CN103643295A - Method for preparing raw material for vapor-method aluminum nitride crystal growth - Google Patents
Method for preparing raw material for vapor-method aluminum nitride crystal growth Download PDFInfo
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- CN103643295A CN103643295A CN201310640427.3A CN201310640427A CN103643295A CN 103643295 A CN103643295 A CN 103643295A CN 201310640427 A CN201310640427 A CN 201310640427A CN 103643295 A CN103643295 A CN 103643295A
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- Prior art keywords
- crucible
- tungsten
- aluminum nitride
- raw material
- warming
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Links
- 238000000034 method Methods 0.000 title claims abstract description 45
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 28
- 239000013078 crystal Substances 0.000 title claims abstract description 28
- 239000002994 raw material Substances 0.000 title claims abstract description 25
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 35
- 239000010937 tungsten Substances 0.000 claims abstract description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012808 vapor phase Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000010792 warming Methods 0.000 claims description 24
- 229910017083 AlN Inorganic materials 0.000 claims description 20
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000005056 compaction Methods 0.000 claims description 3
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 2
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000011010 flushing procedure Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000004821 distillation Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing a raw material for vapor-method aluminum nitride crystal growth. The method comprises the specific steps of soaking a tungsten crucible and a crucible cover which are required to be used in aqua regia for 30-120 minutes, taking out the tungsten crucible and the crucible cover, cleanly flushing, and drying for later use; adding aluminum nitride powder into the tungsten crucible, and carrying out multi-layer compacting treatment; covering the tungsten crucible with the crucible cover, putting in a tungsten-mesh heating furnace, vacuumizing until the pressure is 1*10<-3>Pa, inflating with high-purity nitrogen gas until the pressure is 30kPa, heating to the temperature of 300 DEG C, keeping the temperature constant for 1 hour, heating to the temperature of 800 DEG C, and keeping the temperature constant for 1 hour; inflating the tungsten-mesh heating furnace with high-purity nitrogen gas until the pressure is 50kPa, heating to the temperature of 1800 DEG C, keeping the temperature constant for 5 hours, heating to the temperature of 2,050 DEG C, and keeping the temperature constant for 8 hours; cooling to room temperature, thereby obtaining an aluminum nitride sinter cake which serves as the raw material for vapor-method aluminum nitride crystal growth. According to the method, a compact sintered body is prepared from the aluminum nitride powder, so as to control vapor-phase reaction, thus the requirements of RVT (Physical Vapor Transport)-method aluminum nitride crystal material growth for raw materials are met.
Description
Technical field
The present invention relates to the preparation method of raw material for a kind of vapor phase process growing aluminum nitride crystal.
Background technology
Aluminum-nitride single crystal material is the highly desirable substrate material of a kind of development of new HIGH-POWERED MICROWAVES device and short-wavelength light electrical part, but is also difficult at present obtain aluminum nitride body monocrystal material.Aluminium nitride Theoretical Calculation fusing point is 2800 ℃, and dissociation pressure is 20MPa, is therefore difficult to carry out growing single-crystal as silicon melt vertical pulling method or the temperature gradient solidification law technology of adopting the same as gallium arsenide.One of method more likely is PVT (Physical Vapor Transport, physical vapor transport) method at present.The PVT method growing principle of aluminium nitride is to decompose in the distillation of place, high temperature source region by high-purity aluminium nitride powder, and by the transport of substances process in growth chamber, at low temperature seed crystal, condense in place, and then forms the process of growth of monocrystalline.Adopt PVT legal system for there being many technological difficulties in aluminum-nitride single crystal.Wherein, the highly purified aln raw material of the applicable vapor phase process single crystal growing of acquisition is one of important topic.
Because the affinity of aluminium and oxygen is very strong, adsorb oxygen impurity very easily in aln raw material, oxygen level concentration is up to 10 conventionally
20cm
-3, these impurity participate in reacting generating compound Al
3o
3n etc., have a strong impact on nucleation, two-dimensional growth and the crystal mass of aluminum-nitride single crystal in process of growth.Carbon is also impurity common in a kind of aln raw material, and the heating graphite material using in common heat-processed and lagging material very easily cause carbon to stain.In addition because aluminium nitride powder is spherical in shape, have very high specific surface area, in the process of decomposing in distillation, speed of response is fast, is difficult to control.
