CN102276279B - Preparation method of silicon carbide fiber reinforced silicon carbide composite material - Google Patents
Preparation method of silicon carbide fiber reinforced silicon carbide composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a silicon carbide fiber reinforced silicon carbide composite material. The preparation method comprises the following steps of preparing a SiC fiber knitted piece, placing the SiC fiber knitted piece into a vacuum furnace to carry out chemical vapor deposition through adopting methane or propylene as feed gas and a pressure difference method to deposit a carbon coating on the surface of the SiC fiber knitted piece, carrying out a vacuum impregnation process on the SiC fiber knitted piece deposited with the carbon coating through adopting a liquid SiC ceramic precursor as impregnation liquid, putting the impregnated SiC fiber knitted piece into a mold, carrying out thermal molding crosslinking in a dynamic nitrogen atmosphere, putting the crosslinked SiC fiber knitted piece into a cracking furnace to carry out high temperature cracking in a dynamic nitrogen atmosphere, repeating a vacuum impregnation-thermal molding crosslinking-high temperature cracking cycle so as to finish preparation until the weight increment of a sample obtained after the vacuum impregnation-thermal molding crosslinking-high temperature cracking cycle is less than 1% of the weight increment of the sample obtained after the previous cycle. The preparation method has the advantages of short period, low cost, low pollution and toxic effects, etc.
Description
Technical field
The present invention relates to the carborundum based material field, relate in particular to a kind of preparation method of silicon carbide fiber reinforced silicon carbide composite material.
Background technology
Along with the development of human scientific and technological level, the performance that how further to improve structured material becomes the important breakthrough mouth of accelerating to advance scientific-technical progress gradually.The deadly defects such as the SiC stupalith is large because of fragility, poor reliability have seriously hindered it as the practicalization of structured material.Silicon carbide fiber reinforced silicon carbide (SiC
f/ SiC) matrix material adds the SiC fiber and prepares as second-phase in the SiC stupalith, and it can be in breaking-down process the machine-processed absorbed energy, the intensity of strongthener and toughness such as extracts by crack deflection, fibre breakage and fiber.SiC
fThermal expansion matching between the fiber of/SiC matrix material and matrix, thermal stresses are little, have high specific strength, high ratio modulus, high rigidity, wear-resistant, anti-oxidant, anticorrosive, high-temperature thermal stability is good, thermal conductivity is high, thermal expansivity is little, induce the active excellent properties such as low of radiation, has become the optimal high-temperature structural materials of new generation in field such as aerospace and nuclear power.Such as SiC
f/ SiC matrix material is as the structure unit of aerospace engine, because the advantage of the aspect such as its density is little, intensity is high and can work under ultra high temp, can significantly improve the thrust-weight ratio of engine; SiC
f/ SiC matrix material then embodies the advantages such as its radiation hardness, good stability, safe reliability height, easy care as the heap wall material of atomic reactor.Therefore, for SiC
fThe exploration of/SiC matrix material becomes the forward position of Modern High-Tech's ceramic research and exploitation gradually, and the great attention that is subject to countries in the world also acquires a great achievement.
