CN109629002A - The method that seed crystal, seeding and crystallization situation determine is carried out to the InP crystal ingot of VGF method production - Google Patents
The method that seed crystal, seeding and crystallization situation determine is carried out to the InP crystal ingot of VGF method production Download PDFInfo
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- CN109629002A CN109629002A CN201811640598.5A CN201811640598A CN109629002A CN 109629002 A CN109629002 A CN 109629002A CN 201811640598 A CN201811640598 A CN 201811640598A CN 109629002 A CN109629002 A CN 109629002A
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- crystal
- seed crystal
- seed
- quartz ampoule
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/006—Controlling or regulating
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The InP crystal ingot that the present invention discloses the production of a kind of pair of VGF method take out out of VGF furnace comprising the component including quartz ampoule, boron nitride crucible and crystal ingot after the completion of the method that seed crystal, seeding and crystallization situation determine includes: (1) crystal growth；(2) quartz ampoule is heated, so that the red phosphorus distillation of boron nitride crucible and seed crystal end deposition deposits to the end of quartz ampoule, until the transparency of the boron nitride crucible and the quartz ampoule of seed end point reaches the transparency of setting；(3) crystal ingot in boron nitride crucible is scanned using ultrasonic wave detector from seed crystal end to tail portion, obtains the image of seed crystal and plane of crystal；(4) according to the image of the seed crystal of acquisition and plane of crystal, judge whether plane of crystal crystallization situation and seed crystal seeding situation reach established standards, be to carry out open pipe and the processing of de- crucible；Otherwise it sends the component back to VGF furnace and re-starts growth technique.The growth cost of InP can be effectively reduced in the present invention, improves the utilization rate of former raw material and auxiliary material.
Description
Technical field
The invention belongs to technical field of semiconductor material preparation, and in particular to carry out seed to the InP crystal ingot of VGF method production
The method that brilliant, seeding and crystallization situation determine.
Background technique
Indium phosphide (InP) crystal is important compound semiconductor materials, compared with GaAs (GaAs), superiority master
It is that higher saturated electron drift velocity, thermal conductivity be good and stronger radiation resistance etc..Therefore, inp wafer is usual
For manufacturing high frequency, high speed and HIGH-POWERED MICROWAVES device and circuit.Currently, the growing method of indium phosphide generallys use
VGF method, can also be referred to as vertical gradient solidification, the major advantage of this method be dislocation density defect is low, crystal quality is high,
It can growing large-size crystal.But due to the characteristic of indium phosphide, that there is also growth cycles is long for this growing method,
It is more using raw material and auxiliary material type, can not intuitively observe long brilliant situation, the disadvantages of monocrystalline rate is low, preparation cost is high.Institute
To have seriously affected the application development of indium phosphide single crystal substrate.
The growth that existing VGF legal system makees InP crystal is carried out in closed quartz ampoule, and the crystal ingot come out of the stove is due to nitridation
The influence of red phosphorus, the crystal ingot tail portion boron oxide that boron crucible, quartzy inside pipe wall deposit etc. can not directly judge to crystallize situation and seed crystal
Seeding position, it is necessary to after cutting quartz ampoule, taking out crucible and taking off crystal ingot could judge after crucible to crystallize and seeding situation.Due to
The crystal forming rate of the InP crystal growth of VGF method is low, and the loss of the auxiliary materials such as quartz ampoule caused by this mode is big, at high cost.
Summary of the invention
The present invention is intended to provide a kind of method of non-destructive testing, under the premise of not broken quartzy growth tube, through nitridation
Boron crucible can tentatively judge to connect seed crystal situation, plane of crystal situation.The present invention is realized using following technical scheme:
The InP crystal ingot of a kind of pair of VGF method production carries out the method that seed crystal, seeding and crystallization situation determine, including following step
It is rapid:
(1) it after the completion of crystal growth, takes out out of VGF furnace comprising the component including quartz ampoule, boron nitride crucible and crystal ingot；
(2) quartz ampoule is heated, so that the red phosphorus distillation of boron nitride crucible and seed crystal end deposition deposits to quartz ampoule
End, until the transparency of the quartz ampoule of the boron nitride crucible and seed end point reaches the transparency of setting；
(3) crystal ingot in the boron nitride crucible is scanned using ultrasonic wave detector from seed crystal end to tail portion, is obtained
Obtain the image of seed crystal and plane of crystal；
(4) according to the image of the seed crystal of acquisition and plane of crystal, judge plane of crystal crystallization situation and seed crystal seeding situation
Whether reach established standards, be, carries out open pipe and the processing of de- crucible；Otherwise it sends the component back to VGF furnace and re-starts growth
Technique.
