CN106801258A - A kind of preparation method with hexa-prism aluminium nitride whisker - Google Patents
A kind of preparation method with hexa-prism aluminium nitride whisker Download PDFInfo
- Publication number
- CN106801258A CN106801258A CN201611237098.8A CN201611237098A CN106801258A CN 106801258 A CN106801258 A CN 106801258A CN 201611237098 A CN201611237098 A CN 201611237098A CN 106801258 A CN106801258 A CN 106801258A
- Authority
- CN
- China
- Prior art keywords
- crucible
- preparation
- aln
- hexa
- prism
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C30B29/38—Nitrides
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/007—Growth of whiskers or needles
-
- 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
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of preparation method with hexa-prism aluminium nitride whisker, the preparation method with hexa-prism aluminium nitride whisker, using physical vapor transport, raw material A lN is heated into by gas phase by Frequency Induction Heating mode, it it is 1,700 1750 DEG C by controlling growth temperature, control growth pressure for 200 300 Torr, crystallization forms the AlN whiskers of hexa-prism.The present invention at a lower temperature, six prism AlN whiskers is obtained by Controlling Growth Rate.
Description
Technical field
The invention belongs to one-dimensional semiconductor material with wide forbidden band preparation field, and in particular to one kind is based on physical vapor transport
The method that (Physical vapor transport, PVT) prepares the AlN whiskers of hexagonal prism shape.
Background technology
With the development of semiconductor science and technology, people are pursuing the semi-conducting material of excellent performance always.With silicon
(Si) crystal is that the first generation semi-conducting material of representative supports the development of whole semiconductor industry, with GaAs (GaAs) crystal
For the second generation semi-conducting material for representing is the backing material of telecommunications industry development.With carborundum (SiC), gallium nitride
(GaN) it is that the wide bandgap semiconductor of representative receives attention extensively, and tentatively achieves certain application.In recent years, with more
Aluminium nitride (AlN) crystal of big energy gap is of great interest.
AlN crystalline materials compare other semi-conducting materials, the advantage with following several respects：And wide bandgap semiconductor (1)
SiC (3.2eV), GaN (3.4eV) material are compared, and AlN crystal has bigger energy gap (6.2eV)；(2) AlN crystal has
Excellent thermal conduction characteristic, thermal conductivity at room temperature is 319W/ (m ﹒ K)；(3) AlN crystal and congeners GaN, indium nitride
(InN) direct band-gap semicondictor is, with electricity conversion high, the alloy material of AlN and GaN can be by adjusting element
Ratio realizes the regulation and control (3.4~6.2eV) to energy gap in certain scope.
The elite clone characteristic of AlN crystal can be widely applied to manufacture high temperature, high frequency, high-power, Flouride-resistani acid phesphatase electronic device,
Can be widely applied to the fields such as novel energy-saving power electronic installation, microwave communication field, specular removal semiconductor lighting.At present, PVT
Method is the main method for preparing AlN crystal, because AlN crystal growth has stronger each diversity, PVT method controllable preparations AlN
Crystal is still one of difficult point.
The content of the invention
The characteristics of present invention crystallizes each diversity using the distillation of AlN high temperature and different crystalline phases, by physical vapor transport machine
Reason control crystallization temperature and pressure, prepare the AlN whiskers with hexagonal prism shape.
The present invention provides a kind of preparation method of hexa-prism aluminium nitride whisker herein, and the method is, using physical vapor
Transmission method, gas phase is heated into by Frequency Induction Heating mode by raw material A lN, by controlling growth temperature for 1700-1750 DEG C,
Control growth pressure for 200-300Torr, crystallization forms the AlN whiskers of hexa-prism.The present invention at a lower temperature, passes through
Controlling Growth Rate obtains six prism AlN whiskers.
Preferably, the raw material A lN is AlN powders, particle diameter is 100-300 mesh, and purity is more than 99.99%.