Summary of the invention
The problem existing for prior art, the object of the present invention is to provide the preparation method of raw material for a kind of vapor phase process growing aluminum nitride crystal, utilize raw material prepared by the method to there is the feature of low oxygen and carbon content, low impurity content and high-compactness, suitable for vapor phase process crystal growth raw material.
For achieving the above object, the preparation method of raw material for a kind of vapor phase process growing aluminum nitride crystal of the present invention, is specially:
1) tungsten crucible that will use and crucible cover are soaked in to 30-120 minute in chloroazotic acid, taking-up is rinsed well, dries up standby;
2) in tungsten crucible, add aluminium nitride powder, and carry out some layers of compaction treatment;
3) on tungsten crucible, add a cover crucible cover, put into tungsten net process furnace, be evacuated down to 10
-2-10
-3pa, then be filled with high pure nitrogen to 10-30kPa, being warming up to 300-500 ℃, constant temperature 1-3 hour, is warming up to 800-1000 ℃, constant temperature 1-3 hour;
4) in tungsten net process furnace, be filled with high pure nitrogen to 50-60kPa, be warming up to 1500-1800 ℃, constant temperature 5-6 hour, is warming up to 1950-2050 ℃, constant temperature 8-10 hour;
5) be cooled to room temperature, obtain aluminium nitride agglomerate, as the raw material of vapor phase process aluminum-nitride single crystal growth.
Further, described step 2), concrete steps are: in tungsten crucible, add aluminium nitride powder, while adding to half height of tungsten crucible, will expect compacting, make its face surfacing, interior solid; In tungsten crucible, be dosed to crucible top compacting again again.
Further, in described step 3), be evacuated down to 10
-3pa, then be filled with high pure nitrogen to 30kPa, being warming up to 300 ℃, constant temperature 1 hour, is warming up to 800 ℃, constant temperature 1 hour.
Further, in described step 4), be filled with high pure nitrogen to 50kPa, be warming up to 1800 ℃, constant temperature 5 hours, is warming up to 2050 ℃, constant temperature 8 hours.
The present invention makes fine and close sintered compact by aluminium nitride powder, to control the carrying out of gas-phase reaction, thereby meets the requirement of physical vapor transport growing aluminum nitride crystal material to raw material.
Accompanying drawing explanation
Fig. 1 is the structural representation of tungsten crucible and crucible cover;
Fig. 2 for adding the structural representation after aluminium nitride powder in tungsten crucible;
Fig. 3 for making the structural representation after aluminium nitride agglomerate in tungsten crucible.
Embodiment
Below, with reference to accompanying drawing, the present invention is more fully illustrated, shown in the drawings of exemplary embodiment of the present invention.Yet the present invention can be presented as multiple multi-form, and should not be construed as the exemplary embodiment that is confined to narrate here.But, these embodiment are provided, thereby make the present invention comprehensively with complete, and scope of the present invention is fully conveyed to those of ordinary skill in the art.
For ease of explanation, here can use such as " on ", the space relative terms such as D score " left side " " right side ", the relation for element shown in explanatory view or feature with respect to another element or feature.It should be understood that except the orientation shown in figure, spatial terminology is intended to comprise the different azimuth of device in using or operating.For example, if the device in figure is squeezed, be stated as the element that is positioned at other elements or feature D score will be positioned at other elements or feature " on ".Therefore, exemplary term D score can comprise upper and lower orientation both.Device can otherwise be located (90-degree rotation or be positioned at other orientation), and the relative explanation in space used here can correspondingly be explained.
The technical scheme that the present invention takes is that employing tungsten crucible holds aluminium nitride powder, uses tungsten net process furnace under certain temperature and pressure condition, to process aluminium nitride powder, obtains high-purity aluminum nitride sintered product.