Existing SiC
f/ SiC composite manufacture technique mainly contains: the combination of precursor infiltration and pyrolysis (PIP) technique, chemical vapor infiltration (CVI) technique, nanometer dipping and instantaneous eutectic phase (NITE) technique, hot pressing (HP) technique and reaction sintering (RS) technique and aforementioned several techniques.Wherein, PIP technique and CVI technique have become current SiC
fTwo large main flow techniques of/SiC matrix material preparation.The SiC of CVI technique preparation
f/ SiC matrix material β-SiC purity and degree of crystallinity are high, have good Radiation hardness, but this SiC
fThere is 10%～15% void content in/SiC matrix material, has reduced mechanical property and the antioxidant property of material, and SiC matrix densification rate is low simultaneously, and preparation cycle is longer, and cost is high.The advantages such as compare with CVI technique, it is simple that PIP technique has technique, and cost is low, can prepare large-scale and complex-shaped composite element, and material composition and structure are controlled.Yet the ceramic yield of current ceramic precursor still can not be satisfactory, has a large amount of small molecules to overflow in the cracking process and cause the material porosity higher, and easily form closed pore; Organic precursor method variable density in being converted into the cracking process of inorganic ceramic is large in addition, and volumetric shrinkage is large, directly causes material internal to produce internal stress, and then brings out the generation of tiny crack, is unfavorable for the raising of material property and stable.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that exists for prior art, provides a kind of with chemical vapor deposition (CVD) technique with the preparation method of the silicon carbide fiber reinforced silicon carbide composite material that precursor infiltration and pyrolysis technique combines and preparation cycle is short, cost is low, pollution and toxic action are little.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of preparation method of silicon carbide fiber reinforced silicon carbide composite material is characterized in that, may further comprise the steps:
(1) material is prepared: prepare the SiC fiber braid take the SiC fiber as raw material, and prepare liquid Si C ceramic precursor (LPVCS);
(2) deposit carbon coating: take methane or propylene as unstripped gas, described SiC fiber braid placed adopt pressure differential method to carry out chemical vapour deposition in the vacuum oven, at described SiC fiber braid surface deposition carbon coating;
(3) vacuum impregnation: take described liquid Si C ceramic precursor as steeping fluid, the above-mentioned SiC fiber braid that has deposited carbon coating of vacuum impregnation;
(4) hot moulding is crosslinked: with the mould of packing into of the SiC fiber braid after the above-mentioned vacuum impregnation, it is crosslinked to carry out hot moulding under flowing nitrogen atmosphere;
(5) Pintsch process: the SiC fiber braid after hot moulding is crosslinked is put into pyrolyzer, carries out Pintsch process under flowing nitrogen atmosphere;
Vacuum impregnation-the hot moulding of repeating step (3)～step (5) is crosslinked-the Pintsch process cycle, until sample increases weight less than 1% when this cycle, the sample weightening finish go up end cycle when finishing, finish preparation, and obtain silicon carbide fiber reinforced silicon carbide composite material.
As a further improvement on the present invention:
Among the above-mentioned preparation method, described liquid Si C ceramic precursor preferably contains Si-H and reaches-CH=CH
2Group.
Among the above-mentioned preparation method, the condition optimization of described chemical vapour deposition is: raw gas flow is 0.01 m
3H
-1～0.20m
3H
-1Carrier gas is hydrogen or nitrogen, and the carrier gas atmosphere pressures is 100 Pa～2000Pa, and carrier gas flux is 0.01 m
3H
-1～0.20m
3H
-1Depositing temperature is 800 ℃～1500 ℃, depositing time 1 h～40h.
Among the above-mentioned preparation method, the crosslinked concrete technology parameter of described hot-die is preferably: will be through the SiC fiber braid molding die of packing into of dipping, under flowing nitrogen atmosphere, temperature rise rate with 1 ℃/min～10 ℃/min is warming up to 100 ℃～300 ℃, insulation 0h～5h, continue to be warming up to 200 ℃ ~ 500 ℃ of crosslinking temperatures, insulation 0h～5h keeps molding pressure≤40MPa in intensification and the insulating process.
Among the above-mentioned preparation method, described Pintsch process concrete technology parameter is preferably: will put into pyrolyzer through crosslinked SiC fiber braid, under flowing nitrogen atmosphere, be warming up to 800 ℃～1500 ℃ of cracking temperatures, insulation 1h～10h with the temperature rise rate of 1 ℃/min～50 ℃/min.
Among the above-mentioned preparation method, described vacuum impregnation-hot moulding is crosslinked-and the multiplicity in Pintsch process cycle is preferably 10～20 times.
Compared with prior art, the invention has the advantages that:
1, the preparation method of silicon carbide fiber reinforced silicon carbide composite material of the present invention, by CVD technique in SiC fiber surface deposit carbon coating, not only improve the bonding strength between fiber and the matrix, and in the Pintsch process process, effectively protected the SiC fiber to avoid destroying; So SiC of the present invention's preparation
f/ SiC matrix material is than the SiC of traditional technology preparation
f/ SiC matrix material has better room-temperature mechanical property, as: its room temperature flexural strength can reach more than the 600MPa, and fracture toughness property can reach 30MPa * m
1/2About.
