CN109972120A - A kind of preparation method of multiple elements design carbide coating - Google Patents
A kind of preparation method of multiple elements design carbide coating Download PDFInfo
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- CN109972120A CN109972120A CN201910242863.2A CN201910242863A CN109972120A CN 109972120 A CN109972120 A CN 109972120A CN 201910242863 A CN201910242863 A CN 201910242863A CN 109972120 A CN109972120 A CN 109972120A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
Abstract
The present invention relates to a kind of preparation methods of multiple elements design carbide coating.It successively includes: (1) by TaCl5、HfCl4And ZrCl4Mixed-powder contains in crucible under an inert atmosphere；(2) matrix sample is placed on deposition furnace cradle, and is passed through argon gas, be heated to depositing temperature；(3) it on the lifting support for the low-temperature space that the crucible for filling mixed-powder is put into dual temperature area gasification furnace, is connected to crucible oral area with high-temperature region, sets the heating temperature in low and high temperature area, heating makes mixed-powder be gasified totally；(4) H is passed through into cvd furnace2、CH4, and be passed through in cvd furnace with delivering gas for the mixed gas after being gasified totally, it is deposited in atmospheric conditions.The preparation method can obtain the accurate multicomponent composite coating of each composition stoichiometric ratio, and can guarantee coating and basis material be tightly combined securely, stability it is excellent.
Description
Technical field
The present invention relates to surface heat protective coating technique fields, and in particular to the table of the materials such as C/C composite material and graphite
The protection of face superhigh temperature more particularly to a kind of preparation method of multiple elements design carbide coating.
Background technique
C/C composite material refers to using Carbon fibe or its fabric as reinforced phase, with the pyrolytic carbon or liquid phase of chemical vapor infiltration
Dipping-charing resin carbon, a kind of pure charcoal heterogeneous structure that asphalt carbon is matrix composition.C/C composite material has excellent height
Warm mechanical property and good thermal shock resistance, and be main subliming type thermal-protect ablation material and the material for having high radiant rate,
It is widely used in solid propellant rocket larynx lining, the nose cone of aerospace craft and the contour warm end pieces of radome fairing.But C/C
Compound material antioxygenic property is poor, it is necessary to be modified processing to C/C composite material or prepare protective coating on surface.
Carbide coating, Lai Tigao C/C composite material are prepared in C/C composite material surface currently, being widely used both at home and abroad
Ablation property resistant to high temperatures.For example, the single coatings such as preparation SiC, TaC, HfC, ZrC, these coatings have preferable high temperature resistant
Characteristic, and various high temperature-resistant coating materials have the advantages that different, but are suitable for for 2000 degree of high temperature below；And preparation
The duplex heat treatments such as (Ta, Hf) C, (Hf, Zr) C are suitable for 3000 degree of high temperature below.Wherein, the U.S., Russia and China are equal
Realize the preparation of the coatings such as SiC, TaC, HfC, ZrC, (Ta, Hf) C, (Hf, Zr) C.Duplex heat treatment passes through reasonably at setting up separately
Meter can make each object phase constituent element in coating play synergistic effect, effectively improve the use temperature of C/C composite material.
Chemical vapour deposition technique has that designability is strong, coating purity is high, reaction atmosphere is controllable, easy to operate etc. excellent
Point is the important means for preparing duplex heat treatment.Patent application CN101445392A discloses a kind of graphite matrix flawless TaC painting
Layer and its manufacturing method, patent application CN102093083A disclose a kind of preparation of carbon/carbon composite HfC anti-ablation coating
Method, patent application CN101153384A disclose a kind of manufacturer of unit doublet carbide codeposition fibre-reinforced composite
Method, patent application CN102815971A disclose a kind of Hf (Ta) C superhigh temperature duplex heat treatment and preparation method thereof.
