CN106673710A - HfC nanowire-toughened anti-ablation ceramic coating on surface of carbon/carbon composite material and preparation method - Google Patents
HfC nanowire-toughened anti-ablation ceramic coating on surface of carbon/carbon composite material and preparation method Download PDFInfo
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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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
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Abstract
The invention relates to an HfC nanowire-toughened anti-ablation ceramic coating on the surface of a carbon/carbon composite material and a preparation method, and aims to solve the technical problems that the binding force between an anti-ablation ceramic coating prepared by an existing method and a matrix is low and the ceramic coating is easy to crack and peel in preparation and ablation processes. According to the technical scheme, the preparation method comprises the following steps: firstly preparing an HfC nanowire porous layer on the surface of the carbon/carbon composite material by virtue of a chemical vapor deposition method; and then preparing the HfC coating by virtue of a chemical vapor deposition method. An HfC nanowire and an HfC coating are homogeneous materials and have good physical and chemical compatibility, and the HfC nanowire is introduced into the HfC ceramic coating as an enhancing body, so that the toughness of the HfC coating can be improved and cracking of the coating is reduced, and therefore, the anti-ablation property of the coating is further improved.
Description
Technical field
The invention belongs to carbon/carbon (C/C) composite material surface anti-yaw damper coating and preparation method, it is related to a kind of carbon/carbon multiple
The nanowire-toughened anti-yaw damper ceramic coatings of condensation material surface HfC and preparation method.
Background technology
High temperature is oxidizable, easy ablation be C/C composites be most difficult in actual applications break through bottleneck problem, coating technology
It is the effective means for solving the problem.Superhigh temperature ceramics have high-melting-point, high rigidity and good anti-oxidant, Burning corrosion resistance
Energy.Wherein HfC fusing points are up to 3890 DEG C, are the superhigh temperature ceramics of most infusibility, are the preferable anti-yaw damper coating materials of C/C composites
Material.However, the thermal coefficient of expansion (6.6 × 10 of HfC ceramic coatings-6K-1) it is significantly larger than C/C matrixes (1.2 × 10-6K-1), heat is swollen
Swollen mismatch can cause coating to be ftractureed in preparation and ablation process, peeled off, and cause coating failure.In order to alleviate ceramic coating cracking
Trend, composite coating and introduce secondary phase toughening coating technology and cause the very big concern of researcher.
" the SiC/HfC/SiC ablation resistant coating for carbon/carbon of document 1
composites,Yongjie Wang,Hejun Li,Qiangang Fu,Heng Wu,Dongjia Yao,Hailiang Li,
Surface&Coatings Technology,2012(206):3883-3887 " discloses one kind and prepares compound anti-yaw damper coating
Method, first using investment C/C composite material surfaces prepare SiC undercoating；Secondly using chemical vapor deposition (CVD)
Method prepares HfC coatings, finally prepares SiC external coatings using CVD.The composite coating technology although alleviate to a certain extent
Thermal expansion mismatch between HfC coatings and C/C matrixes, reduces cracking of the HfC coatings in preparation and ablation process, but
HfC coatings and SiC coatings (4.4 × 10-6K-1) thermal coefficient of expansion still mismatch, can be seen that HfC from composite coating sectional view
There is obvious transversal crack in coating, this can cause HfC coatings to be ftractureed in ablation process, peeled off, reduce the anti-yaw damper of coating
Performance.
Document 2 " SiC nanowires toughed HfC ablative coating for C/C composites,
Hejun Li,Yongjie Wang,Qiangang Fu,Yanhui Chu,Journal of Material Science and
Technology,2015(31):70-76 " discloses a kind of method of SiC nanowire toughness reinforcing HfC anti-yaw damper coatings, and the method is first
SiC nanowire porous layer is first prepared in C/C composite material surfaces using chemical gas-phase reaction method, HfC is secondly prepared using CVD
Coating.The technology improves the toughness and Burning corrosion resistance of HfC coatings, but SiC nanowire in ablation environment to a certain extent
Middle rapid oxidation, fusing and washed away by combustion gas stream, this can reduce toughening effect of the SiC nanowire in ablation process.
