CN103194790B - The grower of a kind of phosphorus germanium zinc monocrystal and method - Google Patents
The grower of a kind of phosphorus germanium zinc monocrystal and method Download PDFInfo
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- CN103194790B CN103194790B CN201310115730.1A CN201310115730A CN103194790B CN 103194790 B CN103194790 B CN 103194790B CN 201310115730 A CN201310115730 A CN 201310115730A CN 103194790 B CN103194790 B CN 103194790B
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- MOHPKPMGPNKIKH-UHFFFAOYSA-N [Zn].[Ge].[P] Chemical compound [Zn].[Ge].[P] MOHPKPMGPNKIKH-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 57
- 239000003708 ampul Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000013078 crystal Substances 0.000 claims abstract description 24
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 18
- 238000009413 insulation Methods 0.000 claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 230000007423 decrease Effects 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims 1
- 230000006911 nucleation Effects 0.000 abstract description 6
- 238000010899 nucleation Methods 0.000 abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- QZLIUFNMYYCGQN-UHFFFAOYSA-N [Ge].[P] Chemical compound [Ge].[P] QZLIUFNMYYCGQN-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 238000013461 design Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MRZMQYCKIIJOSW-UHFFFAOYSA-N germanium zinc Chemical compound [Zn].[Ge] MRZMQYCKIIJOSW-UHFFFAOYSA-N 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004297 night vision Effects 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of grower and the method for phosphorus germanium zinc monocrystal.This device includes growth furnace, silica crucible and crucible tray, also includes the insulation powder being filled between silica crucible and crucible tray, is provided with growth ampoule in silica crucible, and crucible tray is placed on pedestal.This device by by the seed crystal end of growth ampoule as in phosphorus germanium zinc polycrystal material, monocrystalline nucleation rate is obviously improved, the temperature of crystal seed end is the most stable, ensure to obtain complete unidirectional seed crystal at the nucleation initial stage, decomposition pressure that the design of internal and external casing simultaneously is higher when can bear phosphorus germanium zinc crystal growth and form relatively flat solid liquid interface when being effectively facilitated growth, thus ensure the phosphorus germanium complete flawless of zinc monocrystalline of growth, and success rate is higher.
Description
Technical field
The present invention relates to the growing technology field of a kind of phosphorus germanium zinc monocrystal, be specifically designed grower and the method for a kind of phosphorus germanium zinc monocrystal.
Background technology
Middle-infrared band (3-5 μm) LASER Light Source suffers from great application prospect at dual-use two aspects.Civilian aspect includes remote sensing, laser radar, atmosphere light communication and range measurement etc..Military aspect includes Infrared jamming, night vision, laser communications etc..And optical parametric oscillator utilizes the nonlinear effect of material can realize the lower conversion of frequency, near-infrared laser is changed to middle-infrared band.Phosphorus germanium zinc crystal is exactly the nonlinear optical crystal of a kind of excellent performance, and it has bigger nonlinear factor, and optics is higher through wide ranges and thermal conductivity.Utilize phosphorus germanium zinc crystal under first kind phase matched, tuning can be obtained in whole middle-infrared band.The U.S. and Russia have grown high-quality phosphorus germanium zinc monocrystal the most in succession, and China is also in developmental stage.
The problem that now growth of phosphorus germanium zinc monocrystal is primarily present is that the size of growth is less, monocrystalline success rate is relatively low, repeated poor and crystal is easy to crack, particularly when utilizing spontaneous nucleation growth monocrystalline, owing to the particularity of seed crystal end causes the warm field instability of seed portion, nucleation probability is relatively low.And seed crystal end first has to form complete quality preferable monocrystalline guarantee and obtains the monocrystal that a monoblock is intact.
Therefore, how to obtain the monocrystalline of good quality, be one of ordinary skill in the art's technical barriers in the urgent need to address.
Summary of the invention
It is an object of the invention to be to provide the grower of a kind of phosphorus germanium zinc monocrystal, it can solve the low success rate of problem of monocrystalline that phosphorus germanium zinc monocrystalline nucleation probability is low and warm field instability causes.
