CN106083192A - There is graphite material of SiC coating and preparation method thereof - Google Patents
There is graphite material of SiC coating and preparation method thereof Download PDFInfo
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- CN106083192A CN106083192A CN201610402410.8A CN201610402410A CN106083192A CN 106083192 A CN106083192 A CN 106083192A CN 201610402410 A CN201610402410 A CN 201610402410A CN 106083192 A CN106083192 A CN 106083192A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
Abstract
The invention discloses a kind of graphite material with SiC coating and preparation method thereof, this graphite material includes graphite matrix and SiC coating, SiC coating includes primary SiC layer and secondary SiC layer, primary SiC layer is penetrated into inside graphite matrix relative to graphite matrix surface, being formed with graphite matrix reaction in-situ for gaseous state silicon, secondary SiC layer is positioned on primary SiC layer.Preparation method includes: (1) carries out gas phase siliconising sintering to graphite material, obtains the graphite material with primary SiC layer;(2 vapour deposition secondary SiC layer.This graphite material with SiC coating has the advantage that SiC coating and graphite material are combined, there is not thermal mismatching, the densification of SiC coating, antioxygenic property height.This preparation method efficiently solves thermal mismatch problem when directly using CVD technique to prepare SiC coating on graphite material surface, it is ensured that coating and the high bond strength of graphite.
Description
Technical field
The invention belongs to graphite material field, particularly relate to a kind of graphite material with SiC coating and preparation method thereof.
Background technology
Graphite material has resistant to elevated temperatures advantage, is all widely used in many thermal structure fields.But, due to stone
Ink material can occur oxide etch under high temperature, oxidation environment, in turn results in component and progressively damages, and therefore graphite material is at some
Coating process the to be carried out during application of particular etch field.Such as, when epitaxial growth monocrystalline GAN material, need to use
To graphite pallet, owing to graphite material can occur to corrode dry linting phenomenon under high temperature, corrosive gas environment, thus powder body is miscellaneous
Matter is incorporated in monocrystal material, and the effective technical way solving graphite pallet etching problem is that graphite substrate applies overall densification
Protective coating.
Highly purified carborundum (SiC) material has low-density, high temperature resistant, antioxidation, resistance to erosion, anticorrosive etc. a series of
Excellent properties, be the ideal material system of graphite material coating for surface protection.Traditional preparation method is typically with chemistry
The method of vapour deposition (CVD) or brushing is in one layer of SiC coating of graphite surface Direct precipitation, but SiC coating and graphite material
Some differences such as coefficient of expansion above existence Physicochemical character is inconsistent, the therefore combination between coating and graphite material
Intensity is the highest, easily comes off;The depositional mode of the employing two-step method also having, first one layer of solid-state Si of deposition, utilizes Si and graphite table
Face reaction primary layer SiC, then redeposited two grades of SiC coatings, but the method solid-state Si and the limited activity of graphite reaction, and instead
Should only be limited in graphite surface, SiC particulate cannot fully penetrate into inside graphite, causes the combination of SiC coating and graphite material
Intensity is the highest.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, it is provided that a kind of SiC coating and graphite material
Be combined, do not exist the high graphite material with SiC coating of thermal mismatching, the densification of SiC coating, antioxidation, corrosion resistance and
Its preparation method.
For solve above-mentioned technical problem, the present invention by the following technical solutions:
A kind of graphite material with SiC coating, including graphite matrix and SiC coating, described SiC coating includes primary
SiC layer and secondary SiC layer, described primary SiC layer is penetrated into inside graphite matrix relative to graphite matrix surface, described primary SiC layer
Being formed with graphite matrix reaction in-situ for gaseous state silicon, described secondary SiC layer is positioned on primary SiC layer.
The above-mentioned graphite material with SiC coating, it is preferred that described primary SiC layer is from graphite matrix surface to graphite
There is composition decreasing gradient in intrinsic silicon, the degree of depth is more than 1mm.
The above-mentioned graphite material with SiC coating, it is preferred that the SiC in described primary SiC layer and secondary SiC layer is equal
For polycrystal Beta-SiC.
The above-mentioned graphite material with SiC coating, it is preferred that the thickness of described secondary SiC layer is 50 μm~100 μm.