Compared with SiC, HfC has fusing point higher, still possesses very in extreme harsh superhigh temperature oxide etch environment
Good chemical stability and thermal shock resistance, its oxide (HfO2) fusing point is up to 2850 DEG C, will not be melted in ablation environment, waved
Hair.Additionally, HfC nano wires belong to homogeneous material with HfC coatings, with good physical chemistry compatibility.Therefore HfC nano wires
The enhancing phase of HfC anti-yaw damper coatings is more suitable for, to improve the mechanical property and Burning corrosion resistance energy of HfC coatings.
The content of the invention
The technical problem to be solved
In order to avoid the deficiencies in the prior art part, the present invention proposes that a kind of surface of carbon/carbon composite HfC nano wires increase
Tough anti-yaw damper ceramic coating and preparation method, overcome existing method prepare HfC anti-yaw damper coatings in preparation and ablation process
Deficiency easy to crack.
Technical scheme
A kind of nanowire-toughened anti-yaw damper ceramic coatings of surface of carbon/carbon composite HfC, it is characterised in that including undercoating
And external coating；The undercoating is HfC nano wire porous layers, and external coating is for HfC coatings and HfC external coatings are around HfC nano wires
Forming core fills the hole of porous layer, obtains the nanowire-toughened HfC ceramic coatings of HfC of densification.
A kind of preparation method of the nanowire-toughened anti-yaw damper ceramic coatings of the surface of carbon/carbon composite HfC, its feature
It is step as follows：
Step 1：C/C composites after treatment are put into the Ni (NO that concentration is 0.5mol/L3)2Soaked in ethanol solution
5h, then takes out and is placed on drying in 80 DEG C of baking oven, obtains surface with Ni (NO3)2C/C matrixes；
Step 2, CVD prepare HfC nano wires：Surface had into Ni (NO3)2C/C matrixes hang on vertical resistance furnace
High-temperature region, by HfCl4Powder is placed in low-temperature space, and resistance furnace is evacuated to after fidelity sky 30min after 2kPa determines that body of heater is air tight
Vavuum pump is opened again, is passed through H2As reducing gas, furnace temperature is risen to 1100~1200 with the programming rate of 8~10 DEG C/min
℃；When in-furnace temperature reaches design temperature, CH is passed through4And Ar, by furnace pressure control in 2kPa~12kPa；Sedimentation time
Stop being passed through CH after 2h4And Ar, by furnace pressure control in 2kPa, heating power supply Temperature fall is closed, whole temperature-fall period leads to H2
Protection, obtains the C/C composites of the surface porous layer of nano wire containing HfC；
The H2Flow is 1000~2000ml/min；The H2It is 3000ml/min, wherein CH with the total flow of Ar4's
Flow is 100~400ml/min；The H2With the volume ratio 1 of Ar:2~2:1；
Step 3, CVD prepare HfC coatings：The C/C composites of surface nano wire containing HfC porous layer are hung on vertical
The high-temperature region of resistance furnace, by HfCl4Powder is placed in low-temperature space, and fidelity sky 30min determines stove after resistance furnace is evacuated into 2kPa
Vavuum pump is opened again after body is air tight, is passed through H2As reducing gas, furnace temperature is risen to the programming rate of 10~15 DEG C/min
1200~1400 DEG C；CH is passed through again4And Ar, sedimentation time be 4h after stop be passed through CH4And Ar, heating power supply Temperature fall is closed,
The whole logical H of temperature-fall period2Protection, obtains the nanowire-toughened anti-yaw damper ceramic coatings of surface of carbon/carbon composite HfC
The H2Flow is 1000~2000ml/min；The H2It is 5000ml/min, wherein CH with the total flow of Ar4's
Flow is 400~800ml/min；The H2With the volume ratio 1 of Ar:4~4:1.
