CN114538897A - Sintering method of gel-casting ceramic green body - Google Patents
Sintering method of gel-casting ceramic green body Download PDFInfo
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- CN114538897A CN114538897A CN202011338375.0A CN202011338375A CN114538897A CN 114538897 A CN114538897 A CN 114538897A CN 202011338375 A CN202011338375 A CN 202011338375A CN 114538897 A CN114538897 A CN 114538897A
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- 238000005245 sintering Methods 0.000 title claims abstract description 83
- 239000000919 ceramic Substances 0.000 title claims abstract description 78
- 238000005266 casting Methods 0.000 title abstract description 7
- 239000002002 slurry Substances 0.000 claims abstract description 83
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
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- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 2
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- MEBJLVMIIRFIJS-UHFFFAOYSA-N hexanedioic acid;propane-1,2-diol Chemical compound CC(O)CO.OC(=O)CCCCC(O)=O MEBJLVMIIRFIJS-UHFFFAOYSA-N 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 229940049964 oleate Drugs 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
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- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6565—Cooling rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The invention provides a sintering method of a gel-casting ceramic green body, which comprises the following steps: a) placing the green body in an oven at 50-80 ℃ for pre-drying for 0.5-3 h; b) and placing the pre-dried green body in a high-temperature kiln for sintering treatment. In the sintering method, the alumina ceramic slurry is subjected to a one-time feeding technology, so that the problem that the ball milling time is difficult to control due to multiple feeding technologies is solved, the stability of different batches of slurry is improved, the binder removal pre-sintering is not required, and the green body treatment process is reduced; the formed ceramic product has size tolerance within 1% and over 30 mm.
Description
Technical Field
The invention relates to a sintering process of a ceramic green body, in particular to a sintering method of a gel-casting ceramic green body.
Background
Sintering is a process of densifying a blank by utilizing heat energy, and the sintering process of ceramics refers to a densification process of a porous ceramic blank under a high-temperature condition, wherein the densification process is characterized by size shrinkage, porosity reduction and mechanical property improvement. In the sintering process of the ceramic body, the change rule of the body in the high-temperature sintering process needs to be mastered, the kiln is correctly selected and designed, the sintering system is scientifically formulated and executed, and the firing operation procedure is strictly executed, so that the aims of improving the product quality, reducing the combustion consumption and obtaining good economic benefit are fulfilled.
For example, the invention patent with the domestic application number of CN200910042518.0 discloses a method for preparing BEO ceramic by utilizing a gel injection molding technology, which comprises the steps of raw material pretreatment, material preparation, ball milling and material mixing, vacuum degassing, gel curing, drying and glue discharging, and sintering; wherein, the sintering is to heat the green body with the moisture content not higher than 10% at the temperature of 400-800 ℃ at the speed of 0.5-5 ℃/min and then preserve the temperature for 0.5-3 h; and then heating to 1000-1500 ℃ at the speed of 10-30 ℃/min, and preserving the heat for 1-5 h. And finally, placing the blank body at 1500-2000 ℃ and preserving heat for 1-5 h.
The invention patent with the application number of CN201010516357.7 discloses a gel casting method and a preparation method of ceramics, wherein, the gel discharging condition comprises the following steps: discharging rubber for 1-6 h at 200-800 ℃; the sintering conditions include: heating to 1000 deg.C within 2h, heating to 1250 deg.C within 25min, and maintaining for 20 min; heating to 1850 ℃ within 1h, and keeping the temperature for 30 min; finally, the temperature is raised to 2150 ℃ within 40min, and the temperature is kept for 1 h. The ceramics obtained by the method have higher mechanical properties.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, the present invention provides a method for sintering a gel-cast ceramic green body, which does not require binder removal and pre-sintering, and reduces the green body processing procedure, thereby solving the problems of the prior art.
To achieve the above objects and other related objects, the present invention includes the following technical solutions.
