CN110451985A - A kind of photocuring silicon carbide ceramics creme and preparation method thereof - Google Patents

A kind of photocuring silicon carbide ceramics creme and preparation method thereof Download PDF

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CN110451985A
CN110451985A CN201910791463.7A CN201910791463A CN110451985A CN 110451985 A CN110451985 A CN 110451985A CN 201910791463 A CN201910791463 A CN 201910791463A CN 110451985 A CN110451985 A CN 110451985A
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powder
sic
mixed
mixing
silicon carbide
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王克杰
鲍崇高
宋索成
许海嫚
卢秉恒
赵纪元
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National Institute Corp of Additive Manufacturing Xian
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National Institute Corp of Additive Manufacturing Xian
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00Materials specially adapted for additive manufacturing
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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
    • C04B35/515Shaped 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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    • 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
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802Powder coating materials
    • C04B35/62805Oxide ceramics
    • C04B35/62807Silica or silicates
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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
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
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Abstract

The invention discloses a kind of photocuring silicon carbide ceramics creme and preparation method thereof, which is made of the mixing of SiC mixed-powder, dispersing agent, monomer, compatilizer and photoinitiator;Wherein the surface of SiC mixed-powder is coated with SiO2Layer reduces refractive index difference between final creme and light-cured resin, and then improves printing effect;SiO2It can be improved the solid concentration of entire slurry, and then in follow-up sintering ceramics, can be improved the mechanical property of the sintered density and finally formed ceramics that are sintered out ceramics;On the one hand dispersing agent is added in the slurry can reduce the agglomeration of slurry, improve dispersibility, on the other hand can be improved the solid concentration of entire slurry;Verifying finds that the solid concentration in the creme can finally reach 40%~60%.

Description

A kind of photocuring silicon carbide ceramics creme and preparation method thereof
[technical field]
The invention belongs to silicon carbide (SiC) creme preparation technical fields, and in particular to a kind of photocuring silicon carbide ceramics Creme and preparation method thereof.
[background technique]
Stereolithography (SLA) is the major technique of ceramic 3D printing currently on the market, and commercialization succeeds relatively Technology.The technology uses a kind of optic-solidified adhesive mixed by ceramic powders, photoinitiator, dispersing agent etc., ultraviolet source Solidified resin is successively scanned according to certain scan path, until printing is completed.SLA stereolithography ceramic technology feature are as follows: Not only reduced cost significantly, and performance is stablized, and has the characteristics that sterile ceramic density is high.Silicon carbide ceramics has antioxygen The property changed is strong, and wear-resisting property is good, and hardness is high, and thermal stability is good, and elevated temperature strength is big, and thermal expansion coefficient is small, and thermal conductivity is big and heat resistanceheat resistant Shake and equal good characteristics resistant to chemical etching.Therefore, it is answered extensively in fields such as petroleum, chemical industry, machinery, aerospace, nuclear energy With being increasingly subject to the attention of people.For example, SiC ceramic can be used as each class bearing, ball, nozzle, sealing element, cutting element, combustion Steam turbine blade, turbocharger rotor, radiation shield and rocket chamber liner etc..
The traditional production method of silicon carbide ceramics has a compression molding, pressureless sintering, hot pressed sintering, HIP sintering and anti- Should be sintered with presoma cracking the methods of.However all there are complex procedures in varying degrees, long in time limit, die wear is big equal scarce Point, it is difficult to realize the design requirement of complex parts.Photocuring technology passes through the method that material gradually adds up, from bottom to top, successively Printing, realizes the manufacturing of entity component, is not necessarily to mold, components produced, not only precision is high, simple process, with biography System manufacturing process is compared, and is also had the characteristics that at low cost, the period is short, molding is diversified, is a kind of with higher formed precision Silicon carbide ceramics forming method.
