CN107032813A - A kind of manufacturing process of fiber reinforced ceramic product - Google Patents

A kind of manufacturing process of fiber reinforced ceramic product Download PDF

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Publication number
CN107032813A
CN107032813A CN201610993524.4A CN201610993524A CN107032813A CN 107032813 A CN107032813 A CN 107032813A CN 201610993524 A CN201610993524 A CN 201610993524A CN 107032813 A CN107032813 A CN 107032813A
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fiber
fiber reinforced
reinforced ceramic
manufacturing process
ceramic product
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赵晓明
徐天文
许海嫚
薛蕾
王俊伟
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Xian Bright Laser Technologies Co Ltd
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Xian Bright Laser Technologies Co Ltd
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/24Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28CPREPARING CLAY; PRODUCING MIXTURES CONTAINING CLAY OR CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28C5/00Apparatus or methods for producing mixtures of cement with other substances, e.g. slurries, mortars, porous or fibrous compositions
    • B28C5/003Methods for mixing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28CPREPARING CLAY; PRODUCING MIXTURES CONTAINING CLAY OR CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28C5/00Apparatus or methods for producing mixtures of cement with other substances, e.g. slurries, mortars, porous or fibrous compositions
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    • C04B35/58Shaped 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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B2235/526Fibers characterised by the length of the fibers
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    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5264Fibers characterised by the diameter of the fibers

Abstract

The invention discloses a kind of manufacturing process of fiber reinforced ceramic product, ceramic material and fibrous material are mixed, fiber reinforcedceramics are obtained;Acrylate and epoxide are mixed, pre-mixed resin is obtained;Fiber reinforcedceramics are added in pre-mixed resin, then adds light trigger under conditions of lucifuge and stirs fiber reinforced ceramic slurry is made, finally, are stood under lucifuge, negative pressure or normal pressure;Using photocuring technology by fiber reinforced ceramic slurry shape needed for part blank, after by degreasing, sintering, obtain.The manufacturing process of fiber reinforced ceramic product of the present invention, realize the densification of product, reduce design of part complexity to the limitation of shaping, avoid fiber introduce with the problem of arrangement, realize the regulation on demand of fiber and matrix proportion, it is possible to reduce defect, raising precision and intensity.

Description

A kind of manufacturing process of fiber reinforced ceramic product
Technical field
The invention belongs to ceramic materials preparation technology field, and in particular to a kind of shaping side of fiber reinforced ceramic product Method.
Background technology
Ceramics have the advantages that hardness height, high temperature resistant, anti-oxidant, resistant to chemical etching, are the knots of application prospect extremely light Structure and functional material, but because it is in fragility, it is difficult to violent mechanical shock and thermal shock is born, its actual application potential is caused Receive serious constraint.It is this people by adding fiber into ceramic matrix, the method for fiber reinforced ceramic is made to it Fragility is improved.Fiber reinforced ceramic on the premise of original ceramic matrix performance is preserved to its fragility due to can change It is kind, the mechanical property such as raising intensity, toughness by a relatively large margin, and then receive from fields such as Aeronautics and Astronautics, national defense construction Extensive concern.
The shaping of existing fiber reinforced ceramic product, using in advance that the mixture briquet of fiber and ceramic matrix is right Sintering setting afterwards, or fiber introducing is carried out in shaping, the method for finally sintering setting is limited by its processing technology, can be deposited In following shortcoming:The structure of product is difficult to complicate;Introducing, the arrangement of fiber have difficulties;Part accuracy is poor, consistency is small, Low intensity.
The content of the invention
It is an object of the invention to provide a kind of manufacturing process of fiber reinforced ceramic product, solve what existing method was obtained The problem of there is the introducing of fiber in ceramic objectses, arrangement difficulty and part accuracy are poor, consistency is small.
