CN1594672A - Visual temperature ladder crystal condensation growth device with low oblique and growth method thereof - Google Patents
Visual temperature ladder crystal condensation growth device with low oblique and growth method thereof Download PDFInfo
- Publication number
- CN1594672A CN1594672A CN 200410043669 CN200410043669A CN1594672A CN 1594672 A CN1594672 A CN 1594672A CN 200410043669 CN200410043669 CN 200410043669 CN 200410043669 A CN200410043669 A CN 200410043669A CN 1594672 A CN1594672 A CN 1594672A
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- growth
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- silica tube
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- 239000013078 crystal Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000009833 condensation Methods 0.000 title claims description 10
- 230000005494 condensation Effects 0.000 title claims description 10
- 230000000007 visual effect Effects 0.000 title claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 8
- 230000001154 acute effect Effects 0.000 claims description 6
- 230000036760 body temperature Effects 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 abstract 2
- 230000001174 ascending effect Effects 0.000 abstract 1
- 239000002775 capsule Substances 0.000 abstract 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract 1
- 239000010931 gold Substances 0.000 abstract 1
- 229910052737 gold Inorganic materials 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000010453 quartz Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 3
- 229910052951 chalcopyrite Inorganic materials 0.000 description 3
- 239000002178 crystalline material Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000003255 drug test Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A visualized small angle inclination temperature gradient condensing unit for crystal growth and its growth method is provided, relating to a crystal material growing device and growing method. Existing growing device has shortcomings that gold plating is not convenient, plating layer is not uniform, and crystal growth has great stress. The inventive growth device is mounted inclining to ground, and in the inclined device, the horizontal elevation of high temperature hot resistance is higher than low temperature hot resistance. The inventive growing method is : placing growing vessel (3) in quartz capsule(4), sealing then placing it in growing device, ascending the oven temperature, keeping the high temperature 1-2 hours, then reducing oven temperature, temperature descending speed being 0.05-0.1K/hr, when whole crystal forming, promoting temperature descending speed to 2-5K/hr until the room temperature. Crystal can orientablly grow in the inventive device, and downward growth of crystal accords with the growth rule than horizontal growth, in downward growth the crystal quality is still better. The inventive method can avoid crystal crack, adapt to the generalized application.
Description
Technical field:
The present invention relates to a kind of growing apparatus and growth method thereof of crystalline material.
Background technology:
Later 1960s, people just recognize that chalcopyrite based semiconductor crystalline material has two outstanding advantages: nonlinear optical coefficients and far infrared region transmitance are very high, utilize them as optical parametric oscillation, optical parameter is amplified, second harmonic, the nonlinear dielectric material of four-time harmonic etc., can in, the frequency inverted aspect of red wave band far away, especially the field that laser power is had relatively high expectations, obtain wide application prospect, as infrared spectra, the Infrared Therapy apparatus, drug testing, infrared photoetching, the monitoring of objectionable impurities in the atmosphere, remote chemical sensitisation, the infrared laser directional jamming, night vision equipment etc.But, have two problems to restrict the application of this crystalloid material always: since serious anisotropic thermal expansion, large-size crystals growth difficulty; Native defect causes photoabsorption and scattering of light, and crystal reduces near and middle infrared transmitance.
This crystalline development and applied research work is all being carried out in U.S. Sanders company, Inrad company, naval laboratory, Stanford University nonlinear optical material center etc., and they mainly adopt transparent horizontal gradient method growing crystal, and size reaches 100mm; The scientific research personnel of Russia Tomsk university, light detection research institute (Institute ofOptic Monitoring) mainly adopts the Bridgman-Stockbarge method for growing crystal; Recent years, Israel has also begun to develop this crystal.But also there is certain defective in these methods, influence crystal mass.Adopt transparent horizontal gradient method this crystal of growing as the U.S., they adopt three layers of silica glasss insulation, and outermost layer silica glass inboard is gold-plated, and its shortcoming is that inner gold-plated inconvenience, uneven coating are even, and heat insulation effect is bad; Growth ship seed crystal end and melt end junction that they adopt are the right angle, and the stress when this makes crystal growth increases, and has increased striation, thereby has reduced crystal mass.Russia etc. adopt this crystalloid of Bridgman-Stockbarge method for growing, and process of growth is invisible, can not the better controlled growth, and in addition, this method can't be avoided this material different and cracking of causing of thermal stresses in different directions.