As a total inventive concept, the present invention also provides for the preparation method of a kind of graphite material with SiC coating,
Comprise the following steps:
(1) graphite material is carried out gas phase siliconising sintering, obtain the graphite material with primary SiC layer;
(2) chemical gaseous phase depositing process is used to have the graphite material surface preparation time of primary SiC layer in step (1) gained
Level SiC layer, obtains the graphite material with SiC coating.
The preparation method of the above-mentioned graphite material with SiC coating, it is preferred that in described step (1), described gas phase is oozed
Silicon sintering technological parameter be: sintering temperature is 1500 DEG C~1650 DEG C, and vacuum is 10Pa~50Pa, temperature retention time be 1h~
4h。
The preparation method of the above-mentioned graphite material with SiC coating, it is preferred that in described step (2), described secondary
The thickness of SiC layer is 50 μm~100 μm.
The preparation method of the above-mentioned graphite material with SiC coating, it is preferred that after described step (1), step (2)
The most further comprising the steps of:
The graphite material that step (1) gained has primary SiC layer is placed in Fluohydric acid. immersion.
The preparation method of the above-mentioned graphite material with SiC coating, it is preferred that the time of described immersion be 24h~
48h。
Compared with prior art, it is an advantage of the current invention that:
1, the graphite material with SiC coating of the present invention, primary SiC layer penetrates into graphite matrix relative to graphite matrix surface
Inside, primary SiC layer is that gaseous state silicon is formed with graphite matrix reaction in-situ, and SiC coating and graphite material form Si-C chemical bond
In conjunction with, the strongest " pinning ", bond strength is high, without thermal stress.Efficiently solve and directly use chemical gaseous phase deposition (CVD) work
Skill prepares thermal mismatch problem during SiC coating on graphite material surface, it is ensured that coating and the high bond strength of graphite.
2, the graphite material with SiC coating of the present invention, further, primary SiC layer is from graphite matrix surface to stone
There is composition decreasing gradient in ink intrinsic silicon, primary SiC layer is deep into graphite matrix internal depth more than 1mm, this primary SiC layer
Defining sufficient pinning, a gradient transition with graphite, SiC particle merges weave in graphite substrate, it is ensured that primary
SiC coating and effective combination of graphite material, further increase bond strength.
3, the present invention the graphite material with SiC coating, the SiC in primary SiC layer and secondary SiC layer is high-purity
Polycrystal Beta-the SiC of degree, has good antioxidant effect.
4, the present invention the graphite material with SiC coating, secondary SiC coating layer thickness is 50~100 microns, can be fully
Graphite material is protected, during overweight coating, still suffers from the danger of cracking;The effect of adequately protecting is not had when crossing thin.
5, the present invention the preparation method of the graphite material with SiC coating, first use gas phase siliconising (GSI) to sinter
Graphite material is sintered by mode, obtains the graphite material with primary SiC layer, then uses chemical gaseous phase deposition (CVD) side
Method prepares secondary SiC layer on the graphite material surface with primary SiC layer.Gas phase siliconising (GSI) sintering process is: first by gas phase
Silicon fully penetrates into inside graphite, and then gas-phase silicon and periphery graphite C fully react primary SiC, the SiC coating of formation and graphite material
Material forms Si-C chemical bonds.Owing to being first prepared for one layer of primary on graphite top layer in the region of internal more than the 1mm degree of depth
SiC coating, primary SiC coating and graphite material are formed in situ the chemical bond of the degree of depth, then are prepared with primary by CVD technique
The secondary SiC coating that SiC layer is well combined, between graphite matrix and primary SiC coating, primary SiC coating and secondary SiC coating
Between the most there is not the problem of thermal mismatching, whole SiC coating and graphite matrix have good bond strength, without thermal stress.Have
Effect solves thermal mismatch problem when directly using CVD technique to prepare SiC coating on graphite material surface, it is ensured that coating and stone
The high bond strength of ink.
Further, since the penetrating power of gas-phase silicon is the strongest, it is possible to penetrate into inside the graphite of the 10mm degree of depth, therefore, this primary
SiC layer and graphite define sufficient pinning, a gradient transition, effectively further improve the combination of SiC and graphite.Separately
Outward, secondary SiC prepared by primary SiC and the CVD technique prepared by GSI method is highly purified polycrystal Beta-SiC, has very well
Antioxidant effect.
