CN105002477B - Graphite deposition device and preparation method thereof - Google Patents
Graphite deposition device and preparation method thereof Download PDFInfo
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- CN105002477B CN105002477B CN201510541467.1A CN201510541467A CN105002477B CN 105002477 B CN105002477 B CN 105002477B CN 201510541467 A CN201510541467 A CN 201510541467A CN 105002477 B CN105002477 B CN 105002477B
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- graphite
- aquadag
- milk solution
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- boron nitride
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Abstract
The invention provides a graphite deposition device and a preparation method thereof. Compared with the prior art, the method has the advantages that the surface of the graphite system is coated with the graphite emulsion solution to form the graphite emulsion thin layer, and the graphite emulsion can be well stripped at high temperature because the thermal expansion coefficient of the graphite emulsion is greater than that of the graphite piece, so that the effect of easily stripping the pyrolytic boron nitride material deposited on the surface of the graphite system is achieved, the damage to the graphite system is reduced, and the treatment method is simple to operate and low in cost.
Description
Technical field
The invention belongs to chemical vapour deposition technique fields more particularly to a kind of graphite deposits device and preparation method thereof.
Background technology
Pyrolytic boron nitride is good a kind of nontoxic, tight, easy processing, surface compact, air-tightness, high temperature resistant, acidproof, resistance to
The material of alkali, salt tolerant and organic reagent, and do not moisten with materials such as most molten metals, semiconductors under high temperature, do not react,
Therefore it is chiefly used in the crucible, the pedestal that prepare semiconductor monocrystal and III~V compounds of group synthesis, fabricated in situ GaAs, InP,
The series such as the LEC series crucible of GaP monocrystalline, the MBE series of molecular beam epitaxy and VGF (vertical gradient solidification), VB methods
Use crucible.
Chemical vapour deposition technique is the main method for preparing pyrolytic boron nitride crucible, manufacture main process be by with earthenware
Mold made of the dense refractories materials such as the identical graphite of crucible shape is placed in CVD chamber, in heating hot conditions
Under, using nitrogen as dilution protective gas, the gas containing hydronitrogen, halogen compounds gas are passed through in stove, on one side into
Gas is extracted out on one side, makes to keep low-voltage vacuum state, at this moment on the graphite jig anticipated, ammonia, halogen chemical combination in stove
Object is all decomposing, and the nitrogen of dehydrogenation is combined to form compound with element B, and be deposited on mold, forms pyrolytic boron nitride；So
Afterwards after cooling down, take out demoulding and obtain boron nitride crucible.
The pyrolytic boron nitride product key for preparing high quality is the pyrolytic boron nitride uniform deposition generated after pyroreaction
In die surface, so as to obtain homogeneous pyrolytic boron nitride product.But generally in deposition process, in addition in graphite jig
Upper to deposit outside by pyrolytic boron nitride, other graphite systems such as pedestal, wall bucket and cover board etc. have pyrolytic boron nitride deposition.Pyrolysis
Boron nitride, which is sticked on graphite, to be peeled off extremely difficult, and the damage that graphite piece can be caused different degrees of in processing procedure,
Cause the wasting of resources.
Invention content
In view of this, the technical problem to be solved in the present invention is to provide a kind of graphite deposits device and preparation method thereof,
This method can make the pyrolytic boron nitride being deposited thereon easily peelable.
The present invention provides a kind of graphite deposits devices, and the graphite system surface in addition to graphite jig is covered with one layer of stone
Black breast layer.
Preferably, the graphite system includes the cavity body wall and graphite base of graphite cover board, graphite deposits device；It is described
Graphite cover board separates the cavity of the cavity of graphite deposits device and raw material feed device；The graphite base is located at graphite deposits
The cavity of device is interior and is provided with graphite jig.
Preferably, the thickness of the aquadag layer is 0.05~0.1mm.
The present invention also provides a kind of preparation method of graphite deposits device, in the graphite system table in addition to graphite jig
Face coats graphite milk solution, forms aquadag layer.
Preferably, the mass ratio of aquadag and solvent is 1 in the graphite milk solution：(1~3).
Preferably, the graphite milk solution is watersoluble plumbago whey solution.
Preferably, the graphite milk solution is the alcoholic solution of solvent type aquadag.
The present invention also provides a kind of chemical gas-phase deposition system, including graphite deposits device.
The present invention provides a kind of graphite deposits device and preparation method thereof, in the graphite system table in addition to graphite jig
Face coats graphite milk solution, forms aquadag layer.Compared with prior art, the present invention is molten in graphite system surface coating aquadag
Liquid forms aquadag thin layer, and under the condition of high temperature, since the coefficient of thermal expansion of aquadag is more than the coefficient of expansion of graphite piece, the two can
Stripping well so as to achieve the effect that make the pyrolytic boron nitride material for being deposited on graphite system surface easily peelable, reduces pair
The damage of graphite system, and the processing method is easy to operate, cost is relatively low.
