CN108249928A - A kind of preparation method of solid-phase sintered silicon carbide ceramics wet moulding low viscosity high solids content water-based slurry - Google Patents
A kind of preparation method of solid-phase sintered silicon carbide ceramics wet moulding low viscosity high solids content water-based slurry Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of solid-phase sintered silicon carbide ceramics wet moulding low viscosity high solids content water-based slurry, after water, water-soluble carbon SiClx dispersant and sintering aid dispersant, add silicon carbide powder and sintering aid, the water-based slurry is obtained through ball milling mixing, the sintering aid powder includes at least one of boron carbide powder, boron powder and carbon black powder；The silicon carbide powder is to be obtained by one kind in silicon carbide in submicro level powder, nano-grade silicon carbide powder and micron order silicon carbide powder by grain composition, the median of the micron order silicon carbide powder is 1.0~50 μm, the median of the silicon carbide in submicro level powder is 0.1~1.0 μm, and the median of the nano-grade silicon carbide powder is 5nm~100nm.
Description
Technical field
The present invention relates to a kind of systems of solid-phase sintered silicon carbide ceramics wet moulding low viscosity high solids content water-based slurry
Preparation Method.Belong to high-performance ceramics field.
Background technology
It is excellent that solid-phase sintered silicon carbide ceramics have that hardness is big, elevated temperature strength is good, thermal conductivity is high, chemical stability is good etc.
Physicochemical characteristics, be widely used as wear-resisting, high temperature resistant, it is anticorrosive or heat transfer structural material, such as axle sleeve, sealing ring,
Bulletproof armour, thermocouple sleeve, heat-exchange tube etc..Since solid-phase sintered silicon carbide ceramics porcelain brittleness is big, hardness is high, unmanageable
Feature, the solid-phase sintered silicon carbide ceramics component of complicated shape usually pass through the side of dry-pressing-isostatic pressed-green body machining-sintering
Formula is produced, and there are the problem of complex process, manufacturing cycle, low yield rate.Wet moulding is that one kind can prepare large scale, complex shape
The effective ways of shape ceramic component can avoid the above problem, including gel casting forming, injection forming and tape casting etc..It is wet
One of key problem is the preparation of high solids content, low viscosity slurry in method forming process, to dry with being dropped in sintering process
Low-shrinkage avoids the generation of defect, promotes yield rate.
The preparation of solid-phase sintered silicon carbide ceramics wet moulding water-based slurry at present is main using sub-micrometer SiC powder
Raw material, since the grain size of submicron powder is small, specific surface area is high, inter-particle force is big, and agglomeration tendency is apparent in the slurry.For
In the case where meeting pouring condition, improve slurry solid content, generally using different dispersants to silicon carbide, boron carbide (or boron powder),
Carbon black carries out the mode of surface modification to realize, for example, Dong Manjiang etc. (Manjiang Dong, Xiaojian Mao,
Zhaoquan Zhang,Qian Liu.Gelcasting of SiC using epoxy resin as gel
former.Ceramics International 2009；35:1363-1366) 0.97, be modified using tetramethylammonium hydroxide
μm SiC powder is prepared for the SiC slurry that volume solid content is 51.3vol%；Swallow blueness waits (Xianhui Li, Qingzhi
Yan,Meiqi Cao,Yingying Mi,Yongjun Han,Changchun Ge.The influence of
granulation on the gelcasting of pressureless-sintered silicon carbide
ceramics.Ceramics International 2014；40:7245-7251) it, is modified using tetramethylammonium hydroxide
0.51 μm of SiC powder is prepared for the SiC slurry that volume solid content is 50vol%；Zhang Jingxian etc. (Jingxian Zhang,
Dongliang Jiang,Qingling Lin,Zhongming Chen,Zhengren Huang.Properties of
silicon carbide ceramics from gelcasting and pressureless sintering.2015；65:
12-16) 0.58 μm of SiC powder being modified using tetramethylammonium hydroxide is prepared for the SiC slurries that volume solid content is 52vol%
Material.Described in summary, it is only capable of obtaining solid-phase sintering of the slurry solid content no more than 52vol% using the mode that dispersant surface is modified
Silicon carbide ceramics wet moulding water-based slurry, slurry solid content need to be further improved (55vol%~58vol%).