As shown in Figure 1, Figure 2, Figure 3 shows, the preparation method of raw material for a kind of vapor phase process growing aluminum nitride crystal of the present invention, concrete steps are:
1) tungsten crucible that will use 1 and crucible cover 2 are soaked in to 30-120 minute in chloroazotic acid, taking-up is rinsed well, dries up standby;
2) in tungsten crucible 1, add aluminium nitride powder 3, and carry out some layers of compaction treatment;
3) on tungsten crucible 1, add a cover crucible cover 2, put into tungsten net process furnace, be evacuated down to 10
-2-10
-3pa, then be filled with high pure nitrogen to 10-30kPa, being warming up to 300-500 ℃, constant temperature 1-3 hour, is warming up to 800-1000 ℃, constant temperature 1-3 hour;
4) in tungsten net process furnace, be filled with high pure nitrogen to 50-60kPa, be warming up to 1500-1800 ℃, constant temperature 5-6 hour, is warming up to 1950-2050 ℃, constant temperature 8-10 hour;
5) be cooled to room temperature, obtain aluminium nitride agglomerate 4, as the raw material of vapor phase process aluminum-nitride single crystal growth.
In general treating processes, step 2) only carry out 2 layers of processing, its concrete steps are: in tungsten crucible 1, add aluminium nitride powder 3, while adding to tungsten crucible 1 half height, will expect compacting, make its face surfacing, interior solid; In tungsten crucible 1, be dosed to crucible top compacting again again.
Optimization numerical value in step 3) is: be evacuated down to 10
-3pa, then be filled with high pure nitrogen to 30kPa, being warming up to 300 ℃, constant temperature 1 hour, is warming up to 800 ℃, constant temperature 1 hour.
Optimization numerical value in step 4) is: be filled with high pure nitrogen to 50kPa, be warming up to 1800 ℃, constant temperature 5 hours, is warming up to 2050 ℃, constant temperature 8 hours.
In the present invention, the aluminium nitride agglomerate 4 after knot high-temperature vacuum sintering is truncated cone-shaped, and material shrinks, and edge is separated with sidewall of crucible, can be used as the raw material of vapor phase process aluminum-nitride single crystal growth after taking-up.
Utilize the preparation method of raw material for vapor phase process growing aluminum nitride crystal of the present invention, can make the raw material of highly purified single crystal growing, present method, in preparation process, has effectively been removed oxygen impurities, prevents from generating Al
3o
3n; Adopt tungsten crucible and lid crucible cover, tungsten net process furnace effectively to avoid the pollution of carbon impurity; Especially this preparation method, has adopted specific temperature, pressure condition after optimizing, processes aluminium nitride powder under this condition, can well control speed of response, obtains high-purity aluminum nitride sintered product.
Claims (4)
1. a preparation method for raw material for vapor phase process growing aluminum nitride crystal, is characterized in that, this preparation method is specially:
1) tungsten crucible that will use and crucible cover are soaked in to 30-120 minute in chloroazotic acid, taking-up is rinsed well, dries up standby;
2) in tungsten crucible, add aluminium nitride powder, and carry out some layers of compaction treatment;
3) on tungsten crucible, add a cover crucible cover, put into tungsten net process furnace, be evacuated down to 10
-2-10
-3pa, then be filled with high pure nitrogen to 10-30kPa, being warming up to 300-500 ℃, constant temperature 1-3 hour, is warming up to 800-1000 ℃, constant temperature 1-3 hour;
4) in tungsten net process furnace, be filled with high pure nitrogen to 50-60kPa, be warming up to 1500-1800 ℃, constant temperature 5-6 hour, is warming up to 1950-2050 ℃, constant temperature 8-10 hour; Be cooled to room temperature, obtain aluminium nitride agglomerate, as the raw material of vapor phase process aluminum-nitride single crystal growth.
2. the preparation method of raw material for vapor phase process growing aluminum nitride crystal as claimed in claim 1, is characterized in that described step 2) in concrete steps be: in tungsten crucible, add aluminium nitride powder, while adding to half height of tungsten crucible, to expect compacting, make its face surfacing, interior solid; In tungsten crucible, be dosed to crucible top compacting again again.
3. the preparation method of raw material for vapor phase process growing aluminum nitride crystal as claimed in claim 1, is characterized in that, in described step 3), is evacuated down to 10
-3pa, then be filled with high pure nitrogen to 30kPa, being warming up to 300 ℃, constant temperature 1 hour, is warming up to 800 ℃, constant temperature 1 hour.
