patents
A kind of gallium phosphide polycrystal body mixes zinc method Download PDFInfo
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- CN103866390B CN103866390B CN201210535514.8A CN201210535514A CN103866390B CN 103866390 B CN103866390 B CN 103866390B CN 201210535514 A CN201210535514 A CN 201210535514A CN 103866390 B CN103866390 B CN 103866390B
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Abstract
A kind of gallium phosphide polycrystal body mixes zinc method, it is that one mixes zinc impurity in gallium phosphide polycrystal building-up process, wherein, zinc is put into the carbon tube of dress gallium, carbon tube is enclosed in crystal reaction tube, put into high pressure area and fuse into stove, the intensification of gallium end, phosphorus end are heated up, after arriving temperature, starts synthesis, mobile crystal reaction tube, phosphorus end is heated up, tests and synthetic mix zinc gallium phosphide polycrystal impurity concentration end to end. It is an advantage of the invention that: drawing can be directly used in and mix zinc monocrystal of gallium phosphide, and when noting be used in crystal-pulling, add zinc impurities in addition, therefore, crystal-pulling process decreases the volatilization of zinc, it is convenient to the observation of crystal pulling process, be conducive to improving monocrystalline yield rate, the doping content of monocrystalline can be controlled again well.
Description
Technical field
The present invention relates to adulterating method in a kind of compound semiconductor crystal, specifically, relate to a kind of gallium phosphide polycrystal body mixes zinc method.
Background technology
GaP crystal divides polycrystalline and monocrystalline. Monocrystal of gallium phosphide material is the main substrate preparing LED, can be used for manufacturing red, yellow, and green look photodiode. Gallium phosphide polycrystal also can be used as the source material of preparation LED simultaneously. When as source material, usual is non-doping gallium phosphide polycrystal, and gallium phosphide non-doped crystal is at room temperature transparent salmon solid. And when being substrate material, it mostly is gallium phosphide N-type or P type monocrystalline. At present not yet obtained undoped partly insulate monocrystal of gallium phosphide, obtaining half insulation monocrystal of gallium phosphide can only as other Group III-V compound semiconductor material, by introduce deep-level impurity, as mix in the elements such as Cr, Fe, O one or both and become semi insulating material. Present industrial N-type monocrystal of gallium phosphide obtains by mixing S, Si, Te impurity usually. And industry preparation P type monocrystal of gallium phosphide obtains by mixing Zn impurity.
Mix Zn monocrystal of gallium phosphide and prepare yellow, yellow-green colour LED for LPE method or VPE method extension. Modern semiconductors industrial production monocrystal of gallium phosphide is all in high-pressure synthesis stove, adopts directional solidification processes synthesis gallium phosphide polycrystal, loads the monocrystalline in high pressure single crystal growing furnace high pressure LEC method growth<111>,<115>crystal orientation after carrying out suitably process. Mix Zn monocrystal of gallium phosphide for obtaining, normally by doping agent Zn with non-mix gallium phosphide polycrystal together with put into quartz crucible, then put into boron oxide insulating covering agent above, load growing single-crystal in high pressure single crystal growing furnace. Due to Zn when gallium phosphide fusing point the saturated vapor pressure of (1467 DEG C) close to 5MPa, therefore in single crystal growth process, Zn is constantly had to evaporate from gallium phosphide melt, make boron oxide insulating covering agent blackening, impact is observed, serious impact is drawn crystalline substance and is controlled crystal diameter with pontoon, makes monocrystalline yield rate become low. Meanwhile, due to the volatilization of Zn, add the effective segregation coefficient that Zn is very low in gallium phosphide, make the doping content of monocrystalline be difficult to control.
Summary of the invention
It is an object of the invention to provide in a kind of gallium phosphide polycrystal body and mix zinc method, adopt the method to can be good at controlled doping concentration, be unlikely to have again too many zinc volatilization when adopting the polycrystalline of this method synthesis to carry out crystal-pulling, it is to increase monocrystalline yield rate.
In order to achieve the above object, present invention employs following technical scheme:
This kind of gallium phosphide polycrystal body mixes zinc method, it is that one mixes zinc impurity in gallium phosphide polycrystal building-up process, wherein, zinc is put into the carbon tube of dress gallium, carbon tube is enclosed in crystal reaction tube, put into high pressure area and fuse into stove, the intensification of gallium end, phosphorus end are heated up, after arriving temperature, starts synthesis, mobile crystal reaction tube, phosphorus end is heated up, tests and synthetic mix zinc gallium phosphide polycrystal impurity concentration end to end.
