CN107746282A - A kind of in-situ carburization silica fibre enhancing liquid phase sintering silicon carbide ceramic and manufacture method - Google Patents

A kind of in-situ carburization silica fibre enhancing liquid phase sintering silicon carbide ceramic and manufacture method Download PDF

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CN107746282A
CN107746282A CN201711051009.5A CN201711051009A CN107746282A CN 107746282 A CN107746282 A CN 107746282A CN 201711051009 A CN201711051009 A CN 201711051009A CN 107746282 A CN107746282 A CN 107746282A
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sintering
carborundum
silicon carbide
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CN107746282B (en
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方锡成
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Ningbo Zhongli Juyuan seal Co.,Ltd.
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FENGHUA ZHONGLI SEALS Co Ltd
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    • C04B35/806
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225Yttrium oxide or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C04B2235/483Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes

Abstract

One kind is using in-situ carburization silica fibre enhancing liquid phase sintering silicon carbide ceramic and manufacture method,It is characterized in that silicon carbide fibre is turned into being bonded the Polycarbosilane strand cracking under 1700 DEG C 1800 DEG C of sintering temperature of the parent silicon-carbide particle of little particle aluminum oxide yttrium oxide sintering aid by VTES and the parent silicon-carbide particle of partial adsorbates Polycarbosilane strand by competitive adsorption," riveting " with other silicon-carbide particles is formed by the growth in liquefied aluminum oxide yttrium oxide sintering aid,The decussating fibers grid and " crack deflection " mechanism formed in the aluminum oxide yttrium oxide sintering aid of residual crystal boundary increases substantially its high-temperature mechanical property,And the reunion in liquid-phase sintering is avoided simultaneously,The situation for being unfavorable for sintering is caused to occur from space steric effect caused by the excessive silicon carbide fibre possibility of particle " riveting " and silicon-carbide particle surface.

Description

A kind of in-situ carburization silica fibre enhancing liquid phase sintering silicon carbide ceramic and manufacture method
Technical field
The present invention relates to a kind of high-strength carborundum ceramics and manufacture method technical field.
Background technology
Thyrite have elevated temperature strength is big, high-temperature oxidation resistance is strong, abrasion resistance properties are good, heat endurance is good, Thermal coefficient of expansion is small, thermal conductivity is big, hardness is high, anti-thermal shock and the good characteristic such as resistant to chemical etching, in automobile, mechanical chemical industry, ring There is increasingly extensive application in the fields such as border protection, space technology, information electronics, the energy, have become a kind of in many industry The irreplaceable structural ceramics of the other materials of field excellent performance.
Dynamic sealing in plant equipment is carried out by the rotational slide of two seal face materials, as sealed end Plane materiel material, it is desirable to which hardness is high, has wear resistance.The hardness of silicon carbide ceramics is at a relatively high and coefficient of friction is small, therefore carborundum is made pottery Porcelain can obtain the sliding properties that other materials are unable to reach as mechanical seal end surface material.On the other hand, two end faces are close Closure material can produce certain heat in rotary movement due to rubbing, so that the local temperature rise of seal face, Therefore face material must also be able to be resistant to certain temperature.In order to avoid end face seal material produces during rotational slide Thermal strain and hot tearing, it is desirable to which the thermal conductivity factor of face material is high, good thermal shock.At present, silicon carbide ceramics is in all kinds of machines Substantial amounts of application is obtained in tool sealing, and very big contribution is made that for the laborsaving of plant equipment and energy-conservation, shows other materials The incomparable superiority of material.Silicon carbide ceramics is also used successfully as various bearings, cutting tool in mechanical industry.
In the automotive industry, in order to improve the thermal efficiency of engine, the energy is made full use of, reduces fuel consumption, is reduced big Gas is polluted, it is desirable to which higher than 1200 DEG C, (according to calculating, the operating temperature of engine is brought up to the operating temperature of engine by 1100 DEG C At 1370 DEG C, 30%) thermal efficiency can increase.Silicon carbide ceramics elevated temperature strength because possessed by, relatively low thermal coefficient of expansion are higher Thermal conductivity factor and preferable thermal-shock resistance and be considered as more than 1200 DEG C most promising candidate materials of temperature in use.Gather around Such as U.S., Germany and the Japan of country for having advanced ceramics technology has been developed that the engine component using silicon carbide ceramics as sent out Motivation stator, rotor, burner and scroll casing simultaneously achieve good using effect, are just being directed to full ceramic engine at present Developmental research.