6, the preparation method of the graphite material with SiC coating of the present invention, further, the sintering temperature of GSI technique
Being 1500~1650 DEG C, vacuum is 10~50Pa, and temperature retention time is 1~4 hour, can make the abundant shape of gas phase Si under this condition
Become, effectively penetrate into graphite reaction internal, abundant formation SiC layer, it is achieved primary layer length of penetration is more than 1mm, it is ensured that primary
SiC coating and effective combination of graphite material.When temperature is less than 1500 DEG C, do not have enough gas phases Si to produce, be unfavorable for reaction
Carrying out;When temperature is higher than 1650 DEG C, gas phase Si excessive concentration, affect length of penetration;Equally, reaction vacuum is too high or too low
All it is unfavorable for the carrying out being effectively formed and reacting of gas-phase silicon.Response time is too short is unfavorable for fully carrying out of reaction, reaches
Certain time reaction just stopped, it is not required that the long time.
7, the preparation method of the graphite material with SiC coating of the present invention, further, also includes removing after GSI sintering
Silicon step, this is because, in the temperature-fall period after GSI, gas phase Si can be at graphite material surface aggregation so that graphite material surface
A small amount of Si is had to remain.The present invention fully removes the residual silicon of specimen surface by the method that Fluohydric acid. corrodes, it is ensured that primary SiC
The high-purity of coating, without other impurity, so fully ensured that effective combination of secondary SiC coating and primary SiC coating.
Accompanying drawing explanation
Fig. 1 is the preparation method flow chart of the graphite material with SiC coating of the present invention.
Fig. 2 is that the cross section SEM of the graphite material with primary SiC layer in the embodiment of the present invention 1 prepared by step (1) shines
Sheet.
Fig. 3 is that in the embodiment of the present invention 1, the graphite material with primary SiC layer prepared by step (1) performs etching and removes
Surface topography SEM photograph after silicon.
Fig. 4 is the cross section SEM photograph of the graphite material with SiC coating prepared by the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with Figure of description and concrete preferred embodiment, the invention will be further described, but the most therefore and
Limit the scope of the invention.
Embodiment 1:
The graphite material with SiC coating of a kind of present invention, including graphite matrix and SiC coating, this SiC coating includes
Primary SiC layer and secondary SiC layer, this primary SiC layer is penetrated into inside graphite matrix relative to graphite matrix surface, for gaseous state silicon and stone
Ink matrix reaction in-situ is formed, and secondary SiC layer is positioned on primary SiC layer.
In the present embodiment, this primary SiC layer from graphite matrix surface to graphite matrix inside there is composition decreasing gradient, deeply
Degree is 2.0mm.
In the present embodiment, the SiC in primary SiC layer and secondary SiC layer is polycrystal Beta-SiC.
In the present embodiment, the thickness of secondary SiC layer is 100 μm.
The preparation method of the graphite material with SiC coating of the present embodiment, as it is shown in figure 1, comprise the following steps:
1) 1500 DEG C, under 50Pa elevated temperature in vacuo, graphite matrix 1 is carried out gas phase siliconising (GSI) and sinters 4 hours,
Preparing one layer and penetrate into the SiC gradient transitional lay within base material from graphite substrate surface, i.e. primary SiC coating 2, the degree of depth is
2.0mm, obtains the graphite material with primary SiC coating;Wherein, in the schematic diagram of Fig. 1, primary SiC coating 2 includes penetrating into
SiC (circle represents) within base material and be positioned at the SiC on graphite substrate surface.
2) at room temperature the graphite material with primary SiC coating is soaked in Fluohydric acid. 24 hours and remove graphite material
In residual Si, obtain noresidue Si has primary SiC coating graphite material;
3) use CVD method noresidue Si have primary SiC coating graphite material surface prepare 100 microns thick secondary
Level SiC coating 3, thus on graphite matrix, it is prepared for double-deck SiC coating, finally be there is the graphite of SiC coating
Finished material.