Invention content
For current solid-phase sintered silicon carbide ceramics wet moulding water-based slurry solid content limited (40-52vol%)
Problem, the purpose of the present invention is to provide a kind of solid-phase sintered silicon carbide ceramics wet moulding water base slurries of low viscosity high solids content
Material and preparation method thereof.
On the one hand, it is water base with low viscosity high solids content the present invention provides a kind of solid-phase sintered silicon carbide ceramics wet moulding
The preparation method of slurry after water, water-soluble carbon SiClx dispersant and sintering aid dispersant, adds carborundum powder
Body and sintering aid obtain the water-based slurry through ball milling mixing, and the sintering aid powder is included in boron carbide powder, boron powder
At least one and carbon black powder；
The silicon carbide powder is by one kind in silicon carbide in submicro level powder, nano-grade silicon carbide powder and micron order carbonization
Silicon powder is obtained by grain composition, and the median of the micron order silicon carbide powder is 1.0~50 μm, the submicron order
The median of silicon carbide powder is 0.1~1.0 μm, and the median of the nano-grade silicon carbide powder is 5nm~100nm.
The present invention is on the basis of the modification of material powder (silicon carbide powder and sintering aid) surface by SiC powder
The mode that grade is matched prepares high solids content SiC water-based slurries.Wherein, by micron order SiC powder (median is 1.0~50 μm)
With sub-micrometer SiC powder (median is 0.1~1.0 μm) or nano grade Sic powder (median is 5nm~100nm)
Grain composition is carried out, is substantially reduced compared to full sub-micron or nano grade Sic powder, surface area, and then between reduction powder granule
Van der Waals force, and be utilized respectively different dispersants (water-soluble carbon SiClx dispersant and sintering aid dispersant) to silicon carbide
Powder, sintering aid (boron carbide powder (or boron powder), carbon black powder) carry out surface modification, and it is intergranular quiet to increase material powder
Electric repulsion and steric hindrance.In addition, the grain composition of silicon carbide powder and the surface of material powder are modified synergistic effect so that solid
Phase sintering silicon carbide ceramics wet moulding water-based slurry has the characteristics of low viscosity, high solids content, is conducive to base after molding
Body, with reducing shrinking percentage in sintering process, avoids deforming or crack, promote yield rate dry.
Preferably, the water-soluble carbon SiClx dispersant is tetramethylammonium hydroxide TMAH, polyethyleneimine PEI, poly- first
Base ammonium acrylate PMAA-NH4, polyethylene glycol PEG, at least one of polyisobutene maleic anhydride；Preferably, the water solubility
The addition of silicon carbide dispersant is 0.1~1.0wt.% of silicon carbide powder.
Preferably, the sintering aid of the boron carbide powder or/and boron powder with dispersant be tetramethylammonium hydroxide TMAH,
Polyethyleneimine PEI, ammonium polymethacrylate PMAA-NH4, polyethylene glycol PEG, polyisobutene maleic anhydride, carboxymethyl cellulose
At least one of plain sodium, addition is boron carbide powder or/and 0.1~1.0wt.% of boron powder gross mass.
Preferably, the sintering aid of the carbon black powder with dispersant is polyvinylpyrrolidone PVP, polyoxyethylene ether,
At least one of poly-maleic anhydride, polymethylacrylic acid, polyacrylic acid, polyvinylbenzenesulfonic acid, addition are carbon powder
0.1~3.0wt.% of body.
Preferably, the grading mass ratio of the micron order silicon carbide powder and silicon carbide in submicro level powder for (2~
0.05)：1 or the grading mass ratio of the micron order silicon carbide powder and nano-grade silicon carbide powder be (2~0.05)：1.
When grading mass ratio is (2~0.05)：When 1, slurry viscosity is substantially reduced and can obtain fine and close SiC ceramic after being sintered.