Aero-Space, atomic energy industry etc., which need to be resistant in the occasion of ultra-high temperature such as nuclear fission and fusion reactor, to be needed That wants bears the heat proof material of 2000 degree or so high temperature;Rocket and aerospace craft surface are used to be resistant to and air severe friction In caused by up to thousands of K temperature thermal insulation tile;Rocket chamber's larynx lining and inner lining material, gas-turbine blade;It is high Top plate, the support of warm stove, and the high-temperature component such as fixture of high temperature experiment also generally use silicon carbide ceramics component.Carborundum Ceramics are also widely used as various corrosion-resistant container and pipelines in petro chemical industry.
Extensive use due to the high-performance of silicon carbide ceramics and in industrial circle, SiC sintering is always material circle The focus of research.But because carborundum is a kind of extremely strong covalent key compound of covalency, at a high temperature of 2100 DEG C, C 1.5 × 10 are also only with Si self-diffusion coefficient-10With 2.5 × 10-13cm2/s.So SiC is difficult sintering, it is necessary to by sintering Auxiliary agent or external pressure are only possible to be densified (Krishi Negita, Effective sintering in 2000 DEG C of implemented below aids for silicon carbide ceramics:reactivities of silicon carbide with Various additives, J.Am.Ceram.Soc., 1986,69 (12):C308-310.).It is understood that in such high temperature Under, if it is possible to certain operating temperature is reduced, energy consumption will sharp reduce, so how to be burnt at alap temperature Knot obtains the silicon carbide ceramics product of high relative density (> 98%), meets different industrial circles to high-end silicon carbide ceramics system The demand of product, it has also become silicon carbide ceramics industry general character key issue urgently to be resolved hurrily.
Hot pressed sintering drives addition in powder or does not add sintering aid, hot pressed sintering reaches before sintering by means of external pressure 98% consistency usually requires 2000 DEG C or so of temperature, and such as east of a river is bright in silicate journal 1981, No.9,133-146 The SiC+1%B under the conditions of 2050 DEG C is reported4Under 45 minutes process conditions of C+3%C architecture heat preservations, density reaches theoretical fine and close The 98.75% of degree.Also system sintering temperature of the part using Al, B, C as sintering aid is less than 2000 DEG C, such as Huang Hanquan In 1991,9 (2):It is reported in 1650 DEG C -1950 DEG C on 70-77, under 50MPa hot pressing condition, relative density height can be obtained In 98% sintered body.But hot pressed sintering can only prepare the silicon carbide components of simple shape, and pass through once sintered process The quantity of prepared product seldom can not be realized and commercially produced.Comparatively speaking, pressureless sintering is high-performance silicon carbide pottery Porcelain industrializes most promising sintering method.It can be divided into solid phase according to from state pressureless sintering of the auxiliary agent in sintering process Sintering and liquid-phase sintering.The method for being occurred without the second phase of melting in sintering process using B, C and Al or its compound is claimed Make solid-phase sintering.Solid phase sintering temperature is higher, and generally more than 2000 DEG C, and the purity requirement to raw material is also very high, such as S.Prochazka (S.Prochazka, Ceramics for High-Performance of GE companies of the U.S. Applications, 1974,239-252.) by adding a small amount of B and C simultaneously in the B-SiC fine powders of high-purity, using nothing Sintering process is pressed, the SiC sintered bodies that density is higher than 98% are obtained in 2020 DEG C.And add Al in sintering system2O3-Y2O3、 AIN-R2O3It is referred to as liquid phase burning by forming the method for binary liquid phase eutectic mixture in sintering process Deng sintering aid Knot.Liquid-phase sintering can sinter to obtain with preferable fracture toughness and bending strength and with complex shape at a lower temperature Shape and large-sized silicon carbide components.Liquid-phase sintering system, particularly SiC-Al2O3-Y2O3, it has also become carborundum burns in recent years Tie the focus of research.But the silicon carbide ceramics of liquid-phase sintering is used, a certain amount of oxide has necessarily been retained between its crystal boundary, The toughness and intensity of silicon carbide ceramics can be greatly lowered in these oxides under higher temperature in use, influence it in extreme ring Performance under the conditions of border, therefore how to carry out improving its elevated temperature strength as far as possible under conditions of liquid-phase sintering using sintering aid And tough sexual development high-performance silicon carbide ceramics are important problems.In recent years, sintering parent or carbon are added to using Polycarbosilane SiClx fiber is directly appended to sinter enhancing silicon carbide ceramics parent in parent and gradually grown up, but these methods are also present Many problems:
If the 1, Polycarbosilane is added to sintering parent using direct sintering, during can produce gas, be carbonized in parent The internal stomata that leaves of silicon ceramics reduces the consistency and mechanical performance of ceramic systems;
2nd, Polycarbosilane is added to the silicon carbide fibre formed after sintering parent cracking or is added directly into system When yardstick itself is small due to having much bigger major diameter compared with parent silicon-carbide particle for silicon carbide fibre, often in parent More serious reunion is formed in silicon carbide ceramics system, causes the heterogeneity of mechanical property;
3rd, because Polycarbosilane is added to the silicon carbide fibre formed after sintering parent cracking or is added directly into system In position of the silicon carbide fibre in parent carborundum system do not know, therefore be often difficult to be formed between silicon-carbide particle " riveting " phenomenon, " crack deflection " mechanism is played, so as to play preferable enhancing effect.