Fig. 2 is the cross section SEM photograph of the graphite material with primary SiC layer prepared by the present embodiment step (1), in figure
Black region is graphite material, and gray area is the primary SiC formed.It can be seen that primary SiC particle fully permeates
Having arrived inside graphite substrate, with base material weave in, defined the strongest " pinning ", its length of penetration reaches 2.0mm.And table
The primary SiC coating of layer is integrally connected together, and consistency is high.
Fig. 3 is the table after the graphite material with primary SiC layer prepared by the present embodiment step (1) performs etching except silicon
Face pattern SEM photograph, it can be seen that except the primary SiC coating after Si is formed, between crystal grain by the SiC crystal grain stacking of crystalline state
It is tightly combined.
Fig. 4 is the cross section SEM photograph of the graphite material with SiC coating prepared by the present embodiment, and outer surface is secondary
CVD SiC coating, intermediate layer is primary gas phase siliconising SiC coating, and bottom is graphite matrix.It will be seen that secondary SiC coating and
It is the best, without sharp interface, pore-free, flawless that primary SiC coating combines.Primary SiC coating and graphite substrate depth integration
, in conjunction with very well, there is not thermal mismatch problem in weave in.Therefore, what the present invention was prepared on graphite matrix is double-deck
SiC coating, efficiently solves SiC coating and the problem of graphite material combination, improves the coating protective capability to graphite, promote
The erosion-resisting performance of antioxidation of graphite material.
Embodiment 2:
The graphite material with SiC coating of a kind of present invention, including graphite matrix and SiC coating, this SiC coating includes
Primary SiC layer and secondary SiC layer, this primary SiC layer is penetrated into inside graphite matrix relative to graphite matrix surface, for gaseous state silicon and stone
Ink matrix reaction in-situ is formed, and secondary SiC layer is positioned on primary SiC layer.
In the present embodiment, this primary SiC layer from graphite matrix surface to graphite matrix inside there is composition decreasing gradient, deeply
Degree is 3.0mm.
In the present embodiment, the SiC in primary SiC layer and secondary SiC layer is polycrystal Beta-SiC.
In the present embodiment, the thickness of secondary SiC layer is 50 μm.
The preparation method of the graphite material with SiC coating of the present embodiment, as it is shown in figure 1, comprise the following steps:
1) 1650 DEG C, under 10Pa elevated temperature in vacuo, graphite matrix 1 is carried out gas phase siliconising (GSI) and sinters 1 hour,
Preparing one layer and penetrate into the SiC gradient transitional lay within base material from graphite substrate surface, i.e. primary SiC coating 2, the degree of depth is
3.0mm, obtains the graphite material with primary SiC coating;
2) at room temperature the graphite material with primary SiC coating is soaked in Fluohydric acid. 48 hours and remove graphite material
In residual Si, obtain noresidue Si has primary SiC coating graphite material;
3) use CVD method noresidue Si have primary SiC coating graphite material surface prepare 50 microns thick secondary
Level SiC coating 3, thus on graphite matrix, it is prepared for double-deck SiC coating, finally be there is the graphite of SiC coating
Finished material.
Embodiment 3:
The graphite material with SiC coating of a kind of present invention, including graphite matrix and SiC coating, this SiC coating includes
Primary SiC layer and secondary SiC layer, this primary SiC layer is penetrated into inside graphite matrix relative to graphite matrix surface, for gaseous state silicon and stone
Ink matrix reaction in-situ is formed, and secondary SiC layer is positioned on primary SiC layer.
In the present embodiment, this primary SiC layer from graphite matrix surface to graphite matrix inside there is composition decreasing gradient, deeply
Degree is 2.5mm.
In the present embodiment, the SiC in primary SiC layer and secondary SiC layer is polycrystal Beta-SiC.
In the present embodiment, the thickness of secondary SiC layer is 75 μm.