The invention provides a sintering method of a gel-casting ceramic green body, which comprises the following steps:
a) placing the green body in an oven at 50-80 ℃ for pre-drying for 0.5-3 h;
b) placing the pre-dried green body in a high-temperature kiln for sintering treatment: raising the temperature from room temperature to 400-500 ℃ at a temperature rise rate of 2-5 ℃/min, preserving the heat at 400-500 ℃ for 0.5-2 h, then continuously raising the temperature to 600-700 ℃ at a temperature rise rate of 5-10 ℃/min, and preserving the heat at 600-700 ℃ for 1-2 h; then, continuously heating to 1500-1600 ℃ at the heating rate of 2.5-5 ℃/min, and preserving the heat for 2-4 h at 1500-1600 ℃; finally, the temperature is reduced to 40-70 ℃ at the cooling rate of 4-8 ℃/min, and then the temperature is cooled to the room temperature along with the furnace.
According to the sintering method, the green body is obtained by adopting the aluminum oxide ceramic slurry to perform cross-linking polymerization reaction with an initiator under the action of a catalyst.
According to the sintering method, the initiator is one or more than two selected from hydrogen peroxide, ammonium persulfate and potassium persulfate.
According to the sintering method, the adding amount of the initiator is not more than 1 wt% of the mass of the alumina ceramic slurry. Preferably, the addition amount of the initiator is not more than 0.01 wt% to 1 wt% of the mass of the alumina ceramic slurry. The initiator is used to cause the slurry to undergo a cross-linking polymerization reaction.
According to the sintering method, the product is dried after the cross-linking polymerization reaction until the water content of the green body is 2 wt% -10 wt%.
According to the sintering method, the drying can be room temperature drying, constant temperature and humidity drying, liquid drying or microwave drying.
According to the sintering method, a catalyst is also adopted in the cross-linking polymerization reaction, and the catalyst is one or more selected from tetramethylethylenediamine, a mixture of cuprous chloride and 2, 2-bipyridine and a mixture of cuprous chloride and ethylenediamine. The catalyst is used for accelerating the reaction rate, the addition amount is excessive, the operable time is too short, the slurry is easily not completely filled into a mold, the cross-linking polymerization reaction is finished, and the defect rate of a green body is increased; on the contrary, the addition amount is insufficient, which results in overlong reaction time and reduced production efficiency.
According to the sintering method, the adding amount of the catalyst is not more than 1 wt% of the mass of the alumina ceramic slurry. Preferably, the adding amount of the catalyst is not more than 0.01 wt% to 1 wt% of the mass of the alumina ceramic slurry.
According to the sintering method, the alumina ceramic slurry comprises the following raw material components in parts by weight:
the pH value of the alumina ceramic slurry is 9-10.
According to the sintering method, the pH regulator is one or more selected from ammonia water, N-methylethanolamine, monoethanolamine, diethanolamine, triethanolamine and butylethanolamine.
According to the sintering method, the particle size of the alumina powder is one or more than two selected from 300-500 meshes, 1000-2000 meshes, 2000-2500 meshes and 3000-5000 meshes.
The sintering method, wherein the sintering aid is selected from SiO2、TiO2、CaCO3、MgO、V2O5、CuO、MnO2、Fe2O3One ofOne or more of them. Preferably, the particle size of the sintering aid is 400-600 meshes. Preferably, the purity of the sintering aid is not less than 99.5%. The ceramic powder does not contain a sintering aid, and a formed product is difficult to form ceramic at the same sintering temperature, so that the strength is low, and the density is low due to the existence of a large number of air holes in the ceramic powder; in the using process, external moisture permeates into the air holes, so that the performance indexes such as the heat conductivity, the pressure resistance value and the like of the water-based composite material can not meet the using requirements.
