CN103184501A - Gallium arsenide polycrystalline ingot casting method - Google Patents
Gallium arsenide polycrystalline ingot casting method Download PDFInfo
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- CN103184501A CN103184501A CN2011104542176A CN201110454217A CN103184501A CN 103184501 A CN103184501 A CN 103184501A CN 2011104542176 A CN2011104542176 A CN 2011104542176A CN 201110454217 A CN201110454217 A CN 201110454217A CN 103184501 A CN103184501 A CN 103184501A
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Abstract
The invention relates to a gallium arsenide polycrystalline ingot casting method comprising the steps of: (1) material loading; (2) heating; (3) material melting; (4) machine processing; (5) cooling; (6) fetching; and (7) sampling and testing. In the fetching process, when the temperature is reduced to below 100 DEG C, quartz tubes are fetched from a monocrystalline furnace; the quartz tubes are broken at a ventilated place, and polycrystalline ingot bars are fetched. In the sampling and testing step, the polycrystalline ingot bars are sampled and tested; when the samples are qualified according to electrical parameter tests, the ingots can be used in monocrystalline growth. The method has the advantages that: synthesis tailings, monocrystalline tailings, and polycrystalline materials caused by gas leakage and power off during a monocrystalline growth process can be re-molten and re-solidified, such that the gallium arsenide polycrystalline ingots are obtained. The operation is convenient, and cost is reduced.
Description
Technical field
The present invention relates to a kind of gallium arsenide polycrystal casting ingot method.
Background technology
In the arsenide gallium monocrystal process of growth, monocrystalline afterbody stoichiometric ratio can be offset, and produces the monocrystalline tailing.In building-up process, also there is kindred circumstances, synthetic tailing is arranged.Fragment and waste material are also arranged in the wafer process process.In single crystal growth process, the polycrystal that gas leakage is also arranged once in a while or cause because of power failure, above-mentioned brilliant material can not directly drop into single crystal growth process, it need be dissolved again, solidifies again.Can drop into single crystal growing after electrical parameter (carrier concentration and the mobility) test passes.More than this method that gallium arsenide polycrystal material and waste material are dissolved again and solidify again be referred to as the gallium arsenide polycrystal ingot casting.
Summary of the invention
The purpose of this invention is to provide a kind of gallium arsenide polycrystal casting ingot method, this method can will be synthesized in tailing, monocrystalline tailing and the single crystal growth process, the polycrystal that gas leakage is also arranged once in a while or cause because of power failure, again dissolve, solidify again, obtain the gallium arsenide polycrystal ingot casting, easy to operate, reduce cost.
To achieve the above object of the invention, the present invention is by the following technical solutions:
This gallium arsenide polycrystal casting ingot method, it comprises following step:
1) charging: the gallium arsenide polycrystal material is put into special-shaped boat, again quartz boat is put into silica tube, puts into the arsenic amount that calculates by the silica tube residual volume, vacuumizes tube sealing then;
2) heat up: will the above-mentioned silica tube of sealing pack in 12 sections horizontal single crystal growing furnaces, heat up, 6 districts of high temperature directly are raised to 1250 ℃ except the Gao Yi district, and interface region and middle warm area are pressed the single crystal growing temperature, and the interface region temperature of lower is lower 20 ℃ than single crystal growing.Beginning material after temperature is raised to.
3) change material: in 4-6 hour, by watching before and after observation window and the body of heater, after affirmation ingot casting material all melts, begin to fall high temperature 2-6 district temperature and exceed 5 ℃ than single crystal growing temperature.Solid-liquid interface district's temperature and middle Wen Wendu are the same.
4) mule carriage: behind the temperature-stable, begin mobile heating member (being commonly called as mule carriage), translational speed is 20mm/h.
5) lower the temperature: after seeing that from window solution all solidifies, the outage cooling.
6) come out of the stove: after waiting to cool to below 100 ℃ silica tube is taken out from single crystal growing furnace, break silica tube in the ventilation, take out the polycrystalline ingot.
