CN106830967A - A kind of fastener of heat-resistant high-strength charcoal/ceramic material and preparation method thereof - Google Patents
A kind of fastener of heat-resistant high-strength charcoal/ceramic material and preparation method thereof Download PDFInfo
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- 239000003610 charcoal Substances 0.000 title claims abstract description 97
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 77
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 42
- 239000003292 glue Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 20
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 235000013312 flour Nutrition 0.000 claims abstract description 11
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 19
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 13
- 239000005011 phenolic resin Substances 0.000 claims description 13
- 229920001568 phenolic resin Polymers 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000001856 Ethyl cellulose Substances 0.000 claims description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 229920001249 ethyl cellulose Polymers 0.000 claims description 3
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004898 kneading Methods 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims description 2
- 230000008023 solidification Effects 0.000 claims description 2
- 238000009738 saturating Methods 0.000 claims 1
- 238000010304 firing Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 13
- 238000005245 sintering Methods 0.000 description 13
- 230000008569 process Effects 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 11
- 239000000919 ceramic Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 7
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 5
- 230000003026 anti-oxygenic effect Effects 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910016006 MoSi Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- RCHKEJKUUXXBSM-UHFFFAOYSA-N n-benzyl-2-(3-formylindol-1-yl)acetamide Chemical compound C12=CC=CC=C2C(C=O)=CN1CC(=O)NCC1=CC=CC=C1 RCHKEJKUUXXBSM-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- -1 phenolic aldehyde Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000007115 recruitment Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
- C04B2235/404—Refractory metals
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/424—Carbon black
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention discloses a kind of fastener of heat-resistant high-strength charcoal/ceramic material and preparation method thereof.The composition of its charcoal/ceramic material is：30~60% unordered Carbon fibe；10~18% carbon black；10~20% silica flour；8~16% molybdenum powder；6~12% carborundum；3~10% zirconium oxide；10~25% glue.Formed through high-temperature firing.The present invention has very excellent resistance to elevated temperatures and excellent mechanical mechanics property at high temperature, while also having good decay resistance, with good processing characteristics, preparation and processing cost can be greatly reduced.
Description
Technical field：
With high temperature resistant and have the ceramic material of high intensity the present invention relates to a kind of, particularly relate to one kind and can be used for all kinds of height
Fastener and connector of the charcoal/ceramic material of warm stove and preparation method thereof.
Background technology：
Superhigh temperature (1500 DEG C of ＞) vacuum drying oven is industrial production, particularly new energy materialses such as monocrystalline silicon, polysilicon, or high
Performance special cermacis such as BN ceramics, the visual plant of nano ceramics production.This kind equipment is related to substantial amounts of under the condition of high temperature
Connector/and fastener, under superelevation temperature state, the connector of common metal material or the service life of fastener are very short,
The heat resistance of the fastener of example steel or irony cannot meet requirement, in addition the intensity of the fastener of existing graphite material
It is low, it is difficult to reach the technical requirements of resistance to 1500 DEG C of high temperature above and bending strength more than 100Mpa.It is existing develop a kind of charcoal/
High temperature resistant fastener prepared by charcoal (C/C) material, it substantially meets above-mentioned technical requirements, and its preparation technology is：Braiding Carbon fiber
(density is ρ=0.5g/cm to dimension precast body3) → precast body high-temperature process (2000 DEG C of ＞) → CVD increases density, and (density is ρ
=1.3g/cm3, the time is 300h) and (density is ρ=1.5g/cm to → high-temperature process (2300 DEG C of ＞) → CVD increase density3, when
Between be 500h)-→ high-temperature process (2400 DEG C of ＞) → processing → CVD increase density (density be ρ=1.7g/cm3, the time is
700h) → high-temperature process (2400 DEG C of ＞) → processing → CVD increases density, and (density is ρ=1.75g/cm3, the time is 900h)
→ high-temperature process (2400 DEG C of ＞) → processed finished products.The raw material that charcoal/Carbon Materials can be seen from process above process are expensive, produce work
Skill is complicated and the production cycle is very long, and energy consumption is big and production cost is high, and product quality is not high in addition, and fastener easily falls tooth, special
Be not charcoal/Carbon Materials antioxygenic property it is low, anti-yaw damper ability causes product service life short, for these reasons, fastening
Part problem turns into one of important key of high temperature furnace manufacture.Due to domestic current superhigh temperature vacuum drying oven have million magnitudes with
On, annual fastener or the usage amount of connector exceed ten million set (part), and the use mission of such as fastener or connector is too short,
The damage or replacement of its own are exactly a huge loss, and the loss such as its related production disruption for causing, maintenance recruitment is more
It is huge.Therefore, the raising of the performance of the fastener or connector of high temperature furnace or equipment has very urgent requirement, and has
Great economic benefit, is a urgent problem.
