CN106242642B - Resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings of one kind and preparation method thereof - Google Patents

Resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings of one kind and preparation method thereof Download PDF

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CN106242642B
CN106242642B CN201610609599.8A CN201610609599A CN106242642B CN 106242642 B CN106242642 B CN 106242642B CN 201610609599 A CN201610609599 A CN 201610609599A CN 106242642 B CN106242642 B CN 106242642B
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low density
density carbon
oxidant
carbon watt
watt
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CN106242642A (en
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徐林
张大海
李兴超
宋永忠
樊桢
倪立勇
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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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
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • 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
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation

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  • Cutting Tools, Boring Holders, And Turrets (AREA)
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Abstract

The present invention relates to a kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof, belong to thermally protective materials technical field.The present invention, to high temperature resistant, lightweight and anti-heat insulating function integration thermally protective materials demand, proposes resistance to 1700 DEG C of low density carbons watt surface oxidation-resistant coating system of one kind and preparation method thereof for novel near space vehicle and Reusable Launch Vehicles thermal protection system.The coating is a kind of composite coating with gradient transition structure, includes: anti-oxidant transition zone, is formed by adulterating the antioxidant compositions such as Si, B, C, O in porous carbon fiber skeleton；Surface refractory anti oxidation layer, by fine and close M (M=Hf, Zr) B2‑MoSi2Superhigh temperature ceramics group is grouped as.

Description

Resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings of one kind and preparation method thereof
Technical field
The present invention relates to a kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof, belong to thermal protection Field of material technology.
Background technique
Thermally protective materials are the key that the designs of advanced thermal protection system and develop, either the weaponry of early stage still In Novel power system, reenters formula aircraft, space probe vehicle, near space vehicle, Reusable Launch Vehicles etc. and grind Key technology is listed in system, performance and reliability plays not associated power system and aircraft advance and reliability Alternative effect.With the development of novel near space vehicle and Reusable Launch Vehicles technology, aircraft nose cone, leading edge And large area regional area proposes high requirement to high temperature resistant, lightweight and anti-heat insulating function integration.
Existing thermally protective materials system is more, and the use that can satisfy different temperatures environment and different quality grade is wanted It asks, but is difficult to meet simultaneously high-temperature oxidation resistant and structure lightened.For example anti-oxidant C/C, C/SiC, UHTCs aoxidize ring for a long time It is more than 1650 DEG C that temperature is used under border, but is high density material, and density is all larger than 1.6g/cm3, heat-proof quality is poor；It is flexible Heat insulation felt density is in 0.1~0.2g/cm3, the use of temperature extremes is only 600 DEG C or so, higher temperature stability use is limited to Raw material property；Ceramic insulation watt density is in 0.2~0.4g/cm3, mature use temperature range is only 1200 DEG C, higher temperature Ceramic insulation watt technology not yet break through.
Low density carbon watt density is low, heat-proof quality is good, and has excellent thermal structure reliability, in integrated light weight There is preferable application potential in anti-heat-barrier material system, however start oxidation under 400 DEG C or more aerobic environments and limit extensively Using needing to solve the problems, such as that its is anti-oxidant.Early period proposes for this problem using the method brushed, crack and pre-oxidized Antioxidant coating is prepared on surface, improves low density carbon watt antioxygenic property.However, the antioxidant coating temperature resistant grade has Limit, 1500 DEG C or more, apparent oxidation ablation can occur for a long time.
Summary of the invention
Technology of the invention solves the problems, such as: overcome the deficiencies in the prior art, proposes a kind of resistance to 1700 DEG C of low density carbons watt Surface oxidation-resistant coating and preparation method thereof, the antioxidant coating enable to low density carbon watt to have excellent high temperature resistant antioxygen Change performance, and this method preparation process is simple, is adapted to small lot preparation.
The technical solution of the invention is as follows:
A kind of antioxidant coating for low density carbon watt, the antioxidant coating include the resistance to height of anti-oxidant transition zone and surface Warm anti oxidation layer；
Wherein, anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, wherein anti-oxidant subcoat is infusibility Metallic compound, the element of the refractory metal compound include Si and C, and the refractory metal compound enters low close Carbon watt inside is spent, the middle layer is consistent with the composition of anti-oxidant subcoat, and the middle layer is located at anti-oxidant basis Above coating and it also is located on the surface of low density carbon watt；The surface refractory anti oxidation layer is HfB2-MoSi2Or ZrB2-MoSi2；The surface refractory anti oxidation layer is located at intermediate layer.