Preferably, selection holds the raw material A lN, such as graphite earthenware to the inactive material of Al steam as the first crucible
Crucible, tungsten crucible, carbonization tantalum crucible etc..It is preferred that use two crucibles, i.e., first the second crucible of crucible overcoat.Second crucible can be
Graphite crucible, tungsten crucible, carbonization tantalum crucible.
It is preferred that the growth time of the AlN whiskers 25~35 hours, e.g., about 30 hours.
It is preferred that the AlN whiskers are wide 300-400 μm, 2-3cm long.
It is preferred that growth atmosphere can be nitrogen.
It is preferred that can be using 4H-SiC that thickness is 1.0~1.5mm as seed crystal.
Brief description of the drawings
Fig. 1 is the PVT method grower schematic diagrames for preparing six prism AlN whiskers；
Fig. 2 is AlN whiskers material object photo prepared by embodiment 1；
Fig. 3 is the electron scanning micrograph of the single whisker of AlN whiskers of embodiment 1；
Fig. 4 is AlN whiskers material object photo prepared by embodiment 2；
Fig. 5 is the optical microscope photograph of the single whisker of AlN whiskers of embodiment 2；
Fig. 6 is AlN whisker Raman spectrum test result figures prepared by PVT methods.
Specific embodiment
With reference to instantiation, the invention will be further described, it should be appreciated that following implementation methods are merely to illustrate this
Invention, is not intended to limit the present invention.
The characteristics of present invention crystallizes each diversity using the distillation of AlN high temperature and different crystalline phases, by physical vapor transport machine
Reason control crystallization temperature and pressure, prepare the AlN whiskers with hexagonal prism shape, whisker 300-400um wide, 2-3cm long.
Referring to Fig. 1, it shows grower schematic diagram, and AlN material powders are put into crucible.Wherein AlN material powders
Can select particle diameter is 100-300 mesh, AlN powder of the purity more than 99.99%.It is inactive to Al steam that crucible can select selection
Material, such as graphite crucible, tungsten crucible, carbonization tantalum crucible.Preferably, two crucibles are can select, i.e., using the first crucible is held
AlN material powders, and in first the second crucible of crucible overcoat.Second crucible and the first crucible are equally selected to Al steam torpescence
Material, for example graphite crucible, tungsten crucible, carbonization tantalum crucible.It is highly preferred that graphite carbon felt also is wound outside the second crucible,
Double crucibles are conducive to improving the stability in radial symmetry gradient and temperature field.Seed crystal is fixed below the top cover of the first crucible, can
Using 4H-SiC seed crystals, seed crystal thickness can be 1.0~1.5mm.Controllable the distance between seed crystal and AlN powder be 25~
35mm.Graphite carbon felt can be set again on the top cover of crucible for insulated roof.
Crucible is placed in the middle of induction coil, the vacuum of growth chamber is evacuated to using mechanical pump and molecular pump<1x 10- 3Pa, then to 200~300Torr, by Frequency Induction Heating, it is 15~20 DEG C/min to control heating rate to inflated with nitrogen, plus
To 1700-1750 DEG C, insulation, pressurize grow 25~35 hours heat.Then proceed to inflated with nitrogen to 600~800Torr, control cooling
Speed is 3~5 DEG C/min, is cooled to room temperature, obtains AlN whiskers, wide 300-400 μm, 2-3cm long.