As a specific technical scheme, the quartz ampoule is heated in step (2), specifically: with heating furnace to the stone
English pipe is heated to 300-400 degree.
As a specific technical scheme, judge that plane of crystal crystallization situation and seed crystal seeding situation refer in step (4), sentence
Whether disconnected seed crystal or plane of crystal have twin crystal line and surface blemish, are then to be not up to the established standards, otherwise reach described and set
Calibration is quasi-.
The present invention first passes through ultrasonic wave judgement before open pipe and the processing of de- crucible, can be selectively to the crystal ingot for growing up to monocrystalline
Open pipe and the processing of de- crucible are carried out, and quartz ampoule and boron nitride crucible of the polycrystalline crystal ingot together with non-open pipe will be grown up to and put back to furnace
It is interior, it reheats fusing and is followed by the long monocrystalline of seed crystal.The present invention can be effectively reduced the growth cost of InP, improve former raw material and
The utilization rate of auxiliary material.
Detailed description of the invention
Fig. 1 is that InP crystal ingot progress seed crystal, seeding and the crystallization situation provided in an embodiment of the present invention to the production of VGF method is sentenced
The flow chart of fixed method.
Specific embodiment
It elaborates with reference to the accompanying drawing to specific embodiments of the present invention:
As shown in Figure 1, the present embodiment provides the InP crystal ingots of a kind of pair of VGF method production to carry out seed crystal, seeding and crystallization situation
The method of judgement, comprising the following steps:
(1) it after the completion of crystal growth, is taken out out of VGF furnace comprising the component including quartz ampoule, boron nitride crucible and crystal ingot,
The component is the component for not carrying out open pipe and the processing of de- crucible.
(2) 300-400 degree is heated to the quartz ampoule with heating furnace so that boron nitride crucible and seed crystal end deposition it is red
Phosphorus, which distils, deposits to the end of quartz ampoule, until the transparency of the boron nitride crucible and the quartz ampoule of seed end point reaches and sets
Fixed transparency.
(3) crystal ingot in the boron nitride crucible is scanned using ultrasonic wave detector from seed crystal end to tail portion, is obtained
Obtain the image of seed crystal and plane of crystal；Ultrasonic wave can through quartz ampoule and boron nitride crucible can indium phosphide to its inside it is brilliant
The case where body carries out noninvasive imaging, can sketch the contours of plane of crystal, once discovery seed crystal or plane of crystal have twin crystal line and surface
Flaw.
(4) according to the image of the seed crystal of acquisition and plane of crystal, judge plane of crystal crystallization situation and seed crystal seeding situation
Whether reach established standards, be, carries out open pipe and the processing of de- crucible；Otherwise it sends the component back to VGF furnace and re-starts growth
Technique (places back in crystal growing furnace, carry out heating melt, connect the isometric brilliant technical process of seed crystal, crystal growth again).
Wherein, judge plane of crystal crystallization situation and seed crystal seeding situation refer to, judge seed crystal or plane of crystal whether have twin crystal line and
Surface blemish is then to be not up to the established standards, otherwise reaches the established standards.
The present invention be not crushed quartzy growth tube by using the technical method of Ultrasonic Nondestructive plane of crystal situation
Under the premise of, breaking and connecting seed crystal situation, plane of crystal situation can be tentatively sentenced through quartz ampoule and boron nitride crucible.By judging,
Open pipe selectively can be carried out to the crystal ingot for growing up to monocrystalline and de- crucible is handled, and polycrystalline crystal ingot will be grown up to together with non-open pipe
Quartz ampoule put back in furnace together, fusing can be reheated and be followed by the long monocrystalline of seed crystal.Former, auxiliary material utilization can be improved
The VGF-InP crystal growth cost of 15%-25% is effectively reduced in rate.
Embodiments described above is intended to the sufficiently open present invention, the range for the protection that is not intended to limit the present invention.This field
Those of ordinary skill should be belonged to based on content disclosed in this invention without the other embodiments that creative work can be obtained
In the invention discloses range.