The element of the refractory metal compound further includes Zr element.
The element of the refractory metal compound further includes B element.
The refractory metal compound enters the position to low density carbon watt top of the internal least significant end of low density carbon watt I.e. the position on low density carbon watt surface, content are incremented by successively.
The anti-oxidant transition zone with a thickness of 2~3mm, wherein anti-oxidant subcoat is with a thickness of 1.5~2.9mm, Intermediate layer thickness is 0.1~0.5mm；The surface refractory anti oxidation layer with a thickness of 100~300 μm.
A kind of the step of preparation method of the antioxidant coating for low density carbon watt, this method includes:
(1) brushing impregnation is carried out to low density carbon watt matrix using ceramic forerunner, is carried out after brushing every time primary Drying obtains the carbon watt material containing half fine and close anti-oxidant transition zone；
(2) Pintsch process is carried out to the carbon watt material that step (1) obtains, obtains the fine and close anti-oxidant transition of the state containing cracking half and applies The low density carbon watt material of layer；
(3) the fine and close anti-oxidant transition of the state containing cracking half that step (2) obtains is applied using the ceramic forerunner in step (1) The low density carbon watt material of layer carries out brushing impregnation, carries out first drying after brushing every time；
(4) Pintsch process is carried out to the product that step (3) obtain；
(5) step (3)-(4) are repeated 1-2 times, obtains the low density carbon watt material containing fine and close anti-oxidant tie coat；
(6) by HfB2Powder and MoSi2Powder either ZrB2Powder and MoSi2Powder carries out at ball milling-spray drying Reason obtains HfB2-MoSi2Mixed powder either ZrB2-MoSi2Mixed powder；
(7) mixed powder that step (6) obtain is contained using what vacuum plasma spray coating method was sprayed on that step (5) obtains The low density carbon watt material surface of fine and close anti-oxidant tie coat, obtains the low density carbon watt containing antioxidant coating.
In the step (1), ceramic forerunner is at least ceramic forerunner containing Si and C.
The ceramic forerunner is Si-C, Si-B-C, Zr-Si-C or Zr-Si-B-C.
The technique of the brushing processing are as follows: ceramic forerunner is dipped to low density carbon watt all outer surfaces using banister brush Brushing processing is carried out, presoma is sucked into material internal through capillary action, by brushing number, presoma viscosity controls transition Profile depth；The drying and processing technique are as follows: temperature is 250~300 DEG C, keeps the temperature 2~3h；The Pintsch process handles work Skill are as follows: 1000~1300 DEG C, keep the temperature 1~3h.
The HfB2Powder, MoSi2Powder, ZrB2The partial size of powder is 20~40 μm, the HfB2Powder with MoSi2The volume ratio of powder is 9:1~7:3, the ZrB2Powder and MoSi2The volume ratio of powder is 9:1~7:3.
Beneficial effect
(1) the invention proposes a kind of novel gradient antioxidant coating and preparation method thereof, low density carbon is further promoted Temperature resistant grade under watt material aerobic environment, provides material base for aircraft nose cone, leading edge and large area localized high temperature regions Plinth and technical support；
(2) present invention is for novel near space vehicle and Reusable Launch Vehicles thermal protection system to high temperature resistant, light Quantization and anti-heat insulating function integration thermally protective materials demand propose a kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistants painting Coating systems and preparation method thereof.The coating is a kind of composite coating with gradient transition structure, includes: anti-oxidant transition zone, It is formed by adulterating the antioxidant compositions such as Si, B, C, O in porous carbon fiber skeleton；Surface refractory anti oxidation layer, by fine and close M (M =Hf, Zr) B2-MoSi2Superhigh temperature ceramics group is grouped as.
(3) anti-oxidant transition zone of the invention includes anti-oxidant subcoat and middle layer, the refractory metal chemical combination The element composition of object includes at least Si and C, can also include Zr or B.On the one hand low density carbon can be improved in anti-oxidant transition zone On the other hand the linear expansion coefficient of low density carbon watt can be improved by introducing the anti-oxidant constituent element of ceramics in watt layer antioxygenic property, Improve the thermal matching energy of low density carbon watt and anti-oxidant subcoat；
(4) surface refractory anti oxidation layer of the invention is HfB2-MoSi2Or ZrB2-MoSi2, structure even compact, thickness 100~300 μm of degree, mainly plays high temperature resistant and antioxidant effect under Service Environment；
(5) preparation process of the invention is simple, the period is short, strong operability, is suitable for mass and stablizes preparation.