Currently, preparing three constituent elements and the above composite coating using chemical vapor deposition method, the anti-burning of coating is further increased
Protective capacities is lost, the research hotspot of superhigh temperature ceramics coating is become.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of multiple elements design carbide coating, which can be obtained
Each composition accurate multicomponent composite coating of stoichiometric ratio, and can guarantee that coating and basis material are tightly combined secured, stability
It can be excellent.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of multiple elements design carbide coating, which is characterized in that successively the following steps are included:
(1) by the TaCl of specific consumption proportion5、HfCl4And ZrCl4Mixed-powder contains under inert atmosphere protection into crucible
It is interior；
(2) matrix sample is placed on deposition furnace cradle, and is passed through argon gas into cvd furnace, exclude furnace air；It reheats
Cvd furnace reaches depositing temperature；
(3) TaCl will be filled5、HfCl4And ZrCl4The crucible of mixed-powder is put into the lifting of the low-temperature space in dual temperature area gasification furnace
On bracket, increasing lifting support is connected to crucible oral area with high-temperature region, sets the heating temperature of low-temperature space in dual temperature area gasification furnace
It is 210 DEG C~450 DEG C, the heating temperature of high-temperature region is 550 DEG C~700 DEG C, and heating makes mixed-powder be gasified totally；
(4) H is passed through into cvd furnace2、CH4, and the TaCl obtained after being gasified totally using argon gas as delivery gas5、HfCl4
And ZrCl4Mixed gas be passed through in cvd furnace, deposition prepares (Ta, Hf, Zr) C composite coating in atmospheric conditions；
(5) after the completion of coating deposition, H is closed2、CH4, and cvd furnace and dual temperature area gasification furnace are closed under protection of argon gas, until furnace
Sample is taken out when temperature drop is down to 200 DEG C or less.
Inventor have passed through permanent repetition test discovery, be prepared in existing method using chemical vapor deposition method at present
When multicomponent composite coating, automatic powder feeding system is mainly that mechanical powder feeding (carries out being vapor-deposited in i.e. direct powder feeding to cvd furnace anti-
Answer), powder feeding of individually gasifying (i.e. every kind of powder raw material be re-fed into after individually gasifying in respective gasification furnace in cvd furnace mix it is heavy
Product).These automatic powder feeding systems cause each raw material powder amount of practical participation reaction inaccurate, each raw material in gained mixed raw material powder
The ratio of powder is not inconsistent with the ratio originally designed, and the mixing of gained mixed raw material powder is uneven, is prepared in addition
All many conditions such as atmospheric condition, temperature influence in journey, eventually lead to obtained solid solution coating high temperature resistance and are affected.
And it is realized in the present invention by combining the conditions such as atmospheric condition, temperature in specific automatic powder feeding system, and setting preparation process
It is accurate that stoichiometric ratio is respectively formed in the multicomponent composite coating of prepared acquisition, the accurate reaction source ratio that controls is to prepare high-performance
The key of multiple elements design carbide coating, also ensure coating and basis material be tightly combined securely, stability it is excellent.
As advanced optimizing, H described in above-mentioned steps (4)2Flow be 500ml/min~1200ml/min, it is described
CH4Flow be 100ml/min~500ml/min；The argon gas as delivery gas when flow be 50ml/min~
1000ml/min。
As advanced optimizing, TaCl described in above-mentioned steps (1)5、HfCl4And ZrCl4Mixed-powder, according to
TaCl5、HfCl4And ZrCl4Mass percent be respectively 55%~75%, 20%~35% and 5%~10% relationship prepare.
As advanced optimizing, the flow of argon gas described in above-mentioned steps (2) is 100ml/min~800ml/min, ventilation
Time is not less than 30min；The depositing temperature is 1200 DEG C~1600 DEG C.
As advanced optimizing, inert atmosphere described in above-mentioned steps (1) is nitrogen or argon gas.
More specifically, the preparation method of above-mentioned multiple elements design carbide coating, which is characterized in that successively include following
Step:
(1) by TaCl5、HfCl4And ZrCl4Mixed-powder contains in alumina crucible under nitrogen or argon, wherein
TaCl5、HfCl4And ZrCl4It is by mass percentage respectively 55%~75%, 20%~35% and 5%~10% preparation；
(2) matrix sample is placed on deposition furnace cradle, and being passed through flow into cvd furnace is 100ml/min~800ml/
The argon gas of min, duration of ventilation is not less than 30min, to exclude furnace air；It is heavy with the heating rate heating of 5~20 DEG C/min again
Product furnace reaches 1200 DEG C~1600 DEG C of depositing temperature；
(3) TaCl will be filled5、HfCl4And ZrCl4The crucible of mixed-powder is put into the lifting of the low-temperature space in dual temperature area gasification furnace
On bracket, increasing lifting support is connected to crucible oral area with high-temperature region, sets the heating temperature of low-temperature space in dual temperature area gasification furnace
It is 210 DEG C~450 DEG C, the heating temperature of high-temperature region is 550 DEG C~700 DEG C, and heating makes mixed-powder be gasified totally；
(4) H that flow is 500ml/min~1200ml/min is passed through into cvd furnace2, flow be 100ml/min~500ml/
The CH of min4, and be passed through in gasification furnace high temperature area, dual temperature area bottom and made with flow for the argon gas of 50ml/min~1000ml/min
To deliver gas, the TaCl obtained after being gasified totally5、HfCl4And ZrCl4Mixed gas be passed through in cvd furnace, in normal pressure item
Deposition prepares (Ta, Hf, Zr) C composite coating under part, and sedimentation time is 1h~50h, and obtaining coating layer thickness is 10 μm~500 μm
(Ta, Hf, Zr) C composite coating；
(5) after the completion of coating deposition, H is closed2、CH4, and cvd furnace and dual temperature area gasification furnace are closed under protection of argon gas, until furnace
Sample is taken out when temperature drop is down to 200 DEG C or less.