The content of the invention
The present invention proposes a kind of using in-situ carburization silica fibre enhancing liquid phase sintering silicon carbide for existing background technology Ceramics and manufacture method, it is characterised in that parent silicon-carbide particle is divided into two parts and is surface-treated respectively, wherein one Divide the competitive adsorption by Polycarbosilane and N- β (aminoethyl) -3- aminopropyltriethoxy dimethoxysilanes so that carborundum The grain a part of region in surface is covered by long chain macromolecule Polycarbosilane, secures Polycarbosilane strand in silicon-carbide particle Relative position;Another part silicon-carbide particle is bonded little particle alumina-yttria by VTES and sintered Auxiliary agent;The cracking of Polycarbosilane strand turns into silicon carbide fibre under 1700 DEG C -1800 DEG C of sintering temperature, by liquefied Growth in alumina-yttria sintering aid forms " riveting " with other silicon-carbide particles, forms the oxygen in residual crystal boundary Change the decussating fibers grid in aluminium-yttrium oxide sintering aid and " crack deflection " mechanism increase substantially its high-temperature mechanical property, And the reunion in liquid-phase sintering is avoided simultaneously, it may draw from the excessive silicon carbide fibre of particle " riveting " and silicon-carbide particle surface The situation that the space steric effect and causing risen is unfavorable for sintering occurs.
It is this that liquid phase sintering silicon carbide ceramic and manufacture method are strengthened using in-situ carburization silica fibre, it is characterised in that by master Raw material carborundum powder is wanted two parts of A and B of quality such as to be divided into, by Polycarbosilane, the 1- of A part carborundum 5-10% mass percents N- β (the aminoethyl) -3- aminopropyltriethoxies dimethoxysilane of 3% mass percent, the toluene of 10-15% mass percents and A part carborundum mixes, after being sufficiently stirred 30-50 minutes and drying 30-60 minutes at a temperature of 80 DEG C -120 DEG C, 20-40 minutes are calcined in 280 DEG C of -350 DEG C of Muffle furnaces, temperature is then increased to 1100 DEG C -1350 DEG C and continues to calcine 5-15 Furnace cooling obtains material I after hour;By the auxiliary agent of B part carborundum 5-15% mass percents, consisting of 30-70wt% Al2O3, 28-65wt%Y2O3And 2-5wt% VTESs, ball is mixed in high energy ball mill with B part carborundum Mill 3-5 hours obtain material II;By material I, material II and material I, material II gross masses 3-5wt% bonding agents in high energy ball By sieving, being molded after mixing and ball milling 5-10 hours in grinding machine, heated up with 5 DEG C -10 DEG C of programming rate in vacuum carbon tube furnace To 1700 DEG C -1800 DEG C and it is incubated the silicon carbide ceramics that high intensity, high tenacity is made in 10-20 hours.
Above-mentioned carborundum powder and Al2O3、Y2O3The granularity difference of sintering aid is larger;The particle of main body carborundum Footpath should be between 0.5-5 microns, Al2O3、Y2O3The particle scale of sintering aid is below 200 nanometers, so as to be advantageous in main body Silicon carbide powder surface forms fine and close, uniform, thin sintering aid clad.
Above-mentioned bonding agent is one kind in phenolic resin, polyvinyl alcohol.
Above-mentioned shaping is that powder is placed in cylindrical die, in 200-250MPa pressure in high tonnage hydraulic Lower static pressure is stripped to obtain biscuit for 5 minutes again, and then biscuit is heat-treated 20 minutes at 250 DEG C, removes bonding agent.