C/C composites after the treatment are：C/C composites are cleaned by ultrasonic with after SiC sand paperings, 80 are put into
Dried in DEG C baking oven.
Ni (the NO3)2Purity for analyze pure, weight/mass percentage composition >=99.8%.
The purity of the ethanol is pure, weight/mass percentage composition >=99.8% of analysis.
The HfCl4To analyze pure, weight/mass percentage composition >=99.8%, granularity is 500 mesh to the purity of powder.
The H2Purity be more than 99.99%.
The CH4Purity be more than 99.99%.
The purity of the Ar is more than 99.99%.
Beneficial effect
The nanowire-toughened anti-yaw damper ceramic coatings of a kind of surface of carbon/carbon composite HfC proposed by the present invention and preparation side
Method, prepares HfC nano wire porous layers using CVD in C/C composite material surfaces first, and then preparing HfC using CVD applies
Layer.The toughness of HfC coatings is improved by introducing HfC nano wires, and then improves the Burning corrosion resistance of HfC coatings.In order to make comparisons, adopt
With same process HfC coatings are prepared in C/C composite material surfaces.
The present invention prepares the nanowire-toughened HfC coatings of HfC using two step CVDs, and HfC is improved by introducing HfC nano wires
The Burning corrosion resistance of the toughness of coating, the cracking for reducing coating and then raising coating.The nanowire-toughened HfC ceramics of HfC of the invention
Coating production is simple, and coating is finer and close after adding HfC nano wires as can be seen from Figure 2, and coated grains are more tiny.
The addition of HfC nano wires as can be seen from Figure 3 can improve the deposition efficiency of coating, avoid coating Transverse Cracks, coated crystal
Structure is changed into equiax crystal from column crystal；The nanowire-toughened HfC coating cross sections of HfC are in sandwich, from coating and the interface of matrix
First reduced to coating surface its consistency increases afterwards.
Brief description of the drawings
Fig. 1 is the HfC nano wire porous layer surface scan electromicroscopic photographs prepared by the embodiment of the present invention 2.
Fig. 2 is respectively HfC coatings (a) and nanowire-toughened HfC coatings (b) surfaces of HfC prepared by the embodiment of the present invention 2
Stereoscan photograph.
Fig. 3 is respectively HfC coatings (a) and nanowire-toughened HfC coatings (b) sections of HfC prepared by the embodiment of the present invention 2
Stereoscan photograph.
Specific embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described：
Embodiment 1：
1) by density 1.7g/cm3C/C composites cut into the square of 10mm × 10mm × 10mm as matrix material
Material, after being polished successively with the SiC sand paper of No. 80, No. 400 and No. 800,1h is cleaned by ultrasonic with absolute ethyl alcohol, and ultrasonic power is set to
80W, is put into dry for standby in 80 DEG C of baking oven.
2) configuration concentration is the Ni (NO of 0.5mol/L3)2Ethanol solution.It is molten that the C/C composites that will be cleaned up are put into this
5h is soaked in liquid, is then taken out and is placed on dry for standby in 80 DEG C of baking oven.
3) CVD prepares HfC nano wires, and specific method is as follows：
By step 2) in surface have Ni (NO3)2C/C matrixes hang on the high-temperature region of vertical resistance furnace, weigh 30g's
HfCl4Powder is placed in low-temperature space in being placed on silica crucible, and resistance furnace is evacuated into 2kPa, turns off vavuum pump fidelity sky 30min
Determine to open vavuum pump again after body of heater is air tight, be passed through H2Used as reducing gas, its flow is 1000ml/min；With 8 DEG C/min
Programming rate furnace temperature is risen to 1100 DEG C；When in-furnace temperature reaches depositing temperature, CH is passed through4And Ar, CH4Flow be
100ml/min, H2It is 3000ml/min (volume ratios 1 with the total flow of Ar:2)；Regulation vacuum pumping speed, by the deposition pressure in stove
Power is controlled in 2kPa；Sedimentation time is 2h；Deposition stops being passed through CH after terminating4And Ar, heating power supply Temperature fall is closed, entirely
Temperature-fall period leads to H2Protection.
