CN106087062A - A kind of tantalum metalwork carbonization method for aluminum-nitride single crystal growth - Google Patents
A kind of tantalum metalwork carbonization method for aluminum-nitride single crystal growth Download PDFInfo
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- CN106087062A CN106087062A CN201610509503.0A CN201610509503A CN106087062A CN 106087062 A CN106087062 A CN 106087062A CN 201610509503 A CN201610509503 A CN 201610509503A CN 106087062 A CN106087062 A CN 106087062A
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- tantalum
- ramet
- metalwork
- carbon
- carbon felt
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/002—Crucibles or containers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of tantalum metalwork carbonization method for aluminum-nitride single crystal growth, described carbonization method comprises the steps: 1) cleaning of ramet part: ramet part is carried out；2) cutting carbon felt sheet: according to geometric shape and the size of ramet part, carbon felt is cut into the carbon felt setting shape；3) assemble: the carbon felt cut, carbon dust, ramet part are placed in cartridge heater with being laminated with order；4) carbonization: heat cartridge heater, to complete the carbonization to ramet part；5) take out ramet part and clean: in Heating tube, take out ramet part and be carried out；6) by step 5) in clean after ramet part be in store for after drying.The carbonization method of the application can make full use of the volume space in Heating tube, improves space availability ratio, efficiently and effectively decreases energy waste, and the carbonization of ramet part is highly uniform.
Description
Technical field
The present invention relates to a kind of tantalum metalwork carbonization method for aluminum-nitride single crystal growth.
Background technology
Aluminium nitride material belongs to III-V race's semiconductor material with wide forbidden band, and its direct band gap is 6.2eV, and aluminium nitride is big
Size single crystal has high thermal conductivity and chemical stability, owing to it has good physicochemical property, so high temperature, high frequency,
High-power component and DUV electronic device and spin semiconductor device aspect are respectively provided with wide application prospect；Aluminum Al again
Being subordinate to of the same clan with gallium Ga, indium In element, itself and nitrogen element all can form the crystalline material of hexagonal wurtzite structure, by artificial
Technological means can realize ternary or quaternary compound, prepares with this and has the adjustable crystalline material of band gap width, enters one
Step can form the adjustable crystalline material of band gap width.Aluminium nitride material is the ideal substrate of GaN epitaxial growth again, so nitrogen
Change aluminum monocrystalline and there is good market using value.
At present, the growth of aluminum nitride body monocrystalline mainly utilizes physical vaporous deposition principle, uses intermediate frequency furnace by former
Material heating, again forms deposition in order on the substrate that temperature is relatively low, thus completes aluminum nitride body list after aln raw material distillation
Brilliant growth.Owing to aluminum nitride body crystal growth temperature is higher, the aluminum atom under negative pressure hot conditions has higher activity, this
Bring certain difficult problem for aluminum-nitride single crystal growth to the crucible selecting which kind of material.It is lazy that ramet has higher chemistry
Property become aluminum-nitride single crystal growth preferred material.The ramet with hard fragility is difficult to machine-shaping, is typically prepared
The technology path of ramet crucible is first to prepare tantalum crucible, then tantalum crucible is carried out high temperature cabonization, the ramet prepared with this
Aluminum-nitride single crystal growth can be met.
Summary of the invention
For problems of the prior art, it is an object of the invention to provide a kind of for aluminum-nitride single crystal growth
Tantalum metalwork carbonization method, the method can make full use of the volume space in Heating tube, improve space availability ratio, conscientiously have
Decrease energy waste to effect, and the carbonization of ramet part is highly uniform.
For achieving the above object, the present invention is by the following technical solutions:
A kind of tantalum metalwork carbonization method for aluminum-nitride single crystal growth, described carbonization method comprises the steps:
1) cleaning of tantalum metalwork: tantalum metalwork is carried out；
2) cutting carbon felt sheet: according to geometric shape and the size of tantalum metalwork, carbon felt is cut into setting shape
Carbon felt；
3) assemble: the carbon felt cut, carbon dust, tantalum metallic member are placed in cartridge heater with being laminated with order；
4) carbonization: heat cartridge heater, to complete the carbonization to tantalum metalwork；
5) take out ramet part and clean: in Heating tube, take out ramet part and be carried out；
6) by step 5) in clean after ramet part be in store for after drying.