2, the preparation method of silicon carbide fiber reinforced silicon carbide composite material of the present invention has adopted mould pressing process, and it can improve the volume fraction of material internal SiC fiber, effectively avoids SiC in preparation process
f/ SiC composite inner produces the hole defective.Therefore, the SiC for preparing of the present invention
f/ SiC matrix material density is higher, and density is at 2.10g/cm
3More than; And porosity is about 6%.
3, among the preparation method of silicon carbide fiber reinforced silicon carbide composite material of the present invention, the Polycarbosilane (PCS) that the market value of the LPVCS that adopts is used far below traditional technology, and the fracture quality retention rate is higher, therefore can shorten the composite manufacture cycle, reduce cost.Simultaneously, LPVCS need not the noxious solvents such as xylol when using, also can not produce poisonous and harmful or inflammable and explosive material in the preparation process, and therefore preparation method of the present invention is safe and reliable, pollution-free.
Description of drawings
Fig. 1 is the SiC that the specific embodiment of the invention 1 prepares
fThe fracture apperance electromicroscopic photograph of/SiC matrix material; Wherein Fig. 1 (A) is the SiC behind the magnify 20
fThe fracture apperance electromicroscopic photograph of/SiC matrix material; Fig. 1 (B) is the SiC after amplifying 200 times
fThe fracture apperance electromicroscopic photograph of/SiC matrix material;
Fig. 2 is the SiC that the specific embodiment of the invention 2 prepares
fThe fracture apperance electromicroscopic photograph of/SiC matrix material; Wherein Fig. 2 (A) is the SiC after amplifying 4500 times
fThe fracture apperance electromicroscopic photograph of/SiC matrix material; Fig. 2 (B) is the SiC after amplifying 5000 times
fThe fracture apperance electromicroscopic photograph of/SiC matrix material.
Embodiment
Below with reference to Figure of description and specific embodiment the present invention is described in further details.
Embodiment 1:
The preparation method of a kind of silicon carbide fiber reinforced silicon carbide composite material of the present invention may further comprise the steps:
(1) material is prepared:
A. take the SiC fiber as raw material, adopt three-dimensional four-way weaving to prepare the SiC fiber braid;
B. preparing to contain Si-H reaches-CH=CH
2The liquid Si C ceramic precursor (LPVCS) of group.
(2) deposit carbon coating: take methane or propylene as unstripped gas, the SiC fiber braid placed adopt pressure differential method to carry out chemical vapour deposition in the vacuum oven, at SiC fiber braid surface deposition carbon coating.The processing condition of chemical vapour deposition are: carbon source is propylene, flow 0.01m
3H
-1Carrier gas is hydrogen, flow 0.10m
3H
-1, atmosphere pressures is 500Pa; 1300 ℃ of depositing temperatures, depositing time 10h.
(3) vacuum impregnation: take the LPVCS for preparing as steeping fluid, the above-mentioned SiC fiber braid that has deposited carbon coating of vacuum impregnation.
(4) hot moulding is crosslinked: will be through the SiC fiber braid molding die of packing into of dipping, place in the multi-functional hot pressing furnace, under flowing nitrogen atmosphere, temperature rise rate with 10 ℃/min is warming up to 200 ℃, insulation 2h continues to be warming up to 400 ℃ of crosslinking temperatures, insulation 2h, keep molding pressure 30MPa in intensification and the insulating process, it is crosslinked to carry out hot moulding.
(5) Pintsch process: will put into pyrolyzer through crosslinked SiC fiber braid, and under flowing nitrogen atmosphere, be warming up to 1300 ℃ of cracking temperatures with the temperature rise rate of 20 ℃/min, insulation 2h carries out Pintsch process.
The dipping of repeating step (3)～step (5)-crosslinked-lytic cycle 13 times until sample increases weight less than 1% when this cycle, the sample weightening finish go up end cycle when finishing, is finished preparation, obtains SiC
f/ SiC matrix material.