The content of the invention：
Goal of the invention of the invention be disclose it is a kind of can be used for the charcoal/ceramic material of the strong mechanical performance of the condition of high temperature or charcoal/
Fastener or connector prepared by ceramic material.
Another goal of the invention of the invention is the preparation method of the fastener of the charcoal/ceramic material for disclosing above-mentioned.
Realizing the composition of described heat-resistant high-strength charcoal/ceramic material is：30~60% unordered Carbon fibe；10~18%
Carbon black；10~20% silica flour；8~16% molybdenum powder；6~12% carborundum；3~10% zirconium oxide；10~25%
Glue.
The further composition of described heat-resistant high-strength charcoal/ceramic material is：30~40% unordered Carbon fibe；10~
12% carbon black；17~20% silica flour；10~12% molybdenum powder；10~12% carborundum；6~10% zirconium oxide；10
~15% glue.
The further composition of described heat-resistant high-strength charcoal/ceramic material is：40~55% unordered Carbon fibe；16~
18% carbon black；10~12% silica flour；8~12% molybdenum powder；6~8% carborundum；8~6% zirconium oxide；12~
25% glue.
Described unordered Carbon fibe is one of short carbon fiber, useless Carbon fibe long, random Carbon fibe or its any combination.
The composition of described glue is：94~98% phenolic resin；0.1~2.0% coupling agent；1.0~4.0%
Ethyl cellulose.
The preparation process of the preparation method of the fastener of described heat-resistant high-strength charcoal/ceramic material is：
A, carbon black, silica flour, molybdenum powder, carborundum and zirconium oxide are mixed to prepare mixing middle material；
B, unordered Carbon fibe is soaked in glue, soak time is 12~24 hours；
C, by above-mentioned mixing middle material and it is mixed with after the glue of unordered Carbon fibe mixes and is made blank；
D, blank is incubated 10~30 minutes at 80 DEG C~120 DEG C, makes blank semi-solid preparation；
E, obtained semi-solid preparation blank is placed in mould first normal temperature pressure, reheats and pressurize, mold temperature is 140 DEG C
~160 DEG C, the briquetting pressure of pressurization is 5~10Mpa, and 1~2 hour is incubated after 180 DEG C~220 DEG C are warming up to afterwards, is obtained solid
Material；
F, under nitrogen protection, solidifying substance is sintered at 1400 DEG C~1800 DEG C and obtains charcoal/ceramic material.
In described step c, mixing middle material be mixed with after the glue of unordered Carbon fibe mix, with kneader kneading 4~
10 hours, or mixing machinery mix 4~10 hours.
In described step c, mixed blank is put 10~30 hours in sealed states, make blank into plasticity shape
State.
After described step f, in the liquid phenolic resin that the charcoal/ceramic material that will be obtained is inserted in autoclave, 1.5 are forced into~
2.0Mpa, so that phenolic resin penetrates into charcoal/ceramic material.
Charcoal/the ceramic material for permeating phenolic resin is placed in high pressure combustion freezing of a furnace, 1500 DEG C~2000 DEG C are warming up to, is obtained more
Highdensity charcoal/ceramic material.
The invention discloses the formula and proportioning of a kind of composition of charcoal/ceramic material fastener, the charcoal/pottery material is also disclosed
The preparation method of material, preparation method of the invention greatly reduces the cost of raw material, process simplification, shortens the production cycle,
And improve the toughness of material.Described charcoal/ceramic material has charcoal element composition higher, therefore with the base of charcoal/Carbon Materials
This performance, at the same in material again contain more ceramic component, these ceramic components generated in high-temperature sintering process MoSi,
Compound between the refractory metals such as ZrC and MoZrSi, produces multivalent effect, improves the mechanical behavior under high temperature of material, improves
The inoxidizability of material and anti-silicon vapor corrosivity.Above-mentioned charcoal/ceramic material can be prepared as various mechanical components, particularly make
Standby is fastener or connector, can be applied to the vacuum drying oven or various high-temperature services of superhigh temperature (1500 DEG C of ＞).Above-mentioned charcoal/pottery
Material or the fastener or connector of preparation have very excellent resistance to elevated temperatures and excellent Mechanics of Machinery at high temperature
Performance, while also there is good decay resistance, particularly oxidation resistent susceptibility and also have close far below metal (such as steel)
Spend and can be applied to aerospace field, and the preparation method of above-mentioned charcoal/ceramic material is relatively simple, and using discarded
Carbon fiber, so production cost is greatly reduced, combination property is extremely superior, with fabulous economic benefit and social benefit.