Compared with prior art, the advantage of the invention is that:Parent silicon-carbide particle is divided into two parts carry out table respectively Face is handled, and a portion is inhaled by Polycarbosilane and the competitive of N- β (aminoethyl) -3- aminopropyltriethoxy dimethoxysilanes It is attached so that a part of region in silicon-carbide particle surface is covered by long chain macromolecule Polycarbosilane, secures Polycarbosilane molecule Relative position of the chain in silicon-carbide particle;Another part silicon-carbide particle is bonded little particle oxygen by VTES Change aluminium-yttrium oxide sintering aid;It is fine to turn into carborundum for the cracking of Polycarbosilane strand under 1700 DEG C -1800 DEG C of sintering temperature Dimension, " riveting " with other silicon-carbide particles is formed by the growth in liquefied alumina-yttria sintering aid, formed Decussating fibers grid and " crack deflection " mechanism in the alumina-yttria sintering aid of residual crystal boundary increase substantially it High-temperature mechanical property, and the reunion in liquid-phase sintering is avoided simultaneously, from the excessive carbon of particle " riveting " and silicon-carbide particle surface SiClx fiber may caused by space steric effect and the causing situation that is unfavorable for sintering occur.Help to obtain high intensity, height The silicon carbide ceramics of toughness.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1:Carborundum powder of the grain diameter between 0.5-5 microns is divided into etc. to two parts of A and B of quality, by A parts The Polycarbosilane of the mass percent of carborundum 5%, N- β (aminoethyl) -3- aminopropyltriethoxy dimethoxies of 1.1% mass percent Base silane, the toluene of 11% mass percent and A part carborundum mix, and are sufficiently stirred 30 minutes and at a temperature of 80 DEG C After drying 35 minutes, calcined in 300 DEG C of Muffle furnaces 20 minutes, temperature is then increased to 1100 DEG C and continues calcining 7 hours Furnace cooling obtains material I afterwards;By the auxiliary agent of the mass percent of B parts carborundum 6%, consisting of grain diameter is received 200 30wt%Al below rice2O3, 65wt%Y2O3And 5wt% VTESs, with B part carborundum in high-energy ball milling Mixing and ball milling obtains material II in 3 hours in machine;By material I, material II and material I, the 3wt% polyvinyl alcohol of material II gross masses Bonding agent in high energy ball mill mixing and ball milling after 5 hours by sieving, powder is fitted into cylindrical die under 200Mpa Stand 5 minutes and obtain biscuit.Biscuit is heat-treated 20 minutes at 250 DEG C, removes polyvinyl alcohol bonding agent.With 6 DEG C of heating speed Biscuit is warming up to 1700 DEG C in vacuum carbon tube furnace and is incubated 12 hours silicon carbide ceramics that high intensity, high tenacity is made by degree.
Embodiment 2:Carborundum powder of the grain diameter between 0.5-5 microns is divided into etc. to two parts of A and B of quality, by A parts The Polycarbosilane of the mass percent of carborundum 7%, N- β (aminoethyl) -3- aminopropyltriethoxy dimethoxys of 2% mass percent Silane, the toluene of 13% mass percent and A part carborundum mix, and are sufficiently stirred 40 minutes and at a temperature of 100 DEG C After drying 45 minutes, calcined in 320 DEG C of Muffle furnaces 30 minutes, temperature is then increased to 1200 DEG C and continues calcining 10 hours Furnace cooling obtains material I afterwards;By the auxiliary agent of the mass percent of B parts carborundum 10%, consisting of grain diameter is received 200 47wt%Al below rice2O3, 50wt%Y2O3And 3wt% VTESs, with B part carborundum in high-energy ball milling Mixing and ball milling obtains material II in 4 hours in machine;By material I, material II and material I, the 4wt% phenolic resin of material II gross masses Bonding agent in high energy ball mill mixing and ball milling after 7 hours by sieving, powder is fitted into cylindrical die under 230Mpa Stand 5 minutes and obtain biscuit.Biscuit is heat-treated 20 minutes at 250 DEG C, removes phenolic resin binder.With 7 DEG C of heating speed Biscuit is warming up to 1750 DEG C in vacuum carbon tube furnace and is incubated 15 hours silicon carbide ceramics that high intensity, high tenacity is made by degree.