Detailed description of the invention
The surface graded tie coat schematic diagram of Fig. 1 low density carbon watt；
The surface graded tie coat macro morphology photo of Fig. 2 low density carbon watt；
The surface graded tie coat microscopic appearance photo of Fig. 3 low density carbon watt.
Specific embodiment
A kind of resistance to 1700 DEG C of antioxidant coatings on low density carbon watt surface, including anti-oxidant transition zone and surface refractory resist Oxide layer.Wherein, anti-oxidant transition zone is the mixing function for adulterating the components such as Si, B, C, O in porous carbon fiber skeleton and being formed Ergosphere, with a thickness of 2~3mm, the main effect for playing two aspects: first is that subsurface carbon watt layer antioxygenic property is improved, second is that Linear expansion coefficient is improved by introducing the anti-oxidant constituent element of ceramics, improves the thermal matching with surface compact fire-resistant oxidation resistant layer Energy；Surface refractory anti oxidation layer is M (M=Hf, Zr) B2-MoSi2, structure even compact 100~300 μm of thickness, mainly exists High temperature resistant and antioxidant effect are played under Service Environment；
A kind of resistance to 1700 DEG C of low density carbons watt surface oxidation-resistant coating preparation method, specific steps are as follows:
1) according to different thermal protection product shape features and size, low density carbon watt is processed, guarantees machining accuracy, Obtain low density carbon watt basis material；
2) brushing dipping is carried out to the low density carbon watt basis material that step 1) obtains using Si, B, C, O ceramic forerunner Processing 2~4 times carries out first drying after brushing every time, drying and processing temperature is 250~300 DEG C, keeps the temperature 2~3h；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, cracking treatment temperature is 1000~1300 DEG C, is protected 1~3h of temperature is every time handled specimen surface after cracking, and removal surface cracks generated soft combination powder granule；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat；
5) select average grain diameter for 20~40 μm of HfB2Or ZrB2、MoSi2Powder, the volume ratios of two kinds of powders be 9:1~ 7:3 obtains M (M=Hf, Zr) B through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, finally obtains the low density carbon watt material used under resistance to 1700 DEG C of aerobic environments Expect exemplar.
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, including anti-oxidant transition zone and surface refractory antioxygen Change layer；
Wherein, anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, wherein anti-oxidant subcoat is infusibility Metallic compound, the content of refractory metal compound is by the position of the lowermost end certain distance apart from low density carbon watt to low-density The position on carbon watt top is incremented by successively；The element composition of the refractory metal compound includes at least Si and C, can also include Zr or B；
The middle layer is consistent with the composition of anti-oxidant subcoat, the described oxidation subcoat and middle layer it is total With a thickness of 2~3mm, wherein anti-oxidant subcoat, with a thickness of 1.5~2.9mm, intermediate layer thickness is 0.1~0.5mm；
Anti-oxidant transition zone mainly plays the effect of two aspects: first is that low density carbon watt layer antioxygenic property is improved, two It is the linear expansion coefficient for improving low density carbon watt by introducing the anti-oxidant constituent element of ceramics, improves low density carbon watt and anti-oxidant basis The thermal matching energy of coating；
The surface refractory anti oxidation layer is M (M=Hf, Zr) B2-MoSi2, structure even compact, thickness 100~ 300 μm, high temperature resistant and antioxidant effect mainly are played under Service Environment.
A kind of preparation method of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, mainly including anti-oxidant transition zone The preparation method of preparation method and surface refractory anti oxidation layer.Wherein, anti-oxidant transition zone is with Si-C, Si-B-C, Zr- The ceramic forerunners such as Si-C or Zr-Si-B-C are carrier, are prepared by brushing dipping, drying, cracking technology；Surface is resistance to High-temperature oxidation resistant layer is to be prepared on anti-oxidant transition zone surface foundation by vacuum plasma spray coating technique, final to obtain The low density carbon watt material of the gradient coating containing fire-resistant oxidation resistant.The specific steps of this method are as follows:
1) according to different thermal protection product shape features and size, low density carbon watt is processed, guarantees machining accuracy, Obtain low density carbon watt basis material；
2) the low density carbon watt basis material that step 1) obtains is carried out using ceramic forerunner brushing impregnation 2~4 It is secondary, first drying is carried out after brushing every time, obtains the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the sample that step 2) obtains, obtains the low of the fine and close anti-oxidant tie coat of the state containing cracking half Density carbon watt material；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat；
5) by M (M=Hf, Zr) B2、MoSi2Powder carries out ball milling-spray drying treatment, obtains M (M=Hf, Zr) B2- MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the specimen material obtained using vacuum plasma spray coating method in step 4) The preparation that surface refractory anti oxidation layer is completed on surface, finally obtains the low density carbon watt used under resistance to 1700 DEG C of aerobic environments Material exemplar.