4) CVD prepares HfC coatings, and specific method is as follows：
The C/C composites that C/C composites and surface contain HfC nano wire porous layers are hung on into vertical resistance furnace
High-temperature region, weighs the HfCl of 60g4Powder is placed in low-temperature space in being placed on silica crucible, and resistance furnace is evacuated into 2kPa, turns off true
Empty pump fidelity sky 30min determines to open vavuum pump again after body of heater is air tight, is passed through H2Used as reducing gas, its flow is
1000ml/min, 1200 DEG C are risen to the programming rate of 10 DEG C/min by furnace temperature；When in-furnace temperature reaches depositing temperature, it is passed through
CH4And Ar, CH4Flow be 400ml/min, H2It is 5000ml/min (volume ratios 1 with the total flow of Ar:4)；Sedimentation time is
4h；Deposition stops being passed through CH after terminating4And Ar, heating power supply Temperature fall is closed, whole temperature-fall period leads to H2Protection.
Through above-mentioned steps, the C/C composite samples for having HfC coatings and HfC nano wire-HfC coatings respectively are prepared for.
Embodiment 2：
1) by density 1.7g/cm3C/C composites cut into the square of 10mm × 10mm × 10mm as matrix material
Material, after being polished successively with the SiC sand paper of No. 80, No. 400 and No. 800,1h is cleaned by ultrasonic with absolute ethyl alcohol, and ultrasonic power is set to
80W, is put into dry for standby in 80 DEG C of baking oven.
2) configuration concentration is the Ni (NO of 0.5mol/L3)2Ethanol solution.It is molten that the C/C composites that will be cleaned up are put into this
5h is soaked in liquid, is then taken out and is placed on dry for standby in 80 DEG C of baking oven.
3) CVD prepares HfC nano wires, and specific method is as follows：
By step 2) in surface have Ni (NO3)2C/C matrixes hang on the high-temperature region of vertical resistance furnace, weigh 30g's
HfCl4Powder is placed in low-temperature space in being placed on silica crucible, and resistance furnace is evacuated into 2kPa, turns off vavuum pump fidelity sky 30min
Determine to open vavuum pump again after body of heater is air tight, be passed through H2Used as reducing gas, its flow is 1500ml/min；With 9 DEG C/min
Programming rate furnace temperature is risen to 1150 DEG C；When in-furnace temperature reaches depositing temperature, CH is passed through4And Ar, CH4Flow be
250ml/min, H2It is 3000ml/min (volume ratios 1 with the total flow of Ar:1)；Regulation vacuum pumping speed, by the deposition pressure in stove
Power is controlled in 7kPa；Sedimentation time is 2h；Deposition stops being passed through CH after terminating4And Ar, by furnace pressure control in 2kPa, close
Heating power supply Temperature fall, whole temperature-fall period leads to H2Protection.
4) CVD prepares HfC coatings, and specific method is as follows：
The C/C composites that C/C composites and surface contain HfC nano wire porous layers are hung on into vertical resistance furnace
High-temperature region, weighs the HfCl of 60g4Powder is placed in low-temperature space in being placed on silica crucible, and resistance furnace is evacuated into 2kPa, turns off true
Empty pump fidelity sky 30min determines to open vavuum pump again after body of heater is air tight, is passed through H2Used as reducing gas, its flow is
1500ml/min, 1300 DEG C are risen to the programming rate of 12 DEG C/min by furnace temperature；When in-furnace temperature reaches depositing temperature, it is passed through
CH4And Ar, CH4Flow be 600ml/min, H2It is 5000ml/min (volume ratios 1 with the total flow of Ar:1)；Sedimentation time is
4h；Deposition stops being passed through CH after terminating4And Ar, heating power supply Temperature fall is closed, whole temperature-fall period leads to H2Protection.
Through above-mentioned steps, the C/C composite samples for having HfC coatings and HfC nano wire-HfC coatings respectively are prepared for.