Preferably, the gross mass of the boron carbide powder or/and boron powder account for carborundum powder weight 0.1~
3.0wt.%, the carbon black powder account for 0.5~7.0wt.% of carborundum powder weight.
Preferably, the rotating speed of the ball milling mixing is 150~600 revs/min, the time is 2~8 hours.
Preferably, the median of the sintering aid is 0.2~1 μm.
On the other hand, the present invention also provides a kind of solid-phase sintered silicon carbide ceramics prepared according to above-mentioned preparation method
Wet moulding water-based slurry, the viscosity of the water-based slurry is 0.1~3Pas, and volume solid content is 55~58vol%.
The method have the characteristics that：The silicon carbide powder of particles used grading is significantly reduced the Van der Waals between powder granule
Power；And be utilized respectively different dispersants and surface modification is carried out to silicon carbide, boron carbide (or boron powder), carbon black, increase material powder
Intergranular electrostatic repulsion and steric hindrance, the grain composition of silicon carbide powder and the surface of powder granule, which are modified synergistic effect, to be made
It obtains solid-phase sintered silicon carbide ceramics wet moulding water-based slurry and has low viscosity (0.1Pas~3Pas), high solids content
The characteristics of (55vol%~58vol%), is conducive to green body after molding dry with reducing shrinking percentage in sintering process, avoids
Deformation or cracking, promote yield rate.The slurry of heretofore described water-based slurry need not add in acrylamide, methylene bisacrylamide
The crosslinking agents such as amide simplify preparation process.The addition of organic matter is reduced, avoids silicon carbide green body cracking in sintering process
Phenomenon.Without adding in the big initiator ammonium persulfate of toxicity and catalyst tetramethyl second two into slurry in solidification process of the present invention
Amine.
Description of the drawings
Fig. 1 is 1,2,3,4 grain composition micron-sized powder grain size of the embodiment of the present invention on slurry viscosity influence figure；
Fig. 2 is 3,5,6,7 solid content of the embodiment of the present invention on slurry viscosity influence figure；
Fig. 3 is the fine and close solid-phase sintered silicon carbide ceramics prepared using high solids content water-based slurry prepared by the embodiment of the present invention 7
Micro-structure diagram.
Specific embodiment
It is further illustrated the present invention below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention using water as solvent, be separately added into water-soluble carbon SiClx dispersant, sintering aid dispersant (including：Carbon
Change boron powder dispersant (or boron powder dispersant) and carbon black powder dispersant), it is uniformly mixed, then sequentially adds micron order carbon
SiClx powder carries out the carborundum powder obtained after grain composition with silicon carbide in submicro level powder (or nano-grade silicon carbide powder)
Body, boron carbide powder (or boron powder), carbon black powder, ball milling mixing obtain solid-phase sintered silicon carbide ceramics wet moulding with water base slurry
Material.The rotating speed of above-mentioned ball milling mixing can be 150~600 revs/min, and the time can be 2~8 hours.Wherein, the micron order carbonization
The median of silicon powder can be 1.0~50 μm.The median of the silicon carbide in submicro level powder can be 0.1~1.0 μm.
The median of the nano-grade silicon carbide powder can be 5nm~100nm.The median of the sintering aid can be 0.2~1
μm.Above-mentioned grain composition is exactly by micron order silicon carbide powder and silicon carbide in submicro level powder (or nanometer silicon carbide powder
Body) in mass ratio (2~0.05)：1 carries out ball milling mixing.The rotating speed of above-mentioned ball milling mixing can be 150~600 revs/min, the time
It can be 2~8 hours.
Optionally, the water-soluble carbon SiClx dispersant can be tetramethylammonium hydroxide (TMAH), polyethyleneimine
(PEI), ammonium polymethacrylate (PMAA-NH4), polyethylene glycol (PEG), in polyisobutene maleic anhydride (Isobam) at least
It is a kind of.The additive amount of the water-soluble carbon SiClx dispersant can be 0.1~1.0wt.% of carborundum powder weight.