According to the sintering method, acrylamide is not contained, and the slurry in the mold can not generate cross-linking polymerization reaction to form a ceramic wet blank; the addition amount of acrylamide is too small, the formed ceramic wet blank has low strength and poor dimensional stability, and is easy to deform after sintering; on the contrary, the addition of the acrylamide is too much, the strength of the ceramic wet blank is too high, and the ceramic wet blank is easy to crack in the demoulding process. For similar reasons, the slurry in the mold does not undergo a cross-linking polymerization reaction to form a ceramic wet blank, and the slurry remains liquid, without the presence of N-N methylene bisacrylamide.
According to the sintering method, the dispersing agent is selected from one or more of acacia gum powder, ammonium polyacrylate, polymethacrylamide, ammonium citrate, sodium polymethacrylate, sodium hexametaphosphate and polyvinyl alcohol. Preferably, the molecular weight of the ammonium polyacrylate is 5000-6000. Preferably, the viscosity of the gum arabic powder at 25 ℃ is 60-130 cps; the pH value of the formed 250g/L aqueous solution is 4-8. The ceramic slurry is free of dispersing agent, the viscosity of the ceramic slurry after ball milling is high under the same solid content condition, the flowing of the slurry in a mould and the discharge of air bubbles are influenced, the surface defects of a wet blank formed after the pouring and condensing reaction are more, and the ceramic yield is low; under high solid content conditions, if no dispersant is contained, even a flowable slurry cannot be formed, and thus cast molding cannot be completed.
According to the sintering method, the raw material components of the alumina ceramic slurry further comprise an oxygen polymerization inhibitor, and the oxygen polymerization inhibitor is one or more than two selected from polyvinylpyrrolidone, polyacrylamide, polyoxyethylene, 1, 4-butanediol and 1, 3-butanetriol. Preferably, the amount of the oxygen polymerization inhibitor added is not more than 2 parts by weight. The ceramic green body obtained by the cross-linking polymerization reaction has the phenomenon of sticking in different degrees in partial high-molecular moulds, and the introduction of a proper amount of oxygen polymerization inhibitor can obviously weaken the phenomenon of sticking, reduce oxygen inhibition, reduce the porosity of the green body and improve the secondary processing capability of the green body. On the contrary, the introduction amount of the oxygen polymerization inhibitor is too large, and the surface of the solidified green body has uneven and uneven phenomena.
According to the sintering method, the raw material components of the alumina ceramic slurry further comprise a plasticizer, and the addition amount of the plasticizer is not more than 1 part by weight. Preferably, the plasticizer is one or more selected from dibutyl phthalate, dioctyl adipate, tricresyl phosphate, butyl epoxy oleate, propylene glycol adipate polyester, triisooctyl 1,2, 4-trimellitate, benzoic acid and propylene glycol. The plasticizer is added to improve the plasticity of the green body and improve the secondary processing capacity of the green body.
According to the sintering method, the raw material components of the alumina ceramic slurry also comprise no more than 0.5 part by weight of defoaming agent; the defoaming agent is selected from one or more of n-butanol, basf A10 and ethanol. During the ball milling preparation and discharging process of the slurry for injection and coagulation, air is inevitably involved to form bubbles, if the bubbles are not completely removed, the problem of oxygen inhibition is caused in the gelation process, and as a result, defects far larger than the size of the bubbles can remain in the interior or on the surface of a gel blank, and become defects of a ceramic body or a cracking source after sintering, and the phenomenon can be obviously improved by introducing the defoaming agent, so that the ceramic yield is improved.
According to the sintering method, the preparation method of the alumina ceramic slurry comprises the following steps: mixing the raw material components and then carrying out ball milling, wherein the discharge granularity of the ball milling is 0.5-3 mu m; meanwhile, a pH regulator is added in the process, so that the pH value of the finally formed alumina ceramic slurry is 9-10. The pH value has great influence on the stability of slurry, the pH values are different, and H is adsorbed on the surface of the powder+Or OH-The difference in the number of ions leads to a difference in the charging condition, which directly affects the electrostatic repulsion between the ions. In the patent, on the premise of ensuring that the die is not corroded, the ceramic is usedThe pH value (9-10) of the slurry is controlled at a position where the absolute value of the Zeta potential is larger, so that higher electrostatic repulsion force among the powder is ensured, and the slurry is ensured to have good dispersibility.