Embodiment 1：
1st, 200 mesh AlN powders are put into carbonization tantalum crucible, cover a graphite crucible, graphite crucible outside outside carbonization tantalum crucible again
Winding graphite carbon felt, a piece of 1mm thickness 4H-SiC seed crystals are fixed below carbonization tantalum crucible top cover, control seed crystal and AlN powders it
Between distance be 30mm, carbonization tantalum crucible above again with graphite carbon felt as insulated roof；
2nd, crucible is placed in the middle of induction coil, then experimental provision as shown in figure 1, start growth.Prepare main as follows：Using
Be evacuated to for the vacuum of growth chamber by mechanical pump and molecular pump<1x 10-3Pa, then inflated with nitrogen is to 200Torr, with 15~20 DEG C/minute
Hot to 1700 DEG C beginning growing AIN whiskers of clock；
3rd, then growth time about 30 hours, inflated with nitrogen to 700Torr starts cooling with 3~5 DEG C/min, treats that temperature is down to room
Temperature takes out sample, and the sample photo of AlN whiskers is shown in accompanying drawing 2；
4th, SEM tests are carried out to the sample for preparing, accompanying drawing 3 is test result, it can be seen that AlN whiskers are presented six from SEM figures
Prism-shaped；
Referring to Fig. 6, it shows AlN whisker Raman spectrum test result figures, the feature of the raman spectra corresponding A lN crystal in figure
Peak, the halfwidth at E2 peaks therein is 10.6cm-1, show that AlN whiskers have good crystalline quality.
Embodiment 2：
1st, 300 mesh AlN powders are put into tungsten crucible, tungsten crucible outside winding graphite carbon felt, below carbonization tantalum crucible top cover
The a piece of 1mm thickness 4H-SiC seed crystals of fixation, control the distance between seed crystal and AlN powders are 30mm, above the tantalum crucible that is carbonized again with
Graphite carbon felt is insulated roof；
2nd, crucible is placed in the middle of induction coil, is evacuated to the vacuum of growth chamber using mechanical pump and molecular pump<1x 10- 3Pa, then inflated with nitrogen is to 300Torr, with 15~20 DEG C/min of heat to 1750 DEG C of beginning growing AIN whiskers；
3rd, then growth time about 30 hours, inflated with nitrogen to 700Torr starts cooling with 3~5 DEG C/min, treats that temperature is down to room
Temperature takes out sample, and the sample photo of AlN whiskers is shown in accompanying drawing 4；
4th, light microscope test is carried out to the sample for preparing, accompanying drawing 5 is test result.From optical microscope photograph it can be seen that
AlN whiskers are presented hexa-prism.
Claims (9)
1. a kind of preparation method with hexa-prism aluminium nitride whisker, it is characterised in that
Using physical vapor transport, raw material A lN is heated into by gas phase by Frequency Induction Heating mode, by controlling growth temperature
It is 1700-1750 DEG C to spend, and controls growth pressure for 200-300 Torr, and crystallization forms the AlN whiskers of hexa-prism.
2. preparation method according to claim 1, it is characterised in that the raw material A lN is AlN powders, and particle diameter is 100-
300 mesh, purity is more than 99.99%.
3. preparation method as claimed in any of claims 1 to 2, it is characterised in that selection is to Al steam torpescence
Material hold the raw material A lN as the first crucible.
4. preparation method according to claim 3, it is characterised in that first crucible is graphite crucible, tungsten crucible, carbon
Change tantalum crucible.
5. the preparation method according to claim 3 or 4, it is characterised in that first crucible is placed in the second crucible, institute
It is graphite crucible, tungsten crucible, carbonization tantalum crucible to state the second crucible.
6. preparation method as claimed in any of claims 1 to 5, it is characterised in that during the growth of the AlN whiskers
Between about 25~35 hours.
7. preparation method as claimed in any of claims 1 to 6, it is characterised in that the AlN whiskers 300- wide
400 μm, 2-3cm long.
8. preparation method as claimed in any of claims 1 to 7, it is characterised in that growth atmosphere is nitrogen.