Photocuring is more difficult relative to the development of other ceramic paste materials with silicon carbide ceramics creme, one side carborundum powder It is difficult the white for having aluminium oxide, zirconium oxide, causes its refractive index higher, is not easy to find matched resin to solidify.It is another Aspect is in order to improve the sintering character of silicon carbide ceramics, it is necessary to improve the solid content of creme, this just needs to reduce the viscosity of creme. Therefore the refractive index difference between monomer and carborundum powder how is reduced, the viscosity of creme is reduced while improving solid content, Play the role of for the printing of photocuring silicon carbide ceramics conclusive.
Application No. is the patent documents of CN108285347A to disclose a kind of 3D printing photocuring ceramic particle and its preparation Method, comprising: the clad for being coated on the ceramic matrix surface is resin layer, and refractive index is 1.40~1.55.The packet Coating with a thickness of 30nm;The resin is selected from paraffin, polyacrylic resin, epoxy resin, alkyd resin, polyvinyl chloride and conjunction At one of fatty acid or a variety of;The patent is a kind of particle surface modification method, is not directed to the preparation of creme, and is made pottery Surface coated porcelain powder is resin, can reduce subsequent creme solid content be unfavorable for follow-up sintering and improve ceramics density with Performance.
[summary of the invention]
It is an object of the invention to overcome the above-mentioned prior art, a kind of photocuring silicon carbide ceramics creme is provided And preparation method thereof;The refractive index difference of the silicon carbide ceramics creme is low, improves the solid content of slurry, is conducive to follow-up sintering Process.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of photocuring silicon carbide ceramics creme, which is characterized in that the silicon carbide ceramics creme includes SiC mixed powder End, dispersing agent, monomer, compatilizer and photoinitiator;The surface of the SiC mixed-powder is coated with SiO2Layer, compatibilizer content It is the 1.5%~3.0% of SiC mixed-powder quality, dispersant is the 0.5%~1.0% of SiC mixed-powder quality, single Body content is the 23.1%~52.3% of SiC mixed-powder quality, and photoinitiator levels are 2.0~4.0wt% of monomer mass.
A further improvement of the present invention is that:
Preferably, the SiC mixed-powder is the spherical SiC powder of d50=0.4um and the spherical SiC of d50=2.5um The surface of the mixture of powder, two spherical SiC powders is coated with SiO2Layer;The ball of d50=0.4um in SiC mixed-powder The quality accounting of shape SiC powder is 20%~50%, and surplus is the spherical SiC powder of d50=2.5um.
Preferably, SiO2Layer with a thickness of 5-15nm.
Preferably, the compatilizer is stearic acid.
Preferably, the dispersing agent be one of Y- glycidyl ether oxygen propyl trimethoxy silicane and Digao 685 or Two kinds of mixture.
Preferably, monomer 1,6 hexanediyl esters, poly- two or six acrylate and trimethylolpropane tris acrylic acid The mixture of ester.
Preferably, 1,6 hexanediyl esters, poly- two or six acrylate and trimethylolpropane trimethacrylate it is mixed Conjunction mass ratio is 7:1:2.
Preferably, one kind of photoinitiator 2,2- dimethoxy -2- phenyl acetophenone and 2- isopropyl thioxanthone or The mixture that two kinds of person.
A kind of preparation method of above-mentioned photocuring silicon carbide ceramics creme, comprising the following steps:
Step 1, one layer of SiO is coated on the SiC powder surface of two kinds of partial sizes respectively by chemical vapour deposition technique2, two kinds The SiC powder of partial size is respectively the spherical SiC powder of d50=0.4um and the spherical SiC powder of d50=2.5um;
Step 2, surface is coated with SiO2The SiC powders of two kinds of partial sizes mix in the ball mill, in mixed process plus Enter stearic acid, obtains SiC mixed-powder;
Step 3, SiC mixed-powder, dispersing agent, monomer, compatilizer and photoinitiator are weighed respectively;
Step 4, SiC mixed-powder, dispersing agent, compatilizer and photoinitiator that step 3 weighs are mixed and stirred for uniformly, Obtain mixture;
Step 5, the mixture and monomer step 4 obtained is uniformly mixed in homogeneous batch mixer, after defoaming, is made A kind of photocuring silicon carbide ceramics creme.