Specific embodiment：
Specific embodiment of the invention is will be given in detail below, it should be noted that specific embodiment of the invention is
Understanding to technical scheme, is not construed as the limitation to claims of the invention.
The concrete composition (by weight percentage) of the first embodiment of charcoal/ceramic material of the invention is：30~60% nothing
Sequence Carbon fibe, 10~18% carbon black, 10~20% silica flour, 8~16% molybdenum powder, 6~12% carborundum, 3~10%
Zirconium oxide and 10~25% glue；Preparation method after above-mentioned each component is mixed through being given in detail below, can fire
Into required charcoal/ceramic material, through high-temperature firing after, above-mentioned charcoal/ceramic material has charcoal molecule and Carbon fibe higher, therefore tool
Have the key property of charcoal/charcoal (C/C) material, at the same above-mentioned material again have more ceramic component, and larger composition constitute
Charcoal/charcoal (C/C) material and ceramic component mixed sintering are constituted, and have above-mentioned charcoal/ceramic material quite excellent comprehensive
Can, wherein unordered Carbon fibe had not only made charcoal/ceramic material have good isotropism but also had made charcoal/ceramic material can be square in preparation process
Just it is molded and the machining property with the later stage.
Further to improve the anti-oxidant and mechanical property of charcoal/ceramic material, the tool of the charcoal/ceramic material of the second embodiment
Body is constituted：30~40% unordered Carbon fibe, 10~12% carbon black, 17~20% silica flour, 10
~12% molybdenum powder, 10~12% carborundum, 6~10% zirconium oxide and 10~15% glue；In the embodiment, due to
With ceramic component higher, therefore its anti-oxidant and mechanical property is further improved, while improve charcoal/ceramic material at high temperature
Mechanical property stability, be more suitable for it is aerobic in the case of use.
Further to improve the resistance to elevated temperatures of charcoal/ceramic material, the concrete composition of the charcoal/ceramic material of the 3rd embodiment
(by weight percentage) it is：40~55% unordered Carbon fibe, 16~18% carbon black, 10~12% silica flour, 8~12%
Molybdenum powder, 6~8% carborundum, 3~6% zirconium oxide and 12~25% glue；In this embodiment, due to higher
Carbon Materials and Carbon fibe percentage, its performance for having more charcoal/Carbon Materials reduce further material fragility, improves
The toughness of material, more resistant to the stability under high temperature and high temperature.
The glue composition (by weight percentage) used in above-mentioned charcoal/ceramic material is specially：94~98% phenolic aldehyde
Resin (article number is PF-5206, the production of Jinan holy well Butterworth company), 0.1~2.0% coupling agent (article number is KH-792,
Tianjin Xiang Fei Materials Co., Ltd produces), (article number is EC, the life of Luzhou north chemical company for 1.0~4.0% ethyl cellulose
Produce)；The glue that above-mentioned composition is constituted mixes with foregoing powdery each component again after being impregnated with unordered Carbon fibe, glue can ensure with
The interface cohesion of unordered Carbon fibe, makes mixed mixture have good plasticity or moldability, and glue and each powder again
The uniform mixing of shape component is also constituted to the charcoal in charcoal/ceramic material, pottery and both crystalline phases very benefit.
Above-mentioned unordered Carbon fibe is one of short carbon fiber, useless Carbon fibe long, random Carbon fibe or its any combination.It is chopped
Carbon fibe is favourable to the isotropic behavior of charcoal/ceramic material；The Carbon fibe long that gives up is strong to improving intensity such as bending strength or stretch-proof
The raising of degree is beneficial, and particularly the performance to the fastening bolt (bar) of final large-sized charcoal/ceramic material size for example long is favourable；
Random Carbon fibe then has the combination property of Carbon fibe short, long, can play coupled action, strengthens the associativity of material, particularly goes up
The Carbon fibe useless long and random Carbon fibe stated can be the waste materials during Carbon fibe production process or use, and this both reduces useless fibre
Tie up the utilization that the influence to environment improves waste again, it is possible to decrease cost of the invention.