Claims (3)
1. the InP crystal ingot of a kind of pair of VGF method production carries out the method that seed crystal, seeding and crystallization situation determine, which is characterized in that packet
Include following steps:
(1) it after the completion of crystal growth, takes out out of VGF furnace comprising the component including quartz ampoule, boron nitride crucible and crystal ingot；
(2) quartz ampoule is heated, so that the red phosphorus distillation of boron nitride crucible and seed crystal end deposition deposits to the end of quartz ampoule
Portion, until the transparency of the boron nitride crucible and the quartz ampoule of seed end point reaches the transparency of setting；
(3) crystal ingot in the boron nitride crucible is scanned using ultrasonic wave detector from seed crystal end to tail portion, obtains seed
Brilliant and plane of crystal image；
(4) according to the image of the seed crystal of acquisition and plane of crystal, judge whether are plane of crystal crystallization situation and seed crystal seeding situation
Reach established standards, be, carries out open pipe and the processing of de- crucible；Otherwise it sends the component back to VGF furnace and re-starts growth technique.
2. the InP crystal ingot according to claim 1 to the production of VGF method carries out the side that seed crystal, seeding and crystallization situation determine
Method, which is characterized in that the quartz ampoule is heated in step (2), specifically: 300- is heated to the quartz ampoule with heating furnace
400 degree.
3. the InP crystal ingot according to claim 1 or 2 to the production of VGF method carries out what seed crystal, seeding and crystallization situation determined
Method, which is characterized in that judge that plane of crystal crystallization situation and seed crystal seeding situation refer in step (4), judge seed crystal or crystalline substance
Whether body surface face has twin crystal line and surface blemish, is then to be not up to the established standards, otherwise reaches the established standards.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811640598.5A CN109629002B (en) | 2018-12-29 | 2018-12-29 | Method for performing seed crystal, seeding and crystallization condition judgment on InP crystal ingot produced by VGF method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811640598.5A CN109629002B (en) | 2018-12-29 | 2018-12-29 | Method for performing seed crystal, seeding and crystallization condition judgment on InP crystal ingot produced by VGF method |
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| CN109629002A true CN109629002A (en) | 2019-04-16 |
| CN109629002B CN109629002B (en) | 2021-03-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113668044A (en) * | 2021-07-14 | 2021-11-19 | 威科赛乐微电子股份有限公司 | Single crystal regrowth method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000018990A1 (en) * | 1998-09-30 | 2000-04-06 | Mitsubishi Materials Silicon Corporation | Method for removing defects of single crystal material and single crystal material from which defects are removed by the method |
| CN101698962A (en) * | 2009-11-03 | 2010-04-28 | 中国科学院上海微系统与信息技术研究所 | Method for accurately controlling growth and characterization of components of quaternary semiconductor direct bandgap material |
| CN206396351U (en) * | 2016-12-08 | 2017-08-11 | 珠海鼎泰芯源晶体有限公司 | A kind of InP crystal growing furnaces based on VGF methods |
-
2018
- 2018-12-29 CN CN201811640598.5A patent/CN109629002B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000018990A1 (en) * | 1998-09-30 | 2000-04-06 | Mitsubishi Materials Silicon Corporation | Method for removing defects of single crystal material and single crystal material from which defects are removed by the method |
| CN101698962A (en) * | 2009-11-03 | 2010-04-28 | 中国科学院上海微系统与信息技术研究所 | Method for accurately controlling growth and characterization of components of quaternary semiconductor direct bandgap material |
| CN206396351U (en) * | 2016-12-08 | 2017-08-11 | 珠海鼎泰芯源晶体有限公司 | A kind of InP crystal growing furnaces based on VGF methods |
Non-Patent Citations (2)
| Title |
|---|
| 侯林峰: "基于超声波法的单晶硅棒内部缺陷检测技术研究", 《万方数据》 * |
| 夏纪真 编著: "《工业无损检测技术 超声检测》", 3 January 2017, 中山大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113668044A (en) * | 2021-07-14 | 2021-11-19 | 威科赛乐微电子股份有限公司 | Single crystal regrowth method |
| CN113668044B (en) * | 2021-07-14 | 2024-03-15 | 威科赛乐微电子股份有限公司 | Single crystal regeneration method |
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