9. preparation method as claimed in any of claims 1 to 8, it is characterised in that with thickness be 1.0~1.5mm
4H-SiC as seed crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611237098.8A CN106801258A (en) | 2016-12-28 | 2016-12-28 | A kind of preparation method with hexa-prism aluminium nitride whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611237098.8A CN106801258A (en) | 2016-12-28 | 2016-12-28 | A kind of preparation method with hexa-prism aluminium nitride whisker |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106801258A true CN106801258A (en) | 2017-06-06 |
Family
ID=58985088
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611237098.8A Pending CN106801258A (en) | 2016-12-28 | 2016-12-28 | A kind of preparation method with hexa-prism aluminium nitride whisker |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106801258A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904661A (en) * | 2017-12-07 | 2018-04-13 | 北京华进创威电子有限公司 | A kind of growing method of low stress nitride aluminium crystal |
| WO2021207904A1 (en) * | 2020-04-14 | 2021-10-21 | 眉山博雅新材料有限公司 | Crystal growth method and device |
| CN115667183A (en) * | 2020-08-07 | 2023-01-31 | 株式会社优迈普 | Ceramic substrate, alN single crystal, alN whisker and AlN whisker composite |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62283900A (en) * | 1986-06-02 | 1987-12-09 | Tokai Carbon Co Ltd | Production of aln whisker |
| JPS6375000A (en) * | 1986-09-18 | 1988-04-05 | Toyota Motor Corp | Production of aluminum nitride whisker |
| JPH09295898A (en) * | 1996-04-26 | 1997-11-18 | Toshiba Ceramics Co Ltd | Aluminum borate whisker coated with aluminum nitride and its production |
| CN1203209A (en) * | 1998-07-24 | 1998-12-30 | 清华大学 | Process for preparing aluminium nitride whisker |
| CN101070618A (en) * | 2007-03-19 | 2007-11-14 | 宁波工程学院 | Monocrystal AIN nano chain |
| JP2009143778A (en) * | 2007-12-17 | 2009-07-02 | Sumitomo Metal Mining Co Ltd | Method for growing aluminum nitride crystal, aluminum nitride substrate and semiconductor device |
| CN101513996A (en) * | 2009-03-23 | 2009-08-26 | 吉林大学 | An aluminum nitride nanometer comb and preparation method thereof |
| CN102618930A (en) * | 2012-03-31 | 2012-08-01 | 哈尔滨工业大学 | Method for preparing AlN crystal |
| CN103060904A (en) * | 2013-02-05 | 2013-04-24 | 中国电子科技集团公司第四十六研究所 | Method for realizing growth of AlN monocrystals by growth mode regulation |
| CN103361718A (en) * | 2012-04-09 | 2013-10-23 | 中国科学院物理研究所 | Method for growing aluminium nitride monocrystal by using physical vapor transport method |
| CN104891458A (en) * | 2015-06-10 | 2015-09-09 | 中国科学院上海光学精密机械研究所 | AlN (aluminium nitride) microparticles with outline of double hexagonal pyramids and preparation method thereof |
-
2016
- 2016-12-28 CN CN201611237098.8A patent/CN106801258A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62283900A (en) * | 1986-06-02 | 1987-12-09 | Tokai Carbon Co Ltd | Production of aln whisker |
| JPS6375000A (en) * | 1986-09-18 | 1988-04-05 | Toyota Motor Corp | Production of aluminum nitride whisker |
| JPH09295898A (en) * | 1996-04-26 | 1997-11-18 | Toshiba Ceramics Co Ltd | Aluminum borate whisker coated with aluminum nitride and its production |
| CN1203209A (en) * | 1998-07-24 | 1998-12-30 | 清华大学 | Process for preparing aluminium nitride whisker |
| CN101070618A (en) * | 2007-03-19 | 2007-11-14 | 宁波工程学院 | Monocrystal AIN nano chain |
| JP2009143778A (en) * | 2007-12-17 | 2009-07-02 | Sumitomo Metal Mining Co Ltd | Method for growing aluminum nitride crystal, aluminum nitride substrate and semiconductor device |
| CN101513996A (en) * | 2009-03-23 | 2009-08-26 | 吉林大学 | An aluminum nitride nanometer comb and preparation method thereof |
| CN102618930A (en) * | 2012-03-31 | 2012-08-01 | 哈尔滨工业大学 | Method for preparing AlN crystal |
| CN103361718A (en) * | 2012-04-09 | 2013-10-23 | 中国科学院物理研究所 | Method for growing aluminium nitride monocrystal by using physical vapor transport method |