Preferably, in step 5, blending process includes with the next stage in homogeneous batch mixer:
Stage 1, with revolving speed 1000rmin-1After mixing 15s, with 2800rmin-1Mix 20s;Stage 2, with revolving speed 2800r·min-1After mixing 20s, with 2000rmin-1Mix 20s;Stage 3, with revolving speed 2000rmin-1After mixing 20s, With 1500rmin-1Mix 10s;Stage 4, with revolving speed 1500rmin-1After mixing 10s, with 800rmin-1Mix 15s.
Compared with prior art, the invention has the following advantages:
The invention discloses a kind of photocuring silicon carbide ceramics cremes, and the creme is by SiC mixed-powder, dispersing agent, list Body, compatilizer and photoinitiator mixing composition;Wherein the surface of SiC mixed-powder is coated with SiO2Layer, SiO2As clad, Itself refractive index is lower, works as SiO2When being coated to surface of SiC, directly participating in cured medium is SiO2With resin (monomer) table Face, therefore the high refractive index difference interface of SiC and resin is effectively avoided, it reduces and is rolled between final creme and light-cured resin Rate difference is penetrated, and then improves printing effect;SiO2It can be improved the curing depth of entire slurry, and then in follow-up sintering ceramics When, it can be improved the mechanical property of the sintered density and finally formed ceramics that are sintered out ceramics;It is added and divides in the slurry On the one hand powder can reduce the agglomeration of slurry, improve dispersibility, and the solid phase that on the other hand can be improved entire slurry contains Amount;Monomer is resin, can be bonded together ceramic powder, and main function is to play solidification;Compatilizer effect is to make It obtains powder and resin preferably combines, and then obtain stable blend;Photoinitiator can absorb certain wavelength in ultraviolet region Energy, generate free radicals, cation etc., to cause monomer polymerization crosslinking curing, to enable creme curing molding;It tests Card discovery, monomer, dispersing agent, compatilizer and photoinitiator is mixed according to a certain percentage, the solid concentration in the creme is most 40%~60% can be reached eventually.
Further, the SiC powder in the present invention uses grain composition, is mixed, is being eventually formed by two kinds of powder Slurry in, short grained SiC powder can fill the SiC powder of bulky grain full, improve the global density of slurry, mention simultaneously The solid concentration of high slurry.
Further, SiO2Layer with a thickness of 5-15nm, SiO2Layer is excessively thin can not to be played the role of reducing refractive index, blocked up The quality that will affect SiC reduces the content of SiC.
Further, compatilizer is stearic acid, the reunion for preventing powder is added when SiC dried bean noodles is ground early period, the later period makes SiC powder is preferably combined with resin.
Further, dispersing agent selects one of glycidyl ether oxygen propyl trimethoxy silicane and Digao 685 or two The mixture of kind, because of glycidyl ether oxygen propyl trimethoxy silicane, silane coupling agent is firmly combined on the surface of SiC, It is added to inside resin, the other end of epoxy group of coupling agent can make with the carboxyl in resin, amino groups reaction SiC powder and resin are firmly combined together by chemical bond;Digao 685 plays the peptizaiton to powder, can be significant Reduce creme viscosity.
Further, monomer 1,6 hexanediyl esters, poly- two or six acrylate and trimethylolpropane tris propylene Acid esters can play the role of letdown resin system, poly- two or six propylene because 1,6 hexanediyl ester concentration is relatively low The intensity for solidifying idiosome can be improved in acid esters, and trimethylolpropane trimethacrylate belongs to high functional group's resin, can be improved solid Change efficiency.
Further, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone and 2- isopropyl thioxanthone, 2,2- bis- Methoxyl group -2- phenyl acetophenone is a kind of efficient ultraviolet light curing initiator, is mainly used as the initiation of ultraviolet light curing reaction Agent, 2- isopropyl thioxanthone is also a kind of photoinitiator, and surface layer initiation effect is extremely significant.