Another object of the present invention is to provide the growing method of a kind of phosphorus germanium zinc monocrystal.
The object of the invention to solve the technical problems realizes by the following technical solutions.According to the grower of a kind of phosphorus germanium zinc monocrystal that the present invention proposes, including crucible tray and silica crucible, it also includes the insulation powder being filled between described crucible tray and described silica crucible；It is provided with growth ampoule in described silica crucible；Described crucible tray is placed on pedestal.
Further, the internal diameter of described crucible tray is 40mm-50mm, its thickness is 5mm-10mm, its a length of 25mm-35mm, the material of crucible tray is aluminium oxide or zirconium oxide, both materials can effectively be kept out thermal shock and be simultaneously worked as good heat insulation effect, and the insulation of tube wall is favourable to forming flat interface.
Further, the material of described insulation powder is alumina powder or zirconia powder, utilizes powder to fill the vibration that can effectively reduce grower, thus avoids the unstable factor in growth course.
Further, the internal diameter of described silica crucible is 19mm-25mm, and its thickness is 2.5mm-3.5mm, its a length of 20mm-30mm, and the external diameter of silica crucible is less than the internal diameter of crucible tray.
Further, the external diameter of described growth ampoule is 18mm-24mm, and its thickness is 1mm-1.5mm, its a length of 15mm-25mm, the external diameter 1mm-2mm less than the internal diameter of silica crucible of growth ampoule, and its material is quartz or boron nitride.Growth ampoule can serve as thermal insulation layer than the space (1mm-2mm) between silica crucible, plays certain heat insulation effect, is so also beneficial to form relatively flat interface.
Further, described silica crucible is positioned on the axis of crucible tray；Described growth ampoule is placed on the axis of silica crucible.
It addition, the invention allows for the growing method of a kind of phosphorus germanium zinc monocrystal, comprise the steps:
1) 5g-20g phosphorus germanium zinc polycrystal material is clayed into power it is filled into the bottom of silica crucible；15g-80g phosphorus germanium zinc polycrystal material is mixed with the red phosphorus of 5g-8g, then fills this blend in growth ampoule, then growth ampoule is placed in silica crucible, then by silica crucible evacuation sealed knot；
2) silica crucible of sealed knot is placed on pedestal, then raises the base into the position measured in advance in growth furnace；Warm field in growth furnace comprises three parts: high-temperature region, gradient zones, low-temperature space；Then the temperature of three warm areas is risen to target temperature from room temperature, and ensure that the lowermost end of silica crucible is in the position of 1027 DEG C；After the temperature in growth furnace rises to target temperature, it is incubated 35-45 hour, then keeps the rotation of pedestal, and begin to decline growth；
3), after growth terminates, phosphorus germanium zinc monocrystal is slowly dropped to 920 DEG C, is then cooled to 650 DEG C, be finally down to room temperature, i.e. obtain phosphorus germanium zinc monocrystal.
Further, in described step 1), the seed crystal end of growth ampoule is immersed in the polycrystal material bottom silica crucible, and silica crucible is evacuated to 10-4Pa。
Further, described step 2) in, the target of described high-temperature region is 1050 DEG C-1060 DEG C, and the thermograde of described gradient zones is 4 DEG C-8 DEG C, and the target temperature of described low-temperature space is 980 DEG C-990 DEG C；Three warm areas of growth furnace rose to target temperature through 6-10 hour from room temperature；The velocity of rotation of described pedestal is 0.5-2rpm, and decrease speed is 0.5-1mm/h.
Further, in described step 3), after growth terminates, phosphorus germanium zinc monocrystal is down to 920 DEG C with 5-15 DEG C/h, is then down to 650 DEG C with 20-25 DEG C/h, is finally down to room temperature with 30-50 DEG C/h.
By technique scheme, the invention have the advantages that and beneficial effect:
1) due to the fact that and the seed crystal end of growth ampoule is immersed in phosphorus germanium zinc polycrystal material, monocrystalline nucleation rate is greatly improved, ensure that the stability of the initial warm field of seed crystal end simultaneously, such that it is able to the perfection of crystal ensured in the incipient stage of crystal growth and the most structural；
2) due to the fact that insulation powder is filled between crucible tray and silica crucible, thus ensure that the stability of quartz ampoule, and the stability of silica crucible serves conclusive effect to the growth of crystal, insulation powder also functions to good heat insulation effect simultaneously, it is ensured that the stability of growth course middle temperature field.