The invention has the following beneficial effects:
The present invention provides a kind of preparation method of multiple elements design carbide coating, it, which passes through, combines specific automatic powder feeding system, with
And the conditions such as atmospheric condition, temperature in setting preparation process, it realizes and whole mixed-powders is gasified totally as gaseous state, ensure that
Into cvd furnace vapor reaction source ratio and pulverulence when ratio (design proportion) it is identical, solve reaction source by design
The problem of deposition accurate in scale, ensure that respectively to form stoichiometric ratio in the multicomponent composite coating of prepared acquisition accurate, also protect
Demonstrate,proved coating and basis material be tightly combined securely, stability it is excellent.The method of the present invention is preparation-obtained to be deposited (Ta,
Hf, Zr) C composite coating C/C composite material, reached the requirement under 3500 DEG C or more hyperthermal environments, anti-superelevation
Warm ablation property is excellent, while after plasma ablation test ablation 38s, composite coating structure is still complete, no to crack and take off
Fall phenomenon, composite coating and C/C composite material be tightly combined securely, stability it is excellent, be suitable for graphite, carbon-to-carbon composite wood
The protection of the superhigh temperature such as material.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of chemical gas-phase deposition system employed in the embodiment of the present invention 1.
Fig. 2 is the cross-sectional structure of the preparation-obtained multiple elements design carbide coating in the embodiment of the present invention 1.
Specific embodiment
The invention will be further described with reference to embodiments, does not therefore limit the present invention to the embodiment described
Within the scope of.
Embodiment 1
A kind of preparation method of multiple elements design carbide coating, successively includes the following steps, wherein used chemical vapor deposition
The specific structure of product system is referring to attached drawing 1:
(1) in argon gas gloves for protection case, by TaCl5、HfCl4And ZrCl4Mixed-powder contains in alumina crucible；Wherein
TaCl5、HfCl4And ZrCl4It is by mass percentage respectively 55%, 35% and 10% preparation；
(2) matrix sample is placed on deposition furnace cradle, and is passed through the argon gas that flow is 200ml/min into cvd furnace
30min, to exclude furnace air；Reach 1300 DEG C of depositing temperature again with the heating rate heating deposition furnace of 5~20 DEG C/min；
(3) TaCl will be filled5、HfCl4And ZrCl4The crucible of mixed-powder is put into the lifting of the low-temperature space in dual temperature area gasification furnace
On bracket, increasing lifting support makes tapered channel on crucible oral area and thermal insulation layer bottom between low-temperature space and high-temperature region
Mouth matches connection, i.e., so that mouth of pot portion is connected to high-temperature region, low-temperature space (gasification zone) adds in setting dual temperature area gasification furnace
Hot temperature is 320 DEG C, and the heating temperature of high-temperature region (mixed zone) is 550 DEG C, and heating makes mixed-powder be gasified totally；
(4) H that flow is 500ml/min is passed through into cvd furnace2, flow be 100ml/min CH4, and gasify in dual temperature area
Furnace high temperature area bottom be passed through using flow for 180ml/min argon gas as delivery gas, obtained after being gasified totally
TaCl5、HfCl4And ZrCl4Mixed gas be passed through in cvd furnace, in atmospheric conditions sedimentation time be 2h；
(5) after the completion of coating deposition, H is closed2、CH4, and cvd furnace and dual temperature area gasification stove heating electricity are closed under protection of argon gas
Source, until furnace temperature takes out sample when being reduced to 200 DEG C or less.
Obtained composite coating bond strength 12.3MPa in this example is tried referring to GJB323A-96 using plasma ablation
Proved recipe method, after ablation 20s, coating structure is complete, no cracking and obscission.The preparation-obtained multiple elements design in this example
The cross-sectional structure of carbide coating is as shown in Fig. 2.
