CN109576776A - A kind of growing method - Google Patents
A kind of growing method Download PDFInfo
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- CN109576776A CN109576776A CN201811645540.XA CN201811645540A CN109576776A CN 109576776 A CN109576776 A CN 109576776A CN 201811645540 A CN201811645540 A CN 201811645540A CN 109576776 A CN109576776 A CN 109576776A
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- Prior art keywords
- quartz ampoule
- crucible
- pnb
- annealing
- growing method
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Classifications
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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
-
- 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
- C30B11/002—Crucibles or containers for supporting the melt
-
- 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
-
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of growing methods, are related to technical field of crystal growth;Using PNB crucible as growing container, including following process flow: S1: the cleaning of quartz ampoule, quartzy sealing cap, PNB crucible;S2: to quartz ampoule, quartzy sealing cap and PNB crucible vacuum annealing;S3: all raw material is packed into PNB crucible, and PNB crucible is put into quartz ampoule, then vacuumizes to quartz ampoule, tube sealing;S4: the temperature of heater is controlled to control heating, constant temperature and the temperature-fall period of PNB crucible, completes crystal growth;S5: make annealing treatment after crystal growth, further eliminates the Investigation of Residual Donor Defects in crystal, reduces residual stress.The microdefect that inp wafer can be significantly eliminated using growing method disclosed in this invention, eliminates the Investigation of Residual Donor Defects of inp wafer, reduces the residual stress of chip, obtains low dislocation, low defect and the few indium phosphide single crystal material of impurity contamination.
Description
Technical field
The present invention relates to electron crystals to grow field, more particularly to a kind of growing method.
Background technique
Indium phosphide is one of great strategic important semiconductor material, in optic communication, millimeter wave high frequency, low noise, width
Integrating equal fields with microelectronics has important application.With the extensive use of indium phosphide device, indium phosphide single crystal prepares work
Skill is just particularly important, and the indium phosphide crystal growing method generally used now is VGF method (vertical temperature gradient method), also at
For temperature gradient solidification hair, this growing method can inhibit the generation in crystal growth Dislocations defect, to obtain low level
The InP substrate of dislocation density defect, plane of crystal do not dissociate, and can be inherently derived diameter without complicated automatic diamenter control system
Uniform crystal (being determined by crucible shape), convenient for large-scale production.
The quality of indium phosphide semiconductor devices and the superiority and inferiority of substrate material are closely connected, and indium phosphide crystal is whole
Uniformity, stability of perfection of lattice and material etc. can all be influenced by fault in material.Since indium phosphide single crystal is as window
Gate material is in the application demand in the fields such as infrared optics instrument, optic test and scientific research, and this requires indium phosphides as window
Gate material must have good light transmittance, and influence indium phosphide single crystal light transmittance it is dense because being known as background free carrier
Degree, residual impurity and defect etc..Therefore, it how to be substantially reduced defect concentration in indium phosphide single crystal growth course, avoids impurity
It stains, keep its stoicheiometry, reduce the grain defect etc. in crystal, be a weight to obtain the good window material of light transmittance
Point is also difficult point.
Traditional growing method only just comes into operation being cleaned to quartz ampoule, specific cleaning process packet
Include the processes such as chloroazotic acid immersion, acetone soak, salt acid soak, deionized water flushing;But it only with the method for cleaning, still has
The residual of a large amount of hydroxyl and other objectionable impurities, will affect the light transmittance of the crystal of growth.
Summary of the invention
The main purpose of the present invention is to provide a kind of growing methods, can obtain the indium phosphide single crystal of high transparency
Material.
To achieve the above object, the following technical solution is employed by the present invention:
A kind of growing method, it is characterised in that including following process flow:
S1: are all made of by under type such as and is cleaned for quartz ampoule, quartzy sealing cap, PNB crucible:
It is cleaned using organic solvent, and is rinsed with deionized water first, then carry out soaking and washing with acid or chloroazotic acid, finally
It is rinsed well, and is dried for standby with deionized water;
S2: vacuum annealing is carried out to quartz ampoule, quartzy sealing cap and PNB crucible;
S3:PNB crucible is placed in quartz ampoule, and required raw material are packed into inside PNB crucible, are then taken out to quartz ampoule
Vacuum covers quartzy sealing cap when vacuum degree reaches design requirement, carries out tube sealing processing to quartz ampoule;
S4: closed quartz ampoule is put into growth furnace, controls warming temperature gradient, thermostatic process and the drop of quartz ampoule
Warm rate completes crystal growth in PNB crucible;
S5: the annealing after crystal growth.