The invention also discloses a kind of photocuring preparation method of silicon carbide ceramics creme, the preparation method passes through table The silica method that bread covers low-refraction reduces the printing of refractive index difference and then raising creme between creme and light-cured resin Efficiency.Simultaneously by the method for spherical carbide silicon particle gradation, small particle silicon carbide powder is made to be adequately filled in big partial size carbonization Between Si powder, the solid concentration of photocuring silicon carbide ceramics creme is improved, to improve the service performance of later product;The system Preparation Method step is simple, and mixing time is shorter, and by homogeneous mixing, is uniformly mixed, so that entire manufacturing cycle is shorter, benefit In industrialization promotion.
In mixed process, using the mixing procedure of high revolving speed short time, the stringent each stage limited in mixing process turns Speed and time, it is ensured that process material is controllable, to prepare uniform photocuring with stable silicon carbide ceramics creme.
[Detailed description of the invention]
Fig. 1 is SiC creme state diagram of the invention;Wherein, (a) figure is the shooting figure at visual angle 1;(b) figure is the bat at visual angle 2 Take the photograph figure;
Fig. 2 is the solidification test chart for the creme that the present invention prepares;
Fig. 3 is the energy spectrum analysis figure for the nano particle that the present invention prepares;Wherein, (a) figure is the energy spectrum analysis figure of A point; (b) figure is the energy spectrum analysis figure of B point;(c) figure is the energy spectrum analysis figure of C point;(d) figure is the energy spectrum analysis figure of D point;(e) figure is Get the location drawing ready.
Fig. 4 is the Analysis of Surface Topography figure for the nano particle that the present invention prepares;
[specific embodiment]
The invention will be described in further detail in the following with reference to the drawings and specific embodiments, and it is solid that the invention discloses a kind of light Change with silicon carbide ceramics creme and preparation method thereof, comprising the following steps:
Step 1, the SiC powder of two kinds of partial sizes is carried out surface to be modified, and coats certain SiO on surface2
Choose the spherical SiC powder of two kinds of size gradings, the spherical SiC powder and d50=of respectively d50=0.4um The spherical SiC powder of 2.5um;By chemical vapor deposition layer (CVD) technique respectively in the SiC powder outer cladding of two kinds of partial sizes SiO2Layer, SiO during cladding2Powder accounts for the 4-8% of all powder quality, and surplus is to be wrapped by powder;Coated by CVD When the spherical SiC powder of d50=0.4um, SiO2The quality accounting of powder is 4-8%, remaining is the spherical SiC of d50=0.4um Powder, when coating the spherical SiC powder of d50=2.5um by CVD, SiO2The quality accounting of powder is 4-8%, remaining is d50 The spherical SiC powder of=2.5um.The SiO being wrapped by2Layer with a thickness of 5-15nm.
Step 2, ball milling mixing
Be wrapped by two kinds of powder are put into ball mill, when mixing is coated with SiO2The SiC of the d50=0.4um of layer Powder quality accounting is 20-50%, and surplus is to be coated with SiO2The SiC powder of the d50=2.5um of layer forms mixing SiC powder End;The stearic acid that mixing SiC powder quality 1% is added in mixing SiC powder carries out ball milling, Ball-milling Time 12h, and revolving speed is 360r/min, so that the SiC powder of two kinds of partial sizes mixes well, ultimately forms uniform SiC mixed-powder by ball milling.