Embodiment 3:Carborundum powder of the grain diameter between 0.5-5 microns is divided into etc. to two parts of A and B of quality, by A parts The Polycarbosilane of the mass percent of carborundum 10%, N- β (aminoethyl) -3- aminopropyltriethoxy diformazans of 2.8% mass percent TMOS, the toluene of 15% mass percent and A part carborundum mix, and are sufficiently stirred 50 minutes and in 120 DEG C of temperature After the lower drying of degree 55 minutes, calcined 40 minutes in 350 DEG C of Muffle furnaces, temperature is then increased to 1350 DEG C and continues calcining 15 Furnace cooling obtains material I after hour;By the auxiliary agent of the mass percent of B parts carborundum 15%, consisting of grain diameter exists Less than 200 nanometers of 65wt%Al2O3, 33wt%Y2O3And 2wt% VTESs, with B part carborundum in high energy Mixing and ball milling obtains material II in 5 hours in ball mill;By material I, material II and material I, the poly- second of 5wt% of material II gross masses Enol bonding agent in high energy ball mill mixing and ball milling after 10 hours by sieving, powder is fitted into cylindrical die 5 minutes, which are stood, under 250Mpa obtains biscuit.Biscuit is heat-treated 20 minutes at 250 DEG C, removes polyvinyl alcohol bonding agent.With 10 DEG C Programming rate in vacuum carbon tube furnace by biscuit be warming up to 1800 DEG C and be incubated the carbonization that high intensity, high tenacity is made in 20 hours Silicon ceramics.
Embodiment 4:Carborundum powder of the grain diameter between 0.5-5 microns is divided into etc. to two parts of A and B of quality, by A parts The Polycarbosilane of the mass percent of carborundum 7%, N- β (aminoethyl) -3- aminopropyltriethoxy dimethoxys of 2% mass percent Silane, the toluene of 12% mass percent and A part carborundum mix, and are sufficiently stirred 35 minutes and are dried at a temperature of 90 DEG C After dry 40 minutes, calcined in 300 DEG C of Muffle furnaces 25 minutes, temperature is then increased to 1120 DEG C and continued after calcining 7 hours Furnace cooling obtains material I;By the auxiliary agent of the mass percent of B parts carborundum 7%, consisting of grain diameter is at 200 nanometers Following 35wt%Al2O3, 62wt%Y2O3And 3wt% VTESs, with B part carborundum in high energy ball mill Middle mixing and ball milling obtains material II in 3 hours;By material I, material II and material I, the 3wt% polyvinyl alcohol knots of material II gross masses Mixture in high energy ball mill mixing and ball milling after 7 hours by sieving, powder is fitted into cylindrical die quiet under 200Mpa Put 5 minutes and obtain biscuit.Biscuit is heat-treated 20 minutes at 250 DEG C, removes polyvinyl alcohol bonding agent.With 6 DEG C of programming rate Biscuit is warming up to 1720 DEG C in vacuum carbon tube furnace and is incubated 15 hours silicon carbide ceramics that high intensity, high tenacity is made.
Embodiment 5:Carborundum powder of the grain diameter between 0.5-5 microns is divided into etc. to two parts of A and B of quality, by A parts The Polycarbosilane of the mass percent of carborundum 8%, N- β (aminoethyl) -3- aminopropyltriethoxy dimethoxies of 1.5% mass percent Base silane, the toluene of 11% mass percent and A part carborundum mix, and are sufficiently stirred 30 minutes and at a temperature of 90 DEG C After drying 35 minutes, calcined in 300 DEG C of Muffle furnaces 20 minutes, temperature is then increased to 1200 DEG C and continues calcining 7 hours Furnace cooling obtains material I afterwards;By the auxiliary agent of the mass percent of B parts carborundum 8%, consisting of grain diameter is received 200 45wt%Al below rice2O3, 50wt%Y2O3And 5wt% VTESs, with B part carborundum in high-energy ball milling Mixing and ball milling obtains material II in 4 hours in machine;By material I, material II and material I, the 3wt% phenolic resin of material II gross masses Bonding agent in high energy ball mill mixing and ball milling after 5 hours by sieving, powder is fitted into cylindrical die under 200Mpa Stand 5 minutes and obtain biscuit.Biscuit is heat-treated 20 minutes at 250 DEG C, removes phenolic resin binder.With 6 DEG C of heating speed Biscuit is warming up to 1750 DEG C in vacuum carbon tube furnace and is incubated 12 hours silicon carbide ceramics that high intensity, high tenacity is made by degree.