The technical solution adopted in the present invention is, a kind of manufacturing process of fiber reinforced ceramic product, specifically according to following Step is implemented:
Step 1, it is 1.5-4 by volume by ceramic material and fibrous material:1 mixing, then adds dispersant in stirring It is uniformly mixed in machine, obtains fiber reinforcedceramics;
Step 2, it is 1-9 by volume by acrylate and epoxide:1 is well mixed, and obtains pre-mixed resin;
Step 3, fiber reinforcedceramics step 1 obtained are added in the pre-mixed resin that step 2 is obtained, then in lucifuge Under conditions of add light trigger, and stir fiber reinforced ceramic slurry be made, finally, under lucifuge, negative pressure or normal pressure 10-48h is stood, to exclude bubble therein;
Step 4, by the three-dimensional part model information to be formed handled well, import in optical soliton interaction equipment, utilize step 3 The blank of part needed for obtained fiber reinforced ceramic slurry is shaped, eventually passes degreasing, sintering, obtains fiber reinforced ceramic Product.
The features of the present invention is also resided in,
A diameter of 0.2-3 μm of ceramic powders in step 1;A diameter of 0.5-4 μm of fibrous material, length be 20-200 μ m。
The speed of mixer is 300-800rad/min in step 1, and mixing time is 1-4h;Dispersant total amount be fiber with The 0.1%-2% of ceramic gross mass.
Acrylate is methyl acrylate or 1,6 hexanediol diacrylate in step 2;Epoxide is sweet to shrink Grease based epoxy resin or cycloaliphatic epoxy resin.
Phase solvent and/or diluent are added in step 2 in pre-mixed resin.
The volume of fiber reinforcedceramics and pre-mixed resin is in step 3, fiber reinforcedceramics:Pre-mixed resin= 9:11-4:1。
Fiber reinforced ceramic slurry time of repose is 10-48h in step 3.
The fiber reinforcedceramics for obtaining step 1 in step 3 are gradually added the pre-mixed resin that step 2 is obtained by several times In, and when adding by several times, while adding defoamer, stir;Defoamer total amount is fiber and the 0.05%- of ceramic gross mass 0.5%, each mixing time 1-5h, stir speed (S.S.) is 100-600r/min.
Light trigger is free radical type initiator and cationic initiators using volume ratio as 1-9 in step 3:1 mixing and , wherein light trigger total amount is fiber and the 0.05%-1.5% of ceramic gross mass, stir speed (S.S.) 150-600r/min, stirring Time 1-3h.
Degreasing process is in step 4:In the environment of the protection of normal pressure, air or argon gas, with 0.1-2 DEG C/min heating speed Rate makes the temperature of blank be increased to furnace cooling after 400-700 DEG C, insulation 2-5h;Then vacuumize, then with 0.1-2 DEG C/min's Heating rate is increased to furnace cooling after 400-700 DEG C, insulation 2-5h.
Sintering process is in step 4:In the environment of argon gas protection, gas pressure 10-200MPa, with 5-10 DEG C/min's Heating rate is raised to furnace cooling after 1000-1800 DEG C, insulation 2-10h.
