CN104446487A - Slurry and method for gelcasting pressureless sintered silicon carbide ceramics - Google Patents
Slurry and method for gelcasting pressureless sintered silicon carbide ceramics Download PDFInfo
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Abstract
The invention provides a slurry for gelcasting pressureless sintered silicon carbide ceramics. The slurry is prepared from the following components by volume fraction: 50-53% of silicon carbide powder including two silicon carbide powder materials of which the medium diameters (D50) are 0.78 micron and 0.41 micron, respectively, 0.4% of 0.93 micron boron carbide, 4.4% of dextrin, 1.3-1.4% of tetramethylammonium hydroxide, 4.2-4.4% of acrylamide, 0.35-0.37% of N,N'-methylenediacrylamide, 0.4-0.8% of ammonium persulfate, 0.8-1.2% of N,N,N',N'-tetramethyldiethylamine and the balance of deionized water. The silicon carbide powder material having the D50 of 0.41 micron in the silicon carbide micropowder accounts for 10-30% by weight. The invention also provides a method for gelcasting the pressureless sintered silicon carbide ceramics by use of the slurry. According to the method for gelcasting the pressureless sintered silicon carbide ceramics by use of the slurry, the porosity of a blank is reduced, and the compactness and bending strength of the formed blank are improved.
Description
Technical field
The invention belongs to the preparation field of silicon carbide ceramics, be specifically related to a kind of slip of gel casting forming pressureless sintering silicon carbide ceramic and utilize the method for this slip pressureless sintering silicon carbide ceramic.
Background technology
Silicon carbide ceramics has excellent physical and chemical performance, as high rigidity, high bending strength, excellent oxidation-resistance, good erosion resistance, high resistance to wearing; In addition, the mechanical behavior under high temperature (as intensity, creep resistance) of silicon carbide ceramics is best in known ceramic material.Based on above-mentioned premium properties, silicon carbide ceramics has been widely used in numerous industrial circles such as oil, chemical industry, aerospace, automobile, nuclear industry.
Compared with other sintering methods, pressureless sintering silicon carbide products better performances, and sintering process is comparatively simple, shape of product and dimensional controllability better, high not as hot pressed sintering to ingredient requirement, be applicable to industrial mass production.Along with pressureless sintering silicon carbide obtains increasingly extensive application as high-performance ceramics, the complicacy of the industrial geometrical shape to silicon carbide ceramics requires more and more higher.But because the hardness of silicon carbide ceramics is very high, the goods processing difficulties after sintering, precise part must carry out mechanical workout with diamond cutter, and price is very expensive.The tooling cost of pottery almost accounts for the 1/3-2/3 of ceramic manufacturing cost.The approach solving this difficult problem has two: (1) prepares the complicated shape base substrate of shaping near net-shape; (2) base substrate has enough intensity, can carry out mechanical workout.
Gel-casting process is a kind of new moulding process be based upon on the basis of traditional ceramics injection forming technology and high molecular theory, is the dead size forming method being realized the formed in situ of slurry by organic monomer polyreaction.The green strength of this technological forming is very high, directly can carry out mechanical workout, obviously be better than the moulding process of other complicated shape ceramic components, and this is highly profitable for very unmanageable stupalith after sintering.Gel-casting process comprises several process: powder is dispersed in the aqueous solution containing organic monomer and linking agent or non-aqueous solution by (1), adds initiator and catalyzer before injection molding, stir and degassed after, slurry is injected mould; (2) under certain temperature condition, cause organic monomer polymerization, slurry viscosity is increased suddenly, thus causes slurry solidify in place, form wet base; (3) after the wet base demoulding, dry at a certain temperature and humidity conditions, obtain high strength base substrate; (4) finally dry body binder removal is sintered, obtain compact components.