Summary of the invention:
The object of the present invention is to provide a kind of crystal can oriented growth, the coating densification, visual small angle inclination temperature ladder condensation growth device of even and crystalline high insulating effect and growth method thereof, the inventive system comprises three layers of silica tube 1, be installed in the thermocouple 2 between second layer silica tube 1-2 and the 3rd layer of silica tube 1-3, be installed in the growth ship 3 in the 3rd layer of silica tube 1-3, be installed in low temperature hot resistance 5-1 and elevated temperature heat resistance 5-2 in the second layer silica tube 1-2, this growing apparatus and ground are inclined to set, in the device after the inclination, the level height of elevated temperature heat resistance 5-2 is higher than the level height of low temperature hot resistance 5-1; Growth method of the present invention is: the growth ship 3 that raw material and seed crystal will be housed places silica tube 4, vacuumize and seal in the silica tube 4 and be placed in the 3rd layer of silica tube 1-3, the seed crystal section 3-1 of growth ship 3 places the body of heater cold zone, the feed end 3-2 of growth ship 3 places the high-temperature zone, the rising furnace temperature, all melting, kept temperature 1～2 hour until seed crystal near thawing 0.1～5mm of feed end 3-2 place and raw material; Reduce furnace body temperature then, rate of temperature fall is 0.05～0.1K/hr, when whole crystal generates in the growth ship 3, rate of temperature fall is brought up to 2～5K/hr, until dropping to room temperature, when temperature-fall period passes through the phase transition point of material, stopped 10～20 hours, and continued to reduce to room temperature then and get final product.Growth furnace of the present invention becomes small angle inclination with horizontal plane, and melting raw material can directly contact with seed crystal, and crystal can oriented growth, simultaneously, the downward growth fraction horizontal growth of crystal, this more meets the crystal growth rule, and crystal mass is better; The second layer silica glass of the present invention outside is gold-plated or silver-plated, advantage be the outside gold-plated or silver-plated easier, coating is finer and close, even, better heat preservation; The present invention ship two places of growing link and to be acute angle, and the stress in the time of can reducing growth reduces striation, improves crystal mass; Growth method of the present invention is compared with the prior art growth method, and its rate of temperature fall is low, can reduce the thermal stresses of crystal growing process like this, thereby avoids crystal cleavage.
Description of drawings:
Fig. 1 is the structural representation of apparatus of the present invention, and Fig. 2 is the structural representation of growth ship 3, and Fig. 3 is the A-A sectional view of Fig. 2.
Embodiment:
Embodiment one: the inventive system comprises three layers of silica tube 1, be installed in the thermocouple 2 between second layer silica tube 1-2 and the 3rd layer of silica tube 1-3, be installed in the growth ship 3 in the 3rd layer of silica tube 1-3, be installed in low temperature hot resistance 5-1 and elevated temperature heat resistance 5-2 in the second layer silica tube 1-2, this growing apparatus and ground are inclined to set, this inclination alpha is 0.1～25 degree, can be 1 degree, 3 degree, 8 degree, 10 degree, 12 degree, 18 degree, 22 degree, in the device after the inclination, the level height of elevated temperature heat resistance 5-2 is higher than the level height of low temperature hot resistance 5-1, outside surface at second layer silica tube 1-2 is gold-plated or silver-plated, and it not only can be incubated but also can be transparent under illumination.