4. the preparation method of raw material for vapor phase process growing aluminum nitride crystal as claimed in claim 1, is characterized in that, in described step 4), is filled with high pure nitrogen to 50kPa, is warming up to 1800 ℃, and constant temperature 5 hours, is warming up to 2050 ℃, constant temperature 8 hours.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637411A (en) * | 2016-12-22 | 2017-05-10 | 苏州奥趋光电技术有限公司 | Growth method of aluminum nitride single crystals |
| CN106757322A (en) * | 2016-12-22 | 2017-05-31 | 苏州奥趋光电技术有限公司 | A kind of aln raw material high temperature purification method |
| CN108147821A (en) * | 2017-12-21 | 2018-06-12 | 北京华进创威电子有限公司 | A kind of high-purity nitride porous aluminium crystallite material source preparation method |
| CN108396384A (en) * | 2018-05-25 | 2018-08-14 | 深圳大学 | A kind of device and method preparing aluminum nitride crystal |
| CN108624957A (en) * | 2018-03-29 | 2018-10-09 | 苏州奥趋光电技术有限公司 | A method of preparing aluminum-nitride single crystal |
| CN109576783A (en) * | 2019-01-23 | 2019-04-05 | 山东大学 | A kind of preprocessing method of raw materials for high quality aluminum nitride crystal growth |
| CN111364104A (en) * | 2020-04-23 | 2020-07-03 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of high-purity raw material for aluminum nitride single crystal growth |
| CN112011825A (en) * | 2020-09-25 | 2020-12-01 | 武汉大学 | Crucible device for growing aluminum nitride crystal |
| CN112979335A (en) * | 2021-02-08 | 2021-06-18 | 哈尔滨化兴软控科技有限公司 | Preparation method of aluminum nitride porous raw material |
| CN115353082A (en) * | 2022-08-29 | 2022-11-18 | 山东大学 | A method for one-step sintering of high-quality aluminum nitride raw materials |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757322A (en) * | 2016-12-22 | 2017-05-31 | 苏州奥趋光电技术有限公司 | A kind of aln raw material high temperature purification method |
| CN106637411A (en) * | 2016-12-22 | 2017-05-10 | 苏州奥趋光电技术有限公司 | Growth method of aluminum nitride single crystals |
| CN106637411B (en) * | 2016-12-22 | 2019-04-05 | 苏州奥趋光电技术有限公司 | A kind of aluminum-nitride single crystal growing method |
| CN108147821B (en) * | 2017-12-21 | 2021-04-27 | 北京华进创威电子有限公司 | A kind of preparation method of high-purity porous aluminum nitride crystal source |
| CN108147821A (en) * | 2017-12-21 | 2018-06-12 | 北京华进创威电子有限公司 | A kind of high-purity nitride porous aluminium crystallite material source preparation method |
| CN108624957A (en) * | 2018-03-29 | 2018-10-09 | 苏州奥趋光电技术有限公司 | A method of preparing aluminum-nitride single crystal |
| CN108396384A (en) * | 2018-05-25 | 2018-08-14 | 深圳大学 | A kind of device and method preparing aluminum nitride crystal |
| CN109576783A (en) * | 2019-01-23 | 2019-04-05 | 山东大学 | A kind of preprocessing method of raw materials for high quality aluminum nitride crystal growth |
| CN111364104A (en) * | 2020-04-23 | 2020-07-03 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of high-purity raw material for aluminum nitride single crystal growth |
| CN112011825A (en) * | 2020-09-25 | 2020-12-01 | 武汉大学 | Crucible device for growing aluminum nitride crystal |
| CN112011825B (en) * | 2020-09-25 | 2021-06-15 | 武汉大学 | Crucible device for growing aluminum nitride crystals |
| CN112979335A (en) * | 2021-02-08 | 2021-06-18 | 哈尔滨化兴软控科技有限公司 | Preparation method of aluminum nitride porous raw material |
| CN112979335B (en) * | 2021-02-08 | 2022-07-01 | 哈尔滨化兴软控科技有限公司 | Preparation method of aluminum nitride porous raw material |
| CN115353082A (en) * | 2022-08-29 | 2022-11-18 | 山东大学 | A method for one-step sintering of high-quality aluminum nitride raw materials |
| CN115353082B (en) * | 2022-08-29 | 2023-10-24 | 山东大学 | Method for sintering high-quality aluminum nitride raw material in one step |
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Application publication date: 20140319 |