In gel casting forming process, solid load, powder condition of surface, powder particle size distribution, dispersion agent, pH value, initiator and catalyzer etc. all can affect gel injection process.High solid loading, low viscosity slip are that this technology is successfully crucial.The high solids content of slip can ensure the quality of molding blank, reduces sintering shrinkage, reduces sintering temperature meter cost, improves the density of goods, be conducive to large-scale production.The quality of phosphoric acid magnitude relationship to become blank shape and the exhaust effect of slurry.Raw material powder size and distribution can affect the rheological property of slip.High solid loading and low viscosity are conflict bodies, especially when the particle diameter of powder is reduced to submicron order, high solid loading inevitably causes the increase of phosphoric acid, and how while reduction phosphoric acid, to realize high solid loading is a still open question.
With the development of ceramic sintering process, powder raw material is also developed to submicron order, nano level by micron order.Because submicron or nanometer grade powder have large specific surface area and surface energy, be very easy to produce reunite, powder flowing property and dispersing property poor, employing conventional ball mill-drying powder handling technique oneself be not suitable for.In pressureless sintering silicon carbide, usually adopting wet ball grinding batch mixing-mist projection granulating, is carry out spraying dry after fluidization process to powder, by the slip Direct spraying that mixes in warm air, at very short time inner drying, obtains the spherical powder of regular shape.Atomizing granulating technology is applied in special cermacis is produced, effectively can avoid the reunion again of each component and settlement separate, keep the original homogeneity of slurry, and slurry atomization evenly, gained powder is spheroidal particle, and epigranular distributes, good fluidity, be applicable to continuous automatic moulding, also can improve biscuit homogeneity, be conducive to the sintering of pottery.What mist projection granulating obtained is regular shape, ganoid spheroidal particle.
Patent of invention CN 103964854A discloses " a kind of layer-built armor SiC ceramic thin layer bullet resistant material and preparation method thereof ", raw material powder in the method comprises silicon carbide micro-powder 100 parts, boron carbide micro powder 0.5-2 part, acrylamide monomer 20-35 part, N ' N methylene-bisacrylamide 1-3 part, Tetramethylammonium hydroxide 0.5-1.5 part, tributyl phosphate 0.2-0.8 part, deionized water 30-45 part; Wherein silicon carbide micro-powder median size is 0.45 μm; Boron carbide micro powder median size is 1.5-3.5 μm.This patent solves Gel-casting process and prepares the problem easily producing warpage, cracking in large size thin ceramic product drying, sintering process.But still do not solve the problem that preparation low viscosity slip realizes high solid volume fraction simultaneously.
Summary of the invention
According to prior art Problems existing, the invention provides a kind of slip and method of gel casting forming pressureless sintering silicon carbide ceramic.The present invention, by carrying out pre-treatment to raw material powder, improves powder particles size and distribution thereof, thus improves the rheological property of slip, improves performance and the workability of base substrate, and then improves the mechanical property of sintered compact.
Technical scheme of the present invention:
The slip of gel casting forming pressureless sintering silicon carbide ceramic, by volume number meter, composed of the following components: sic powder: to comprise D
50be respectively two kinds of sic powders of 0.78 μm and 0.41 μm, 50-53%; The norbide of 0.93 μm, 0.4%; Dextrin, 4.4%; Tetramethylammonium hydroxide, 1.3-1.4%; Acrylamide, 4.2-4.4%; N, N'-methylene-bisacrylamide, 0.35-0.37%; Ammonium persulphate 0.4-0.8%; N, N, N', N'-tetramethyl-diethylamine 0.8-1.2%; Surplus is deionized water.D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 10-30%.