Embodiment 2
A kind of preparation method of multiple elements design carbide coating, successively includes the following steps, wherein used chemical vapor deposition
The structure of product system is same as Example 1:
(1) in argon gas gloves for protection case, by TaCl5、HfCl4And ZrCl4Mixed-powder contains in alumina crucible；Wherein
TaCl5、HfCl4And ZrCl4It is by mass percentage respectively 75%, 20% and 5% preparation；
(2) matrix sample is placed on deposition furnace cradle, and is passed through the argon gas that flow is 200ml/min into cvd furnace
30min, to exclude furnace air；Reach 1400 DEG C of depositing temperature again with the heating rate heating deposition furnace of 5~20 DEG C/min；
(3) TaCl will be filled5、HfCl4And ZrCl4The crucible of mixed-powder is put into the lifting of the low-temperature space in dual temperature area gasification furnace
On bracket, increasing lifting support makes tapered channel on crucible oral area and thermal insulation layer bottom between low-temperature space and high-temperature region
Mouth matches connection, i.e., so that mouth of pot portion is connected to high-temperature region, low-temperature space (gasification zone) adds in setting dual temperature area gasification furnace
Hot temperature is 400 DEG C, and the heating temperature of high-temperature region (mixed zone) is 600 DEG C, and heating makes mixed-powder be gasified totally；
(4) H that flow is 800ml/min is passed through into cvd furnace2, flow be 200ml/min CH4, and gasify in dual temperature area
Furnace high temperature area bottom be passed through using flow for 300ml/min argon gas as delivery gas, obtained after being gasified totally
TaCl5、HfCl4And ZrCl4Mixed gas be passed through in cvd furnace, in atmospheric conditions sedimentation time be 3h；
(5) after the completion of coating deposition, H is closed2、CH4, and cvd furnace and dual temperature area gasification stove heating electricity are closed under protection of argon gas
Source, until furnace temperature takes out sample when being reduced to 200 DEG C or less.
The composite coating bond strength 11.5MPa that the present embodiment obtains is tried referring to GJB323A-96 using plasma ablation
Proved recipe method, after ablation 30s, coating structure is complete, no cracking and obscission.
Embodiment 3
A kind of preparation method of multiple elements design carbide coating, successively includes the following steps, wherein used chemical vapor deposition
The structure of product system is same as Example 1:
(1) in argon gas gloves for protection case, by TaCl5、HfCl4And ZrCl4Mixed-powder contains in alumina crucible；Wherein
TaCl5、HfCl4And ZrCl4It is by mass percentage respectively 60%, 30% and 10% preparation；
(2) matrix sample is placed on deposition furnace cradle, and is passed through the argon gas that flow is 200ml/min into cvd furnace
30min, to exclude furnace air；Reach 1400 DEG C of depositing temperature again with the heating rate heating deposition furnace of 5~20 DEG C/min；
(3) TaCl will be filled5、HfCl4And ZrCl4The crucible of mixed-powder is put into the lifting of the low-temperature space in dual temperature area gasification furnace
On bracket, increasing lifting support makes tapered channel on crucible oral area and thermal insulation layer bottom between low-temperature space and high-temperature region
Mouth matches connection, i.e., so that mouth of pot portion is connected to high-temperature region, low-temperature space (gasification zone) adds in setting dual temperature area gasification furnace
Hot temperature is 450 DEG C, and the heating temperature of high-temperature region (mixed zone) is 650 DEG C, and heating makes mixed-powder be gasified totally；
(4) H that flow is 100ml/min is passed through into cvd furnace2, flow be 250ml/min CH4, and gasify in dual temperature area
Furnace high temperature area bottom be passed through using flow for 420ml/min argon gas as delivery gas, obtained after being gasified totally
TaCl5、HfCl4And ZrCl4Mixed gas be passed through in cvd furnace, in atmospheric conditions sedimentation time be 4h；
(5) after the completion of coating deposition, H is closed2、CH4, and cvd furnace and dual temperature area gasification stove heating electricity are closed under protection of argon gas
Source, until furnace temperature takes out sample when being reduced to 200 DEG C or less.
The composite coating bond strength 10.7MPa that the present embodiment obtains is tried referring to GJB323A-96 using plasma ablation
Proved recipe method, after ablation 38s, coating structure is complete, no cracking and obscission.