It comprises following concrete steps:
1. 1��8 gram of zinc is placed in the carbon tube loading gallium, it is placed on 1/2��2/3 place from carbon tube head;
2. being enclosed in crystal reaction tube by carbon tube, put into high pressure area and fuse into stove, zone length is set as 8��13cm;
3. gallium end temperature is risen to 1450��1500 DEG C, phosphorus end temperature to 520��540 DEG C are started synthesis;
4. move crystal reaction tube with the speed of 7��8 lis ms/h, with the temperature rise rate of 30��40 DEG C/h, phosphorus end is heated up simultaneously, complete building-up process;
5. mix after zinc gallium phosphide polycrystal takes out by synthetic, test its impurity concentration end to end. The gallium phosphide polycrystal doping content obtained is not less than 2 �� 1018cm-3��
It is known equipment that high pressure area fuses into stove,
The melting zone of suitable width refers to gallium end carbon tube heating zone length.
It is an advantage of the invention that:
Owing to adopting high pressure area to fuse into, zinc is placed on correct position, by control phosphorus end temperature, so that control phosphorus vapour pressure, inhibiting the evaporation of zinc, the melting zone of suitable width can make again zinc in whole gallium phosphide polycrystal ingot evenly distribute.
Adopt the gallium phosphide polycrystal of the present invention's synthesis, it is possible to be directly used in drawing and mix zinc monocrystal of gallium phosphide, and when noting be used in crystal-pulling, add zinc impurities in addition. Therefore, crystal-pulling process decreases the volatilization of zinc, is convenient to the observation of crystal pulling process, is conducive to improving monocrystalline yield rate, can control again the doping content of monocrystalline well.
Accompanying drawing explanation
Fig. 1 is the FB(flow block) mixing zinc method in a kind of gallium phosphide polycrystal body of the present invention.
Embodiment
Mixing zinc method in a kind of gallium phosphide polycrystal body of the present invention adopts equipment to be high-pressure synthesis stove.
With specific embodiment, the present invention will be further described below:
Embodiment 1:
1. 1 gram of zinc is placed in the carbon tube loading gallium, it is placed on 1/2 place from carbon tube head;
2. being enclosed in crystal reaction tube by carbon tube, put into high pressure area and fuse into stove and add thermal synthesis, zone length is set as 8cm;
3. gallium end temperature is risen to 1470 DEG C, phosphorus end temperature to 520 DEG C is started synthesis;
4. move crystal reaction tube with the speed of 7 lis ms/h, with the temperature rise rate of 30 DEG C/h, phosphorus end is heated up simultaneously, complete building-up process;
5. mix after zinc gallium phosphide polycrystal takes out by synthetic, test its impurity concentration end to end. The gallium phosphide polycrystal head doping content obtained is 3.6 �� 1018cm-3��
Embodiment 2:
1. 3 grams of zinc are placed in the carbon tube loading gallium, it are placed on 1/2 place from carbon tube head;
2. being enclosed in crystal reaction tube by carbon tube, put into high pressure area and fuse into stove, zone length is set as 9cm;
3. gallium end temperature is risen to 1480 DEG C, phosphorus end temperature to 525 DEG C is started synthesis;
4. move crystal reaction tube with the speed of 7.5 lis ms/h, with the temperature rise rate of 35 DEG C/h, phosphorus end is heated up simultaneously, complete building-up process;
5. mix after zinc gallium phosphide polycrystal takes out by synthetic, test its impurity concentration end to end. The gallium phosphide polycrystal head doping content obtained is 8.4 �� 1018cm-3��
Embodiment 3:
1. 4 grams of zinc are placed in the carbon tube loading gallium, it are placed on 5/9 place from carbon tube head;
2. being enclosed in crystal reaction tube by carbon tube, put into high pressure area and fuse into stove, zone length is set as 10cm;
3. gallium end temperature is risen to 1485 DEG C, phosphorus end temperature to 530 DEG C is started synthesis;
4. move crystal reaction tube with the speed of 7.6 lis ms/h, with the temperature rise rate of 33 DEG C/h, phosphorus end is heated up simultaneously, complete building-up process;
5. mix after zinc gallium phosphide polycrystal takes out by synthetic, test its impurity concentration end to end. The gallium phosphide polycrystal head doping content obtained is 1.5 �� 1019cm-3��
Embodiment 4:
1. 7 grams of zinc are placed in the carbon tube loading gallium, it are placed on 2/3 place from carbon tube head;