Adopt the method for the slip pressureless sintering silicon carbide ceramic of above-mentioned gel casting forming pressureless sintering silicon carbide ceramic, comprise the following steps:
(1) raw materials pretreatment: proportionally take silicon carbide micro-powder, boron carbide micro powder, carbon source and dispersion agent, is put in tetrafluoroethylene ball grinder, adds ethanol in proper amount, after magnetic agitation, be made into suspension.Silicon carbide micro-powder comprises D
50be respectively two kinds of sic powders of 0.78 μm and 0.41 μm, D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 10-30%, boron carbide micro powder is D
50be 0.93 μm, carbon source is dextrin, and dispersion agent is Tetramethylammonium hydroxide (TMAH).In this step, count by weight, Tetramethylammonium hydroxide is 0.5% of silicon carbide micro-powder.Being placed on planetary ball mill by adding ball milling ball in gained suspension, carrying out ball mill mixing.Then by gained slip, under Rotary Evaporators 70 ~ 80 DEG C of conditions, dry 2 ~ 4h, obtains Homogeneous phase mixing powder.Adopt the silicon carbide micro-powder of two kinds of different-grain diameters, utilize grain composition principle, after even batch mixing, fine particle is made to be dispersed in coarse grained surrounding, in shaping pressing process, fine particle is filled in tightly packed the formed space of coarse particles, thus reduces base substrate porosity, improves molding blank degree of compactness;
(2) pelletizing preparation: powder step (1) obtained, at the closely knit base substrate of the pressure system of chilling press 60 ~ 90MPa, after fragmentation, is crossed 60 mesh sieves, obtained particle diameter continuous distribution, shaggy Polygons pelletizing.This process effectively avoids the reunion again of each feed composition and settlement separate, keeps the original homogeneity of each raw material powder in step (1);
(3) premixed liquid preparation: organic monomer and linking agent are dissolved in deionized water by the mass ratio of 11-13:1, and add Tetramethylammonium hydroxide, mechanical stirring is to mixing under constant temperature, obtains premixed liquid; In this step, by volume mark meter, described organic monomer is acrylamide (AM), add-on 4.2-4.4%, and described linking agent is N, N'-methylene-bisacrylamide (MBAM), add-on 0.35-0.37%; The add-on of described Tetramethylammonium hydroxide is the 1.3-1.4% of total slip;
(4) Pulp preparation: joined by the pelletizing that step (2) obtains in the premixed liquid that step (3) obtains, mechanical stirring 6h, prepares the silicon carbide dispersion slip that solid content is 50-53vol%; In mud dispersivity process, water molecules aligns in solid particles surface region, forms fixing water molecule layer.Raw material powder is after granulation, and pelletizing particle diameter increases, and specific surface area reduces, and reduces, phosphoric acid is reduced at the water molecules volume of solid particles surface sizing arrangement.Thus solve in gel forming technique, the problem that silicon carbide in submicro level preparation phosphoric acid is large;
(5) vacuum stripping: owing to often producing bubble in ceramic size preparation process, therefore slurry need carry out de-bubble through vacuumizing mode.Slurry vacuum tightness be-0.1MPa under the degasification 10-30min obtained by step (4), thoroughly to get rid of the bubble in slurry, improves the density of biscuit.In above-mentioned slip, add initiator ammonium persulfate (APS) and catalyst n, N, N', N'-tetramethyl-diethylamine (TEMED), after fully stirring, repeat degassing procedure 5-10min, obtaining can the ceramic slurry of injection molding.
(6) casting: the slip that step (5) obtains injects mould, is heated to 60 DEG C, keep 30-90min, organic monomer crosslinking curing, obtains having larger elastic wet base;
(7) body drying: moved into by wet base in the drying installation of high humidity (70-80%) after the demoulding immediately, dry 4-6h, to avoid the cracking that causes due to rapid drying and ununiform shrinkage; Then base substrate is moved in the drying installation of low humidity (20-30%), dry 48h;
(8) binder removal process: dried base substrate is placed in vacuum oven, is warming up at a slow speed 800 DEG C, temperature rise rate 1 DEG C/min, and insulation 30min, obtains biscuit body.Pelletizing particle diameter continuous distribution, and surface irregularity, have irregularly shaped, is conducive to engaging each other between particle, is conducive to the degree of compactness improving biscuit, improves biscuit intensity;
(9) blank sintering: gained biscuit body is placed in non-pressure sintering furnace, under 1atmAr atmosphere, is warming up to 2200 DEG C, and insulation 1h, obtains sintered compact after cooling.Heating, cooling speed is 10 DEG C/min.