The beneficial effects of the invention are as follows, the manufacturing process of fiber reinforced ceramic product of the present invention, by by fibrous material with Ceramic matrix is uniformly blended into photosensitive resin by a certain percentage, the blank of product needed for being shaped using photocuring technology, then is passed through Degreasing, sintering realize the densification of product, reduce design of part complexity to the limitation of shaping, avoid fiber introduce with The problem of arrangement, the regulation on demand for realizing fiber and matrix proportion, it is possible to reduce defect, improve precision and intensity.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of manufacturing process of fiber reinforced ceramic product of the present invention, specifically implements according to following steps:
Step 1, it is that 20-200 μm of fibrous material is pressed by a diameter of 0.2-3 μm of ceramic material and a diameter of 0.5-4 μm, length Volume ratio is 1.5-4:1 mixing, then adds dispersant in mixer using speed as 300-800rad/min, stirs as 1- 4h, obtains fiber reinforcedceramics;Wherein dispersant total amount is fiber and the 0.1%-2% of ceramic gross mass;
Step 2, acrylate (methyl acrylate or 1,6- hexanediyl ester) (is shunk sweet with epoxide Grease based epoxy resin or cycloaliphatic epoxy resin) it is 1-9 by volume:1 mixing, then adds phase solvent (such as polyalcohol) And/or diluent (such as acrylic glycidol ether), using speed as 100-500rad/min in mixer, 1-4h is stirred, is obtained Obtain pre-mixed resin;
Step 3, fiber reinforcedceramics substep step 1 obtained is gradually added in the pre-mixed resin that step 2 is obtained (volume of fiber reinforcedceramics and pre-mixed resin is, fiber reinforcedceramics:Pre-mixed resin=9:11-4:1), every All add defoamer (such as mineral oil) when once adding and stir, the defoamer total amount of addition is fiber and ceramic gross mass 0.05%-0.5%, each mixing time 1-5h, stir speed (S.S.) is 100-600r/min;Light is added under conditions of lucifuge again Initiator, and stir fiber reinforced ceramic slurry is made, light trigger is free radical type initiator (such as dialkoxy benzene second Ketone, benzoin system etc.) with cationic initiators (such as sulfosalt, salt compounded of iodine) using volume ratio as 1-9:1 is obtained by mixing, wherein Light trigger total amount is fiber and the 0.05%-1.5%, stir speed (S.S.) 150-600r/min, mixing time 1- of ceramic gross mass 3h, finally, 10-48h is stood under lucifuge, negative pressure or normal pressure, to exclude bubble therein;
Step 4, by the three-dimensional part model information to be formed handled well, import in optical soliton interaction equipment, utilize step 3 The blank of part needed for obtained fiber reinforced ceramic slurry is shaped, eventually passes degreasing, sintering, obtains fiber reinforced ceramic Product.
Degreasing process is in step 4:In the environment of the protection of normal pressure, air or argon gas, with 0.1-2 DEG C/min heating speed Rate makes the temperature of blank be increased to furnace cooling after 400-700 DEG C, insulation 2-5h;Then vacuumize, then with 0.1-2 DEG C/min's Heating rate is increased to furnace cooling after 400-700 DEG C, insulation 2-5h.
Sintering process is in step 4:In the environment of argon gas protection, gas pressure 10-200MPa, with 5-10 DEG C/min's Heating rate is raised to furnace cooling after 1000-1800 DEG C, insulation 2-10h.
The present invention uses optical soliton interaction technology, passes through previously-introduced fiber and mixed uniformly method, it is to avoid fiber Introduce, arrangement and proportion adjustment problem, and relieve product shaping limited by its complex degree of structure.
Meanwhile, using the preparing process of above-mentioned slurry, ensure that slurry is 45-80% in volume fraction shared by its solid phase In the range of can obtain good mixed effect, in addition combined with above-mentioned degreasing, sintering process step, it is ensured that molded part With high consistency and adhesion strength, the comprehensive mechanical property of formation of parts is improved.
Embodiment 1
Optical soliton interaction fibre reinforced Al2O3Ceramic objectses
1. the preparation of fiber reinforcedceramics and the premixing of resin material.It is first according to Volume fraction, Al2O3Powder End:Fiber C=3:1 ratio, weighs 270g diameters 1um, length 50-100um fiber C and 1620g, d50=1um Al2O3 Powder, then adds 18.90g dispersants (fiber and the 1% of strong ceramic gross mass) in mixer with 300rad/min speed Rate, stirring 3h is well mixed the two, obtains fiber reinforcedceramics;By volume, acrylate:Epoxide=4: 1 ratio, measures methyl acrylate 320ml, ethylene oxidic ester 80ml, and add a small amount of phase solvent (polyalcohol), diluent (acrylic glycidol ether), with 150rad/min speed in mixer, pre-mixed resin is made in stirring 1h.