According to the preparation method of the alumina ceramic slurry, the step of eliminating bubbles is also included, and the step can be natural defoaming or vacuum defoaming. Preferably, the gas bubbles remaining in the slurry are eliminated by vacuum treatment.
According to the sintering method, the viscosity of the ceramic slurry at 25 ℃ is 100-500 mPa & s. When the product is used for preparing ceramic by gel casting, bubbles in the ceramic slurry can easily escape from pores of the mold during the forming process, thereby reducing the surface defects of the ceramic green body and improving the compactness.
In accordance with the sintering method described above, a method of drying a green body formed from a ceramic slurry is also disclosed herein, comprising the steps of:
1) mixing raw materials for forming a green body under the environment with the temperature of 15-25 ℃ and the humidity of 30% -50%, reacting in a mold, and taking out from the mold;
2) then placing the mixture on a flat and breathable mesh screen, and standing the mixture for 8-12 hours in an environment with the temperature of 10-25 ℃ and the humidity of 70-90%;
3) then placing the mixture in an organic solvent or an organic solvent water solution for soaking for 0.5 to 4 hours;
4) taking out the mixture from the organic solvent or the organic solvent water solution, wiping the mixture to remove surface liquid, and standing the mixture in a well-ventilated environment with the temperature of 15-25 ℃ and the humidity of 20-45% for 6-12 hours.
According to the drying method, the material of the mold is one or two selected from glass and stainless steel. According to the preparation method, in the step 3), the organic solvent is one or more than two selected from ethanol, propanol, ethanone, acetone, methyl ether, ethyl ether, polyethylene glycol, acetaldehyde and propionaldehyde.
The sintering method has the advantages of mild drying conditions, short drying time and simple operation; the problems that heating and drying are easy to cause green body deformation, pure solvent drying production cost is high, solvent concentration is uncontrollable, potential safety hazards are brought, and room temperature drying production efficiency is low are solved, and finally formed green bodies are low in deformation rate, small in shrinkage rate and high in size stability.
The alumina ceramic slurry provided by the invention is prepared by a one-time feeding technology, so that the problem that the ball milling time is difficult to control due to a multiple-time feeding technology is solved, the stability of slurries in different batches is improved, the method does not need to carry out binder removal pre-sintering, the green body treatment process is reduced, and the ceramic product formed by adopting the sintering method is in the size range of more than 30mm, and the size tolerance can be controlled within 1%.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
In the examples, the viscosity of the slurry was measured using a rotational viscometer.
In the embodiment of the application, the particle size of the alumina powder is one or more selected from 120-150 meshes, 300-500 meshes, 1000-2000 meshes, 2000-2500 meshes and 3000-5000 meshes.
In the embodiment of the application, the dispersing agent is selected from one or more of acacia gum powder, ammonium polyacrylate, polymethacrylamide, ammonium citrate, sodium polymethacrylate, sodium hexametaphosphate and polyvinyl alcohol.
In the embodiment, the viscosity of the gum arabic powder at 25 ℃ is 60-130 cps; the pH value of the formed 250g/L aqueous solution is 4-8.
In the embodiment, the molecular weight of the ammonium polyacrylate is 5000-6000.
In this embodiment, a pH adjuster selected from one or more of ammonia, N-methylethanolamine, monoethanolamine, diethanolamine, triethanolamine, and butylethanolamine is used to adjust the pH of the ceramic slurry. Specifically, monoethanolamine may be selected.
The preparation method of the ceramic slurry in the embodiment comprises the following steps: mixing the raw material components, performing ball milling, adding a pH regulator in the ball milling process to adjust the pH value of the slurry, wherein the discharge granularity of the ball milling is 0.5-3 mu m.