Beneficial effect of the present invention: the present invention adopts the silicon carbide micro-powder of two kinds of different-grain diameters, utilize grain composition principle, after even batch mixing, fine particle is made to be dispersed in coarse grained surrounding, in moulding process, fine particle is filled in tightly packed the formed space of coarse particles, thus reduces base substrate porosity, improves molding blank degree of compactness.By carrying out granulation to powder, obtain particle diameter large, and continuous distribution, the irregularly shaped pelletizing of tool uneven surface, reduce the viscosity of silicon carbide ceramics slip, solve in gel forming technique, the problem that the phosphoric acid that submicron silicon carbide particle obtains is larger, improve degree of compactness and the flexural strength of biscuit body, base substrate workability strengthens.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1:
The slip of gel casting forming pressureless sintering silicon carbide ceramic, by volume number meter, composed of the following components: sic powder: to comprise D
50be respectively two kinds of sic powders of 0.78 μm and 0.41 μm, 50%; The norbide of 0.93 μm, 0.4%; Dextrin, 4.4%; Tetramethylammonium hydroxide, 1.4%; Acrylamide, 4.4%; N, N'-methylene-bisacrylamide, 0.37%; Ammonium persulphate 0.4%; N, N, N', N'-tetramethyl-diethylamine 0.8%; Surplus is deionized water.D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 20%.
Adopt the method for the slip pressureless sintering silicon carbide ceramic of above-mentioned gel casting forming pressureless sintering silicon carbide ceramic, comprise the following steps:
(1) raw materials pretreatment: proportionally take silicon carbide micro-powder, boron carbide micro powder, carbon source and dispersion agent, is put in tetrafluoroethylene ball grinder, adds ethanol in proper amount, after magnetic agitation, be made into suspension.Silicon carbide micro-powder comprises D
50be respectively two kinds of sic powders of 0.78 μm and 0.41 μm, D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 20%, boron carbide micro powder is D
50be 0.93 μm, carbon source is dextrin, and dispersion agent is Tetramethylammonium hydroxide (TMAH).In this step, count by weight, Tetramethylammonium hydroxide is 0.5% of silicon carbide micro-powder.Being placed on planetary ball mill by adding ball milling ball in gained suspension, carrying out ball mill mixing.Then by gained slip, under Rotary Evaporators 70 ~ 80 DEG C of conditions, dry 2 ~ 4h, obtains Homogeneous phase mixing powder.Adopt the silicon carbide micro-powder of two kinds of different-grain diameters, utilize grain composition principle, after even batch mixing, make fine particle be dispersed in coarse grained surrounding, in moulding process, fine particle is filled in tightly packed the formed space of coarse particles, thus reduce base substrate porosity, improve molding blank degree of compactness;
(2) pelletizing preparation: powder step (1) obtained, at the closely knit base substrate of the pressure system of chilling press 60 ~ 90MPa, after fragmentation, is crossed 60 mesh sieves, obtained particle diameter continuous distribution, shaggy Polygons pelletizing.This process effectively avoids the reunion again of each feed composition and settlement separate, keeps the original homogeneity of each raw material powder in step (1);
(3) premixed liquid preparation: organic monomer and linking agent are dissolved in deionized water by the mass ratio of 12:1, and add Tetramethylammonium hydroxide, mechanical stirring is to mixing under constant temperature, obtains premixed liquid; In this step, by volume mark meter, described organic monomer is acrylamide, add-on 4.4%, and described linking agent is N, N'-methylene-bisacrylamide, add-on 0.37%; The add-on of described Tetramethylammonium hydroxide is 1.4% of total slip;
(4) Pulp preparation: joined by the pelletizing that step (2) obtains in the premixed liquid that step (3) obtains, mechanical stirring 6h, prepares the silicon carbide dispersion slip that solid content is 50vol%; In mud dispersivity process, water molecules aligns in solid particles surface region, forms fixing water molecule layer.Raw material powder is after granulation, and pelletizing particle diameter increases, and specific surface area reduces, and reduces, phosphoric acid is reduced at the water molecules volume of solid particles surface sizing arrangement.Thus solving in gel forming technique, silicon carbide in submicro level particle prepares the large problem of phosphoric acid;
(5) vacuum stripping: owing to often producing bubble in ceramic size preparation process, therefore slurry need carry out de-bubble through vacuumizing mode.Slurry vacuum tightness be-0.1MPa under the degasification 10-30min obtained by step (4), thoroughly to get rid of the bubble in slurry, improves the density of biscuit.In above-mentioned slip, add initiator ammonium persulfate (APS) and catalyst n, N, N', N'-tetramethyl-diethylamine (TEMED), after fully stirring, repeat degassing procedure 5-10min, obtaining can the ceramic slurry of injection molding.