7) sampling and testing: polycrystalline ingot sampling and testing, can drop into single crystal growing after electrical parameter (carrier concentration and the mobility) test passes.
Substandard product can be used for reclaiming gallium.
Description of drawings
Fig. 1: casting ingot process FB(flow block)
Among Fig. 1, input: GaAs polycrystal, quartz, ingot casting is got the raw materials ready, and charging-heat up-change material-mule carriage-outage lowers the temperature-comes out of the stove-sampling and testing-dispose respectively by test result.
Embodiment
The present invention adopts 12 sections horizontal single crystal growing furnaces (a kind of 12 sections heating zone horizontal single crystal growing furnace heating member patent No.s: ZL200820078527.6) as the heating member of gallium arsenide polycrystal ingot casting.
Charging: aforesaid gallium arsenide polycrystal material is put into quartz boat, and (single crystal growing is with the special-shaped boat patent No.: ZL200520130545.0).Again quartz boat is put into silica tube, put into the arsenic amount that calculates by the silica tube residual volume, calculate and undertaken by desirable gas equation.Vacuumize tube sealing then.
Heat up: the above-mentioned silica tube of sealing is packed in 12 sections horizontal single crystal growing furnaces.Heat up, 6 districts of high temperature directly are raised to 1260 ℃ except the Gao Yi district, and Gao Yiqu is 1200 ℃; The interface region temperature of lower is 1250 ℃, and the side temperature is 1232 ℃; In warm area one district be 1190 ℃, in two in four be 1180 ℃, the Zhong Wu district is 1100 ℃.Beginning material after being raised to.
Change material: in 4-6 hour, by watching before and after observation window and the body of heater, after affirmation ingot casting material all melted, beginning to fall high temperature 2-6 district temperature was 1245 ℃.Solid-liquid interface district's temperature and middle Wen Wendu are the same.
Mule carriage: behind the temperature-stable, begin mobile heating member (being commonly called as mule carriage), translational speed is 20mm/h.
Lower the temperature: after seeing that from window melt all solidifies, the outage cooling.
Come out of the stove: after waiting to cool to below 100 ℃ silica tube is taken out from single crystal growing furnace, break silica tube in the ventilation, take out the polycrystalline ingot.
Sampling and testing: polycrystalline ingot sampling and testing, (acceptance condition is: its conduction type of ingot casting polycrystal is N-type to electrical parameter (conduction type, carrier concentration and mobility) test passes, and mobility is in the qualified gallium arsenide material of subordinate list one " mixing silicon horizontal gallium arsenide monocrystalline concentration and mobility relation curve " zone.Be referred to as the qualified gallium arsenide material of μ, it expects to carry out ingot casting end to end, and rest part enters crystal pulling.Be in defective gallium arsenide material zone as its mobility, be referred to as the defective gallium arsenide material of μ, as the waste recovery gallium.Its conduction type of ingot casting polycrystal is the P type, regards it as qualified P type crystal pulling polycrystal.)
Acceptance condition is judged: utilizing the data of subordinate list one, is longitudinal axes (Y-axis) with the mobility, and carrier concentration is transverse axis (X-axis); Connecting each point draw carrier concentration and mobility curve figure, is qualified gallium arsenide material zone above the curve, is defective gallium arsenide material zone below.Be " mixing silicon horizontal gallium arsenide monocrystalline concentration and mobility relation curve ".
Embodiment 1
Ingot casting numbering: 11-casting-110.Charging 5800g, surplus arsenic amount: 3.4g.Shove charge on April 19 in 2011, on April 21st, 2011 came out of the stove.Test result: carrier concentration: head: 1.05E+18, mobility: 2540; Afterbody: 4.08E18, mobility: 1620, qualified by aforementioned judgement, enter crystal pulling.