Step 3, SiC mixed-powder, dispersing agent, monomer, compatilizer and photoinitiator are weighed respectively, wherein SiC mixed powder It is handled after end is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 1.5wt%~3.0wt%, dispersing agent Content be SiC mixed-powder 0.5wt%~1.0wt%, content of monomer be SiC mixed-powder 23.1wt%~ 52.3wt%, photoinitiator levels are 2.0wt%~4.0wt% of monomer mass;Compatilizer is stearic acid;Dispersing agent Y- shrinks One or both of glycerol ether oxygen propyl trimethoxy silicane or Digao 685 mixture mix matter when for two kinds of mixtures Amount is than being (1.3~2): 1;Monomer is 1,6 hexanediyl esters (HDDA), poly- two or six acrylate (DPHA) and three hydroxyl first The mixture of base propane triacrylate (TMPTA), mixing mass ratio 7:1:2.Photoinitiator is 2,2- dimethoxy -2- One or two kinds of mixture of phenyl acetophenone or 2- isopropyl thioxanthone, when for two kinds of mixtures, mixing quality Than for (1~2): 1.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture;
Step 5, the mixture and monomer step 4 obtained mixes, and stirs simultaneously in mixed process, homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage:
Stage 1, with revolving speed 1000rmin-1After mixing 15s, with 2800rmin-1Mix 20s;
Stage 2, with revolving speed 2800rmin-1After mixing 20s, with 2000rmin-1Mix 20s;
Stage 3, with revolving speed 2000rmin-1After mixing 20s, with 1500rmin-1Mix 10s;
Stage 4, with revolving speed 1500rmin-1After mixing 10s, with 800rmin-1Mix 15s.
After homogeneous mixing, the bubble in creme is removed, a kind of photocuring silicon carbide porcelain creme is made.
Embodiment 1
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 8nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 20%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 1g, monomer 34.69g, compatilizer 3g and photoinitiator are weighed respectively 0.69g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 3wt%, dispersant are the 1wt% of SiC mixed-powder, and content of monomer is the 34.69wt% of SiC mixed-powder, light-initiated Agent content is the 2wt% of monomer mass;Compatilizer is stearic acid, dispersing agent is Digao 685, monomer HDDA, DPHA and TMPTA Mixture, mixing mass ratio 7:1:2, photoinitiator be 2- isopropyl thioxanthone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are stirred, are mixed Close object.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 49.8%.
The creme prepared by the embodiment as shown in Figure 1, it can be seen from the figure that the mobility of the creme is preferable, And modest viscosity.
Creme prepared by the embodiment is done into solidification test, after result is as shown in Fig. 2, as can be seen from the figure solidify Solidification test is with a thickness of 60um.
(e) figure in Fig. 3 is the energy got position ready, scheme that (a)-figure (d) is corresponding different location that energy spectrum analysis carries out Spectrogram, it can be seen from the figure that oxygen content is apparently higher than close to centre close to the A point (figure (a)) and D point (figure (d)) of outer layer The oxygen content of B point is schemed (b);And the oxygen content for scheming (c) corresponding C point is then between B point and A point;It can from figure SiC particulate surface oxygen content is apparently higher than inside out, illustrates Surface Creation SiO2
Fig. 4 is that surface is coated with SiO in step 1 in the embodiment2SiC particulate surface topography map, can be with from figure Find out, particle be divided into it is inside and outside, and be two kinds of substances, from energy spectrum analysis above it can be concluded that outside is SiO2, interior The substance in portion is SiC.
Embodiment 2
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 8nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 30%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.7g, monomer 23.1g, compatilizer 2.5g and light-initiated are weighed respectively Agent 0.46g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 2.5wt%, dispersant are the 0.7wt% of SiC mixed-powder, and content of monomer is the 23.1wt% of SiC mixed-powder, and light draws Send out the 2wt% that agent content is monomer mass;Compatilizer is stearic acid, dispersing agent is Y- glycidol ether that mass ratio is 1.5:1 The mixture of oxygen propyl trimethoxy silicane and the mixture of Digao 685, monomer HDDA, DPHA and TMPTA, mixing quality Than for 7:1:2, photoinitiator is 2, the 2- dimethoxy -2- phenyl acetophenone and 2- isopropyl thioxanthone that mass ratio is 1:1 Mixture.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 60%.
Embodiment 3
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 10nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 40%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.6g, monomer 30g, compatilizer 1.5g and photoinitiator are weighed respectively 0.66g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 1.5wt%, dispersant are the 0.6wt% of SiC mixed-powder, and content of monomer is the 30wt% of SiC mixed-powder, light-initiated Agent content is the 2.2wt% of monomer mass;Compatilizer is stearic acid, dispersing agent is Y- glycidyl ether oxygen propyl trimethoxy silicon The mixture of alkane, monomer HDDA, DPHA and TMPTA, mixing mass ratio 7:1:2, photoinitiator 2,2- dimethoxy- 2- phenyl acetophenone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 53.6%.