Description of the drawings
Fig. 1 is the peeling effect photo of 2 pyrolytic boron nitride of the embodiment of the present invention.
Specific embodiment
Below in conjunction with the attached drawing of the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Ground describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained without making creative work
Example is applied, shall fall within the protection scope of the present invention.
The present invention provides a kind of graphite deposits devices, and the graphite system surface in addition to graphite jig is covered with one layer of stone
Black breast layer.
Wherein, the graphite system preferably includes the cavity body wall and graphite base of graphite cover board, graphite deposits device；Institute
Graphite cover board is stated to separate the cavity of the cavity of graphite deposits device and raw material feed device；The graphite base sinks positioned at graphite
The cavity of product device is interior and is provided with graphite jig.
The thickness of the aquadag layer is preferably 0.05~0.1mm.Aquadag thin layer is too thin not to have easily peelable effect,
It is too thick, cause the stripping of aquadag thin layer unclean, can equally cause the wasting of resources.
The present invention also provides a kind of preparation method of above-mentioned graphite deposits device, in the graphite system in addition to graphite jig
System surface coating graphite milk solution, forms aquadag layer.
The graphite system is same as above, and details are not described herein.According to the present invention, in order to avoid the interference of other impurities,
It is preferred that graphite system is cleaned out in advance.
Graphite milk solution is coated on graphite system surface, wherein the method for the coating is well known to those skilled in the art
Method has no special limitation, preferably sprays or brush in the present invention.Aquadag and solvent in the graphite milk solution
Mass ratio be preferably 1：(1~3), more preferably 1：1.Aquadag in the graphite milk solution can be watersoluble plumbago breast,
It can be solvent type aquadag；When the aquadag is watersoluble plumbago breast, solvent is water, and graphite milk solution is preferably aqueous stone
Black whey solution；When the aquadag is solvent type aquadag, solvent is organic solvent；The organic solvent is this field
It can dissolve the organic solvent of solvent type aquadag known to technical staff, have no special limitation, be preferably in the present invention
Alcoholic solvent, more preferably ethyl alcohol；At this point, the graphite milk solution is preferably the alcoholic solution of solvent type aquadag, it is more preferably molten
The ethanol solution of dosage form aquadag.
Graphite milk solution is coated, after dry, forms aquadag thin layer；The drying preferably spontaneously dries at room temperature
It can.The present invention is under graphite system surface coating graphite milk solution formation aquadag thin layer, the condition of high temperature, due to the heat of aquadag
The coefficient of expansion is more than the coefficient of expansion of graphite piece, and the two can be removed, make to be deposited on graphite system surface so as to reach well
The easily peelable effect of pyrolytic boron nitride material reduces the damage to graphite system, and this method is easy to operate, cost is relatively low,
It can economize on resources simultaneously.
The present invention also provides a kind of chemical gas-phase deposition system, including above-mentioned graphite deposits device.
In order to further illustrate the present invention, with reference to embodiments to a kind of processing side of graphite surface provided by the invention
Method is described in detail.
Reagent used in following embodiment is commercially available.
Embodiment 1
By watersoluble plumbago breast and water according to mass ratio 1:2 ratio is uniformly mixed, and obtains watersoluble plumbago milk solution；It will be aqueous
Graphite milk solution is uniformly brushed in the graphite deposits device for pyrolytic boron nitride cleaned out in advance except graphite jig
Graphite system (graphite base, graphite body wall and graphite cover board) surface, after being positioned over indoor seasoning, you can for chemical deposition
Pyrolytic boron nitride is prepared, after coming out of the stove, the aquadag on graphite system surface is brushed and is played with the pyrolytic boron nitride being deposited thereon
Peeling effect, but be not completely exfoliated.
Embodiment 2
By watersoluble plumbago breast and water according to mass ratio 1:1 ratio is uniformly mixed, and obtains watersoluble plumbago milk solution；It will be aqueous
Graphite milk solution uniformly brushes the stone that graphite jig is removed in the graphite deposits device for pyrolytic boron nitride cleaned out in advance
Ink system (graphite base, graphite body wall and graphite cover board) surface, after being positioned over indoor seasoning, you can for chemical deposition legal system
Standby pyrolytic boron nitride after coming out of the stove, is brushed the aquadag on graphite system surface and is played with the pyrolytic boron nitride being deposited thereon
Good peeling effect, entire pyrolytic boron nitride are directly detached from, and photo is as shown in Figure 1.
Embodiment 3
By watersoluble plumbago breast and water according to mass ratio 1:3 ratio is uniformly mixed, and obtains watersoluble plumbago milk solution；It will be aqueous
Graphite milk solution uniformly brushes the stone that graphite jig is removed in the graphite deposits device for pyrolytic boron nitride cleaned out in advance
Ink system (graphite base, graphite body wall and graphite cover board) surface, after being positioned over indoor seasoning, you can for chemical deposition legal system
Standby pyrolytic boron nitride after coming out of the stove, is brushed the aquadag on graphite system surface and is played with the pyrolytic boron nitride being deposited thereon
Peeling effect, but be not completely exfoliated.