As a specific technical scheme, organic solvent described in S1 is acetone or alcohol;It is described to be soaked with acid or chloroazotic acid
Steeping the time is 8-12 hours.
It as a specific technical scheme, is 1200 to the vacuum annealing temperature of quartz ampoule, quartzy sealing cap and PNB crucible in S2
DEG C, annealing time is 30 hours, vacuum degree 10-4MmHg or more.
As a specific technical scheme, the raw material being packed into PNB crucible in S3 are as follows: coverture boron oxide, red phosphorus,
Indium phosphide polycrystal and dopant iron.
As a specific technical scheme, in S3 the water content of coverture boron oxide in 300ppm hereinafter, purity be 6N;Red phosphorus
Content be red phosphorus vapour pressure when guaranteeing crystal growth in quartz ampoule not less than 2.8MP;The concentration of indium phosphide polycrystal is lower than
5x1015/cm3, mobility is higher than 4000cm2/ Vs, the field trashes such as no package indium;Concentration range (3-10) x10 of dopant iron15/
cm3。
As a specific technical scheme, the annealing in S5 after crystal growth is specially following manner: to the crystalline substance of growth
Body stick carries out slicing treatment, is put into crystal cut and red phosphorus in quartz ampoule, covers quartzy sealing cap, made annealing treatment, annealing temperature
Degree is 950 DEG C, and annealing time is ± 10 hours 60 hours.
As a specific technical scheme, the tube sealing processing that quartz ampoule carries out is sealed to be sintered with oxyhydrogen flame in S3.
The method have the benefit that by carrying out cleaning and vacuum to quartz ampoule, quartzy sealing cap and PNB crucible
The dual clean of annealing, the objectionable impurities including capable of sufficiently removing comprising hydroxyl;Using crystal growth disclosed in this invention
Method can significantly eliminate the microdefect of inp wafer, eliminate the Investigation of Residual Donor Defects of inp wafer, reduce the residual of chip
It stays stress, obtains low dislocation, low defect and the few indium phosphide single crystal material of impurity contamination.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of growth furnace used in growing method of the invention.
In figure: 1- furnace body, 21- primary heater, 22- secondary heater, 23- third heater, 3- graphite crucible support, 4-
Quartz ampoule, 5-PNB crucible, 6- temperature thermocouple.
Specific embodiment
In order to which technical solution of the present invention is more clearly understood, the present invention is made below in conjunction with attached drawing and specific embodiment
It further illustrates.
Growth furnace used by growth method of the invention as shown in Figure 1, the growth furnace be crystal growth routinely use growth furnace,
Including furnace body 1, heater 2, graphite crucible support 3;The PNB crucible 5 for installing raw material is put into quartz ampoule 4, and quartz ampoule 4 (belongs to
Conventional components, the construction of quartz ampoule 4 does not indicate complete in figure) quartzy sealing cap in top cover (conventional components, figure in do not show), so
After be put into graphite crucible support 3;Graphite crucible support 3 is located in the furnace chamber of furnace body 1, is used to support quartz ampoule 4;Heater setting exists
Around graphite crucible support 3, in crystal growing process, the warm area of crystal growth uses three warm areas herein, with three heaters
The temperature of three warm areas is controlled respectively, and primary heater 21 controls the temperature of the first warm area, second temperature of the control of secondary heater 22
The temperature in area, third heater 23 control the temperature of third warm area;Each heater is separately connected a temperature thermocouple 6.