(6) casting: the slip that step (5) obtains injects mould, is heated to 60 DEG C, keep 30-90min, organic monomer crosslinking curing, obtains having larger elastic wet base;
(7) body drying: moved into by wet base in the drying installation of high humidity (70-80%) after the demoulding immediately, to avoid the cracking that causes due to rapid drying and ununiform shrinkage; After contraction stops, base substrate is moved in the drying installation of low humidity (20-30%), dry 48h;
(8) binder removal process: dried base substrate is placed in vacuum oven, is warming up at a slow speed 800 DEG C, temperature rise rate 1 DEG C/min, and insulation 30min, obtains biscuit body.Pelletizing particle diameter continuous distribution, and surface irregularity, have irregularly shaped, is conducive to engaging each other between particle, is conducive to the degree of compactness improving biscuit, improves biscuit intensity;
(9) blank sintering: gained biscuit body is placed in non-pressure sintering furnace, under 1atmAr atmosphere, is warming up to 2200 DEG C, and insulation 1h, obtains sintered compact after cooling.Heating, cooling speed is 10 DEG C/min.
Embodiment 2:
As different from Example 1, sic powder: comprise D
50be respectively two kinds of sic powders of 0.78 μm and 0.41 μm, 53%; Tetramethylammonium hydroxide, 1.4%; Acrylamide, 4.2%; N, N'-methylene-bisacrylamide, 0.37%; Ammonium persulphate 0.4%; N, N, N', N'-tetramethyl-diethylamine 1.2vol%; Surplus is deionized water.D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 10%.
Embodiment 3:
As different from Example 1, in the slip of gel casting forming pressureless sintering silicon carbide ceramic, the volume fraction of Tetramethylammonium hydroxide is 1.3%, and the volume fraction of acrylamide is the volume fraction of 4.4%, N, N'-methylene-bisacrylamide is 0.35%; The volume fraction of ammonium persulphate is 0.8%; The volume fraction of N, N, N', N'-tetramethyl-diethylamine is 0.8%; D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 30%.
Adopt the method for the slip pressureless sintering silicon carbide ceramic of above-mentioned gel casting forming pressureless sintering silicon carbide ceramic, carry out accommodation.
Embodiment 4:
As different from Example 1, in the slip of gel casting forming pressureless sintering silicon carbide ceramic, the volume fraction of Tetramethylammonium hydroxide is 1.35%, and the volume fraction of acrylamide is the volume fraction of 4.3%, N, N'-methylene-bisacrylamide is 0.36%; The volume fraction of ammonium persulphate is 0.6%; The volume fraction of N, N, N', N'-tetramethyl-diethylamine is 1.0%; D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 20%.
Adopt the method for the slip pressureless sintering silicon carbide ceramic of above-mentioned gel casting forming pressureless sintering silicon carbide ceramic, carry out accommodation.