Embodiment 4
By solvent type aquadag and alcohol according to mass ratio 1:1 ratio is uniformly mixed, and obtains graphite milk solution；By graphite
Milk solution uniformly brushes the graphite that graphite jig is removed in the graphite deposits device for pyrolytic boron nitride gas cleaned out in advance
System (graphite base, graphite body wall and graphite cover board) surface, after being positioned over indoor rapidly drying, you can for chemical deposition
Method prepares pyrolytic boron nitride, after coming out of the stove, brushes the aquadag on graphite system surface and is risen with the pyrolytic boron nitride being deposited thereon
Good peeling effect is arrived, entire pyrolytic boron nitride is directly detached from.
Claims (6)
1. a kind of graphite deposits device, which is characterized in that the graphite system surface in addition to graphite jig is covered with one layer of graphite
Newborn layer；The thickness of the aquadag layer is 0.05~0.1mm.
2. graphite deposits device according to claim 1, which is characterized in that the graphite system includes graphite cover board, stone
The cavity body wall and graphite base of black precipitation equipment；The graphite cover board is by the cavity and raw material feed device of graphite deposits device
Cavity separate；The graphite base is located in the cavity of graphite deposits device and is provided with graphite jig.
3. a kind of preparation method of graphite deposits device, which is characterized in that applied on the graphite system surface in addition to graphite jig
Graphite milk solution is covered, forms aquadag layer；The mass ratio of aquadag and solvent is 1 in the graphite milk solution：(1~3).
4. preparation method according to claim 3, which is characterized in that the graphite milk solution is molten for watersoluble plumbago whey
Liquid.
5. preparation method according to claim 3, which is characterized in that the graphite milk solution is the alcohol of solvent type aquadag
Solution.
6. a kind of chemical gas-phase deposition system, which is characterized in that including the graphite deposits described in claim 1~2 any one
Graphite deposits device prepared by device or claim 3~5 any one.
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| CN105002477B true CN105002477B (en) | 2018-06-29 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105483642A (en) * | 2016-01-22 | 2016-04-13 | 山东国晶新材料有限公司 | Preparation method of PBN (pyrolytic boron nitride) crucible mold with long service life |
| CN105970186B (en) * | 2016-07-04 | 2018-05-15 | 山东国晶新材料有限公司 | A kind of method of efficiently production pyrolytic boron nitride product |
| CN114044698A (en) * | 2021-11-04 | 2022-02-15 | 广东先导微电子科技有限公司 | Preparation method of boron nitride film of graphite stirrer |
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| CN1507652A (en) * | 2001-05-09 | 2004-06-23 | ���������ƴ���ʽ���� | Coating agent, plasma-resistant component having coating film fomed by the coating agent, plasma processing device provided with the plasma-resistant component |
| CN1898783A (en) * | 2003-12-24 | 2007-01-17 | 三菱重工业株式会社 | Plasma processing apparatus |
| JP2008291299A (en) * | 2007-05-23 | 2008-12-04 | Texas Instr Japan Ltd | Structure for preventing peeling of metal film in apparatus for forming metal film, and method for manufacturing semiconductor device using the structure |
| WO2010143525A1 (en) * | 2009-06-11 | 2010-12-16 | 三菱重工業株式会社 | Plasma processing apparatus and plasma processing method |
| CN102796995A (en) * | 2012-08-27 | 2012-11-28 | 北京博宇半导体工艺器皿技术有限公司 | Vapor deposition furnace and method for preparing pyrolytic boron nitride product |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1507652A (en) * | 2001-05-09 | 2004-06-23 | ���������ƴ���ʽ���� | Coating agent, plasma-resistant component having coating film fomed by the coating agent, plasma processing device provided with the plasma-resistant component |
| CN1898783A (en) * | 2003-12-24 | 2007-01-17 | 三菱重工业株式会社 | Plasma processing apparatus |
| JP2008291299A (en) * | 2007-05-23 | 2008-12-04 | Texas Instr Japan Ltd | Structure for preventing peeling of metal film in apparatus for forming metal film, and method for manufacturing semiconductor device using the structure |
| WO2010143525A1 (en) * | 2009-06-11 | 2010-12-16 | 三菱重工業株式会社 | Plasma processing apparatus and plasma processing method |
| CN102796995A (en) * | 2012-08-27 | 2012-11-28 | 北京博宇半导体工艺器皿技术有限公司 | Vapor deposition furnace and method for preparing pyrolytic boron nitride product |
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Effective date of registration: 20220524 Address after: No. 1116-1, building 1, Dianzhong Business Plaza, Dianzhong new area, Kunming, Yunnan 650000 Patentee after: Kunming forerunner New Material Technology Co.,Ltd. Address before: 511517 Guangdong Industrial Development Zone, Qingxian County, Qingyuan, Guangdong (beside the fish dam road) Guangdong pioneer thin material Limited by Share Ltd Patentee before: FIRST RARE MATERIALS Co.,Ltd. |