| CN103060904A (en) * | 2013-02-05 | 2013-04-24 | 中国电子科技集团公司第四十六研究所 | Method for realizing growth of AlN monocrystals by growth mode regulation |
| CN104891458A (en) * | 2015-06-10 | 2015-09-09 | 中国科学院上海光学精密机械研究所 | AlN (aluminium nitride) microparticles with outline of double hexagonal pyramids and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| H.Q.BAO ET AL.: ""The sublimation growth of AlN fibers: transformations in morphology & fiber direction"", 《APPLIED PHYSICS A》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904661A (en) * | 2017-12-07 | 2018-04-13 | 北京华进创威电子有限公司 | A kind of growing method of low stress nitride aluminium crystal |
| CN107904661B (en) * | 2017-12-07 | 2021-04-27 | 北京华进创威电子有限公司 | Growth method of low-stress aluminum nitride crystal |
| WO2021207904A1 (en) * | 2020-04-14 | 2021-10-21 | 眉山博雅新材料有限公司 | Crystal growth method and device |
| US11926922B2 (en) | 2020-04-14 | 2024-03-12 | Meishan Boya Advanced Materials Co., Ltd. | Methods for crystal growth by replacing a sublimated target source material with a candidate source material |
| CN115667183A (en) * | 2020-08-07 | 2023-01-31 | 株式会社优迈普 | Ceramic substrate, alN single crystal, alN whisker and AlN whisker composite |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6141609B2 (en) | 100mm silicon carbide wafer with low micropipe | |
| TWI516648B (en) | Apparatus for producing silicon carbide crystals with multi-seeds | |
| JP5841339B2 (en) | 100mm high purity semi-insulating single crystal silicon carbide wafer | |
| EP2653591A1 (en) | Process for growing silicon carbide single crystal by physical vapor transport method and annealing silicon carbide single crystal in situ | |
| EP2072646A1 (en) | Process for producing single crystal of silicon carbide | |
| CN105463575B (en) | A kind of seed crystal processing method for growing silicon carbide crystal with high quality | |
| JP2010159185A (en) | Multilayer substrate and method for manufacturing the same, and diamond film and method for manufacturing the same | |
| CN103060904B (en) | A kind of method being realized AlN single crystal growing by growth pattern regulation and control | |
| CN106801258A (en) | A kind of preparation method with hexa-prism aluminium nitride whisker | |
| CN104562206A (en) | Method for improving crystal form stability of 4H-SiC crystals by virtue of physical vapor transport method | |
| KR100287793B1 (en) | SINGLE CRYSTAL SiC AND PROCESS FOR PREPARING THE SAME | |
| JPS60145992A (en) | Preparation of silicon carbide single crystal base | |
| EP0921214B1 (en) | Single crystal silicon carbide and process for preparing the same | |
| CN110306239A (en) | A kind of silicon carbide material seed crystal support | |
| CN111394788A (en) | Method and device for preparing cubic silicon carbide crystals | |
| CN108946735A (en) | A kind of synthetic method of the big partial size sic powder of growing silicon carbice crystals | |
| CN109628998B (en) | Silicon carbide crystal and method for producing same | |
| CN114438588B (en) | Preparation method of silicon carbide single crystal, silicon carbide supporting system and single crystal growth furnace | |
| JP2006143511A (en) | Seed crystal fixing part and method of fixing seed crystal | |
| WO2020006772A1 (en) | Gallium nitride single crystal material and preparation method therefor | |
| JP2013047159A (en) | Method of producing silicon carbide single crystal, silicon carbide single crystal ingot, and silicon carbide single crystal substrate | |
| CN101275075A (en) | Preparation for luminous silicon carbide thin film | |
| WO2009128224A1 (en) | Process for producing crystalline silicon carbide substrate | |
| CN112744816B (en) | Preparation method of silicon carbide powder for silicon carbide single crystal growth | |
| KR20230169109A (en) | How to Grow High-Quality Single Crystal Silicon Carbide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170606 |
|
| WD01 | Invention patent application deemed withdrawn after publication |