Performance test:
Test SiC obtained above
fThe density of/SiC matrix material and mechanical property, can get its porosity is 6.25%, density is 2.11g/cm
3, flexural strength is 619Mpa, fracture toughness property is 29.13MPa * m
1/2
With SiC obtained above
f/ SiC matrix material carries out the electron-microscope scanning test, obtains fracture apperance electromicroscopic photograph as shown in Figure 1.Can find out that from Fig. 1 (A) fracture of matrix material is uneven, have a large amount of fibers to extract, and the length of extracting be longer, show obvious ductile rupture characteristic; From Fig. 1 (B), can find out, fiber is extracted from matrix under extraneous load effect, and very tight because of interface combination between fiber and the matrix when extracting, it is cracked that huge frictional force causes matrix to be pullled, consume simultaneously the energy of extraneous load, thereby reached raising SiC
fThe purpose of/SiC matrix material flexural strength and fracture toughness property.
Embodiment 2:
The preparation method of a kind of silicon carbide fiber reinforced silicon carbide composite material of the present invention may further comprise the steps:
(1) material is prepared:
A. take the SiC fiber as raw material, adopt three-dimensional four-way weaving to prepare the SiC fiber braid;
B. preparing to contain Si-H reaches-CH=CH
2The liquid Si C ceramic precursor (LPVCS) of group.
(2) deposit carbon coating: take methane or propylene as unstripped gas, the SiC fiber braid placed adopt pressure differential method to carry out chemical vapour deposition in the vacuum oven, at SiC fiber braid surface deposition carbon coating.The processing condition of chemical vapour deposition are: carbon source is propylene, flow 0.05m
3H
-1Carrier gas is hydrogen, flow 0.20m
3H
-1, atmosphere pressures is 1500Pa; 1200 ℃ of depositing temperatures, depositing time 6h.
(3) vacuum impregnation: take the LPVCS for preparing as steeping fluid, the above-mentioned SiC fiber braid that has deposited carbon coating of vacuum impregnation.
(4) hot moulding is crosslinked: will be through the SiC fiber braid molding die of packing into of dipping, place in the multi-functional hot pressing furnace, under flowing nitrogen atmosphere, temperature rise rate with 5 ℃/min is warming up to 150 ℃, insulation 3h continues to be warming up to 350 ℃ of crosslinking temperatures, insulation 3h, keep molding pressure 40MPa in intensification and the insulating process, it is crosslinked to carry out hot moulding.
(5) Pintsch process: will put into pyrolyzer through crosslinked SiC fiber braid, and under flowing nitrogen atmosphere, be warming up to 1400 ℃ of cracking temperatures with the temperature rise rate of 30 ℃/min, insulation 5h carries out Pintsch process.
The dipping of repeating step (3)～step (5)-crosslinked-lytic cycle 15 times until sample increases weight less than 1% when this cycle, the sample weightening finish go up end cycle when finishing, is finished preparation, obtains SiC
f/ SiC matrix material.
Performance test:
Test SiC obtained above
fThe density of/SiC matrix material and mechanical property, can get its porosity is 5.63%, density is 2.14g/cm
3, flexural strength is 591Mpa, fracture toughness property is 29.54MPa * m
1/2
With SiC obtained above
f/ SiC matrix material carries out the electron-microscope scanning test, obtains fracture apperance electromicroscopic photograph as shown in Figure 2.From Fig. 2 (A), can find out, the carbon coating of CVD process deposits has produced the disbonding phenomenon in breaking-down process, illustrate that coating can improve the interfacial combined function between SiC fiber and the SiC matrix, so that fiber effective consumed energy in the debonding and pull-out process improves composite materials property; Can find out that from Fig. 2 (B) the SiC fiber surface is smooth, be not damaged, illustrate that the carbon coating of CVD process deposits can effectively protect the SiC fiber to avoid oxidation, corrosion equivalent damage in the material preparation process.