Embodiment 4
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 5nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 20%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.5g, monomer 40g, compatilizer 1.8g and photoinitiator are weighed respectively 0.96g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 1.8wt%, dispersant are the 0.5wt% of SiC mixed-powder, and content of monomer is the 40wt% of SiC mixed-powder, light-initiated Agent content is the 2.4wt% of monomer mass;Compatilizer is stearic acid, dispersing agent be Digao 685, monomer HDDA, DPHA and The mixture of TMPTA, mixing mass ratio 7:1:2, photoinitiator are 2- isopropyl thioxanthone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 46.5%.
Embodiment 5
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 11nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 30%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.8g, monomer 23.1g, compatilizer 1.7g and light-initiated are weighed respectively Agent 0.58g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 1.7wt%, dispersant are the 0.8wt% of SiC mixed-powder, and content of monomer is the 23.1wt% of SiC mixed-powder, and light draws Send out the 2.51wt% that agent content is monomer mass;Compatilizer is stearic acid, dispersing agent is that the Y- mixed according to mass ratio 1.3:1 contracts The mixture of water glycerol ether oxygen propyl trimethoxy silicane and the mixture of Digao 685, monomer HDDA, DPHA and TMPTA, Mixing mass ratio is 7:1:2, photoinitiator is according to mass ratio be 2:1 mixing 2,2- dimethoxy -2- phenyl acetophenone and The mixture of 2- isopropyl thioxanthone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 60%.
Embodiment 6
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 12nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 50%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.9g, monomer 25g, compatilizer 1.9g and photoinitiator are weighed respectively 0.63g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 1.9wt%, dispersant are the 0.9wt% of SiC mixed-powder, and content of monomer is the 25wt% of SiC mixed-powder, light-initiated Agent content is the 2.52wt% of monomer mass;Compatilizer is stearic acid, dispersing agent is that the Y- shrink that mix according to mass ratio 2:1 is sweet The mixture of oily ether oxygen propyl trimethoxy silicane and the mixture of Digao 685, monomer HDDA, DPHA and TMPTA, mixing Mass ratio is 7:1:2, and photoinitiator is different according to mass ratio 1.5:1 2, the 2- dimethoxy -2- phenyl acetophenone mixed and 2- The mixture of propyl thioxanthone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 58.1%.
Embodiment 7
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 8nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 45%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.5g, monomer 35g, compatilizer 2g and photoinitiator are weighed respectively 0.98g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 2wt%, dispersant are the 0.5wt% of SiC mixed-powder, and content of monomer is the 35wt% of SiC mixed-powder, photoinitiator Content is the 2.8wt% of monomer mass;Compatilizer is stearic acid, dispersing agent is that the Y- shrink that mix according to mass ratio 1.4:1 is sweet The mixture of oily ether oxygen propyl trimethoxy silicane and the mixture of Digao 685, monomer HDDA, DPHA and TMPTA, mixing Mass ratio is 7:1:2, and photoinitiator is different according to mass ratio 1.3:1 2, the 2- dimethoxy -2- phenyl acetophenone mixed and 2- The mixture of propyl thioxanthone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 49.8%.
Embodiment 8
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 15nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 25%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.7g, monomer 45g, compatilizer 2.2g and photoinitiator are weighed respectively 1.35g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 2.2wt%, dispersant are the 0.7wt% of SiC mixed-powder, and content of monomer is the 45wt% of SiC mixed-powder, light-initiated Agent content is the 3wt% of monomer mass;Compatilizer is stearic acid, dispersing agent is that the Y- shrink that mix according to mass ratio 1.8:1 is sweet The mixture of oily ether oxygen propyl trimethoxy silicane and the mixture of Digao 685, monomer HDDA, DPHA and TMPTA, mixing Mass ratio is 7:1:2, photoinitiator 2,2- dimethoxy -2- phenyl acetophenone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 43.5%.