2. the preparation of fiber reinforced ceramic slurry.Fiber reinforcedceramics substep is gradually added in pre-mixed resin (fine Dimension strengthens ceramic material and the volume of pre-mixed resin is, fiber reinforcedceramics:Pre-mixed resin=3:2), added each time When all add defoamer (mineral oil) and stir, the defoamer total amount of addition is fiber and strong ceramic gross mass 0.5% (9.45g), each mixing time 3h, stir speed (S.S.) is 400r/min;Fiber and strong pottery are added under conditions of lucifuge again 1% light trigger (18.90g) of porcelain gross mass, and stir fiber reinforced ceramic slurry is made, light trigger is dioxane Epoxide acetophenone is with sulfosalt using volume ratio as 4:1 is obtained by mixing, and mixing parametric used is, stir speed (S.S.) 200r/min, stirs Mix time 2h;Finally, 24h is stood under the conditions of lucifuge.
3. the optical soliton interaction of fiber reinforced ceramic product blank.By the fiber C REINFORCED Al handled well2O3Ceramic slurry is filled Enter in optical soliton interaction equipment, and import treated three-dimensional part model to be formed, the blank of product needed for shaping.
4. it is degreasing sintered.Degreasing process is:Under normal pressure, ar gas environment, it is increased to 0.1 DEG C/min heating rate 400 DEG C, it is incubated furnace cooling after 2h;Then vacuumize, identical temperature is raised to identical heating rate, undergo equal guarantor Furnace cooling again after the warm time.Sintering process is:In the environment of argon pressure is 50MPa, with 5 DEG C/min heating rate It is raised to furnace cooling after 1520 DEG C, insulation 2h.
Embodiment 2
Optical soliton interaction SiC fiber reinforcements SiO2Ceramic objectses
1. the preparation of fiber reinforcedceramics and the premixing of resin material.Volume fraction after mixing is first according to, SiO2Powder:SiC fibers account for=4:1 ratio, weigh 325g diameters 4um, length 150-200um SiC fibers and 1144g, d50=2um SiO2Powder, then add 14.69g dispersants (fiber and the 1% of strong ceramic gross mass) in mixer with 500rad/min speed, stirring 2h is well mixed the two, obtains fiber reinforcedceramics;By volume, acrylate: Epoxide=17:3 ratio, measures 1,6- hexanediyl ester 297.5ml, cycloaliphatic epoxy resin 52.5ml, And a small amount of phase solvent (polyalcohol), diluent (acrylic glycidol ether) are added, with 200rad/min's in mixer Pre-mixed resin is made in speed, stirring 2h.
2. the preparation of fiber reinforced ceramic slurry.Fiber reinforcedceramics substep is gradually added in pre-mixed resin (fine Dimension strengthens ceramic material and the volume of pre-mixed resin is, fiber reinforcedceramics:Pre-mixed resin=13:7), add each time Fashionable all to add defoamer (mineral oil) and stir, the defoamer total amount of addition is fiber and strong ceramic gross mass 0.4% (5.876g), each mixing time 2.5h, stir speed (S.S.) is 350r/min;Again under conditions of lucifuge add fiber with 1% light trigger (14.69g) of strong ceramics gross mass, and stir fiber reinforced ceramic slurry is made, light trigger is two Alkoxy benzene ethyl ketone is with sulfosalt using volume ratio as 17:3 are obtained by mixing, and mixing parametric used is, stir speed (S.S.) 380r/min, Mixing time 2h;Finally, 12h is stood under conditions of lucifuge, pressure≤- 0.06MPa.
3. the optical soliton interaction of fiber reinforced ceramic product blank.By the SiC fiber reinforcements SiO handled well2Ceramic slurry It is fitted into optical soliton interaction equipment, and imports treated three-dimensional part model to be formed, the blank of product needed for shaping.
4. it is degreasing sintered.Degreasing process is:Under normal pressure, ar gas environment, 500 are increased to 1 DEG C/min heating rate DEG C, furnace cooling after insulation 2h;Then vacuumize, identical temperature is raised to identical heating rate, undergo equal insulation Furnace cooling again after time.Sintering process is:In the environment of argon pressure is 50MPa, with 10 DEG C/min heating rate It is raised to furnace cooling after 1000 DEG C, insulation 10h.