In this example, the method for testing the ceramic density was: in this experiment, the bulk density of the sample was determined according to the archimedes' principle of drainage. Firstly, drying a fired ceramic sample in an oven at 100 ℃, cooling the ceramic sample to room temperature in a dryer, weighing the ceramic sample, and repeating the step until the weight is constant to obtain the dry weight of the sample; and then boiling the sample in boiling water for 6 hours to open pores in the ceramic material, taking out the sample, and measuring the float weight and the wet weight. And finally, calculating the density according to a formula listed below:
ρ＝m1*ρliquid for treating urinary tract infection/(m3-m2)(m1Is the dry weight of the sample; m is3Is the saturated wet weight of the ceramic sample; m is2The weight of the sample in the test liquid, pLiquid for treating urinary tract infectionRefers to the specific gravity of water).
In the embodiments of the present application, the green body is dried before the sintering method is performed, and the drying method specifically includes:
1) mixing raw materials for forming a green body at 20 ℃ and under the environment with the humidity of 40%, reacting in a mold, and taking out from the mold; the mould is made of glass;
2) placing the green body on a flat and breathable mesh screen, and standing for 10 hours in an environment with the temperature of 20 ℃ and the humidity of 80%;
3) then placing the mixture into 30 wt% ethanol water solution for soaking treatment for 2 h;
4) the solution was taken out of the aqueous ethanol solution, wiped to remove surface liquid, and then left to stand in a well-ventilated environment at 20 ℃ and a humidity of 40% for 8 hours.
Example 1
The ceramic slurry in the embodiment comprises the following raw material components in parts by weight:
and adjusting the pH value of the ceramic slurry to 9-10 by using a pH regulator.
The sintering aid is SiO2And TiO2The mixture formed according to 1: 1.
The dispersant in this example was gum powder.
The preparation method of the ceramic slurry in the embodiment comprises the following steps: mixing the raw material components, performing ball milling, adding a pH regulator in the ball milling process to adjust the pH value of the slurry, wherein the discharge granularity of the ball milling is 0.5-3 mu m; and finally, removing gas in the slurry by adopting vacuum defoaming.
The viscosity of the slurry in this example was 175 mPas, and no significant delamination occurred after 15 days at room temperature.
Example 2
The ceramic slurry in the embodiment comprises the following raw material components in parts by weight:
and adjusting the pH value of the ceramic slurry to 9-10 by using a pH regulator.
The dispersant in this example was gum powder.
The sintering aid is SiO2And CaCO3The mixture formed according to 1: 1.
The preparation method of the ceramic slurry in the embodiment comprises the following steps: mixing the raw material components, performing ball milling, adding a pH regulator in the ball milling process to adjust the pH value of the slurry, wherein the discharge granularity of the ball milling is 0.5-3 mu m; and finally, removing the internal gas of the slurry by adopting vacuum defoaming.
And (3) testing results: the viscosity of the slurry prepared by the method is 330 mPa.s, and the slurry is placed at room temperature for 15 days without obvious layering.
Example 3
The ceramic slurry in the embodiment comprises the following raw material components in parts by weight:
and adjusting the pH value of the ceramic slurry to 9-10 by using a pH regulator.
The dispersant in this example is ammonium polyacrylate.
In this example, the sintering aid is TiO2。
The preparation method of the ceramic slurry in the embodiment comprises the following steps: mixing the raw material components, performing ball milling, adding a pH regulator in the ball milling process to adjust the pH value of the ceramic slurry, wherein the discharge granularity of the ball milling is 0.5-3 mu m; and finally, removing gas in the slurry by adopting vacuum defoaming.
And (3) testing results: the viscosity of the slurry prepared by the method is 350 mPas, and the slurry is placed at room temperature for 15 days without obvious layering.