The growth method of present embodiment is: the growth ship 3 that raw material and seed crystal will be housed places silica tube 4, vacuumize and seal in the silica tube 4 and be placed in the 3rd layer of silica tube 1-3, body of heater is divided into low temperature and two heating zone of high temperature, resistive heating, body of heater temperature ladder is 1～2K/cm, furnace body temperature is measured and control by two thermopairs and precise temperature control instrument, the seed crystal section 3-1 of growth ship 3 places the body of heater cold zone, the feed end 3-2 of growth ship 3 places the high-temperature zone, the rising furnace temperature, all melting, kept temperature 1～2 hour until seed crystal near thawing 0.1～5mm of feed end 3-2 place and raw material; Reduce furnace body temperature then, rate of temperature fall is 0.05～0.1K/hr, can be 0.06K/hr, 0.07K/hr 0.08K/hr is when whole crystal generates in the growth ship 3, rate of temperature fall is brought up to 2～5K/hr, until dropping to room temperature, rate of temperature fall can be 2.5K/hr, 3.5K/hr, 4.5K/hr, when temperature-fall period passes through the phase transition point of material, stopped 10～20 hours, continue to reduce to room temperature then and get final product.
Embodiment two: the seed crystal end 3-1 and the melt end 3-2 junction of present embodiment growth ship 3 are acute angle, and this acute angles beta is 1～60 degree, can be 5 degree, 10 degree, 20 degree, 30 degree, 40 degree, 50 degree.
Growing apparatus of the present invention and growth method can be used for the growth of chalcopyrite based semiconductor crystalline material, and polycrystal raw material places the growth ship, and growth ship material is graphite, vitrifying graphite, the silica glass that scribbles boron nitride coating.
Chalcopyrite based semiconductor material comprises IB-IIIA-VIA
2And IIB-IVA-VA
2Compounds of group.IB family element comprises Cu, Ag, and IIIA family element comprises Al, Ga, In, and VIA family element comprises S, Se, Te; IIB family element comprises Zn, Cd, Hg, and IVA family element comprises Si, Ge, Sn, and VA family element comprises P, As.
Claims (7)
1, the visual small angle inclination temperature ladder of a kind of crystalline condensation growth device, it comprises three layers of silica tube (1), is installed in the thermocouple (2) between second layer silica tube (1-2) and the 3rd layer of silica tube (1-3), be installed in the growth ship (3) in the 3rd layer of silica tube (1-3), be installed in low temperature hot resistance (5-1) and elevated temperature heat resistance (5-2) in the second layer silica tube (1-2), it is characterized in that this growing apparatus and ground are inclined to set, in the device after the inclination, the level height of elevated temperature heat resistance (5-2) is higher than the level height of low temperature hot resistance (5-1).
2, the visual small angle inclination temperature ladder of crystalline according to claim 1 condensation growth device, the angle (α) that it is characterized in that this growing apparatus and terrain slope is 0.1～25 degree.
3, the visual small angle inclination temperature ladder of crystalline according to claim 1 and 2 condensation growth device is characterized in that at the outside surface of second layer silica tube (1-2) gold-plated or silver-plated.
4, the visual small angle inclination temperature ladder of crystalline according to claim 1 and 2 condensation growth device is characterized in that the seed crystal end (3-1) of described growth ship (3) and melt end (3-2) junction are acute angle.
5, the visual small angle inclination temperature ladder of crystalline according to claim 3 condensation growth device is characterized in that the seed crystal end (3-1) of described growth ship (3) and melt end (3-2) junction are acute angle.
6, the visual small angle inclination temperature ladder of crystalline according to claim 5 condensation growth device is characterized in that described acute angle (β) is 1～60 degree.