3) present invention has reserved the space between growth ampoule and quartz ampoule, and the space of this section tiny serves the effect of heat-insulation layer, is favourable to forming smooth growth interface.
4) present device is simple, decomposition pressure that the design of internal and external casing simultaneously is higher when can bear phosphorus germanium zinc crystal growth and form relatively flat solid liquid interface when being effectively facilitated growth, thus ensure the phosphorus germanium complete flawless of zinc monocrystalline of growth, and success rate is higher；And it is easily controlled growthing process parameter, beneficially automatization's growth.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the grower of phosphorus germanium zinc monocrystal of the present invention；
Fig. 2 is the phosphorus germanium zinc monocrystalline of the embodiment of the present invention 1 growth；
Fig. 3 is the X-ray rocking curve of the phosphorus germanium zinc monocrystalline of the embodiment of the present invention 1 growth；
Fig. 4 is the phosphorus germanium zinc monocrystalline of the embodiment of the present invention 2 growth；
Fig. 5 is the X-ray rocking curve of the phosphorus germanium zinc monocrystalline of the embodiment of the present invention 2 growth.
1: crucible tray 2: insulation material
3: silica crucible 4: growth ampoule
5: growth furnace 6: phosphorus germanium zinc monocrystal
7: phosphorus germanium zinc polycrystal material 8: pedestal
Detailed description of the invention
The present invention is described in further detail to combine accompanying drawing below by concrete preferred embodiment, but the present invention is not limited in below example.
Wherein, in following embodiment, drop tube furnace used by phosphorus germanium zinc single crystal growth is field of crystal growth prior art.
Embodiment 1
In the present embodiment, the grower of phosphorus germanium zinc monocrystal, as it is shown in figure 1, its structure includes crucible tray 1 and silica crucible 3, also includes the insulation powder 2 being filled between crucible tray 1 and silica crucible 3, being provided with growth ampoule 4 in silica crucible 3, crucible tray 1 is placed on pedestal 8.
The internal diameter of crucible tray 1 used is 40mm, and its thickness is 5mm, its a length of 25mm, and the material of crucible tray 1 is aluminium oxide.
The material of insulation powder 2 used is alumina powder.
The internal diameter of this silica crucible 3 is 15mm, and its thickness is 2.5mm, its a length of 20mm.
The external diameter of this growth ampoule 4 is 14mm, and its thickness is 1.5mm, its a length of 15mm-25mm, and its material is quartz.
The growing method of the phosphorus germanium zinc monocrystal in the present embodiment, comprises the steps:
1) 10g phosphorus germanium zinc polycrystal material 7 is clayed into power it is filled into the bottom of silica crucible 3；The red phosphorus of 25g phosphorus germanium zinc polycrystal material and 5g is mixed, then fill this blend in growth ampoule 4, then growth ampoule 4 is placed in silica crucible 3, and the seed crystal end of growth ampoule 3 is immersed in the polycrystal material bottom silica crucible 4, then silica crucible 3 is evacuated to 10-4Pa sealed knot.
2) silica crucible 3 of sealed knot is placed on pedestal 8, then pedestal 8 is promoted in growth furnace 5 position of mensuration in advance.Warm field in growth furnace comprises three parts: high-temperature region, gradient zones, low-temperature space；The target of high-temperature region is 1050 DEG C-1060 DEG C, and the thermograde of gradient zones is 4 DEG C-8 DEG C, and the target temperature of low-temperature space is 980 DEG C-990 DEG C.Then the temperature of three warm areas was risen to target temperature through 6-10 hour from room temperature, and ensure that the lowermost end of silica crucible 3 is in the position of 1027 DEG C.After the temperature in growth furnace rises to target temperature, it is incubated 35-45 hour, then keeps the rotation of pedestal, and begin to decline growth.The velocity of rotation of pedestal is 0.5-2rpm, and decrease speed is 0.5-1mm/h.