The nano wire layer for preparing as can be seen from Figure 1 is porous network structure, nanowire diameter between 300-500nm,
Length is between tens to hundreds of microns.Coating is finer and close after adding HfC nano wires as can be seen from Figure 2, coated grains
It is more tiny.As can be seen from Figure 3 the addition of HfC nano wires can improve coating deposition efficiency, avoid coating Transverse Cracks,
Coating structure is changed into equiax crystal from column crystal；The nanowire-toughened HfC coating cross sections of HfC are in sandwich, from coating and matrix
Interface first reduces to coating surface its consistency to be increased afterwards.
Embodiment 3：
1) by density 1.7g/cm3C/C composites cut into the square of 10mm × 10mm × 10mm as matrix material
Material, after being polished successively with the SiC sand paper of No. 80, No. 400 and No. 800,1h is cleaned by ultrasonic with absolute ethyl alcohol, and ultrasonic power is set to
80W, is put into dry for standby in 80 DEG C of baking oven.
2) configuration concentration is the Ni (NO of 0.5mol/L3)2Ethanol solution.It is molten that the C/C composites that will be cleaned up are put into this
5h is soaked in liquid, is then taken out and is placed on dry for standby in 80 DEG C of baking oven.
3) CVD prepares HfC nano wires, and specific method is as follows：
By step 2) in surface have Ni (NO3)2C/C matrixes hang on the high-temperature region of vertical resistance furnace, weigh 30g's
HfCl4Powder is placed in low-temperature space in being placed on silica crucible, and resistance furnace is evacuated into 2kPa, turns off vavuum pump fidelity sky 30min
Determine to open vavuum pump again after body of heater is air tight, be passed through H2Used as reducing gas, its flow is 2000ml/min；With 10 DEG C/min
Programming rate furnace temperature is risen to 1200 DEG C；When in-furnace temperature reaches depositing temperature, CH is passed through4And Ar, CH4Flow be
400ml/min, H2It is 3000ml/min (volume ratios 2 with the total flow of Ar:1)；Regulation vacuum pumping speed, by the deposition pressure in stove
Power is controlled in 12kPa；Sedimentation time is 2h；Deposition stops being passed through CH after terminating4And Ar, by furnace pressure control in 2kPa, close
Heating power supply Temperature fall is closed, whole temperature-fall period leads to H2Protection.
4) CVD prepares HfC coatings, and specific method is as follows：
The C/C composites that C/C composites and surface contain HfC nano wire porous layers are hung on into vertical resistance furnace
High-temperature region, weighs the HfCl of 60g4Powder is placed in low-temperature space in being placed on silica crucible, and resistance furnace is evacuated into 2kPa, turns off true
Empty pump fidelity sky 30min determines to open vavuum pump again after body of heater is air tight, is passed through H2Used as reducing gas, its flow is
2000ml/min, 1400 DEG C are risen to the programming rate of 15 DEG C/min by furnace temperature；When in-furnace temperature reaches depositing temperature, it is passed through
CH4And Ar, CH4Flow be 800ml/min, H2It is 5000ml/min (volume ratios 4 with the total flow of Ar:1)；Sedimentation time is
4h；Deposition stops being passed through CH after terminating4And Ar, heating power supply Temperature fall is closed, whole temperature-fall period leads to H2Protection.
Through above-mentioned steps, the C/C composite samples for having HfC coatings and HfC nano wire-HfC coatings respectively are prepared for.
In all embodiments, described Ni (NO3)2Analysis pure (weight/mass percentage composition >=99.8%) is with ethanol,
HfCl4The purity of powder is 500 mesh, CH to analyze pure (weight/mass percentage composition >=99.8%), granularity4, Ar and H2Purity is to be more than
99.99% high-purity gas.
Claims (9)
1. nanowire-toughened anti-yaw damper ceramic coatings of a kind of surface of carbon/carbon composite HfC, it is characterised in that including undercoating and
External coating；The undercoating is HfC nano wire porous layers, and external coating is for HfC coatings and HfC external coatings are linear around HfC nanometers
Core fills the hole of porous layer, obtains the nanowire-toughened HfC ceramic coatings of HfC of densification.