The preparation method of the graphite material with SiC coating of the present embodiment, as it is shown in figure 1, comprise the following steps:
1) 1575 DEG C, under 35Pa elevated temperature in vacuo, graphite matrix 1 carries out gas phase siliconising (GSI), and to sinter 2.5 little
Time, to prepare one layer and penetrate into the SiC gradient transitional lay within base material from graphite substrate surface, i.e. primary SiC coating 2, the degree of depth is
2.5mm, obtains the graphite material with primary SiC coating;
2) at room temperature the graphite material with primary SiC coating is soaked in Fluohydric acid. 36 hours and remove graphite material
In residual Si, obtain noresidue Si has primary SiC coating graphite material;
3) use CVD method noresidue Si have primary SiC coating graphite material surface prepare 75 microns thick secondary
Level SiC coating 3, thus on graphite matrix, it is prepared for double-deck SiC coating, finally be there is the graphite of SiC coating
Finished material.
Comparative example 1:
Use CVD method to prepare 100 microns of thick SiC coatings in graphite substrate, obtain the graphite with CVD SiC coating
Finished material.
Graphite material and the present invention to uncoated graphite material, comparative example 1 preparation with CVD SiC coating implement
The graphite material with SiC coating of example 1 preparation is combined intensity and antioxygenic property test, and acquired results is listed in table 1.
The uncoated graphite material of table 1, comparative example 1 sample and the performance test results of embodiment 1 sample
From table 1, the double-deck SiC coating that the present invention is prepared on graphite matrix and graphite matrix have very well
Bond strength, use stripping method when being combined strength test, when intensity is 10MPa, graphite substrate is the most separated, and
Double-deck SiC coating and graphite do not separate, and illustrate that the bond strength between this SiC coating and graphite substrate is more than 10MPa.
Comparative example 1 directly uses one layer of SiC coating of CVD process deposits on graphite substrate surface, and its bond strength is 5.2MPa.It addition,
Graphite matrix is played a very good protection by double-deck SiC coating prepared by the present invention, carries out under the same conditions
When oxidation control tests, its antioxygenic property is substantially better than comparative example 1 and without coating graphite material.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned enforcement
Example.All technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It it is noted that for the art
Those of ordinary skill for, improvements and modifications under the premise without departing from the principles of the invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. there is a graphite material for SiC coating, including graphite matrix and SiC coating, it is characterised in that described SiC coating
Including primary SiC layer and secondary SiC layer, described primary SiC layer is penetrated into inside graphite matrix relative to graphite matrix surface, described at the beginning of
Level SiC layer is that gaseous state silicon is formed with graphite matrix reaction in-situ, and described secondary SiC layer is positioned on primary SiC layer.
The graphite material with SiC coating the most according to claim 1, it is characterised in that described primary SiC layer is from graphite
There is composition decreasing gradient in matrix surface inside graphite matrix, the degree of depth is more than 1mm.
The graphite material with SiC coating the most according to claim 1 and 2, it is characterised in that described primary SiC layer and
SiC in secondary SiC layer is polycrystal Beta-SiC.
The graphite material with SiC coating the most according to claim 1 and 2, it is characterised in that described secondary SiC layer
Thickness is 50 μm~100 μm.
5. there is a preparation method for the graphite material of SiC coating, comprise the following steps:
(1) graphite material is carried out gas phase siliconising sintering, obtain the graphite material with primary SiC layer;
(2) chemical gaseous phase depositing process is used to have the graphite material surface preparation secondary of primary SiC layer in step (1) gained
SiC layer, obtains the graphite material with SiC coating.
The preparation method of the graphite material with SiC coating the most according to claim 5, it is characterised in that described step
(1) in, described gas phase siliconising sintering technological parameter be: sintering temperature is 1500 DEG C~1650 DEG C, vacuum be 10Pa~
50Pa, temperature retention time is 1h~4h.
The preparation method of the graphite material with SiC coating the most according to claim 6, it is characterised in that described step
(2), in, the thickness of described secondary SiC layer is 50 μm~100 μm.
8. according to the preparation method of the graphite material with SiC coating described in any one of claim 5~7, it is characterised in that
After described step (1), before step (2) the most further comprising the steps of:
The graphite material that step (1) gained has primary SiC layer is placed in Fluohydric acid. immersion.
The preparation method of the graphite material with SiC coating the most according to claim 8, it is characterised in that described immersion
Time be 24h~48h.
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CN112391675B (en) * | 2020-11-16 | 2021-08-31 | 南京工业大学 | Graphite base plate with transition layer structure for semiconductor and preparation method thereof |
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