Further, step 1) particularly as follows: by tantalum metalwork submergence in acetone, supersound process 2～taking-up after 30 minutes, then
Supersound process 0～5 minutes twice in dehydrated alcohol；After cleaning with pure water, tantalum metalwork being placed in concentration is 5%～65%
Supersound process 3～60 minutes in potassium hydrogen sulfate solution, after taking-up in the hydrochloric acid solution that concentration is suitable supersound process 0～30 points
Clock, after cleaning with pure water again with washes of absolute alcohol once, dries up standby.
Further, step 3) particularly as follows:
The most first Heating tube is cleared up, afterwards by evenly laid out for carbon dust bottom Heating tube, during its thickness tired paving 5mm thickness, will
The carbon felt cut gently is placed on carbon dust layer；
B. the last layer that tiles equably in the carbon felt inserted sets the carbon dust of thickness, more gently puts on carbon dust layer
Put the carbon felt cut, depending on the geometry of carbon felt, size, modes of emplacement are based on tantalum metalwork；
C. tantalum metalwork is fixed in carbon felt, afterwards carbon dust is uniformly filled between carbon felt and tantalum metalwork, directly
Flooding wherein to carbon dust by tantalum metalwork, carbon dust face layer is higher than tantalum metalwork face layer；
D. atresia carbon felt is put down gently on carbon dust layer, then carbon dust is laid in atresia carbon felt equably；
E. repetitive operation step a, b, c, d, until all tantalum metallic member are laminated with order ground, it tired is placed in Heating tube.
Further, step 4) particularly as follows: cartridge heater is heated, little at high temperature 2050～2300 DEG C of holdings 8～100
Time, pressure is maintained at 1～90,000 handkerchiefs.
Further, step 5) particularly as follows: after ramet part after the carbonization taken out in Heating tube, by ramet object table
The bur in face wipes out；Ramet object is immersed in acetone or alcohol liquid supersound process 2～30 minutes, again will after taking-up
Ramet object is placed in pure water supersound process 1～3 times, each 0.5～5 minute；The most again ramet object is placed on dense
In sulfuric acid solution, in Ultrasound Instrument, heating in water bath is to 50～70 DEG C, maintains 20～60 minutes, afterwards by ramet object from dense sulfur
Acid is taken out, after being removed by the concentrated sulphuric acid of ramet object surface with pure water, then ramet object is placed on hydrochloric acid solution
Middle supersound process 5～30 minutes, then by ramet object pure water ultrasonic cleaning 1～5 times.
The present invention has a following Advantageous Effects:
The ramet part carbonization method of the present invention can make full use of the volume space in Heating tube, improves space utilization
Rate, efficiently and effectively decreases energy waste, and the carbonization of ramet part is highly uniform.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the ramet part carbonization method multiple tantalum crucible lids of assembling of the present invention；
Fig. 2 is that the ramet part carbonization method of the present invention assembles a tantalum crucible lid and the schematic diagram of a tantalum crucible body；
Detailed description of the invention
Below, with reference to accompanying drawing, the present invention is more fully illustrated, shown in the drawings of the exemplary enforcement of the present invention
Example.But, the present invention can be presented as multiple multi-form, is not construed as the exemplary enforcement being confined to describe here
Example.And it is to provide these embodiments, so that the present invention is fully and completely, and will fully convey the scope of the invention to this
The those of ordinary skill in field.
For ease of explanation, here can use such as " on ", the space relative terms such as D score " left " " right ", be used for
Shown in bright figure a element or feature are relative to another element or the relation of feature.It should be understood that except in figure
Outside the orientation illustrated, spatial terminology is intended to include device different azimuth in use or operation.Such as, if in figure
Device is squeezed, be stated as being positioned at the element of other elements or feature D score will be located into other elements or feature " on ".Cause
This, exemplary term D score can comprise upper and lower both orientation.Device can otherwise position (90-degree rotation or be positioned at
Other orientation), relatively illustrate used herein of space correspondingly to explain.