Example 4
The ceramic slurry in the embodiment comprises the following raw material components in parts by weight:
and adjusting the pH value of the ceramic slurry to 9-10 by using a pH regulator.
The dispersant in this example is ammonium polyacrylate.
In this embodiment, the sintering aid is SiO2And CaCO3The mixture formed according to 1: 3.
The preparation method of the ceramic slurry in the embodiment comprises the following steps: mixing the raw material components, performing ball milling, adding a pH regulator in the ball milling process to adjust the pH value of the ceramic slurry, wherein the discharge granularity of the ball milling is 0.5-3 mu m; and finally, removing gas in the slurry by adopting vacuum defoaming.
And (3) testing results: the viscosity of the slurry prepared by the method is 220 mPas, and the slurry is placed at room temperature for 15 days without obvious layering.
Example 5
In this example, the alumina ceramic slurry formed in example 1 was mixed with an initiator, ammonium persulfate, and a catalyst, tetramethylethylenediamine, and subjected to a cross-linking polymerization reaction to obtain a green compact.
In this embodiment, the sintering method includes the steps of:
a) placing the green body in a 50 ℃ oven for pre-baking for 1h before high-temperature sintering;
b) placing the pre-dried green body in a high-temperature kiln for sintering treatment: heating from room temperature to 450 ℃ at the heating rate of 2 ℃/min, and preserving the heat at 450 ℃ for 1 h; then heating from 450 ℃ to 650 ℃ at the heating rate of 5 ℃/min, and preserving the heat at 650 ℃ for 2 h; heating from 650 ℃ to 1550 ℃ at the heating rate of 4 ℃/min, and keeping the temperature at 1550 ℃ for 4 h; finally, the temperature is reduced from 1550 ℃ to 50 ℃ at the cooling rate of 4 ℃/min, and then the temperature is cooled to the room temperature along with the furnace.
And (3) testing results: the yield of the ceramic fired from the green body of the batch is 96.5 percent, and the ceramic density is 3.78g/cm3(ii) a The formed ceramic product has size tolerance within 1% and over 30 mm.
Example 6
In this example, the alumina ceramic slurry formed in example 2 was mixed with an initiator, ammonium persulfate, and a catalyst, tetramethylethylenediamine, and subjected to a cross-linking polymerization reaction to obtain a green compact.
In this embodiment, the sintering method includes the steps of:
a) placing the green body in a 60 ℃ oven for pre-drying for 0.5h before high-temperature sintering;
b) placing the pre-dried green body in a high-temperature kiln for sintering treatment: heating from room temperature to 450 ℃ at the heating rate of 2 ℃/min, and preserving the heat at 450 ℃ for 1.5 h; heating from 450 ℃ to 650 ℃ at the heating rate of 8 ℃/min, and keeping the temperature at 650 ℃ for 1 h; heating from 650 ℃ to 1550 ℃ at the heating rate of 2.5 ℃/min, and preserving heat for 3h at 1550 ℃; the temperature is reduced from 1550 ℃ to 50 ℃ at the cooling rate of 6 ℃/min, and then the temperature is cooled to the room temperature along with the furnace.
And (3) testing results: the yield of the ceramic fired from the green body of the batch is 96 percent, and the ceramic density is 3.74g/cm3(ii) a The formed ceramic product has size tolerance within 1% and over 30 mm.
Example 7
In this example, the alumina ceramic slurry formed in example 3 was mixed with an initiator, ammonium persulfate, and a catalyst, tetramethylethylenediamine, and subjected to a cross-linking polymerization reaction to obtain a green compact.