Above-mentioned steps 2) in, the ceramic forerunners such as Si-C, Si-B-C, Zr-Si-C, Zr-Si-B-C are liquid at room temperature, tool There is certain fluidity, there is preferable wellability with carbon fiber；
Above-mentioned steps 2) in, it is all to low density carbon watt outer to dip ceramic forerunner using banister brush to brush impregnation technology Surface carries out brushing processing, and presoma is sucked material internal through capillary action, and by brushing number, presoma viscosity controls Tie coat depth；
Above-mentioned steps 2) in, drying and processing temperature is 250~300 DEG C, keeps the temperature 2~3h；
Above-mentioned steps 3) in, cracking treatment temperature is 1000~1300 DEG C, 1~3h is kept the temperature, every time to sample after cracking Surface is handled, and removal surface cracks generated soft combination powder granule；
Above-mentioned steps 5) in, M (M=Hf, Zr) B2、MoSi2Powder diameter is 20~40 μm, M (M=Hf, Zr) B2With MoSi2Volume ratio is 9:1~7:3.
The gradient coatings with superior oxidation resistance energy can be prepared on low density carbon watt surface by the above method, The anti-oxidant transition zone and 100~300 μ formed comprising adulterating the components such as Si, B, C, O in 2~3mm thickness porous carbon fiber skeleton M thickness M (M=Hf, Zr) B2-MoSi2Surface refractory anti oxidation layer.Obtained low density carbon watt surface oxidation-resistant coating combine compared with It is good, there is preferable lightweight, high temperature resistant, antioxygenic property.
Below with reference to embodiment, the invention will be further described.But the contents of the present invention are not only confined to following Embodiment:
Embodiment 1
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.1~2.5mm, and the element composition of refractory metal compound includes Si and C；The member of the middle layer Element group becomes Si and C, and the surface refractory anti oxidation layer is HfB2-MoSi2, with a thickness of 210~260 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.20~ 0.22g/cm3；
2) brushing leaching is carried out to all faces of low density carbon watt basis material that step 1) obtains using Si-C ceramic forerunner Stain is handled 2~4 times, and sample is put into convection oven after brushing every time and is thermally dried, and 250 DEG C of drying temperature, is kept the temperature 2h, is obtained To the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the sample that step 2) obtains, treatment temperature is 1300 DEG C, and it is fine and close to obtain the state containing cracking half The low density carbon watt material of anti-oxidant tie coat, it is 0.46~0.48g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.68~0.71g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of HfB2And MoSi2Ceramic powders are raw material, are 7:3 according to the two volume ratio It is weighed, then obtains HfB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.85~0.88g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.1~2.5mm Change transition zone and 210~260 μm of surface refractory anti oxidation layer, antioxidant coating photomacrograph and cross-section morphology are as schemed Shown in 2 and Fig. 3.Cylindrical body exemplar after preparation has passed through the lower 1650 DEG C/60s of atmospheric environment, 1720 DEG C/60s plasma torch Experiment examination, overall structure is intact after test, and appearance does not have significant change, and line ablation amount is zero, and quality is increased slightly, weight gain speed Rate is 3.2~3.8 × 10-6g/cm2s。
Embodiment 2
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.0~2.7mm, and the element composition of refractory metal compound includes Si, B, C；The middle layer Element group becomes Si, B, C, and the surface refractory anti oxidation layer is ZrB2-MoSi2, with a thickness of 160~220 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.20~ 0.22g/cm3；
2) all faces of low density carbon watt basis material that step 1) obtains are brushed using Si, B, C ceramic forerunner Impregnation 2~4 time, sample is put into convection oven after brushing every time and is thermally dried, 250 DEG C of drying temperature, keeps the temperature 2h, Obtain the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, treatment temperature is 1300 DEG C, obtains the state containing cracking The low density carbon watt material of half fine and close anti-oxidant tie coat, it is 0.45~0.49g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.65~0.70g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of ZrB2And MoSi2Ceramic powders are raw material, are 4:1 according to the two volume ratio It is weighed, then obtains ZrB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.87~0.90g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.0~2.7mm Change transition zone and 160~220 μm of surface refractory anti oxidation layer.Cylindrical body exemplar after preparation has passed through under atmospheric environment 1700 DEG C, 300s plasma torch experiment examination, overall structure is intact after test, and appearance does not have significant change, and line ablation amount is Zero, quality is increased slightly, and rate of gain is 2.7~3.3 × 10-6g/cm2s。
Embodiment 3