Embodiment 9
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 14nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 35%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.8g, monomer 52.3g, compatilizer 2.3g and light-initiated are weighed respectively Agent 1.67g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 2.3wt%, dispersant are the 0.8wt% of SiC mixed-powder, and content of monomer is the 52.3wt% of SiC mixed-powder, and light draws Send out the 3.19wt% that agent content is monomer mass;Compatilizer is stearic acid, dispersing agent is that the Y- mixed according to mass ratio 1.6:1 contracts The mixture of water glycerol ether oxygen propyl trimethoxy silicane and the mixture of Digao 685, monomer HDDA, DPHA and TMPTA, Mixing mass ratio is 7:1:2, photoinitiator be 2, the 2- dimethoxy -2- phenyl acetophenone that mix according to mass ratio 1.7:1 with The mixture of 2- isopropyl thioxanthone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are mixed evenly, are obtained To mixture.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 40%.
Embodiment 10
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 12nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 45%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 0.6g, monomer 50g, compatilizer 2.4g and photoinitiator are weighed respectively 1.7g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 2.4wt%, dispersant are the 0.6wt% of SiC mixed-powder, and content of monomer is the 50wt% of SiC mixed-powder, light-initiated Agent content is the 3.4wt% of monomer mass;Compatilizer is stearic acid, dispersing agent is Y- glycidyl ether oxygen propyl trimethoxy silicon The mixture of alkane, monomer HDDA, DPHA and TMPTA, mixing mass ratio 7:1:2, photoinitiator 2,2- dimethoxy- 2- phenyl acetophenone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are stirred, are mixed Close object.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 41%.
Embodiment 11
Step 1, by CVD method respectively in the spherical SiC powder of the spherical SiC powder of d50=0.4um and d50=2.5um The surface at end coats one layer of SiO2, SiO2Layer with a thickness of 10nm.
Step 2, be wrapped by two kinds of powder are put into ball mill, wherein the SiC powder quality of d50=0.4um accounts for Than being 50%, surplus is the SiC powder of d50=2.5um, and the stearic acid of the SiC powder quality 1% of addition carries out ball milling, ball milling 12h, rotational speed of ball-mill 360r/min form SiC mixed-powder after ball milling.
Step 3, SiC mixed-powder 100g, dispersing agent 1g, monomer 23.1g, compatilizer 2.8g and photoinitiator are weighed respectively 0.92g is handled after wherein SiC mixed-powder is dry by 100 mesh screen sievings;Compatibilizer content is SiC mixed-powder 2.8wt%, dispersant are the 1wt% of SiC mixed-powder, and content of monomer is the 23.1wt% of SiC mixed-powder, light-initiated Agent content is the 4wt% of monomer mass;Compatilizer is stearic acid, dispersing agent is Y- glycidyl ether oxygen propyl trimethoxy silicon The mixture of alkane, monomer HDDA, DPHA and TMPTA, mixing mass ratio 7:1:2, photoinitiator 2,2- dimethoxy- 2- phenyl acetophenone.
Step 4, the weighed SiC mixed-powder of step 3, dispersing agent, compatilizer and photoinitiator are stirred, are mixed Close object.
Step 5, mixture step 4 obtained is added in monomer, and adition process stirs simultaneously, and homogeneous is put into after mixing Homogeneous mixing is carried out in batch mixer;Homogeneous mixing includes the following four stage: the stage 1, with revolving speed 1000rmin-1 mixing 15s Afterwards, with 2800rmin-1 mixing 20s;Stage 2 is mixed after revolving speed 2800rmin-1 mixing 20s with 2000rmin-1 20s;Stage 3, after revolving speed 2000rmin-1 mixing 20s, with 1500rmin-1 mixing 10s;Stage 4, with revolving speed After 1500rmin-1 mixing 10s, with 800rmin-1 mixing 15s;After homogeneous mixing, the bubble in creme is removed, is made one The kind high solid phase silicon carbide porcelain creme of photocuring, wherein the solid content of silicon carbide is 60%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of photocuring silicon carbide ceramics creme, which is characterized in that the silicon carbide ceramics creme includes SiC mixed powder End, dispersing agent, monomer, compatilizer and photoinitiator;The surface of the SiC mixed-powder is coated with SiO2Layer, compatibilizer content It is the 1.5%~3.0% of SiC mixed-powder quality, dispersant is the 0.5%~1.0% of SiC mixed-powder quality, single Body content is the 23.1%~52.3% of SiC mixed-powder quality, and photoinitiator levels are 2.0~4.0wt% of monomer mass.