Embodiment 3
Optical soliton interaction SiC fiber reinforcements Si3N4Ceramic objectses
1. the preparation of fiber reinforcedceramics and the premixing of resin material.Volume fraction after mixing is first according to, Si3N4Powder:SiC fiber=7:3 ratio, weigh 562.5g diameters 3um, length 100-150um SiC fibers and 1680g, d50=3um Si3N4Particle, then adds 11.2125g dispersants (fiber and the 0.5% of strong ceramic gross mass) in mixer The interior speed with 400rad/min, stirring 2.5h is well mixed the two;By volume, acrylate:Epoxide= 1.5:1 ratio, measures methyl acrylate 150ml, cycloaliphatic epoxy resin 100ml, and it is (polynary to add a small amount of phase solvent Alcohol), diluent (acrylic glycidol ether), with 300rad/min speed in mixer, stirring 1.5h be made premix tree Fat, is made pre-mixed resin.
2. fiber reinforcedceramics substep is gradually added into (fiber reinforcedceramics and pre-mixed resin in pre-mixed resin Volume be, fiber reinforcedceramics:Pre-mixed resin=3:1), defoamer (mineral oil) is all added simultaneously when adding each time Stir, the defoamer total amount of addition is fiber and 0.05% (1.1213g) of strong ceramic gross mass, each mixing time 2h, stir speed (S.S.) is 200r/min;Fiber and 0.5% light trigger of strong ceramic gross mass are added under conditions of lucifuge again (11.2125g), and stir fiber reinforced ceramic slurry is made, light trigger be Dialkoxy acetophenones with sulfosalt with Volume ratio is 1.5:1 is obtained by mixing, and mixing parametric used is, stir speed (S.S.) 420r/min, mixing time 1.5h;Finally, exist 12h is stood under conditions of lucifuge, pressure≤- 0.06MPa.
3. the optical soliton interaction of fiber reinforced ceramic product blank.By the SiC fiber reinforcements Si handled well3N4Ceramic slurry It is fitted into optical soliton interaction equipment, and imports treated three-dimensional part model to be formed, the blank of product needed for shaping.
4. it is degreasing sintered.Degreasing process is:Under normal pressure, air ambient, it is increased to 1.5 DEG C/min heating rate 700 DEG C, it is incubated furnace cooling after 2h;Then vacuumize, identical temperature is raised to identical heating rate, undergo equal guarantor Furnace cooling again after the warm time.Sintering process is:In the environment of argon pressure is 100MPa, with 5 DEG C/min heating speed Rate is raised to furnace cooling after 1650 DEG C, insulation 2h.
Embodiment 4
Optical soliton interaction SiC fiber reinforcements SiO2Ceramic objectses
1. the preparation of fiber reinforcedceramics and the premixing of resin material.Volume fraction after mixing is first according to, SiO2Powder:SiC fiber=1.5:1 ratio, weighs 450g diameters 0.5um, length 20-50um fiber C and 594g, d50= 0.2um SiO2Powder, then add 20.88g dispersants (fiber and the 2% of strong ceramic gross mass) in mixer with 600rad/min speed, stirring 1h is well mixed the two, obtains fiber reinforcedceramics;By volume, acrylate: Epoxide=9:1 ratio, measures methyl acrylate 495ml, cycloaliphatic epoxy resin 55ml, and add a small amount of mix Agent (polyalcohol), diluent (acrylic glycidol ether), with 100rad/min speed in mixer, stirring 3h is made pre- Mixed resin.