Embodiment one
A kind of growing method, including following process flow:
S1: are all made of by under type such as and is cleaned for quartz ampoule 4, quartzy sealing cap, PNB crucible 5:
It is cleaned with organic solvent-acetone or alcohol, and is rinsed with deionized water first, then using in acid or chloroazotic acid
8-12 hour is impregnated, finally rinsed well with deionized water and is dried for use, contamination or the residue on surface are removed;
S2: the objectionable impurities removal of quartz ampoule 4, quartzy sealing cap, PNB crucible 5:
To quartz ampoule 4, quartzy sealing cap and 5 vacuum annealing of PNB crucible, sufficiently removes hydroxyl therein and other nocuousness are miscellaneous
Matter;Vacuum annealing temperature is 1200 DEG C, and annealing time is 30 hours, vacuum degree 10-4MmHg or more, in the present embodiment, vacuum
Degree is preferably 2*10-4mmHg;
S3: charging and vacuumizes, closed quartz tube 4
PNB crucible 5 is put into quartz ampoule 4, the indium phosphide polycrystal that coverture boron oxide, high-purity red phosphorus, high-purity are matched
And dopant iron is packed into inside PNB crucible 5, is then vacuumized to quartz ampoule 4, and when vacuum degree reaches design requirement, lid
Upper quartz sealing cap, is sintered quartz ampoule 4 with oxyhydrogen flame and seals;
The sequence that is put into of each raw material is coverture boron oxide-red phosphorus-indium phosphide polycrystal-dopant iron, preferred to cover
The water content of agent boron oxide is in 300ppm hereinafter, purity is 6N;The content of red phosphorus is phosphorus when guaranteeing crystal growth in quartz ampoule 4
Vapour pressure is advisable not less than 2.8MP, so that growth conditions is micro- rich phosphorus state in quartz ampoule 4;The concentration of indium phosphide polycrystal is lower than
5x1015/cm3, mobility is higher than 4000cm2/ Vs, the field trashes such as no package indium;Concentration range (3-10) x10 of dopant iron15/
cm3, can sufficiently occupy indium position and activation becomes acceptor and reaches to compensate to the Investigation of Residual Donor impurity in crystal
To the purpose for reducing background carrier concentration;
The water content of coverture boron oxide is 200ppm in the present embodiment, and the content of red phosphorus is quartz when guaranteeing crystal growth
Phosphorous vapor pressure in pipe 4 is 2.8MP, and the concentration of indium phosphide polycrystal is 2x1015/cm3, mobility 5000cm2/ Vs, dopant
The concentration of iron is 5x1015/cm3;
S4: crystal growth
Closed quartz ampoule 4 is put into growth furnace, controls the liter of quartz ampoule 4 by controlling the temperature of three heaters
Warm temperature gradient, thermostatic process and rate of temperature fall complete crystal growth in PNB crucible 5;To guarantee the rate of crystal growth
It is maintained at 2-3mm/h;The rate control of crystal growth is 2.5mm/h in the present embodiment, and the slow speed of growth effectively avoids
The generation of particle microdefect;
S5: the annealing after crystal growth
Slicing treatment is carried out to the crystal bar of growth, crystal cut and red phosphorus is put into quartz ampoule 4, covers quartzy sealing cap,
To making annealing treatment after 4 tube sealing of quartz ampoule, annealing temperature is 950 DEG C, and annealing time is 60 hours, can further eliminate crystalline substance
Investigation of Residual Donor Defects in body reduces residual stress.
By carrying out the dual clean of cleaning with vacuum annealing, Neng Gouchong to quartz ampoule 4, quartzy sealing cap and PNB crucible 5
Divide and removes hydroxyl therein and other objectionable impurities;Phosphatization can significantly be eliminated using growing method disclosed in this invention
The microdefect of indium chip eliminates the Investigation of Residual Donor Defects of inp wafer, reduces the residual stress of chip, obtains low dislocation, low
Defect and the few indium phosphide single crystal material of impurity contamination.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of growing method, it is characterised in that including following process flow:
S1: are all made of by under type such as and is cleaned for quartz ampoule, quartzy sealing cap, PNB crucible:
It is cleaned using organic solvent, and is rinsed with deionized water first, then carried out soaking and washing with acid or chloroazotic acid, finally spend
Ionized water is rinsed well, and is dried for standby;
S2: vacuum annealing is carried out to quartz ampoule, quartzy sealing cap and PNB crucible;
S3:PNB crucible is placed in quartz ampoule, and required raw material are packed into inside PNB crucible, then take out to quartz ampoule true
Sky covers quartzy sealing cap when vacuum degree reaches design requirement, carries out tube sealing processing to quartz ampoule;
S4: closed quartz ampoule is put into growth furnace, controls warming temperature gradient, thermostatic process and the cooling speed of quartz ampoule
Rate completes crystal growth in PNB crucible;
S5: the annealing after crystal growth.