Embodiment 3:
The preparation method of a kind of silicon carbide fiber reinforced silicon carbide composite material of the present invention may further comprise the steps:
(1) material is prepared:
A. take the SiC fiber as raw material, adopt three-dimensional four-way weaving to prepare the SiC fiber braid;
B. preparing to contain Si-H reaches-CH=CH
2The liquid Si C ceramic precursor (LPVCS) of group.
(2) deposit carbon coating: take methane or propylene as unstripped gas, the SiC fiber braid placed adopt pressure differential method to carry out chemical vapour deposition in the vacuum oven, at SiC fiber braid surface deposition carbon coating.The processing condition of chemical vapour deposition are: carbon source is propylene, flow 0.10m
3H
-1Carrier gas is hydrogen, flow 0.15m
3H
-1, atmosphere pressures is 200Pa; 1400 ℃ of depositing temperatures, depositing time 30h.
(3) vacuum impregnation: take the LPVCS for preparing as steeping fluid, the above-mentioned SiC fiber braid that has deposited carbon coating of vacuum impregnation.
(4) hot moulding is crosslinked: will be through the SiC fiber braid molding die of packing into of dipping, place in the multi-functional hot pressing furnace, under flowing nitrogen atmosphere, temperature rise rate with 10 ℃/min is warming up to 250 ℃, insulation 1h continues to be warming up to 450 ℃ of crosslinking temperatures, insulation 1h, keep molding pressure 25MPa in intensification and the insulating process, it is crosslinked to carry out hot moulding.
(5) Pintsch process: will put into pyrolyzer through crosslinked SiC fiber braid, and under flowing nitrogen atmosphere, be warming up to 1250 ℃ of cracking temperatures with the temperature rise rate of 25 ℃/min, insulation 10h carries out Pintsch process.
The dipping of repeating step (3)～step (5)-crosslinked-lytic cycle 17 times until sample increases weight less than 1% when this cycle, the sample weightening finish go up end cycle when finishing, is finished preparation, obtains SiC
f/ SiC matrix material.
Performance test:
Test SiC obtained above
fThe density of/SiC matrix material and mechanical property, can get its porosity is 6.44%, density is 2.13g/cm
3, flexural strength is 629Mpa, fracture toughness property is 29.73MPa * m
1/2
Embodiment 4:
The preparation method of a kind of silicon carbide fiber reinforced silicon carbide composite material of the present invention may further comprise the steps:
(1) material is prepared:
A. take the SiC fiber as raw material, adopt three-dimensional four-way weaving to prepare the SiC fiber braid;
B. preparing to contain Si-H reaches-CH=CH
2The liquid Si C ceramic precursor (LPVCS) of group.
(2) deposit carbon coating: take methane or propylene as unstripped gas, the SiC fiber braid placed adopt pressure differential method to carry out chemical vapour deposition in the vacuum oven, at SiC fiber braid surface deposition carbon coating.The processing condition of chemical vapour deposition are: carbon source is propylene, flow 0.20m
3H
-1Carrier gas is hydrogen, flow 0.20m
3H
-1, atmosphere pressures is 2000Pa; 1350 ℃ of depositing temperatures, depositing time 30h.
(3) vacuum impregnation: take the LPVCS for preparing as steeping fluid, the above-mentioned SiC fiber braid that has deposited carbon coating of vacuum impregnation.
(4) hot moulding is crosslinked: will be through the SiC fiber braid molding die of packing into of dipping, place in the multi-functional hot pressing furnace, under flowing nitrogen atmosphere, temperature rise rate with 5 ℃/min is warming up to 300 ℃, insulation 1h continues to be warming up to 500 ℃ of crosslinking temperatures, insulation 1h, keep molding pressure 35MPa in intensification and the insulating process, it is crosslinked to carry out hot moulding.
(5) Pintsch process: will put into pyrolyzer through crosslinked SiC fiber braid, and under flowing nitrogen atmosphere, be warming up to 1450 ℃ of cracking temperatures with the temperature rise rate of 50 ℃/min, insulation 8h carries out Pintsch process.