This application provides a kind of ramet part carbonization method for aluminum-nitride single crystal growth, described carbonization method includes
Following steps:
1) cleaning of tantalum metalwork: tantalum metalwork is carried out；Tantalum crucible, tantalum crucible cover through machining molding
After, there is more physically or chemically adsorbate on tantalum metalwork surface, such as the adhesion oil contamination on tantalum metalwork surface, meanwhile, by
In machining and being chronically exposed in air, tantalum metalwork surface adsorption has oxygen atom and other atoms；By tantalum metalwork
Submergence in acetone, supersound process 2～take out after 30 minutes, then supersound process 0～5 minutes twice in dehydrated alcohol；With pure
Tantalum metalwork is placed in the potassium hydrogen sulfate solution that concentration is 5%～65% supersound process 3～60 minutes by water after cleaning, after taking-up
Supersound process 0～30 minutes in the hydrochloric acid solution that concentration is suitable, after cleaning with pure water again with washes of absolute alcohol once, dry up
Standby.
2) cutting carbon felt sheet: according to geometric shape and the size of tantalum metalwork, the cutting mould using carbon felt will
Carbon felt is cut into the carbon felt of definite shape；In order to preferably increase in Heating tube space availability ratio and effectively reduce energy waste,
Make to have being more uniformly distributed of tantalum metalwork carbonization of irregular figure simultaneously, need fault in Heating tube to place several layers of carbon with having order
Felt.Carbon felt is cut into the disk being sized for by the cutting mould utilizing carbon felt, according to profile and the size of tantalum metalwork
Size, cuts out the ring-type carbon felt being sized for.
3) assemble: the carbon felt cut, carbon dust, tantalum metallic member are placed in cartridge heater with being laminated with order；During assembling
Make to be evenly distributed with around tantalum metalwork certain thickness carbon dust possibly, so that there being enough carbon atoms in carbonisation greatly
Spread to tantalum metal inside and be bonded.Graphite felt after cutting, carbon dust, ramet part are placed on cartridge heater with being laminated with order
In.
4) carbonization: heat cartridge heater, to complete the carbonization to tantalum metalwork；Uniformly heating, slow cooling.From room
Temperature is in high-temperature heating process, and temperature rate is all unsuitable too fast；Especially rate of temperature fall should suitably reduce.At high temperature 2050～
2300 DEG C keep 8～100 hours, and pressure is maintained at 1～90,000 handkerchiefs.
5) take out ramet part and clean: in Heating tube, take out ramet part and be carried out；Ramet after carbonization
Surface adhesion has a lot of carbon dust, needs to clean.After the ramet object taken out in Heating tube, need gluing ramet surface
Addendum wipes out；Ramet object is immersed in acetone or alcohol liquid supersound process 2～30 minutes, again by ramet after taking-up
Object is placed in pure water supersound process 1～3 times, each 0.5～5 minute；The most again ramet object is placed on concentrated sulphuric acid molten
In liquid, in Ultrasound Instrument, heating in water bath is to 50～70 DEG C, time 20～60 minutes, afterwards ramet object is taken from concentrated sulphuric acid
Go out, after the concentrated sulphuric acid of ramet object surface being removed with pure water, then ramet object is placed in hydrochloric acid solution ultrasonic
Process 5～30 minutes, then by ramet object pure water ultrasonic cleaning 1～5 times.
6) by step 5) in clean after ramet part be in store for after drying.
Below in conjunction with specific embodiment, the assembling process of the application is further described:
As it is shown in figure 1, Heating tube is first cleared up by 1., afterwards by evenly laid out for carbon dust bottom Heating tube, the tired paving of its thickness
During 5mm thickness, the atresia carbon felt cut gently is placed on carbon dust layer.