The step of preparation method of above-mentioned charcoal/ceramic material is：
A, carbon black, silica flour, molybdenum powder, carborundum and zirconium oxide are mixed to prepare mixing middle material；
B, unordered Carbon fibe is soaked in glue, soak time is 12~24 hours；
C, by above-mentioned mixing middle material and it is mixed with after the glue of unordered Carbon fibe mixes and is made blank；
D, blank is incubated 10~30 minutes at 80 DEG C~120 DEG C, makes blank semi-solid preparation；
E, obtained semi-solid preparation blank is placed in mould first normal temperature pressure, reheats and pressurize, mold temperature is 140 DEG C
~160 DEG C, the briquetting pressure of pressurization is 5~10Mpa, and 1~2 hour is incubated after 180 DEG C~220 DEG C are warming up to afterwards, is obtained solid
Material；
F, under nitrogen protection, solidifying substance is sintered at 1400 DEG C~1800 DEG C and obtains charcoal/ceramic material.
In above-mentioned step a, foregoing carbon black, silica flour, molybdenum powder, carborundum and zirconium oxide are mixed and then prepares mixing
Middle material, with standby, or inserts mix grinding 2~4 hours in ball mill by above-mentioned mixing middle material, prepare each component granularity compared with
It is the mixing middle material of uniform smaller particle size, the specific surface area on the one hand increasing each component improves the mutual of mixing middle material again
Packing and mutual permeability, improve the crystallinity of reaction rate and charcoal, pottery in sintering process；In above-mentioned step b,
Unordered Carbon fibe is soaked in glue, soak time be 12~24 hours, substantially from microstructure Carbon fibe due to
Technique causes it to have a small hole, and when Carbon fibe is soaked in glue, the molecule of glue can enter charcoal within a certain period of time
Micro-pore in fiber surface and/or top layer, this enters needs the regular hour, into carbon fiber surface and/or top layer
The glue of hole forms a transition zone after sintering, and increases the interfacial effect between Carbon fibe and charcoal/ceramic material structure, carries
The mechanical strength of charcoal/ceramic material high；It is by above-mentioned mixing middle material and the glue for being mixed with unordered Carbon fibe in above-mentioned step c
Blank is made after mixing, is further to improve the uniformity of mixing and enable glue more preferably and be fully infiltrated into foregoing each component
Particle top layer, inserts above-mentioned blank kneader and mediates 4~10 hours, or above-mentioned blank is placed in into mixing machinery mixing 4
~10 hours, mixed blank was put 10~30 hours under being placed in sealing state, preferably 15~24 hours, can make glue and charcoal
Fiber and solid particle fully permeate, moisten, spread and merge, and make blank into mecystasis, in sintering stage below, are impregnated with
The each component of glue to the larger benefit that is combined with of the crystallization of charcoal/ceramic material, above-mentioned blank be prepared as through mould needed for
Template blank or other shapes of blank；In above-mentioned step d, after blank is incubated 10~30 minutes at 80 DEG C~120 DEG C, base
Material semi-solid preparation, making the blank of semi-solid preparation turns into the thixotroping blank with certain plasticity；In step e, by obtained semi-solid preparation base
Material is placed in mould first normal temperature pressure, reheats and pressurizes, and the blank of thixotroping is placed on into normal temperature pressure on press produces blank
Plastic deformation, volume contraction, density increases, and thermal conductivity is improved, and this can ensure that base substrate temperature is consistent in hot pressing below,
Then heat up, mold temperature is 140 DEG C~160 DEG C, the briquetting pressure of pressurization is 5~10Mpa, can tentatively by the volatilization in blank
Thing is discharged, and insulation 1~3 is small after being incubated 1~2 hour or be warming up to 180 DEG C~250 DEG C after 180 DEG C~200 DEG C being warming up to afterwards
When, then natural cooling, then can substantially drain volatile matter and make ingot solidification and turn into solidifying substance, due to semi-solid preparation blank tool
Have the dimensions, volatile substance is discharged in lower temperature, while higher temperature is except continuing to discharge volatile substance, can trigger
Chemically react and semi-solid preparation blank is turned into solidifying substance；In step f, under nitrogen protection by solidifying substance 1400 DEG C~1800
Sintering obtains charcoal/ceramic material at DEG C, and sintering temperature in this step has been higher than the sintering temperature of general ceramic material, the sintering
Temperature depends on the component and formula and proportioning of foregoing charcoal/ceramic material, and in sintering process, it is heat that phenolic resin will be carbonized
Solution charcoal and increase total carbon content of charcoal/ceramic material, the charcoal/ceramic material after above-mentioned sintering has had at a relatively high superhigh temperature resistant
Energy and high intensity, can use, as connector or fastener due to making above-mentioned charcoal/pottery with a relatively high ceramic component
Material has good oxidation resistance energy again, and this compensate for Carbon Materials or charcoal/Carbon Materials antioxygenic property defect not high.