Optionally, the carbonization borated dispersant is identical with boron powder dispersant the selection of material, may be, for example, tetramethyl hydroxide
Ammonium (TMAH), polyethyleneimine (PEI), ammonium polymethacrylate (PMAA-NH4), polyethylene glycol (PEG), polyisobutene Malaysia
At least one of acid anhydrides (Isobam), sodium carboxymethylcellulose etc..The additive amount of the carbonization borated dispersant can be boron carbide
0.1~1.0wt.% of powder quality.The boron carbide powder (or boron powder) accounts for silicon carbide powder (that is, the carbon after grain composition
SiClx powder) quality 0.1wt.%~3.0wt.%.
Optionally, the carbon black powder dispersant can be polyvinylpyrrolidone (PVP), polyoxyethylene ether, poly- maleic
At least one of polymer of dicarboxylic anhydride, methacrylic acid, acrylic acid, vinyl benzenesulfonic acid etc..The carbon black powder dispersant
Additive amount can be carbon black powder 0.1~3.0wt.%.The carbon black powder accounts for silicon carbide powder (that is, after grain composition
Silicon carbide powder) quality 0.5wt%~7.0wt%.
Preparation method as a solid-phase sintered silicon carbide ceramics wet moulding low viscosity high solids content water-based slurry
Example, prepared by following steps：(1) it is water is uniform with dispersant：Using water as solvent, it is separately added into water-soluble carbonization
Silicon dispersant, boron carbide powder dispersant (or boron powder dispersant) and carbon black powder dispersant are uniformly mixed.(2) it and then adds in
Silicon carbide powder after grain composition：By micron order silicon carbide powder and silicon carbide in submicro level powder (or nano carborundum powder
Body grade) according to grading mass ratio be (2~0.05)：1 carries out grain composition.(3) sintering aid powder is eventually adding, ball milling obtains
Required slurry：The sintering aid powder is boron carbide powder (or boron powder) and carbon black powder.
The present invention uses rheometer to measure the viscosity of water-based slurry as 0.1~3Pas.
In the present invention, the viscosity of the water base silicon carbide ceramics slurry of gained can be 0.1~3Pas, and volume solid content can be
55vol%~58vol%.It should be noted that above-mentioned water-based slurry can be used for solid-phase sintered silicon carbide ceramics wet moulding, base is obtained
Body.Wherein, the wet process forming method includes but not limited to gel casting forming, injection forming and tape casting.
Above-mentioned green body at 2000~2200 DEG C is sintered, obtains silicon carbide ceramics.The time being wherein sintered can be
0.5~4 hour.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.If without specified otherwise, the carbon in following embodiments
The median for changing boron powder is 200~500nm, and the median of the carbon black powder is 500nm~2 μm.
Embodiment 1
Using the water of 50g as solvent, addition account for silicon carbide powder and boron carbide powder gross mass 0.5wt.% tetramethylammonium hydroxide,
The polyvinylpyrrolidone for accounting for carbon black powder quality 1wt.% is dispersant, is uniformly mixed, and then sequentially adds 0.5 μm of 151g
SiC powder, account for the B of carborundum powder weight 0.5wt.%4C, the carbon black powder of 5wt.%, 300r/min, ball milling are after 4 hours
Obtain the solid-phase sintered silicon carbide ceramics wet moulding water-based slurry that volume solid content is 50vol%.After tested, 100s-1When,
The viscosity of the slurry is 14.06Pas (see C0.5-100 curves in Fig. 1).
Embodiment 2
Using the water of 50g as solvent, addition account for silicon carbide powder and boron carbide powder gross mass 0.5wt.% tetramethylammonium hydroxide,
The polyvinylpyrrolidone of carbon black powder quality 1wt.% is accounted for as dispersant, is uniformly mixed, then sequentially adds 1 μm of 151g
SiC powder accounts for the B of carborundum powder weight 0.5wt.%4C, the carbon black powder of 5wt.%, 300r/min, ball milling obtain after 4 hours
To the solid-phase sintered silicon carbide ceramics wet moulding water-based slurry that volume solid content is 50vol%.After tested, 100s-1When, it should
The viscosity of slurry is 6.82Pas (see C1-100 curves in Fig. 1).