Claims (3)

1. a kind of manufacture method for strengthening liquid phase sintering silicon carbide ceramic using in-situ carburization silica fibre, it is characterised in that will be main Raw material carborundum powder such as is divided at two parts of A and B of quality, by Polycarbosilane, the 1-3% of A part carborundum 5-10% mass percents N- β (the aminoethyl) -3- aminopropyltriethoxies dimethoxysilane of mass percent, the toluene of 10-15% mass percents and A parts Carborundum mixes, after being sufficiently stirred 30-50 minutes and drying 30-60 minutes at a temperature of 80 DEG C -120 DEG C, 280 20-40 minutes are calcined in DEG C -350 DEG C of Muffle furnaces, temperature is then increased to 1100 DEG C -1350 DEG C and continues to calcine 5-15 hours Furnace cooling obtains material I afterwards;By the auxiliary agent of B part carborundum 5-15% mass percents, consisting of 30-70wt%Al2O3、 28-65wt%Y2O3And 2-5wt% VTESs, with B part carborundum mixing and ball milling 3-5 in high energy ball mill Hour obtains material II;By material I, material II and material I, material II gross masses 3-5wt% bonding agents in high energy ball mill By sieving, being molded after middle mixing and ball milling 5-10 hours, it is warming up to 5 DEG C -10 DEG C of programming rate in vacuum carbon tube furnace 1700 DEG C -1800 DEG C and it is incubated the silicon carbide ceramics that high intensity, high tenacity is made in 10-20 hours.
2. manufacture method according to claim 1, it is characterised in that the grain diameter of carborundum between 0.5-5 microns, Al2O3、Y2O3The particle scale of sintering aid is below 200 nanometers;Bonding agent is one kind in phenolic resin, polyvinyl alcohol.
3. manufacture method according to claim 1, shaping is that powder is placed in cylindrical die, in hydraulic press Static pressure is stripped to obtain biscuit for 5 minutes again under 200-250MPa pressure, and then biscuit is heat-treated 20 minutes at 250 DEG C, is removed Bonding agent.
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CN108911773A (en) * 2018-06-20 2018-11-30 浙江立泰复合材料股份有限公司 A kind of preparation method of silicon carbide fibre enhancing boron carbide ceramics material
CN110746193A (en) * 2019-10-16 2020-02-04 上海德宝密封件有限公司 Carbon fiber reinforced normal-pressure sintered silicon carbide
CN112250450A (en) * 2020-09-15 2021-01-22 航天特种材料及工艺技术研究所 Preparation method of heat insulation tile blank capable of resisting high temperature of 2000 DEG C
CN115385706A (en) * 2022-08-23 2022-11-25 广西三元华鑫特种陶瓷有限公司 Method for improving impact toughness of micro-nano fiber reinforced silicon carbide material

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CN101928148A (en) * 2009-07-20 2010-12-29 宁波大学 Method for manufacturing low-temperature high-density silicon carbide ceramics based on silane coupling agent
CN103864446A (en) * 2014-03-27 2014-06-18 中钢集团洛阳耐火材料研究院有限公司 Silicon carbide bonded carbon-containing fireproof material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
US20030064220A1 (en) * 2001-10-03 2003-04-03 Hiroyuki Yamaoka Silicon carbide fiber having boron nitride layer in fiber surface and process for the production thereof
CN101928148A (en) * 2009-07-20 2010-12-29 宁波大学 Method for manufacturing low-temperature high-density silicon carbide ceramics based on silane coupling agent
CN103864446A (en) * 2014-03-27 2014-06-18 中钢集团洛阳耐火材料研究院有限公司 Silicon carbide bonded carbon-containing fireproof material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108911773A (en) * 2018-06-20 2018-11-30 浙江立泰复合材料股份有限公司 A kind of preparation method of silicon carbide fibre enhancing boron carbide ceramics material
CN110746193A (en) * 2019-10-16 2020-02-04 上海德宝密封件有限公司 Carbon fiber reinforced normal-pressure sintered silicon carbide
CN112250450A (en) * 2020-09-15 2021-01-22 航天特种材料及工艺技术研究所 Preparation method of heat insulation tile blank capable of resisting high temperature of 2000 DEG C
CN115385706A (en) * 2022-08-23 2022-11-25 广西三元华鑫特种陶瓷有限公司 Method for improving impact toughness of micro-nano fiber reinforced silicon carbide material

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