2. a kind of photocuring silicon carbide ceramics creme according to claim 1, which is characterized in that the SiC mixed powder End is the mixture of the spherical SiC powder of d50=0.4um and the spherical SiC powder of d50=2.5um, two spherical SiC powders Surface be coated with SiO2Layer;In SiC mixed-powder the quality accounting of the spherical SiC powder of d50=0.4um be 20%~ 50%, surplus is the spherical SiC powder of d50=2.5um.
3. a kind of photocuring silicon carbide ceramics creme according to claim 1, which is characterized in that SiO2Layer with a thickness of 5-15nm。
4. a kind of photocuring silicon carbide ceramics creme according to claim 1, which is characterized in that the compatilizer is hard Resin acid.
5. a kind of photocuring silicon carbide ceramics creme according to claim 1, which is characterized in that the dispersing agent is Y- The mixture of one or both of glycidyl ether oxygen propyl trimethoxy silicane and Digao 685.
6. a kind of photocuring silicon carbide ceramics creme according to claim 1, which is characterized in that monomer 1,6 oneself two The mixture of alcohol diacrylate, poly- two or six acrylate and trimethylolpropane trimethacrylate.
7. a kind of photocuring silicon carbide ceramics creme according to claim 6, which is characterized in that 1,6 hexylene glycol dipropyl The mixing mass ratio of olefin(e) acid ester, poly- two or six acrylate and trimethylolpropane trimethacrylate is 7:1:2.
8. a kind of photocuring silicon carbide ceramics creme according to claim 1, which is characterized in that photoinitiator 2,2- One or two kinds of mixture of dimethoxy -2- phenyl acetophenone and 2- isopropyl thioxanthone.
9. a kind of preparation method of photocuring described in claim 1 silicon carbide ceramics creme, which is characterized in that including following Step:
Step 1, one layer of SiO is coated on the SiC powder surface of two kinds of partial sizes respectively by chemical vapour deposition technique2, two kinds of partial sizes SiC powder is respectively the spherical SiC powder of d50=0.4um and the spherical SiC powder of d50=2.5um;
Step 2, surface is coated with SiO2The SiC powders of two kinds of partial sizes mix in the ball mill, be added in mixed process stearic Acid obtains SiC mixed-powder;
Step 3, SiC mixed-powder, dispersing agent, monomer, compatilizer and photoinitiator are weighed respectively;
Step 4, SiC mixed-powder, dispersing agent, compatilizer and photoinitiator that step 3 weighs are mixed and stirred for uniformly, obtaining Mixture;
Step 5, the mixture and monomer step 4 obtained is uniformly mixed in homogeneous batch mixer, and after defoaming, one kind is made Photocuring silicon carbide ceramics creme.
10. a kind of preparation method of photocuring silicon carbide ceramics creme according to claim 9, which is characterized in that step In rapid 5, blending process includes with the next stage in homogeneous batch mixer:
Stage 1, with revolving speed 1000rmin-1After mixing 15s, with 2800rmin-1Mix 20s;Stage 2, with revolving speed 2800r min-1After mixing 20s, with 2000rmin-1Mix 20s;Stage 3, with revolving speed 2000rmin-1After mixing 20s, with 1500r·min-1Mix 10s;Stage 4, with revolving speed 1500rmin-1After mixing 10s, with 800rmin-1Mix 15s.
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