2. the preparation of fiber reinforced ceramic slurry.Fiber reinforcedceramics substep is gradually added in pre-mixed resin (fine Dimension strengthens ceramic material and the volume of pre-mixed resin is, fiber reinforcedceramics:Pre-mixed resin=9:11), add each time Fashionable all to add defoamer (mineral oil) and stir, the defoamer total amount of addition is fiber and strong ceramic gross mass 0.4% (8.352g), each mixing time 1h, stir speed (S.S.) is 100r/min;Fiber is added under conditions of lucifuge again and strong 1.5% light trigger (31.32g) of ceramic gross mass, and stir fiber reinforced ceramic slurry is made, light trigger is two Alkoxy benzene ethyl ketone is with sulfosalt using volume ratio as 9:1 is obtained by mixing, and mixing parametric used is, stir speed (S.S.) 150r/min, Mixing time 1h;Finally, 10h is stood under lucifuge, normal pressure.
3. the optical soliton interaction of fiber reinforced ceramic product blank.By the SiC fiber reinforcements SiO handled well2Ceramic slurry It is fitted into optical soliton interaction equipment, and imports treated three-dimensional part model to be formed, the blank of product needed for shaping.
4. it is degreasing sintered.Degreasing process is:Under normal pressure, ar gas environment, 500 are increased to 1 DEG C/min heating rate DEG C, furnace cooling after insulation 3h;Then vacuumize, identical temperature is raised to identical heating rate, undergo equal insulation Furnace cooling again after time.Sintering process is:In the environment of argon pressure is 10MPa, with 8 DEG C/min heating rate liter To 1800 DEG C, furnace cooling after insulation 6h.
Embodiment 5
Optical soliton interaction SiC fiber reinforcements Si3N4Ceramic objectses
1. the preparation of fiber reinforcedceramics and the premixing of resin material.Volume fraction after mixing is first according to, Si3N4Powder:SiC fiber=3:1 ratio, weighs 500g diameters 2um, length 50-100um SiC fibers and 1920g, d50 =1.5um Si3N4Particle, then add 24.2g dispersants (fiber and the 1% of strong ceramic gross mass) in mixer with 800rad/min speed, stirring 4h is well mixed the two;By volume, acrylate:Epoxide=1:1 ratio Example, measures 1,6- hexanediyl ester 100ml, glycidyl ester epoxy resin 100ml, and add a small amount of phase solvent (polyalcohol), diluent (acrylic glycidol ether), with 500rad/min speed in mixer, premix is made in stirring 4h Resin, is made pre-mixed resin.
2. fiber reinforcedceramics substep is gradually added into (fiber reinforcedceramics and pre-mixed resin in pre-mixed resin Volume be, fiber reinforcedceramics:Pre-mixed resin=4:1), defoamer (mineral oil) is all added simultaneously when adding each time Stir, the defoamer total amount of addition is fiber and 0.1% (2.42g), each mixing time 5h of strong ceramic gross mass, is stirred Speed is mixed for 600r/min;Fiber and 0.05% light trigger of strong ceramic gross mass are added under conditions of lucifuge again (1.21g), and stir fiber reinforced ceramic slurry is made, light trigger be Dialkoxy acetophenones with sulfosalt with volume Than for 3:1 is obtained by mixing, and mixing parametric used is, stir speed (S.S.) 600r/min, mixing time 3h;Finally, in lucifuge, pressure 48h is stood under conditions of≤- 0.06MPa.
3. the optical soliton interaction of fiber reinforced ceramic product blank.By the SiC fiber reinforcements Si handled well3N4Ceramic slurry It is fitted into optical soliton interaction equipment, and imports treated three-dimensional part model to be formed, the blank of product needed for shaping.
4. it is degreasing sintered.Degreasing process is:Under normal pressure, air ambient, 400 are increased to 2 DEG C/min heating rate DEG C, furnace cooling after insulation 5h;Then vacuumize, identical temperature is raised to identical heating rate, undergo equal insulation Furnace cooling again after time.Sintering process is:In the environment of argon pressure is 200MPa, with 6 DEG C/min heating rate It is raised to furnace cooling after 1300 DEG C, insulation 8h.