3), after growth terminates, phosphorus germanium zinc monocrystal 6 is down to 920 DEG C with 5-15 DEG C/h, is then down to 650 DEG C with 20-25 DEG C/h, is finally down to room temperature with 30-50 DEG C/h.
Fig. 2 show the phosphorus germanium zinc monocrystal of acquisition, and the complete flawless of monocrystal, size reaches: diameter 11mm, length 60mm.
The X-ray rocking curve that Fig. 3 measures after showing axially cutting.According to Fig. 3, it is thus achieved that phosphorus germanium zinc monoclinic crystal structure fine.
Embodiment 2
The present embodiment difference from embodiment 1 is: the material of crucible tray 1 is zirconium oxide；Other structures of device and technical process are the most identical.
Embodiment 3
The present embodiment difference from embodiment 1 is: the material of growth ampoule 4 is boron nitride；Other structures of device and technical process are the most identical.
Embodiment 4
The present embodiment difference from embodiment 2 is: the material of growth ampoule 4 is boron nitride；Other structures of device and technical process are the most identical.
Embodiment 5
In the present embodiment, the grower of phosphorus germanium zinc monocrystal as shown in Figure 1: including crucible tray 1 and silica crucible 3, also include the insulation powder 2 being filled between crucible tray 1 and silica crucible 3, be provided with growth ampoule 4 in silica crucible 3, crucible tray 1 is placed on pedestal 8.
The internal diameter of crucible tray 1 used is 40mm, and its thickness is 5mm, its a length of 25mm, and the material of crucible tray 1 is aluminium oxide.
The material of insulation powder 2 used is alumina powder.
The internal diameter of described silica crucible 3 is 19mm, and its thickness is 3mm, its a length of 20mm.
The external diameter of described growth ampoule 4 is 18mm, and its thickness is 1.5mm, its a length of 15mm-25mm, and its material is quartz.
The growing method of the phosphorus germanium zinc monocrystal in the present embodiment, comprises the steps:
1) 11g phosphorus germanium zinc polycrystal material 7 is clayed into power it is filled into the bottom of silica crucible 3；The red phosphorus of 50g phosphorus germanium zinc polycrystal material and 6.5g is mixed, then fill this blend in growth ampoule 4, then growth ampoule 4 is placed in silica crucible 3, and the seed crystal end of growth ampoule 3 is immersed in the polycrystal material bottom silica crucible 4, then silica crucible 3 is evacuated to 10-4Pa sealed knot.
2) silica crucible 3 of sealed knot is placed on pedestal 8, then pedestal 8 is promoted in growth furnace 5 position of mensuration in advance.Warm field in growth furnace comprises three parts: high-temperature region, gradient zones, low-temperature space；The target of high-temperature region is 1050 DEG C-1060 DEG C, and the thermograde of gradient zones is 4 DEG C-8 DEG C, and the target temperature of low-temperature space is 980 DEG C-990 DEG C.Then the temperature of three warm areas was risen to target temperature through 6-10 hour from room temperature, and ensure that the lowermost end of silica crucible is in the position of 1027 DEG C.After the temperature in growth furnace rises to target temperature, it is incubated 35-45 hour, then keeps the rotation of pedestal, and begin to decline growth.The velocity of rotation of pedestal is 0.5-2rpm, and decrease speed is 0.5-1mm/h.
3), after growth terminates, phosphorus germanium zinc monocrystal 6 is down to 920 DEG C with 5-15 DEG C/h, is then down to 650 DEG C with 20-25 DEG C/h, is finally down to room temperature with 30-50 DEG C/h.
Fig. 3 show the phosphorus germanium zinc monocrystal of acquisition, and the complete flawless of monocrystal, size reaches: diameter 15mm, length 70mm.
Fig. 4 show axially cutting after measure X-ray rocking curve, according to Fig. 4, it is thus achieved that phosphorus germanium zinc monoclinic crystal structure fine.
Embodiment 6
The present embodiment difference from embodiment 5 is: the material of crucible tray 1 is zirconium oxide.