Characterization result in table 1 gel casting forming pressureless sintering silicon carbide ceramic
Interpretation of result is carried out for embodiment 1:
(1) properties of powder analysis
The powder that step 1 adopts two kinds of granularities different carries out mixture, and in particle packing process, fine-grained powder is dispersed in around coarse particles powder.In pine dress and jolt ramming process, fine particle fills tightly packed the formed space of coarse particles, and therefore the loose density of step 1 gained powder and tap density are 0.56g/cm
3and 0.8g/cm
3higher than single powder (D
50=0.78 μm) loose density and tap density 0.48g/cm
3and 0.7g/cm
3.Step 2 gained pelletizing is made up of the irregular particle with coarse particles surface, particle diameter continuous distribution, and do not have 1-100 μm not etc., granulation loose density and tap density are 0.63g/cm
3and 0.9g/cm
3.
(2) the rheological property analysis of slip
Solids in pulp amount is 50vol%, when shearing rate is 100s
-1, the viscosity that raw material powder prepares slip is 483MPas, and the viscosity that step 2 gained pelletizing prepares slip is 134MPas, and phosphoric acid reduces.This is because in aqueous gel process, in the arrangement of solid particles surface regional water molecular orientation, form water of constitution, after granulation for powders, particle diameter increases, and specific surface area reduces, and water of constitution volume reduces, and viscosity reduces.Therefore when identical solid load, the far low and single powder phosphoric acid of the viscosity of slip prepared by pelletizing.
(3) body crack defects analysis
Obtain biscuit body through gel casting forming, preform structure is closely knit, without obvious pore.Biscuit relative density is 52%, and flexural strength is 28MPa, can carry out mechanical workout.The relative density of the biscuit that its parameter value is prepared higher than single powder material and flexural strength.This is because fine particle fills the space of thick tightly packed formation, and play the effect improving base substrate degree of compactness, pelletizing surface irregularity and irregular pattern thereof, be also conducive to combining closely of particle simultaneously.
(4) sintered compact performance analysis
In sintering process, particle re-arrangement, pore is got rid of gradually, and sintered compact is closely knit gradually, and irregular pattern pelletizing is destroyed, and the performance of raw material powder directly affects solid phase diffusion in sintering process, particle re-arrangement, volumetric shrinkage etc.Adopt the raw material powder of two kinds of granularities, the density of its sintered compact is 3.1g/cm
3, flexural strength is the sintered compact of 430Mpa higher than single preparation.
Claims (6)
1. the slip of gel casting forming pressureless sintering silicon carbide ceramic, is characterized in that: by volume number meter, composed of the following components: sic powder: to comprise D
50be respectively two kinds of sic powders of 0.78 μm and 0.41 μm, 50-53%; The norbide of 0.93 μm, 0.4%; Dextrin, 4.4%; Tetramethylammonium hydroxide, 1.3-1.4%; Acrylamide, 4.2-4.4%; N, N'-methylene-bisacrylamide, 0.35-0.37%; Ammonium persulphate 0.4-0.8%; N, N, N', N'-tetramethyl-diethylamine 0.8-1.2%; Surplus is deionized water.
2. the slip of gel casting forming pressureless sintering silicon carbide ceramic according to claim 1, is characterized in that: D in described silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 10-30%.