Due in above-mentioned sintering process, it is difficult to avoid the presence of small bubble, and the density of charcoal/ceramic material is not also most
It is good, therefore in liquid phenolic resin in charcoal/ceramic material that above-mentioned step f is obtained inserts autoclave, it is forced into 1.5~
2.0Mpa, so that phenolic resin penetrates into charcoal/ceramic material, under stress, the micro-bubble that phenolic resin enters in charcoal/ceramic material
It is interior；Charcoal/the ceramic material for permeating phenolic resin is placed in high pressure combustion freezing of a furnace, 1500 DEG C~2000 DEG C sintering, phenolic aldehyde tree are warming up to
Further increase the density of charcoal/ceramic material after fat charing, highdensity charcoal/ceramic material has more preferably high temperature resistant and mechanics high
Performance such as bending strength and tensile strength, above-mentioned charcoal/ceramic material can be prepared through certain machining on demand
Specific fastener or connector or other structures part.
Charcoal/ceramic material prepared by the present invention has non-than fastener prepared by charcoal/charcoal (C/C) material of prior art etc.
Often big advantage, such as cost of raw and processed materials can save 70% or so, and the production cycle reduces 4/5ths or so, and yield rate is improved
15%, production cost decline 75%, antioxygenic property improve cause service life to double, improve mechanical strength, because charcoal/
The uniformity of ceramic material and improve processability and can produce large-sized fastener etc., the present invention has very superior
Combination property, has many advantages, such as charcoal/ceramic material and ceramic material, is the composite of a new generation.
Claims (10)
1. a kind of fastener of heat-resistant high-strength charcoal/ceramic material, it is characterised in that the composition of charcoal/ceramic material is：
2. the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 1, it is characterised in that it is in charcoal/ceramic material
Composition is：
3. the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 1, it is characterised in that it is in charcoal/ceramic material
Composition is：
4. the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 1 or 2 or 3, it is characterised in that described glue
It is：
Phenolic resin 94~98%；
Coupling agent 0.1~2.0%；
Ethyl cellulose 1.0~4.0%.
5. the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 1 or 2 or 3 or 4, it is characterised in that described
Unordered Carbon fibe is one of short carbon fiber, useless Carbon fibe long, random Carbon fibe or any combination.
6. the preparation method of the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 1 or 2 or 3 or 4 or 5, it is special
Levy is that its preparation process is as follows：
A, carbon black, silica flour, molybdenum powder, carborundum and zirconium oxide are mixed to prepare mixing middle material；
B, unordered Carbon fibe is soaked in glue, soak time is 12~24 hours；
C, by above-mentioned mixing middle material and it is mixed with after the glue of unordered Carbon fibe mixes and is made blank；
D, blank is incubated 10~30 minutes at 80 DEG C~120 DEG C, makes blank semi-solid preparation；
E, obtained semi-solid preparation blank being placed in mould first normal temperature pressure, reheat and pressurize, mold temperature is 140 DEG C~
160 DEG C, the briquetting pressure of pressurization is 5~10Mpa, and 1~2 hour is incubated after 180 DEG C~220 DEG C are warming up to afterwards, and solidification is obtained
Material；
F, under nitrogen protection, solidifying substance is sintered at 1400 DEG C~1800 DEG C and obtains charcoal/ceramic material.
7. the preparation method of the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 6, it is characterised in that described
In step c, mixing middle material be mixed with after the glue of unordered Carbon fibe mix, with kneader kneading 4~10 hours, or mixer
Tool mixes 4~10 hours.
8. the preparation method of the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 7, it is characterised in that described
In step c, mixed blank is put 10~30 hours in sealed states, make blank into mecystasis.
9. the preparation method of the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 6 or 7 or 8, it is characterised in that
After described step f, in the liquid phenolic resin that the charcoal/ceramic material that will be obtained is inserted in autoclave, 1.5~2.0Mpa is forced into,
So that phenolic resin penetrates into charcoal/ceramic material.
10. the preparation method of the fastener of the heat-resistant high-strength charcoal/ceramic material as described in claim 9, it is characterised in that will ooze
Charcoal/the ceramic material of saturating phenolic resin is placed in high pressure combustion freezing of a furnace, is warming up to 1500 DEG C~2000 DEG C, and prepared more highdensity charcoal/
Ceramic material.
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| CN114790121A (en) * | 2022-05-12 | 2022-07-26 | 宁波金鼎紧固件有限公司 | Heat-resistant high-strength carbon/ceramic fastener and preparation method thereof |
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