Embodiment 2
Ingot casting numbering: 11-casting-111.Charging 6200g, surplus arsenic amount: 3.4g.Shove charge on April 20 in 2011, on April 22nd, 2011 came out of the stove.Test result: carrier concentration: head: 1.18E+18, mobility: 2190; Afterbody: 4.04E17, mobility: 1450, qualified by aforementioned judgement, enter crystal pulling
Embodiment 3
Ingot casting numbering: 11-casting-182.Charging 5800g, surplus arsenic amount: 3.4g.Shove charge on June 20 in 2011, on June 21st, 2011 came out of the stove.Test result: carrier concentration: head: 1.20E+18, mobility: 1280; Afterbody: 7.45E17 because inhomogeneous, does not have the mobility data, and is defective by aforementioned judgement, reclaims gallium.
Subordinate list 1: mix silicon horizontal gallium arsenide monocrystalline concentration and mobility mapping table
| Monocrystalline concentration | Mobility | Monocrystalline concentration | Mobility | Monocrystalline concentration | Mobility |
| ＜9E+16 | ≥3000 | 1.4E+18 | 1850 | 2.8E+18 | 1540 |
| 1E+17 | 2850 | 1.5E+18 | 1800 | 2.9E+18 | 1520 |
| 2E+17 | 2730 | 1.6E+18 | 1770 | 3.0E+18 | 1510 |
| 3E+17 | 2600 | 1.7E+18 | 1730 | 3.1E+18 | 1500 |
| 4E+17 | 2500 | 1.8E+18 | 1700 | 3.2E+18 | 1480 |
| 5E+17 | 2400 | 1.9E+18 | 1670 | 3.3E+18 | 1450 |
| 6E+17 | 2330 | 2.0E+18 | 1650 | 3.4E+18 | 1420 |
| 7E+17 | 2250 | 2.1E+18 | 1640 | 3.5E+18 | 1370 |
| 8E+17 | 2180 | 2.2E+18 | 1620 | 3.6E+18 | 1280 |
| 9E+17 | 2120 | 2.3E+18 | 1600 | 3.7E+18 | 1180 |
| 1E+18 | 2050 | 2.4E+18 | 1580 | 3.8E+18 | 1100 |
| 1.1E+18 | 2000 | 2.5E+18 | 1570 | 3.9E+18 | 1040 |
| 1.2E+18 | 1950 | 2.6E+18 | 1560 | 4.0E+18 | ≥1000 |
| 1.3E+18 | 1900 | 2.7E+18 | 1550 | ＞4.1E+18 | ≥1000 |
Claims (2)
1. gallium arsenide polycrystal casting ingot method, it is characterized in that: it comprises following step:
1) charging: the gallium arsenide polycrystal material is put into special-shaped boat, again quartz boat is put into silica tube, puts into the arsenic amount that calculates by the silica tube residual volume, vacuumizes tube sealing then;
2) heat up: the above-mentioned silica tube of sealing is packed in 12 sections horizontal single crystal growing furnaces, heat up, 6 districts of high temperature directly are raised to 1250 ℃ except the Gao Yi district, and interface region and middle warm area are by the single crystal growing temperature, the interface region temperature of lower is lower 20 ℃ than single crystal growing, beginning material after temperature is raised to;
3) change material: in 4-6 hour, by watching before and after observation window and the body of heater, after affirmation ingot casting material all melts, begin to fall high temperature 2-6 district temperature and exceed 5 ℃ than single crystal growing temperature, solid-liquid interface district's temperature and middle Wen Wendu are the same.
4) mule carriage: behind the temperature-stable, begin mobile heating member, translational speed is 20mm/h;
5) lower the temperature: after seeing that from window solution all solidifies, the outage cooling;
6) come out of the stove: after waiting to cool to below 100 ℃ silica tube is taken out from single crystal growing furnace, break silica tube in the ventilation, take out the polycrystalline ingot;
7) sampling and testing: polycrystalline ingot sampling and testing, can drop into single crystal growing after the electrical parameter test passes.