Claims (6)
1. a kind of preparation method of multiple elements design carbide coating, which is characterized in that successively the following steps are included:
(1) by the TaCl of specific consumption proportion5、HfCl4And ZrCl4Mixed-powder contains under inert atmosphere protection into crucible
It is interior；
(2) matrix sample is placed on deposition furnace cradle, and is passed through argon gas into cvd furnace, exclude furnace air；It reheats
Cvd furnace reaches depositing temperature；
(3) TaCl will be filled5、HfCl4And ZrCl4The crucible of mixed-powder is put into the lifting of the low-temperature space in dual temperature area gasification furnace
On bracket, increasing lifting support is connected to crucible oral area with high-temperature region, sets the heating temperature of low-temperature space in dual temperature area gasification furnace
It is 210 DEG C~450 DEG C, the heating temperature of high-temperature region is 550 DEG C~700 DEG C, and heating makes mixed-powder be gasified totally；
(4) H is passed through into cvd furnace2、CH4, and the TaCl obtained after being gasified totally using argon gas as delivery gas5、HfCl4With
ZrCl4Mixed gas be passed through in cvd furnace, deposition prepares (Ta, Hf, Zr) C composite coating in atmospheric conditions；
(5) after the completion of coating deposition, H is closed2、CH4, and cvd furnace and dual temperature area gasification furnace are closed under protection of argon gas, until furnace temperature
Sample is taken out when being reduced to 200 DEG C or less.
2. the preparation method of multiple elements design carbide coating as described in claim 1, it is characterised in that: institute in the step (4)
State H2Flow be 500ml/min~1200ml/min, the CH4Flow be 100ml/min~500ml/min；The argon gas
Flow when as delivery gas is 50ml/min~1000ml/min.
3. the preparation method of multiple elements design carbide coating as claimed in claim 1 or 2, it is characterised in that: in the step (1)
The TaCl5、HfCl4And ZrCl4Mixed-powder, according to TaCl5、HfCl4And ZrCl4Mass percent be respectively 55%~
75%, 20%~35% and 5%~10% relationship is prepared.
4. the preparation method of multiple elements design carbide coating as described in claim 1-3 is any, it is characterised in that: the step
(2) flow of argon gas described in is 100ml/min~800ml/min, and duration of ventilation is not less than 30min；The depositing temperature is
1200 DEG C~1600 DEG C.
5. the preparation method of multiple elements design carbide coating as described in claim 1-4 is any, it is characterised in that: the step
(1) inert atmosphere described in is nitrogen or argon gas.
6. the preparation method of multiple elements design carbide coating as described in claim 1, which is characterized in that successively include following step
It is rapid:
(1) by TaCl5、HfCl4And ZrCl4Mixed-powder contains in alumina crucible under nitrogen or argon, wherein
TaCl5、HfCl4And ZrCl4It is by mass percentage respectively 55%~75%, 20%~35% and 5%~10% preparation；
(2) matrix sample is placed on deposition furnace cradle, and being passed through flow into cvd furnace is 100ml/min~800ml/
The argon gas of min, duration of ventilation is not less than 30min, to exclude furnace air；It is heavy with the heating rate heating of 5~20 DEG C/min again
Product furnace reaches 1200 DEG C~1600 DEG C of depositing temperature；
(3) TaCl will be filled5、HfCl4And ZrCl4The crucible of mixed-powder is put into the lifting of the low-temperature space in dual temperature area gasification furnace
On bracket, increasing lifting support is connected to crucible oral area with high-temperature region, sets the heating temperature of low-temperature space in dual temperature area gasification furnace
It is 210 DEG C~450 DEG C, the heating temperature of high-temperature region is 550 DEG C~700 DEG C, and heating makes mixed-powder be gasified totally；
(4) H that flow is 500ml/min~1200ml/min is passed through into cvd furnace2, flow be 100ml/min~500ml/
The CH of min4, and be passed through in gasification furnace high temperature area, dual temperature area bottom and made with flow for the argon gas of 50ml/min~1000ml/min
To deliver gas, the TaCl obtained after being gasified totally5、HfCl4And ZrCl4Mixed gas be passed through in cvd furnace, in normal pressure item
Deposition prepares (Ta, Hf, Zr) C composite coating under part, and sedimentation time is 1h~50h；
(5) after the completion of coating deposition, H is closed2、CH4, and cvd furnace and dual temperature area gasification furnace are closed under protection of argon gas, until furnace temperature
Sample is taken out when being reduced to 200 DEG C or less.
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| CN201910242863.2A CN109972120B (en) | 2019-03-28 | 2019-03-28 | Preparation method of multi-element composite carbide coating |
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| CN113235066A (en) * | 2021-05-19 | 2021-08-10 | 重庆大学 | Organic platinum group metal chemical vapor deposition device and method |
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| CN113684471B (en) * | 2021-08-02 | 2023-04-11 | 江苏鎏溪光学科技有限公司 | System and method for monitoring reaction atmosphere in chemical vapor deposition process |
| CN113860917B (en) * | 2021-10-09 | 2022-11-25 | 航天特种材料及工艺技术研究所 | Ablation-resistant ceramic matrix composite and preparation method thereof |
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