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.1~2.5mm, and the element composition of refractory metal compound includes Zr, Si, C；The middle layer Element group becomes Zr, Si, C, and the surface refractory anti oxidation layer is ZrB2-MoSi2, with a thickness of 150~220 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.20~ 0.22g/cm3；
2) all faces of low density carbon watt basis material that step 1) obtains are brushed using Zr, Si, C ceramic forerunner Impregnation 2~4 time, sample is put into convection oven after brushing every time and is thermally dried, 270 DEG C of drying temperature, keeps the temperature 2h, Obtain the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, treatment temperature is 1500 DEG C, obtains the state containing cracking The low density carbon watt material of half fine and close anti-oxidant tie coat, it is 0.46~0.50g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.65~0.72g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of ZrB2And MoSi2Ceramic powders are raw material, are 4:1 according to the two volume ratio It is weighed, then obtains ZrB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.88~0.91g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.1~2.5mm Change transition zone and 150~220 μm of surface refractory anti oxidation layer.
Embodiment 4
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.2~2.8mm, and the element composition of refractory metal compound includes Zr, Si, B, C；The middle layer Element group become Zr, Si, B, C, the surface refractory anti oxidation layer be ZrB2-MoSi2, with a thickness of 150~210 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.20~ 0.22g/cm3；
2) all faces of low density carbon watt basis material that step 1) obtains are brushed using Zr, Si, B ceramic forerunner Impregnation 2~4 time, sample is put into convection oven after brushing every time and is thermally dried, 270 DEG C of drying temperature, keeps the temperature 2h, Obtain the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, treatment temperature is 1500 DEG C, obtains the state containing cracking The low density carbon watt material of half fine and close anti-oxidant tie coat, it is 0.45~0.49g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.63~0.71g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of ZrB2And MoSi2Ceramic powders are raw material, are 4:1 according to the two volume ratio It is weighed, then obtains ZrB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.87~0.90g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.2~2.8mm Change transition zone and 150~210 μm of surface refractory anti oxidation layer.
Embodiment 5
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.1~2.5mm, and the element composition of refractory metal compound includes Si, C；The member of the middle layer Element group becomes Si, C, and the surface refractory anti oxidation layer is ZrB2-MoSi2, with a thickness of 210~260 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.20~ 0.22g/cm3；
2) brushing leaching is carried out to all faces of low density carbon watt basis material that step 1) obtains using Si-C ceramic forerunner Stain is handled 2~4 times, and sample is put into convection oven after brushing every time and is thermally dried, and 250 DEG C of drying temperature, is kept the temperature 2h, is obtained To the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, treatment temperature is 1300 DEG C, obtains the state containing cracking The low density carbon watt material of half fine and close anti-oxidant tie coat, it is 0.46~0.49g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.67~0.70g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of ZrB2And MoSi2Ceramic powders are raw material, are 7:3 according to the two volume ratio It is weighed, then obtains ZrB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.85~0.88g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.1~2.5mm Change transition zone and 210~260 μm of surface refractory anti oxidation layer.
Embodiment 6
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.0~2.6mm, and the element composition of refractory metal compound includes Si, B, C；The middle layer Element group becomes Si, B, C, and the surface refractory anti oxidation layer is HfB2-MoSi2, with a thickness of 150~230 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.21~ 0.22g/cm3；
2) all faces of low density carbon watt basis material that step 1) obtains are brushed using Si, B, C ceramic forerunner Impregnation 2~4 time, sample is put into convection oven after brushing every time and is thermally dried, 250 DEG C of drying temperature, keeps the temperature 2h, Obtain the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, treatment temperature is 1300 DEG C, obtains the state containing cracking The low density carbon watt material of half fine and close anti-oxidant tie coat, it is 0.45~0.49g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.66~0.70g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of HfB2And MoSi2Ceramic powders are raw material, are 4:1 according to the two volume ratio It is weighed, then obtains HfB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.88~0.91g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.0~2.6mm Change transition zone and 150~230 μm of surface refractory anti oxidation layer.