The dipping of repeating step (3)～step (5)-crosslinked-lytic cycle 14 times until sample increases weight less than 1% when this cycle, the sample weightening finish go up end cycle when finishing, is finished preparation, obtains SiC
f/ SiC matrix material.
Performance test:
Test density and the mechanical property of SiCf/SiC matrix material obtained above, can get its porosity is 7.35%, and density is 2.11g/cm
3, flexural strength is 657Mpa, fracture toughness property is 26.80MPa * m
1/2
Below only be preferred implementation of the present invention, protection scope of the present invention also not only is confined to above-described embodiment, conceives various process programs without substantial differences all in protection scope of the present invention with the present invention.
Claims (2)
1. the preparation method of a silicon carbide fiber reinforced silicon carbide composite material is characterized in that, may further comprise the steps:
(1) material is prepared: three-dimensional four-way weaving prepares the SiC fiber braid as raw material adopts take the SiC fiber, and prepares liquid Si C ceramic precursor; Described liquid Si C ceramic precursor contains Si-H and reaches-CH=CH
2Group;
(2) deposit carbon coating: take methane or propylene as unstripped gas, described SiC fiber braid placed adopt pressure differential method to carry out chemical vapour deposition in the vacuum oven, at described SiC fiber braid surface deposition carbon coating; The condition of described chemical vapour deposition is: raw gas flow is 0.01 m
3H
-1～0.20m
3H
-1Carrier gas is hydrogen or nitrogen, and the carrier gas atmosphere pressures is 100 Pa～2000Pa, and carrier gas flux is 0.01 m
3H
-1～0.20m
3H
-1Depositing temperature is 800 ℃～1500 ℃, depositing time 1 h～40h;
(3) vacuum impregnation: take described liquid Si C ceramic precursor as steeping fluid, the above-mentioned SiC fiber braid that has deposited carbon coating of vacuum impregnation;
(4) hot moulding is crosslinked: with the mould of packing into of the SiC fiber braid after the above-mentioned vacuum impregnation, it is crosslinked to carry out hot moulding under flowing nitrogen atmosphere; The crosslinked concrete technology parameter of described hot moulding is: the temperature rise rate with 1 ℃/min～10 ℃/min is warming up to 100 ℃～300 ℃, be incubated 0 h～5h, continue to be warming up to 200 ℃ ~ 500 ℃ of crosslinking temperatures, insulation 0h～5h keeps molding pressure≤40MPa in intensification and the insulating process;
(5) Pintsch process: the SiC fiber braid after hot moulding is crosslinked is put into pyrolyzer, carries out Pintsch process under flowing nitrogen atmosphere; Described Pintsch process concrete technology parameter is: the temperature rise rate with 1 ℃/min～50 ℃/min is warming up to 800 ℃～1500 ℃ of cracking temperatures, insulation 1h～10h;
Vacuum impregnation-the hot moulding of repeating step (3)～step (5) is crosslinked-the Pintsch process cycle, until sample increases weight less than 1% when this cycle, the sample weightening finish go up end cycle when finishing, finish preparation, and obtain silicon carbide fiber reinforced silicon carbide composite material.
2. the preparation method of silicon carbide fiber reinforced silicon carbide composite material according to claim 1 is characterized in that, and described vacuum impregnation-hot moulding is crosslinked-and the multiplicity in Pintsch process cycle is 10～20 times.
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| CN114315400A (en) * | 2022-01-05 | 2022-04-12 | 湖南远辉复合材料有限公司 | Composite material preparation method based on hot die pressing cracking |
| CN115385704A (en) * | 2022-08-23 | 2022-11-25 | 广西三元华鑫特种陶瓷有限公司 | Method for reducing drying stress deformation of micro-nano fiber reinforced silicon carbide material semi-finished product |
| CN115819099A (en) * | 2023-02-24 | 2023-03-21 | 中国人民解放军国防科技大学 | High-performance SiC f Preparation method of/SiC composite material |
| CN116903382A (en) * | 2023-07-21 | 2023-10-20 | 湖南泽睿新材料有限公司 | Equipment for rapidly depositing carbon coating on surface of continuous silicon carbide fiber and application method |
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