Embodiment 3
Using the water of 50g as solvent, addition account for silicon carbide powder and boron carbide powder gross mass 0.5wt.% tetramethylammonium hydroxide,
The polyvinylpyrrolidone for accounting for carbon black powder quality 1wt.% is dispersant, is uniformly mixed, and then sequentially adds the quality of 151g
Than being 1.86:2 μm of 1 mixing and 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 0.5wt.%4C、
The carbon black powder of 5wt.%, 300r/min, ball milling obtain the solid-phase sintered silicon carbide that volume solid content is 50vol% after 4 hours
Ceramic wet molding water-based slurry.After tested, 100s-1When, the viscosity of the slurry is (bent see C2-65 in Fig. 1 for 0.59Pas
Line is shown in 50vol% curves in Fig. 2).
Embodiment 4
Using the water of 50g as solvent, addition account for silicon carbide powder and boron carbide powder gross mass 0.5wt.% tetramethylammonium hydroxide,
The polyvinylpyrrolidone for accounting for carbon black powder quality 1wt.% is dispersant, is uniformly mixed, and then sequentially adds the quality of 151g
Than being 1.86:5 μm of 1 mixing and 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 0.5wt.%4C、
The carbon black powder of 5wt.%, 300r/min, ball milling obtain the solid-phase sintered silicon carbide that volume solid content is 50vol% after 4 hours
Ceramic wet molding water-based slurry.After tested, 100s-1When, the viscosity of the slurry is (bent see C5-30 in Fig. 1 for 0.53Pas
Line).
Embodiment 5
Using the water of 44.6g as solvent, addition accounts for silicon carbide powder and boron carbide powder gross mass 0.5wt.% tetramethyl hydroxides
Ammonium accounts for the polyvinylpyrrolidone of carbon black powder quality 1wt.% as dispersant, is uniformly mixed, then sequentially adds the matter of 151g
Amount is than being 1.86:2 μm of 1 mixing and 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 0.5wt.%4C、
The carbon black powder of 5wt.%, 300r/min, ball milling obtain the solid-phase sintered silicon carbide that volume solid content is 52vol% after 4 hours
Ceramic wet molding water-based slurry.After tested, 100s-1When, the viscosity of the slurry is 1.13Pas (see 52vol% in Fig. 2
Curve).
Embodiment 6
Using the water of 41g as solvent, addition account for silicon carbide powder and boron carbide powder gross mass 0.5wt.% tetramethylammonium hydroxide,
The polyvinylpyrrolidone for accounting for carbon black powder quality 1wt.% is dispersant, is uniformly mixed, and then sequentially adds the quality of 151g
Than being 1.86:2 μm of 1 mixing and 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 0.5wt.%4C、
The carbon black powder of 5wt.%, 300r/min, ball milling obtain the solid-phase sintered silicon carbide that volume solid content is 54vol% after 4 hours
Ceramic wet molding water-based slurry.After tested, 100s-1When, the viscosity of the slurry is 2.28Pas (see 54vol% in Fig. 2
Curve).
Embodiment 7
Using the water of 39g as solvent, the tetramethyl hydroxide for accounting for silicon carbide powder and boron carbide powder gross mass 0.5wt.% is added in
Ammonium accounts for the polyvinylpyrrolidone of carbon black powder quality 1wt.% as dispersant, is uniformly mixed, then sequentially adds the matter of 151g
Amount is than being 1.86:2 μm of 1 mixing and 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 0.5wt.%4C、
The carbon black powder of 5wt.%, 300r/min, ball milling obtain the solid-phase sintered silicon carbide that volume solid content is 55vol% after 4 hours
Ceramic wet molding water-based slurry.After tested, 100s-1When, the viscosity of the slurry is 2.36Pas (see 55vol% in Fig. 2
Curve).SiC ceramic manufactured in the present embodiment passes through gel-casting method, under conditions of 2100 DEG C of solid-phase sinterings, sintering
It obtains within 0.5 hour.