2. the preparation side of the nanowire-toughened anti-yaw damper ceramic coatings of surface of carbon/carbon composite HfC described in a kind of claim 1
Method, it is characterised in that step is as follows：
Step 1：C/C composites after treatment are put into the Ni (NO that concentration is 0.5mol/L3)25h is soaked in ethanol solution, so
Take out afterwards and be placed on drying in 80 DEG C of baking oven, obtain surface with Ni (NO3)2C/C matrixes；
Step 2, CVD prepare HfC nano wires：Surface had into Ni (NO3)2C/C matrixes hang on the high temperature of vertical resistance furnace
Area, by HfCl4Powder is placed in low-temperature space, and fidelity sky 30min determines to be beaten again after body of heater is air tight after resistance furnace is evacuated to 2kPa
Vavuum pump is driven, H is passed through2As reducing gas, furnace temperature is risen to 1100~1200 DEG C with the programming rate of 8~10 DEG C/min；When
When in-furnace temperature reaches design temperature, CH is passed through4And Ar, by furnace pressure control in 2kPa~12kPa；Stop after sedimentation time 2h
Only it is passed through CH4And Ar, by furnace pressure control in 2kPa, heating power supply Temperature fall is closed, whole temperature-fall period leads to H2Protection,
Obtain the C/C composites of the surface porous layer of nano wire containing HfC；
The H2Flow is 1000~2000ml/min；The H2It is 3000ml/min, wherein CH with the total flow of Ar4Flow
It is 100~400ml/min；The H2With the volume ratio 1 of Ar:2~2:1；
Step 3, CVD prepare HfC coatings：The C/C composites of surface nano wire containing HfC porous layer are hung on into vertical resistance
The high-temperature region of stove, by HfCl4Powder is placed in low-temperature space, and fidelity sky 30min determines body of heater not after resistance furnace is evacuated into 2kPa
Vavuum pump is opened after gas leakage again, H is passed through2As reducing gas, furnace temperature is risen to 1200 with the programming rate of 10~15 DEG C/min
~1400 DEG C；CH is passed through again4And Ar, sedimentation time be 4h after stop be passed through CH4And Ar, heating power supply Temperature fall is closed, entirely
Temperature-fall period leads to H2Protection, obtains the nanowire-toughened anti-yaw damper ceramic coatings of surface of carbon/carbon composite HfC
The H2Flow is 1000~2000ml/min；The H2It is 5000ml/min, wherein CH with the total flow of Ar4Flow
It is 400~800ml/min；The H2With the volume ratio 1 of Ar:4~4:1.
3. preparation method according to claim 2, it is characterised in that：C/C composites after the treatment are：By C/C
Composite is cleaned by ultrasonic with after SiC sand paperings, is put into drying in 80 DEG C of baking ovens.
4. preparation method according to claim 2, it is characterised in that：Ni (the NO3)2Purity for analyze pure, quality hundred
Divide content >=99.8%.
5. preparation method according to claim 2, it is characterised in that：The purity of the ethanol is pure, the quality percentage of analysis
Content >=99.8%.
6. preparation method according to claim 2, it is characterised in that：The HfCl4The purity of powder is pure, the quality hundred of analysis
Divide content >=99.8%, granularity is 500 mesh.
7. preparation method according to claim 2, it is characterised in that：The H2Purity be more than 99.99%.
8. preparation method according to claim 2, it is characterised in that：The CH4Purity be more than 99.99%.
9. preparation method according to claim 2, it is characterised in that：The purity of the Ar is more than 99.99%.