7, the visual small angle inclination temperature ladder of a kind of crystalline condensation growth method, it is characterized in that: the growth ship (3) that raw material and seed crystal will be housed places silica tube (4), vacuumize and seal in the silica tube (4) and be placed in the 3rd layer of silica tube (1-3), the seed crystal section (3-1) of growth ship (3) places the body of heater cold zone, the feed end (3-2) of growth ship (3) places the high-temperature zone, the rising furnace temperature, locating to melt 0.1～5mm and raw material all melts until seed crystal near feed end (3-2), keeping temperature 1～2 hour; Reduce furnace body temperature then, rate of temperature fall is 0.05～0.1K/hr, when whole crystal generates in the growth ship (3), rate of temperature fall is brought up to 2～5K/hr, until reducing to room temperature, when temperature-fall period passes through the phase transition point of material, stopped 10～20 hours, and continued to reduce to room temperature then and get final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100436695A CN1307329C (en) | 2004-06-30 | 2004-06-30 | Visual temperature ladder crystal condensation growth device with low oblique and growth method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100436695A CN1307329C (en) | 2004-06-30 | 2004-06-30 | Visual temperature ladder crystal condensation growth device with low oblique and growth method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1594672A true CN1594672A (en) | 2005-03-16 |
| CN1307329C CN1307329C (en) | 2007-03-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100436695A Expired - Fee Related CN1307329C (en) | 2004-06-30 | 2004-06-30 | Visual temperature ladder crystal condensation growth device with low oblique and growth method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN1307329C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105714372A (en) * | 2016-03-28 | 2016-06-29 | 中国科学院福建物质结构研究所 | Crystal growing device |
| CN105734668A (en) * | 2016-03-28 | 2016-07-06 | 中国科学院福建物质结构研究所 | Growth method of Ba3P3O10Cl monocrystal |
| CN105926031A (en) * | 2016-06-08 | 2016-09-07 | 中国工程物理研究院化工材料研究所 | Inspection window applied to tubular single crystal growth furnace |
| CN108239787A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波材料技术与工程研究所 | A kind of method for preparing SnSe crystal |
| CN114574971A (en) * | 2021-12-23 | 2022-06-03 | 中国科学院福建物质结构研究所 | Visual CVT sulfide crystal growth device and method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001181084A (en) * | 1999-12-27 | 2001-07-03 | Natl Space Development Agency Of Japan | Single crystal-growing unit |
| FR2826377B1 (en) * | 2001-06-26 | 2003-09-05 | Commissariat Energie Atomique | DEVICE FOR MANUFACTURING COOLING ALLOY CRYSTALS AND CONTROLLED SOLIDIFICATION OF A LIQUID MATERIAL |
-
2004
- 2004-06-30 CN CNB2004100436695A patent/CN1307329C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105714372A (en) * | 2016-03-28 | 2016-06-29 | 中国科学院福建物质结构研究所 | Crystal growing device |
| CN105734668A (en) * | 2016-03-28 | 2016-07-06 | 中国科学院福建物质结构研究所 | Growth method of Ba3P3O10Cl monocrystal |
| CN105714372B (en) * | 2016-03-28 | 2018-08-28 | 中国科学院福建物质结构研究所 | A kind of crystal growing apparatus |
| CN105734668B (en) * | 2016-03-28 | 2018-09-28 | 中国科学院福建物质结构研究所 | A kind of Ba3P3O10The growing method of Cl monocrystalline |
| CN105926031A (en) * | 2016-06-08 | 2016-09-07 | 中国工程物理研究院化工材料研究所 | Inspection window applied to tubular single crystal growth furnace |
| CN105926031B (en) * | 2016-06-08 | 2018-11-09 | 中国工程物理研究院化工材料研究所 | A kind of observation window for tubular type monocrystal growing furnace |
| CN108239787A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院宁波材料技术与工程研究所 | A kind of method for preparing SnSe crystal |
| CN114574971A (en) * | 2021-12-23 | 2022-06-03 | 中国科学院福建物质结构研究所 | Visual CVT sulfide crystal growth device and method |
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| Publication number | Publication date |
|---|---|
| CN1307329C (en) | 2007-03-28 |
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Effective date of registration: 20190722 Address after: 150000 Heilongjiang Province, Harbin City Economic Development Zone haping Road District Dalian road and Xingkai road junction Patentee after: HIT ROBOT GROUP Co.,Ltd. Address before: 150001 Harbin, Nangang, West District, large straight street, No. 92 Patentee before: Harbin Institute of Technology |
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