Embodiment 8
Using 50g water as solvent, the tetramethylammonium hydroxide for accounting for silicon carbide powder and boron carbide powder gross mass 1wt.% is added in, is accounted for
The polyoxyethylene ether of carbon black powder quality 3wt.% is uniformly mixed, and it is 0.05 then to sequentially add 151g mass ratioes:The 2 of 1 mixing
μm with 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 0.1wt.%4C, the carbon black powder of 0.5wt.%,
300r/min, ball milling obtain solid-phase sintered silicon carbide ceramics wet moulding that volume solid content is 50vol% with water base after 4 hours
Slurry.
Embodiment 9
Using 50g water as solvent, addition accounts for silicon carbide powder and boron carbide powder gross mass 0.1wt.% polyethyleneimines, accounts for carbon black
The poly-maleic anhydride of powder quality 1wt.% is dispersant, is uniformly mixed, and it is 1.86 then to sequentially add 151g mass ratioes:
2 μm of 1 mixing and 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 3wt.%4C, the carbon powder of 7wt.%
Body, 300r/min, ball milling obtain the solid-phase sintered silicon carbide ceramics wet moulding that volume solid content is 50vol% and use after 4 hours
Water-based slurry.
Embodiment 10
Using 50g water as solvent, addition accounts for silicon carbide powder and boron carbide powder gross mass 0.1wt.% ammonium polymethacrylates, accounts for
The polymethylacrylic acid of carbon black powder quality 3wt.% is dispersant, is uniformly mixed, then sequentially adding 151g mass ratioes is
1.86:2 μm of 1 mixing and 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 0.1wt.%4C, 5wt.%
Carbon black powder, 300r/min, ball milling obtain the solid-phase sintered silicon carbide ceramics wet method that volume solid content is 50vol% after 4 hours
Molding water-based slurry.
Embodiment 11
Using 50g water as solvent, addition accounts for silicon carbide powder and boron carbide powder gross mass 1wt.% polyethylene glycol, accounts for carbon black powder
The polyacrylic acid of quality 0.1wt.% is dispersant, is uniformly mixed, and it is 1.86 then to sequentially add 151g mass ratioes:The 2 of 1 mixing
μm with 0.5 μm of SiC powder, account for the B of grain composition carborundum powder weight 3wt.%4C, the carbon black powder of 0.5wt.%,
300r/min, ball milling obtain solid-phase sintered silicon carbide ceramics wet moulding that volume solid content is 50vol% with water base after 4 hours
Slurry.
Embodiment 12
Using the water of 50g as solvent, addition accounts for silicon carbide powder and boron carbide powder gross mass 0.5wt.% tetramethylammonium hydroxide,
It is uniformly mixed, the mass ratio for then sequentially adding 151g is 1.86:2 μm of 1 mixing and 0.5 μm of SiC powder, account for grain composition
The B of carborundum powder weight 0.5wt.%4C, the carbon black powder of 5wt.%, 300r/min, ball milling obtain volume after 4 hours and contain admittedly
Measure the solid-phase sintered silicon carbide ceramics wet moulding water-based slurry for 50vol%.After tested, 100s-1When, the viscosity of the slurry
For 2Pas.