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| CN108395279A (en) * | 2018-02-08 | 2018-08-14 | 西北工业大学 | The method that chemical gaseous phase co-electrodeposition method prepares HfC-SiC complex phase gradient coatings |
| CN111253171A (en) * | 2020-03-18 | 2020-06-09 | 西北工业大学 | Densification preparation method of fiber-reinforced hafnium carbide ceramic matrix composite material |
| CN114853507A (en) * | 2022-07-06 | 2022-08-05 | 湖南泰坦未来科技有限公司 | Composite carbon material and preparation method and application thereof |
| CN115259900A (en) * | 2022-03-23 | 2022-11-01 | 西北工业大学 | Very long (Ta)xHf1-x) C ultra-high temperature ceramic solid solution nanowire and preparation method thereof |
| CN115403397A (en) * | 2022-08-09 | 2022-11-29 | 西北工业大学 | Core-shell structure toughened (Hf, ta) C solid solution ultrahigh-temperature ceramic coating and one-step preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101563801A (en) * | 2005-11-21 | 2009-10-21 | 纳米***公司 | Nanowire structures comprising carbon |
| CN103951470A (en) * | 2014-04-04 | 2014-07-30 | 西北工业大学 | Hafnium carbide nanowire-toughened ceramic coating layer of surface of carbon/carbon composites and preparation method thereof |
| CN103964883A (en) * | 2014-04-25 | 2014-08-06 | 西北工业大学 | Preparation method for thin wall or tapered member made from one-dimensional nanofiber reinforced and toughened carbon-ceramic composite |
| CN104150938A (en) * | 2014-08-06 | 2014-11-19 | 西北工业大学 | Preparation method for one-dimensional HfC (hafnium carbide) modified carbon/carbon composite material |
-
2016
- 2016-12-02 CN CN201611093835.1A patent/CN106673710A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101563801A (en) * | 2005-11-21 | 2009-10-21 | 纳米***公司 | Nanowire structures comprising carbon |
| CN103951470A (en) * | 2014-04-04 | 2014-07-30 | 西北工业大学 | Hafnium carbide nanowire-toughened ceramic coating layer of surface of carbon/carbon composites and preparation method thereof |
| CN103964883A (en) * | 2014-04-25 | 2014-08-06 | 西北工业大学 | Preparation method for thin wall or tapered member made from one-dimensional nanofiber reinforced and toughened carbon-ceramic composite |
| CN104150938A (en) * | 2014-08-06 | 2014-11-19 | 西北工业大学 | Preparation method for one-dimensional HfC (hafnium carbide) modified carbon/carbon composite material |
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| CN108395279A (en) * | 2018-02-08 | 2018-08-14 | 西北工业大学 | The method that chemical gaseous phase co-electrodeposition method prepares HfC-SiC complex phase gradient coatings |
| CN111253171A (en) * | 2020-03-18 | 2020-06-09 | 西北工业大学 | Densification preparation method of fiber-reinforced hafnium carbide ceramic matrix composite material |
| CN111253171B (en) * | 2020-03-18 | 2022-05-03 | 西北工业大学 | Densification preparation method of fiber-reinforced hafnium carbide ceramic matrix composite material |
| CN115259900A (en) * | 2022-03-23 | 2022-11-01 | 西北工业大学 | Very long (Ta)xHf1-x) C ultra-high temperature ceramic solid solution nanowire and preparation method thereof |
| CN115259900B (en) * | 2022-03-23 | 2024-01-30 | 西北工业大学 | Extremely long (Ta x Hf 1-x ) C superhigh temperature ceramic solid solution nanowire and preparation method thereof |
| CN114853507A (en) * | 2022-07-06 | 2022-08-05 | 湖南泰坦未来科技有限公司 | Composite carbon material and preparation method and application thereof |
| CN115403397A (en) * | 2022-08-09 | 2022-11-29 | 西北工业大学 | Core-shell structure toughened (Hf, ta) C solid solution ultrahigh-temperature ceramic coating and one-step preparation method |
| CN115403397B (en) * | 2022-08-09 | 2023-10-24 | 西北工业大学 | Core-shell structure toughened (Hf, ta) C solid solution ultrahigh-temperature ceramic coating and one-step preparation method |
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