Embodiment 7
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.1~2.8mm, and the element composition of refractory metal compound includes Zr, Si, C；The middle layer Element group becomes Zr, Si, C, and the surface refractory anti oxidation layer is HfB2-MoSi2, with a thickness of 150~200 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Wherein, anti-oxidant subcoat is refractory metal compound, the element group of refractory metal compound become Zr, Si, C；The element group of the middle layer becomes Zr, Si, C.The surface refractory anti oxidation layer is HfB2-MoSi2。
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.21~ 0.22g/cm3；
2) all faces of low density carbon watt basis material that step 1) obtains are brushed using Zr, Si, C ceramic forerunner Impregnation 2~4 time, sample is put into convection oven after brushing every time and is thermally dried, 270 DEG C of drying temperature, keeps the temperature 2h, Obtain the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, treatment temperature is 1500 DEG C, obtains the state containing cracking The low density carbon watt material of half fine and close anti-oxidant tie coat, it is 0.45~0.52g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.66~0.72g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of HfB2And MoSi2Ceramic powders are raw material, are 4:1 according to the two volume ratio It is weighed, then obtains HfB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.89~0.92g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.1~2.8mm Change transition zone and 150~200 μm of surface refractory anti oxidation layer.
Embodiment 8
A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings, which includes anti-oxidant transition zone and table Face fire-resistant oxidation resistant layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, as shown in Figure 1；It is wherein anti-oxidant Subcoat is refractory metal compound, and the refractory metal compound enters the position of the internal least significant end of low density carbon watt To low density carbon watt top, that is, low density carbon watt surface position, content is incremented by successively；The anti-oxidant subcoat and The overall thickness of middle layer is 2.1~3.0mm, and the element composition of refractory metal compound includes Zr, Si, B, C；The middle layer Element group become Zr, Si, B, C, the surface refractory anti oxidation layer be HfB2-MoSi2, with a thickness of 150~205 μm；
For Φ 25mm size cylinder exemplar, designs and be prepared for a kind of anti-oxidant painting of low density carbon watt surface refractory Layer, the coating are a kind of composite coatings with gradient transition structure, including anti-oxidant transition zone and surface refractory it is anti-oxidant Layer；Anti-oxidant transition zone includes anti-oxidant subcoat and middle layer.
Specific preparation step are as follows:
1) low density carbon watt is processed according to drawing requirement, guarantees machining accuracy, obtain having a size of Φ 25mm × The low density carbon watt cylindrical body exemplar of 40mm, quality is weighed after processing and be calculated low density carbon watt density be 0.20~ 0.22g/cm3；
2) all faces of low density carbon watt basis material that step 1) obtains are brushed using Zr, Si, B ceramic forerunner Impregnation 2~4 time, sample is put into convection oven after brushing every time and is thermally dried, 270 DEG C of drying temperature, keeps the temperature 2h, Obtain the carbon watt material containing half fine and close anti-oxidant transition zone；
3) Pintsch process is carried out to the intermediate state sample that step 2) obtains, treatment temperature is 1500 DEG C, obtains the state containing cracking The low density carbon watt material of half fine and close anti-oxidant tie coat, it is 0.46~0.49g/cm that cylinder density, which increases, after processing3；
4) step 2)~3 are repeated) 1~2 time, obtain the low density carbon watt material containing fine and close anti-oxidant tie coat, processing It is 0.64~0.72g/cm that cylindrical body exemplar density, which increases, afterwards3；
5) select average grain diameter for 20~40 μm of HfB2And MoSi2Ceramic powders are raw material, are 4:1 according to the two volume ratio It is weighed, then obtains HfB through ball milling-spray drying2-MoSi2Mixed powder；
6) mixed powder that step 5) is obtained, the meso sample obtained using vacuum plasma spray coating method in step 4) The preparation of surface refractory anti oxidation layer is completed on material, it is 0.88~0.90g/cm that cylindrical body exemplar density, which increases, after preparation3, most The low density carbon watt material exemplar used under resistance to 1700 DEG C of aerobic environments is obtained afterwards.