2. growing method according to claim 1, which is characterized in that organic solvent described in S1 is acetone or wine
Essence;It is described that with acid or chloroazotic acid, to carry out soaking time be 8-12 hours.
3. growing method according to claim 1, which is characterized in that quartz ampoule, quartzy sealing cap and PNB earthenware in S2
The vacuum annealing temperature of crucible is 1200 DEG C, and annealing time is 30 hours, vacuum degree 10-4MmHg or more.
4. growing method according to claim 1, which is characterized in that the former material being packed into PNB crucible in S3
Material are as follows: coverture boron oxide, red phosphorus, indium phosphide polycrystal and dopant iron.
5. growing method according to claim 4, which is characterized in that the water content of coverture boron oxide exists in S3
300ppm is hereinafter, purity is 6N;The content of red phosphorus is that red phosphorus vapour pressure when guaranteeing crystal growth in quartz ampoule is not less than
2.8MP;The concentration of indium phosphide polycrystal is lower than 5x1015/cm3, mobility is higher than 4000cm2/ Vs, the field trashes such as no package indium;It mixes
Concentration range (3-10) x10 of miscellaneous dose of iron15/cm3。
6. growing method according to claim 4, which is characterized in that the annealing in S5 after crystal growth is specific
For following manner: carrying out slicing treatment to the crystal bar of growth, be put into crystal cut and red phosphorus in quartz ampoule, cover quartzy envelope
Cap is made annealing treatment, and annealing temperature is 950 DEG C, and annealing time is ± 10 hours 60 hours.
7. according to claim 1 to growing method described in 6 any one, which is characterized in that carried out in S3 to quartz ampoule
Tube sealing processing for oxyhydrogen flame be sintered seal.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110725008A (en) * | 2019-11-28 | 2020-01-24 | 珠海鼎泰芯源晶体有限公司 | Annealing and de-panning method after crystal growth and crystal preparation method |
CN110952133A (en) * | 2019-12-31 | 2020-04-03 | 珠海鼎泰芯源晶体有限公司 | Quartz sealing cap for crystal growth based on VGF method, crystal growth device and crystal growth process |
CN111041550A (en) * | 2019-12-31 | 2020-04-21 | 珠海鼎泰芯源晶体有限公司 | Gas phase doping crystal growth method based on VGF method |
CN111763988A (en) * | 2020-07-09 | 2020-10-13 | 练小正 | Method for synthesizing indium-arsenic-antimony polycrystalline raw material |
CN113638048A (en) * | 2021-07-15 | 2021-11-12 | 云南鑫耀半导体材料有限公司 | Method for growing indium phosphide single crystal by VGF method |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110725008A (en) * | 2019-11-28 | 2020-01-24 | 珠海鼎泰芯源晶体有限公司 | Annealing and de-panning method after crystal growth and crystal preparation method |
CN110952133A (en) * | 2019-12-31 | 2020-04-03 | 珠海鼎泰芯源晶体有限公司 | Quartz sealing cap for crystal growth based on VGF method, crystal growth device and crystal growth process |
CN111041550A (en) * | 2019-12-31 | 2020-04-21 | 珠海鼎泰芯源晶体有限公司 | Gas phase doping crystal growth method based on VGF method |
CN111041550B (en) * | 2019-12-31 | 2021-10-12 | 珠海鼎泰芯源晶体有限公司 | Gas phase doping crystal growth method based on VGF method |
CN111763988A (en) * | 2020-07-09 | 2020-10-13 | 练小正 | Method for synthesizing indium-arsenic-antimony polycrystalline raw material |
CN111763988B (en) * | 2020-07-09 | 2021-12-14 | 进化半导体(深圳)有限公司 | Method for synthesizing indium-arsenic-antimony polycrystalline raw material |
CN113638048A (en) * | 2021-07-15 | 2021-11-12 | 云南鑫耀半导体材料有限公司 | Method for growing indium phosphide single crystal by VGF method |
CN113638048B (en) * | 2021-07-15 | 2022-07-15 | 云南鑫耀半导体材料有限公司 | Method for growing indium phosphide single crystal by VGF method |
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Application publication date: 20190405 |