Claims (10)

1. a kind of manufacturing process of fiber reinforced ceramic product, it is characterised in that comprise the following steps:
Step 1, it is 1.5-4 by volume by ceramic material and fibrous material:1 mixing, then adds dispersant in mixer It is uniformly mixed, obtains fiber reinforcedceramics;
Step 2, it is 1-9 by volume by acrylate and epoxide:1 is well mixed, and obtains pre-mixed resin;
Step 3, fiber reinforcedceramics step 1 obtained are added in the pre-mixed resin that step 2 is obtained, then in the bar of lucifuge Light trigger is added under part, and stirs fiber reinforced ceramic slurry is made, finally, is stood under lucifuge, negative pressure or normal pressure, To exclude bubble therein;
Step 4, by the three-dimensional part model information to be formed handled well, import in optical soliton interaction equipment, obtained using step 3 Fiber reinforced ceramic slurry shape needed for part blank, eventually pass degreasing, sintering, obtain fiber reinforced ceramic system Part.
2. the manufacturing process of fiber reinforced ceramic product according to claim 1, it is characterised in that ceramic powder in step 1 A diameter of 0.2-3 μm of end;A diameter of 0.5-4 μm of fibrous material, length be 20-200 μm.
3. the manufacturing process of fiber reinforced ceramic product according to claim 1 or 2, it is characterised in that stirred in step 1 The speed of machine is 300-800rad/min, and mixing time is 1-4h;Dispersant total amount is fiber and the 0.1%- of ceramic gross mass 2%.
4. the manufacturing process of fiber reinforced ceramic product according to claim 1, it is characterised in that acrylic acid in step 2 Ester is methyl acrylate or 1,6 hexanediol diacrylate;Epoxide is glycidyl ester epoxy resin or alicyclic Epoxy resin.
5. the manufacturing process of the fiber reinforced ceramic product according to claim 1 or 4, it is characterised in that pre- in step 2 Phase solvent and/or diluent are added in mixed resin.
6. the manufacturing process of fiber reinforced ceramic product according to claim 1, it is characterised in that fiber increases in step 3 The volume ratio of strong ceramic material and pre-mixed resin is 9:11-4:1;The fiber reinforced ceramic slurry time of repose is 10-48h.
7. the manufacturing process of the fiber reinforced ceramic product according to claim 1 or 6, it is characterised in that will step in step 3 Rapid 1 obtained fiber reinforcedceramics are gradually added in the pre-mixed resin that step 2 is obtained by several times, and when adding by several times, simultaneously Defoamer is added, is stirred;Defoamer total amount is fiber and the 0.05%-0.5%, each mixing time 1- of ceramic gross mass 5h, stir speed (S.S.) is 100-600r/min.
8. the manufacturing process of fiber reinforced ceramic product according to claim 1, it is characterised in that light-initiated in step 3 Agent is free radical type initiator and cationic initiators using volume ratio as 1-9:1 is obtained by mixing, and wherein light trigger total amount is Fiber and the 0.05%-1.5%, stir speed (S.S.) 150-600r/min, mixing time 1-3h of ceramic gross mass.
9. the manufacturing process of fiber reinforced ceramic product according to claim 1, it is characterised in that degreasers in step 4 Skill is:In the environment of the protection of normal pressure, air or argon gas, the temperature for making blank with 0.1-2 DEG C/min heating rate is increased to 400-700 DEG C, it is incubated furnace cooling after 2-5h;Then vacuumize, then 400- is increased to 0.1-2 DEG C/min heating rate 700 DEG C, it is incubated furnace cooling after 2-5h.
10. the manufacturing process of the fiber reinforced ceramic product according to claim 1 or 9, it is characterised in that burnt in step 4 Knot technique is:In the environment of argon gas protection, gas pressure 10-200MPa is raised to 1000- with 5-10 DEG C/min heating rate 1800 DEG C, it is incubated furnace cooling after 2-10h.
CN201610993524.4A 2016-11-08 2016-11-08 A kind of manufacturing process of fiber reinforced ceramic product Pending CN107032813A (en)

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