3. adopt the method for the slip pressureless sintering silicon carbide ceramic of the gel casting forming pressureless sintering silicon carbide ceramic described in claim 1 or 2, it is characterized in that: comprise the following steps:
1. raw materials pretreatment: proportionally take silicon carbide micro-powder, boron carbide micro powder, carbon source and dispersion agent, adds ethanol in proper amount and is made into suspension; Described silicon carbide micro-powder comprises D
50be respectively two kinds of sic powders of 0.78 μm and 0.41 μm, D in silicon carbide micro-powder
50be the parts by weight of the sic powder of 0.41 μm be 10-30%, described boron carbide micro powder is D
50be 0.93 μm, described carbon source is dextrin, and described dispersion agent is Tetramethylammonium hydroxide; In this step, count by weight, Tetramethylammonium hydroxide is 0.5% of silicon carbide micro-powder; After ball mill mixing, drying obtains dry powder;
2. prepare pelletizing: powder pressing step 1. obtained obtains closely knit base substrate, then fragmentation is sieved, and obtains pelletizing;
3. premixed liquid preparation: by soluble in water for the mass ratio that organic monomer and linking agent press 11-13:1, and add Tetramethylammonium hydroxide, be stirred to and mix, obtain premixed liquid; Described organic monomer is acrylamide, and described linking agent is N, N'-methylene-bisacrylamide; In this step, by volume mark meter, the add-on of described Tetramethylammonium hydroxide is the 1.3-1.4% of total slip;
4. Pulp preparation: pelletizing step 2. obtained joins in the premixed liquid that 3. step obtain, stirs and obtains silicon carbide dispersion slip;
5. casting: the slip that 4. step obtains injects mould, is heated to 60 DEG C, keeps 30-90min, obtains having larger elastic wet base;
6. base substrate binder removal: after the wet base drying that 5. step is obtained, be placed in vacuum oven, be warming up at a slow speed 800 DEG C, insulation 30min, obtains biscuit body;
7. blank sintering: gained biscuit body is placed in non-pressure sintering furnace, under 1atm Ar atmosphere, is warming up to 2200 DEG C, and insulation 1h, obtains sintered compact after cooling, namely final product.
4. the method for the slip pressureless sintering silicon carbide ceramic of employing according to claim 3 gel casting forming pressureless sintering silicon carbide ceramic according to claim 1, is characterized in that: described step 4. and step 5. between also comprise vacuum stripping step: slip step 4. obtained is degasification 10-30min under vacuum tightness is the condition of-0.1Mpa; Then in above-mentioned slip, add initiator and catalyzer, after fully stirring, repeat degassing procedure 5-10min, obtaining can the ceramic slurry of injection molding; Described initiator is ammonium persulphate, and described catalyzer is N, N, N', N'-tetramethyl-diethylamine.
5. the method for the slip pressureless sintering silicon carbide ceramic of employing according to claim 4 gel casting forming pressureless sintering silicon carbide ceramic according to claim 1, it is characterized in that: described step 6. in wet bad drying be specially: the wet base after the demoulding is moved in the drying installation of high humidity immediately, dry 4-6h; Then base substrate is moved in the drying installation of low humidity, dry 48h.Described high humidity is 70-80%, and described low humidity is 20-30%.
6. the method for the slip pressureless sintering silicon carbide ceramic of employing according to claim 4 gel casting forming pressureless sintering silicon carbide ceramic according to claim 1, it is characterized in that: the heating step of described base substrate binder removal is 1 DEG C/min, and the heating, cooling speed of described blank sintering is 10 DEG C/min.
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| CN107449324A (en) * | 2017-09-13 | 2017-12-08 | 山东汇金新材料有限公司 | One kind is without pressure solid-phase sintering boron carbide helmet and preparation method thereof |
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| CN108546128A (en) * | 2018-05-19 | 2018-09-18 | 奉化市飞固凯恒密封工程有限公司 | A kind of silicon carbide ceramics non-pressure sintering technology |
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| CN114988880A (en) * | 2022-07-15 | 2022-09-02 | 河南淅川平煤三责精密陶瓷有限公司 | Preparation method for preparing silicon carbide ceramic through gel injection molding and pressureless sintering |
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| CN114230346A (en) * | 2021-12-27 | 2022-03-25 | 宁波伏尔肯科技股份有限公司 | Silicon carbide composite powder for additive manufacturing and preparation method thereof |
| CN114988880A (en) * | 2022-07-15 | 2022-09-02 | 河南淅川平煤三责精密陶瓷有限公司 | Preparation method for preparing silicon carbide ceramic through gel injection molding and pressureless sintering |
| CN114988880B (en) * | 2022-07-15 | 2023-03-31 | 河南淅川平煤三责精密陶瓷有限公司 | Preparation method for preparing silicon carbide ceramic through gel injection molding and pressureless sintering |
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