Fig. 1 be 1,2,3,4 grain composition micron-sized powder grain size of the embodiment of the present invention on slurry viscosity influence figure, from figure
Understand that 4 kinds of formulas can obtain the silicon carbide slurry with certain fluidity, with the increase of micron-sized powder grain size, slurry glues
Degree is substantially reduced.Shear rate is 100s-1When, viscosity is reduced to 0.53Pas from 14.06Pas.Therefore in identical solid content
When, grain composition can effectively reduce the viscosity of slurry；
Fig. 2 is 3,5,6,7 solid content of the embodiment of the present invention on slurry viscosity influence figure, as we know from the figure with solid content from
50vol% increases to 55vol%, and the viscosity of slurry significantly increases.Shear rate is 100s-1When, viscosity reduces from 0.59Pas
For 2.36Pas.The viscosity of slurry be Van der Waals force between powder with caused by the capillary force in aggregate duct, with solid
The distance between the increase of content, the opposite reduction of decentralized medium, powder granule reduction, Van der Waals force increase.Correspondingly, unit
The aggregate of powder also increases in volume slurry, and capillary force is caused to increase.The factor of these two aspects causes slurry viscosity
Increase；
Fig. 3 is the fine and close solid-phase sintered silicon carbide ceramics prepared using high solids content water-based slurry prepared by the embodiment of the present invention 7
Micro-structure diagram, as we know from the figure grain composition silicon carbide slurry sintering after crystal grain be evengranular equi-axed crystal, grain
Diameter size is~20 μm.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of solid-phase sintered silicon carbide ceramics wet moulding water-based slurry, which is characterized in that by water, water-soluble
After property silicon carbide dispersant and sintering aid dispersant, silicon carbide powder and sintering aid are added, through ball milling mixing
The water-based slurry is obtained, the sintering aid powder includes at least one of boron carbide powder, boron powder and carbon black powder；
The silicon carbide powder is by one kind in silicon carbide in submicro level powder, nano-grade silicon carbide powder and micron order carbonization
Silicon powder is obtained by grain composition, and the median of the micron order silicon carbide powder is 1.0~50 μm, the submicron order
The median of silicon carbide powder is 0.1~1.0 μm, and the median of the nano-grade silicon carbide powder is 5nm~100nm.
2. preparation method according to claim 1, which is characterized in that the water-soluble carbon SiClx dispersant is tetramethyl hydrogen
Amine-oxides TMAH, polyethyleneimine PEI, ammonium polymethacrylate PMAA-NH4, polyethylene glycol PEG, polyisobutene maleic anhydride
At least one of；Preferably, the addition of the water-soluble carbon SiClx dispersant is the 0.1~1.0 of silicon carbide powder
wt.%。
3. preparation method according to claim 1 or 2, which is characterized in that the sintering of the boron carbide powder or/and boron powder
Auxiliary agent with dispersant is tetramethylammonium hydroxide TMAH, polyethyleneimine PEI, ammonium polymethacrylate PMAA-NH4, poly- second two
At least one of alcohol PEG, polyisobutene maleic anhydride, sodium carboxymethylcellulose, addition are boron carbide powder or/and boron powder
0.1~1.0wt.% of gross mass.
4. preparation method according to claim 1 or 2, which is characterized in that the sintering aid dispersion of the carbon black powder
Agent is polyvinylpyrrolidone PVP, polyoxyethylene ether, poly-maleic anhydride, polymethylacrylic acid, polyacrylic acid, polyethylene
At least one of benzene sulfonic acid, addition are 0.1~3.0wt.% of carbon black powder.
5. according to the preparation method described in any one of claim 1-4, which is characterized in that the micron order silicon carbide powder and
The grading mass ratio of silicon carbide in submicro level powder is（2~0.05）：1 or the micron order silicon carbide powder and nanoscale
The grading mass ratio of silicon carbide powder is（2~0.05）：1.
6. preparation method according to any one of claims 1-5, which is characterized in that the boron carbide powder or/and boron
The gross mass of powder accounts for 0.1~3.0wt.% of carborundum powder weight, the carbon black powder account for carborundum powder weight 0.5~
7.0wt.%。
7. according to the preparation method described in any one of claim 1-6, which is characterized in that the rotating speed of the ball milling mixing is
150~600r/ minutes, the time was 2~8 hours.
8. according to the preparation method described in any one of claim 1-7, which is characterized in that the median of the sintering aid
It is 0.2~1 μm.
9. solid-phase sintered silicon carbide ceramics wet moulding prepared by a kind of preparation method according to claim 1-8 is with water base
Slurry, which is characterized in that the viscosity of the water-based slurry is 0.1~3 Pas, and volume solid content is 55~58vol%.
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| CN108892509A (en) * | 2018-08-03 | 2018-11-27 | 宁波哈泰雷碳化物有限公司 | A kind of preparation method of the nanometer silicon carbide slurry for ceramic moulding by casting |
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