2. a kind of gallium arsenide polycrystal casting ingot method according to claim 1 is characterized in that: behind sampling and testing, substandard product is used for reclaiming gallium.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103726100A (en) * | 2013-11-25 | 2014-04-16 | 青岛盛嘉信息科技有限公司 | Polycrystalline gallium arsenide synthetic method without liquid encapsulation |
| CN106319630A (en) * | 2015-07-02 | 2017-01-11 | 广东先导先进材料股份有限公司 | Growing method of gallium arsenide monocrystalline |
| CN106894092A (en) * | 2015-12-21 | 2017-06-27 | 有研光电新材料有限责任公司 | A kind of method that seed crystal is connect in Horizontal Bridgman Method arsenide gallium monocrystal pulling process |
| CN107829141A (en) * | 2017-11-10 | 2018-03-23 | 北京鼎泰芯源科技发展有限公司 | The circulation utilization method of rich indium indium phosphide polycrystal material |
| CN108570708A (en) * | 2018-07-25 | 2018-09-25 | 汉能新材料科技有限公司 | A kind of gallium arsenide polycrystal synthesizer |
| CN108866630A (en) * | 2018-07-25 | 2018-11-23 | 汉能新材料科技有限公司 | A kind of gallium arsenide polycrystal synthetic method |
| CN113652752A (en) * | 2021-08-17 | 2021-11-16 | 广东先导微电子科技有限公司 | Preparation method of gallium arsenide polycrystal |
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| CN2885891Y (en) * | 2006-02-09 | 2007-04-04 | 姚荣华 | Temperature control furnace for growth of arsenide gallium monocrystal |
| CN201172700Y (en) * | 2008-01-14 | 2008-12-31 | 北京有色金属研究总院 | Heating body of horizontal single crystal furnace with twelve-segment heating zones |
| CN101538741A (en) * | 2009-03-09 | 2009-09-23 | 新乡市神舟晶体科技发展有限公司 | Synthetic utilization method of gallium arsenide polycrystal tail |
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- 2011-12-30 CN CN201110454217.6A patent/CN103184501B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2885891Y (en) * | 2006-02-09 | 2007-04-04 | 姚荣华 | Temperature control furnace for growth of arsenide gallium monocrystal |
| CN201172700Y (en) * | 2008-01-14 | 2008-12-31 | 北京有色金属研究总院 | Heating body of horizontal single crystal furnace with twelve-segment heating zones |
| CN101538741A (en) * | 2009-03-09 | 2009-09-23 | 新乡市神舟晶体科技发展有限公司 | Synthetic utilization method of gallium arsenide polycrystal tail |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103726100A (en) * | 2013-11-25 | 2014-04-16 | 青岛盛嘉信息科技有限公司 | Polycrystalline gallium arsenide synthetic method without liquid encapsulation |
| CN106319630A (en) * | 2015-07-02 | 2017-01-11 | 广东先导先进材料股份有限公司 | Growing method of gallium arsenide monocrystalline |
| CN106894092A (en) * | 2015-12-21 | 2017-06-27 | 有研光电新材料有限责任公司 | A kind of method that seed crystal is connect in Horizontal Bridgman Method arsenide gallium monocrystal pulling process |
| CN107829141A (en) * | 2017-11-10 | 2018-03-23 | 北京鼎泰芯源科技发展有限公司 | The circulation utilization method of rich indium indium phosphide polycrystal material |
| CN108570708A (en) * | 2018-07-25 | 2018-09-25 | 汉能新材料科技有限公司 | A kind of gallium arsenide polycrystal synthesizer |
| CN108866630A (en) * | 2018-07-25 | 2018-11-23 | 汉能新材料科技有限公司 | A kind of gallium arsenide polycrystal synthetic method |
| CN113652752A (en) * | 2021-08-17 | 2021-11-16 | 广东先导微电子科技有限公司 | Preparation method of gallium arsenide polycrystal |
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