In this embodiment, the sintering method includes the steps of:
a) before high-temperature sintering, placing the green body in an oven at 80 ℃ for pre-drying for 0.5 h;
b) placing the pre-dried green body in a high-temperature kiln for sintering treatment: heating from room temperature to 450 ℃ at the heating rate of 4 ℃/min; keeping the temperature at 450 ℃ for 2 h; then heating from 450 ℃ to 650 ℃ at the heating rate of 6 ℃/min, and preserving the heat at 650 ℃ for 1 h; heating from 650 ℃ to 1550 ℃ at the heating rate of 5 ℃/min, and keeping the temperature at 1550 ℃ for 2 h; finally, the temperature is reduced from 1550 ℃ to 50 ℃ at the cooling rate of 7 ℃/min, and then the temperature is cooled to the room temperature along with the furnace.
And (3) testing results: the yield of the ceramic fired by the green body of the batch is 99 percent, and the ceramic density is 3.85g/cm3(ii) a The formed ceramic product has size tolerance within 1% and over 30 mm.
Example 8
In this example, the alumina ceramic slurry formed in example 4 was mixed with an initiator, ammonium persulfate, and a catalyst, tetramethylethylenediamine, and subjected to a cross-linking polymerization reaction to obtain a green compact.
In this embodiment, the sintering method includes the steps of:
a) before high-temperature sintering, placing the green body in a 50 ℃ oven for pre-baking for 2 hours;
b) placing the pre-dried green body in a high-temperature kiln for sintering treatment, heating the green body from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving heat at 450 ℃ for 1 h; heating from 450 ℃ to 650 ℃ at the heating rate of 5 ℃/min, and keeping the temperature at 650 ℃ for 2 h; heating from 650 ℃ to 1550 ℃ at the heating rate of 3.5 ℃/min, and keeping the temperature at 1550 ℃ for 2 h; cooling from 1550 ℃ to 50 ℃ at a cooling rate of 8 ℃/min, and then naturally cooling to room temperature.
And (3) testing results: the yield of the ceramic fired by the green body of the batch is 98.2 percent, and the ceramic density is 3.82g/cm3(ii) a The formed ceramic product has size tolerance within 1% and over 30 mm.
Comparative example 1
The same procedure as in example 1 was repeated except that the sintering aid was not contained in example 1.
The ceramic powder does not contain a sintering aid, and a formed product cannot be completely ceramic at the same sintering temperature, so that the strength is low, and the density is low and is only 2.83g/cm due to the existence of a large number of air holes in the ceramic powder3(ii) a During the use process, external moisture permeates into the air holes, so that the performance indexes such as the heat conductivity, the pressure resistance value and the like of the water-based composite material can not meet the use requirements.
Comparative example 2
The same procedure as in example 1 was repeated except that acrylamide was not contained in example 1.
The ceramic wet blank does not contain acrylamide, and the slurry in the mold does not undergo a cross-linking polymerization reaction to form a ceramic wet blank; the addition amount of acrylamide is too small, the formed ceramic wet blank has low strength and poor dimensional stability, and is easy to deform after sintering; on the contrary, the addition of the acrylamide is too much, the strength of the ceramic wet blank is too high, and the ceramic wet blank is easy to crack in the demoulding process.
Comparative example 3
The same procedure as in example 1 was repeated except that N-N methylene bisacrylamide was not contained in example 1.
The slurry in the mould does not contain N-N methylene-bisacrylamide, the cross-linking polymerization reaction of the slurry in the mould does not occur to form a ceramic wet blank, and the slurry still keeps liquid state.
Comparative example 4
The procedure was as in example 1 except that the dispersant was not contained in example 1.
The slurry prepared by the method has the viscosity of 820mPa & s, obvious layering phenomenon can occur after the slurry is placed at room temperature for 1 day, the surface defects of a wet blank formed after the injection coagulation reaction are more, and the yield of the wet blank is only 40%.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method of sintering a green gel-cast ceramic body comprising the steps of:
a) placing the green body in an oven at 50-80 ℃ for pre-drying for 0.5-3 h;
b) placing the pre-dried green body in a high-temperature kiln for sintering treatment: raising the temperature from room temperature to 400-500 ℃ at a temperature rise rate of 2-5 ℃/min, preserving the heat at 400-500 ℃ for 0.5-2 h, then continuously raising the temperature to 600-700 ℃ at a temperature rise rate of 5-10 ℃/min, and preserving the heat at 600-700 ℃ for 1-2 h; then, continuously heating to 1500-1600 ℃ at the heating rate of 2.5-5 ℃/min, and preserving the heat for 2-4 h at 1500-1600 ℃; finally, the temperature is reduced to 40-70 ℃ at the cooling rate of 4-8 ℃/min, and then the temperature is cooled to the room temperature along with the furnace.