Embodiment 7
The present embodiment difference from embodiment 5 is: the material of growth ampoule 4 is boron nitride；Other structures of device and technical process are the most identical.
Embodiment 8
The present embodiment difference from embodiment 6 is: the material of growth ampoule 4 is boron nitride；Other structures of device and technical process are the most identical.
The above, it it is only presently preferred embodiments of the present invention, not the present invention is made any pro forma restriction, therefore it is every without departing from technical solution of the present invention content, any simple modification, equivalent variations and the modification made above example according to the technical spirit of the present invention, all still falls within the range of technical solution of the present invention.
Claims (4)
1. the growing method of a phosphorus germanium zinc monocrystal, it is characterised in that comprise the steps:
1) being clayed into power by 10g-20g phosphorus germanium zinc polycrystal material the bottom of the silica crucible being filled into grower, described grower includes growth furnace, crucible tray and silica crucible, and the insulation powder being filled between described crucible tray and described silica crucible；Described silica crucible is positioned on the axis of crucible tray；Described growth ampoule is placed on the axis of silica crucible；The material of described insulation powder is alumina powder or zirconia powder；The external diameter of described silica crucible is less than the internal diameter of described crucible tray；It is provided with growth ampoule in described silica crucible；The external diameter 1mm-2mm less than the internal diameter of silica crucible of described growth ampoule, its material is quartz or boron nitride；Described crucible tray is placed on pedestal；The material of described crucible tray is aluminium oxide or zirconium oxide；15g-80g phosphorus germanium zinc polycrystal material is mixed with the red phosphorus of 5g-8g, then fills this blend in growth ampoule, then growth ampoule is placed in silica crucible, then by silica crucible evacuation sealed knot；
2) silica crucible of sealed knot is placed on pedestal, then raises the base into the position measured in advance in growth furnace；Warm field in growth furnace comprises three parts: high-temperature region, gradient zones, low-temperature space；The target of described high-temperature region is 1050 DEG C-1060 DEG C, and the thermograde of described gradient zones is 4 DEG C-8 DEG C, and the target temperature of described low-temperature space is 980 DEG C-990 DEG C；Then the temperature of three warm areas is risen to target temperature from room temperature, and ensure that the lowermost end of silica crucible is in the position of 1027 DEG C；After the temperature in growth furnace rises to target temperature, it is incubated 35-45 hour, then keeps the rotation of pedestal, and begin to decline growth；
3), after growth terminates, phosphorus germanium zinc monocrystal is down to 920 DEG C with 5-15 DEG C/h, is then down to 650 DEG C with 20-25 DEG C/h, is finally down to room temperature with 30-50 DEG C/h, i.e. obtain phosphorus germanium zinc monocrystal.
The growing method of phosphorus germanium zinc monomer the most according to claim 1, it is characterised in that: the internal diameter of described crucible tray is 40mm-50mm, and its thickness is 5mm-10mm, its a length of 25mm-35mm；The internal diameter of described silica crucible is 15mm-25mm, and its thickness is 2.5mm-3.5mm, its a length of 20mm-30mm；The external diameter of described growth ampoule is 14mm-24mm, and its thickness is 1mm-1.5mm, its a length of 15mm-25mm.
The growing method of phosphorus germanium zinc monocrystal the most according to claim 1, it is characterised in that: described step 1) in, the seed crystal end of growth ampoule is immersed in the polycrystal material bottom silica crucible, and silica crucible is evacuated to 10-4Pa。
The growing method of phosphorus germanium zinc monocrystal the most according to claim 1, it is characterised in that: described step 2) in, three warm areas of growth furnace rose to target temperature through 6-10 hour from room temperature；The velocity of rotation of described pedestal is 0.5-2rpm, and decrease speed is 0.5-1mm/h.
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| CN107268070A (en) * | 2017-06-10 | 2017-10-20 | 中国科学院合肥物质科学研究院 | A kind of method of low absorption phosphorus germanium zinc crystal growth |
| CN110042461B (en) * | 2019-04-30 | 2021-06-08 | 哈尔滨工业大学 | Growth method of large-size zinc germanium phosphide crystal for increasing heat transfer |
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