2. being enclosed in crystal reaction tube by carbon tube, put into high pressure area and fuse into stove, zone length is set as 12cm;
3. gallium end temperature is risen to 1490 DEG C, phosphorus end temperature to 535 DEG C is started synthesis;
4. move crystal reaction tube with the speed of 8 lis ms/h, with the temperature rise rate of 36 DEG C/h, phosphorus end is heated up simultaneously, complete building-up process;
5. mix after zinc gallium phosphide polycrystal takes out by synthetic, test its impurity concentration end to end. The gallium phosphide polycrystal head doping content obtained is 2.3 �� 1019cm-3��
Embodiment 5:
1. 8 grams of zinc are placed in the carbon tube loading gallium, it are placed on 2/3 place from carbon tube head;
2. being enclosed in crystal reaction tube by carbon tube, put into high pressure area and fuse into stove, zone length is set as 13cm;
3. gallium end temperature is risen to 1500 DEG C, phosphorus end temperature to 540 DEG C is started synthesis;
4. move crystal reaction tube with the speed of 8 lis ms/h, with the temperature rise rate of 40 DEG C/h, phosphorus end is heated up simultaneously, complete building-up process;
5. mix after zinc gallium phosphide polycrystal takes out by synthetic, test its impurity concentration end to end. The gallium phosphide polycrystal head doping content obtained is 3.8 �� 1019cm-3��
Claims (1)
1. a gallium phosphide polycrystal body mixes zinc method, it is characterized in that: it is that one mixes zinc impurity in gallium phosphide polycrystal building-up process, wherein, zinc is put into the carbon tube of dress gallium, carbon tube is enclosed in crystal reaction tube, put into high pressure area and fuse into stove, the intensification of gallium end, phosphorus end are heated up, after arriving temperature, starts synthesis, mobile crystal reaction tube, phosphorus end is heated up, tests and synthetic mix zinc gallium phosphide polycrystal impurity concentration end to end; Specifically comprise the following steps:
1). 1��8 gram of zinc is placed in the carbon tube loading gallium, is placed on 1/2��2/3 place from carbon tube head;
2). being enclosed in crystal reaction tube by carbon tube, put into high pressure area and fuse into stove, zone length is set as 8��13cm;
3). gallium end temperature is risen to 1450��1500 DEG C, phosphorus end temperature to 520��540 DEG C are started synthesis;
4). move crystal reaction tube with the speed of 7��8 lis ms/h, with the temperature rise rate of 30��40 DEG C/h, phosphorus end is heated up simultaneously, complete building-up process;
5). mixing after zinc gallium phosphide polycrystal takes out by synthetic, test its impurity concentration end to end, the gallium phosphide polycrystal doping content obtained is not less than 2 �� 1018cm-3��
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3937700B2 (en) * | 2000-07-26 | 2007-06-27 | 日立電線株式会社 | Method for producing GaAs semiconductor single crystal doped with conductive impurities |
| CN101660207A (en) * | 2008-08-26 | 2010-03-03 | 北京有色金属研究总院 | Method for synthesizing gallium phosphide polycrystal |
| CN102040204A (en) * | 2009-10-16 | 2011-05-04 | 北京有色金属研究总院 | Method for casting ingots by using gallium phosphide polycrystal |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59137400A (en) * | 1983-01-26 | 1984-08-07 | Sumitomo Electric Ind Ltd | P type gallium arsenide single crystal with low dislocation density and its manufacture |
| JPH0761917B2 (en) * | 1988-03-09 | 1995-07-05 | 株式会社ジャパンエナジー | InP compound semiconductor polycrystalline synthesis method |
| JP2712594B2 (en) * | 1989-07-20 | 1998-02-16 | 旭硝子株式会社 | Method for producing group 3-5 compound semiconductor single crystal |
| JPH06329492A (en) * | 1993-05-21 | 1994-11-29 | Asahi Glass Co Ltd | Production of gaas compound semiconductor crystal |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3937700B2 (en) * | 2000-07-26 | 2007-06-27 | 日立電線株式会社 | Method for producing GaAs semiconductor single crystal doped with conductive impurities |
| CN101660207A (en) * | 2008-08-26 | 2010-03-03 | 北京有色金属研究总院 | Method for synthesizing gallium phosphide polycrystal |
| CN102040204A (en) * | 2009-10-16 | 2011-05-04 | 北京有色金属研究总院 | Method for casting ingots by using gallium phosphide polycrystal |
Non-Patent Citations (2)
| Title |
|---|
| Electrical and optical properties of Mg, Ca, and Zndoped InP crystals grown by the synthesis, solute diffusion technique;Eishi Kubota,et al.;《Journal of Applied Physics》;19840515;第55卷;第3779-3784页 * |
| The Behaviour of Zinc in Gap Synthesis by the SSD Technique;H. KOI，et al.;《Crystal Res. & Technol》;19821231;第17卷(第12期);第1501-1512页 * |
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