2. the last layer that tiles equably in the carbon felt inserted sets the carbon dust of thickness, and such as thickness is 5mm, then at carbon
Gently placing a piece of carbon felt cut on bisque, the pore size of carbon felt is with tantalum crucible lid outside dimension as foundation.
3. tantalum crucible lid is placed in the hole slot of carbon felt 3, afterwards carbon dust is uniformly filled in carbon felt and tantalum metalwork
Between, until tantalum metalwork is flooded wherein by carbon dust, carbon dust face layer is higher than tantalum metalwork face layer；Preferably, carbon dust upper strata
Face is higher than tantalum metalwork face layer 5mm.
4. atresia carbon felt is put down gently on carbon dust layer, then carbon dust is laid in atresia carbon felt equably.
5. repetitive operation step 1,2,3,4, multiple tantalum crucible cap rocks are laminated with order ground, and it tired is placed in Heating tube.
In Fig. 1,1 is heating cover, and 2 is gap, and 3 is carbon felt with holes, and 4,5,9,10 is carbon dust layer, and 6 is tantalum crucible lid, 7
For atresia carbon felt, 8 is Heating tube.
As in figure 2 it is shown, Heating tube is first cleared up by 1., afterwards by evenly laid out for carbon dust bottom Heating tube, the tired paving of its thickness
During 5mm thickness, the atresia carbon felt cut gently is placed on carbon dust layer.
2. the last layer that tiles equably in the carbon felt inserted sets the carbon dust of thickness, and such as thickness is 5mm, then at carbon
Gently placing a piece of carbon felt cut on bisque, the pore size of carbon felt is with tantalum crucible lid outside dimension as foundation.
3. tantalum crucible lid is placed in the hole slot of carbon felt 3 with holes, afterwards carbon dust is uniformly filled in carbon felt and tantalum gold
Belonging between part, until tantalum metalwork is flooded wherein by carbon dust, carbon dust face layer is higher than tantalum metalwork face layer；Preferably, carbon dust
Face layer is higher than tantalum metalwork face layer 5mm.
4. atresia carbon felt is put down gently on carbon dust layer, then carbon dust is laid in atresia carbon felt equably.
5. repetitive operation step 1,2, tantalum crucible body is placed in the hole of carbon felt with holes, and ensures that vertical centrage is coaxial,
Again by carbon dust load wherein, according on crucible body mouth along position, carbon dust is evenly laid out, the carbon dust layer after tiling is placed with holes
Carbon felt, loads onto carbon dust layer and Karbate carpet veneer simultaneously successively.
6. edge on cleaning Heating tube, covers heating cover；Have between the superiors' carbon felt in guarantee heating cover and Heating tube
Certain interval.
In Fig. 2,1-generates heat cover, 2-gap, 3-carbon felt with holes, 4,5,9,10-carbon dust, 6-tantalum crucible lid, 7-Karbate
Felt, 8-Heating tube, 11-tantalum crucible body.
Described above simply to illustrate that the present invention, it is understood that to the invention is not limited in above example, meet
The various variants of inventive concept are all within protection scope of the present invention.
Claims (5)
1. one kind for aluminum-nitride single crystal growth tantalum metalwork carbonization method, it is characterised in that described carbonization method include as
Lower step:
1) cleaning of tantalum metalwork: tantalum metalwork is carried out；
2) cutting carbon felt sheet: according to geometric shape and the size of tantalum metalwork, carbon felt is cut into the carbon setting shape
Felt；
3) assemble: the carbon felt cut, carbon dust, tantalum metallic member are placed in cartridge heater with being laminated with order；
4) carbonization: heat cartridge heater, to complete the carbonization to tantalum metalwork；
5) take out ramet part and clean: in Heating tube, take out ramet part and be carried out；
6) by step 5) in clean after ramet part be in store for after drying.