Low density carbon watt surface refractory antioxidant coating by above method development includes the antioxygen of 2.1~3.0mm Change transition zone and 190~280 μm of surface refractory anti oxidation layer.

Claims (9)

1. a kind of antioxidant coating for low density carbon watt, it is characterised in that: the antioxidant coating includes anti-oxidant transition zone With surface refractory anti oxidation layer；
Wherein, anti-oxidant transition zone includes anti-oxidant subcoat and middle layer, wherein anti-oxidant subcoat is refractory metal Compound, the element of the refractory metal compound include Si and C, and the refractory metal compound enters low density carbon Watt inside, the middle layer is consistent with the composition of anti-oxidant subcoat, and the middle layer is located at anti-oxidant subcoat Above and it also is located on the surface of low density carbon watt；The surface refractory anti oxidation layer is HfB2-MoSi2Or ZrB2- MoSi2；The surface refractory anti oxidation layer is located at intermediate layer；
The preparation method of the antioxidant coating, step include:
(1) brushing impregnation is carried out to low density carbon watt matrix using ceramic forerunner, carries out first drying after brushing every time, Obtain the carbon watt material containing half fine and close anti-oxidant transition zone；
(2) Pintsch process is carried out to the carbon watt material that step (1) obtains, obtains the fine and close anti-oxidant tie coat of the state containing cracking half Low density carbon watt material；
(3) step (2) is obtained using the ceramic forerunner in step (1) the fine and close anti-oxidant tie coat of the state containing cracking half Low density carbon watt material carries out brushing impregnation, carries out first drying after brushing every time；
(4) Pintsch process is carried out to the product that step (3) obtain；
(5) step (3)-(4) are repeated 1-2 times, obtains the low density carbon watt material containing fine and close anti-oxidant tie coat；
(6) by HfB2Powder and MoSi2Powder either ZrB2Powder and MoSi2Powder carries out ball milling-spray drying treatment, obtains HfB2-MoSi2Mixed powder either ZrB2-MoSi2Mixed powder；
(7) by mixed powder that step (6) obtain using vacuum plasma spray coating method be sprayed on that step (5) obtains containing densification The low density carbon watt material surface of anti-oxidant tie coat, obtains the low density carbon watt containing antioxidant coating.
2. a kind of antioxidant coating for low density carbon watt according to claim 1, it is characterised in that: the infusibility The element of metallic compound further includes Zr element.
3. a kind of antioxidant coating for low density carbon watt according to claim 1 or 2, it is characterised in that: described The element of refractory metal compound further includes B element.
4. a kind of antioxidant coating for low density carbon watt according to claim 1, it is characterised in that: the infusibility Metallic compound enters the position to the i.e. low density carbon watt surface in low density carbon watt top of the internal least significant end of low density carbon watt Position, content are incremented by successively.
5. a kind of antioxidant coating for low density carbon watt according to claim 1, it is characterised in that: the antioxygen Change transition zone with a thickness of 2~3mm, wherein anti-oxidant subcoat is with a thickness of 1.5~2.9mm, intermediate layer thickness is 0.1~ 0.5mm；The surface refractory anti oxidation layer with a thickness of 100~300 μm.
6. a kind of antioxidant coating for low density carbon watt according to claim 1, it is characterised in that: the step (1) in, ceramic forerunner is at least ceramic forerunner containing Si and C.
7. a kind of antioxidant coating for low density carbon watt according to claim 1, it is characterised in that: the ceramics Presoma is Si-C, Si-B-C, Zr-Si-C or Zr-Si-B-C.
8. a kind of antioxidant coating for low density carbon watt according to claim 1, it is characterised in that: the brushing The technique of processing are as follows: ceramic forerunner is dipped using banister brush, brushing processing is carried out to low density carbon watt all outer surfaces, passed through Presoma is sucked material internal by capillarity, and by brushing number, presoma viscosity controls tie coat depth；The baking Dry process are as follows: temperature is 250~300 DEG C, keeps the temperature 2~3h；The Pintsch process treatment process are as follows: 1000~1300 DEG C, keep the temperature 1~3h.
9. a kind of antioxidant coating for low density carbon watt according to claim 1, it is characterised in that: the HfB2 Powder, MoSi2Powder, ZrB2The partial size of powder is 20~40 μm, the HfB2Powder and MoSi2The volume ratio of powder is 9:1~7:3, the ZrB2Powder and MoSi2The volume ratio of powder is 9:1~7:3.
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