2. The sintering method according to claim 1, wherein the green body is obtained by a cross-linking polymerization reaction of an alumina ceramic slurry and an initiator under the action of a catalyst.
3. The sintering method according to claim 2, wherein the initiator is one or more selected from the group consisting of hydrogen peroxide, ammonium persulfate, and potassium persulfate;
and/or the addition amount of the initiator is not more than 1 wt% of the mass of the alumina ceramic slurry.
4. The sintering method according to claim 2, further comprising drying the product after the cross-linking polymerization reaction until the water content of the green compact is 2 wt% to 10 wt%.
5. The sintering method according to claim 2, wherein the catalyst is one or more selected from the group consisting of tetramethylethylenediamine, a mixture of cuprous chloride and 2, 2-bipyridine, and a mixture of cuprous chloride and ethylenediamine.
6. The sintering method according to claim 2, wherein the alumina ceramic slurry comprises the following raw material components in parts by weight:
the pH value of the alumina ceramic slurry is 9-10.
7. Sintering method according to claim 6, characterised in that the sintering aid is selected from SiO2、TiO2、CaCO3、MgO、V2O5、CuO、MnO2、Fe2O3One or more of the above;
and/or the dispersing agent is selected from one or more of the group consisting of gum arabic powder, ammonium polyacrylate, polymethacrylamide, ammonium citrate, sodium polymethacrylate, sodium hexametaphosphate and polyvinyl alcohol.
8. The sintering method according to claim 6, wherein the raw material composition of the alumina ceramic slurry further comprises not more than 2 parts by weight of an oxygen polymerization inhibitor, and the oxygen polymerization inhibitor is one or more selected from polyvinylpyrrolidone, polyacrylamide, polyoxyethylene, 1, 4-butanediol, and 1, 3-butanetriol.
9. The sintering method according to claim 6, wherein the raw material composition of the alumina ceramic slurry further comprises not more than 1 part by weight of a plasticizer selected from one or more of dibutyl phthalate, dioctyl adipate, tricresyl phosphate, butyl epoxy oleate, propylene glycol adipate polyester, triisooctyl 1,2, 4-trimellitate, benzoic acid, and propylene glycol;
and/or the raw material components of the alumina ceramic slurry also comprise no more than 0.5 weight part of defoaming agent; the defoaming agent is one or more selected from n-butanol, basf A10, and ethanol
And/or the preparation method of the alumina ceramic slurry comprises the following steps: mixing the raw material components and then carrying out ball milling, wherein the discharge granularity of the ball milling is 0.5-3 mu m.
10. The sintering method according to claim 1, wherein the green body is subjected to a drying process before the sintering process, the drying process being:
1) mixing raw materials for forming a green body under the environment with the temperature of 15-25 ℃ and the humidity of 30% -50%, reacting in a mold, and taking out from the mold; 2) then placing the mixture on a flat and breathable mesh screen, and standing the mixture for 8-12 hours in an environment with the temperature of 10-25 ℃ and the humidity of 70-90%;
3) then placing the mixture in an organic solvent or an organic solvent water solution for soaking for 0.5 to 4 hours;
4) taking out the mixture from the organic solvent or the organic solvent water solution, wiping the mixture to remove surface liquid, and standing the mixture in a well-ventilated environment with the temperature of 15-25 ℃ and the humidity of 20-45% for 6-12 hours.
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