Tantalum metalwork carbonization method the most according to claim 1, it is characterised in that step 1) particularly as follows: by tantalum metalwork
Submergence in acetone, supersound process 2～take out after 30 minutes, then supersound process 0～5 minutes twice in dehydrated alcohol；With pure
Tantalum metalwork is placed in the potassium hydrogen sulfate solution that concentration is 5%～65% supersound process 3～60 minutes by water after cleaning, after taking-up
Supersound process 0～30 minutes in the hydrochloric acid solution that concentration is suitable, after cleaning with pure water again with washes of absolute alcohol once, dry up
Standby.
Tantalum metalwork carbonization method the most according to claim 1, it is characterised in that step 3) particularly as follows:
The most first Heating tube is cleared up, afterwards by evenly laid out for carbon dust bottom Heating tube, during its thickness tired paving 5mm thickness, by cutting
Good carbon felt is gently placed on carbon dust layer；
B. the last layer that tiles equably in the carbon felt inserted sets the carbon dust of thickness, more gently places sanction on carbon dust layer
The carbon felt sheared, depending on the geometry of carbon felt, size, modes of emplacement are based on tantalum metalwork；
C. tantalum metalwork is fixed in carbon felt, afterwards carbon dust is uniformly filled between carbon felt and tantalum metalwork, until carbon
Tantalum metalwork is flooded wherein by powder, and carbon dust face layer is higher than tantalum metalwork face layer；
D. atresia carbon felt is put down gently on carbon dust layer, then carbon dust is laid in atresia carbon felt equably；
E. repetitive operation step a, b, c, d, until all tantalum metallic member are laminated with order ground, it tired is placed in Heating tube.
Tantalum metalwork carbonization method the most according to claim 1, it is characterised in that step 4) particularly as follows: cartridge heater is entered
Row heating, keeps 8～100 hours high temperature 2050～2300 DEG C, and pressure is maintained at 1～90,000 handkerchiefs.
Tantalum metalwork carbonization method the most according to claim 1, it is characterised in that step 5) particularly as follows: in Heating tube
After ramet part after the carbonization taken out, the bur of ramet object surface is wiped out；Ramet object is immersed acetone
Or supersound process 2～30 minutes in alcohol liquid, ramet object is placed in pure water supersound process 1～3 times again, often after taking-up
Secondary 0.5～5 minute；Being placed in concentrated sulfuric acid solution by ramet object, in Ultrasound Instrument, heating in water bath is to 50～70 the most again
DEG C, maintain 20～60 minutes, afterwards ramet object is taken out from concentrated sulphuric acid, with pure water by the dense sulfur of ramet object surface
After acid removes, then ramet object is placed in hydrochloric acid solution supersound process 5～30 minutes, then by ramet object pure water
Ultrasonic cleaning 1～5 times.
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| CN201610509503.0A CN106087062A (en) | 2016-06-30 | 2016-06-30 | A kind of tantalum metalwork carbonization method for aluminum-nitride single crystal growth |
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| CN201610509503.0A CN106087062A (en) | 2016-06-30 | 2016-06-30 | A kind of tantalum metalwork carbonization method for aluminum-nitride single crystal growth |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939569A (en) * | 2021-03-19 | 2021-06-11 | 哈尔滨化兴软控科技有限公司 | Method for recycling tantalum carbide crucible material for PVT (physical vapor transport) method |
| CN113846383A (en) * | 2021-09-27 | 2021-12-28 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Graphite heater for simultaneously carbonizing tantalum crucibles of different sizes and using method |
| CN115819088A (en) * | 2023-02-21 | 2023-03-21 | 宁波合盛新材料有限公司 | Silicon carbide crystal growth device, filter material thereof and preparation method of filter material |
| CN115874279A (en) * | 2023-02-28 | 2023-03-31 | 中国电子科技集团公司第四十六研究所 | Preparation method of tantalum carbide substrate for growing aluminum nitride on silicon carbide |
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| CN115819088A (en) * | 2023-02-21 | 2023-03-21 | 宁波合盛新材料有限公司 | Silicon carbide crystal growth device, filter material thereof and preparation method of filter material |
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