CN1174933C - Liquid-solid gel reaction process of synthesizing ceramic powder - Google Patents
Liquid-solid gel reaction process of synthesizing ceramic powder Download PDFInfo
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- CN1174933C CN1174933C CNB01130801XA CN01130801A CN1174933C CN 1174933 C CN1174933 C CN 1174933C CN B01130801X A CNB01130801X A CN B01130801XA CN 01130801 A CN01130801 A CN 01130801A CN 1174933 C CN1174933 C CN 1174933C
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Abstract
The present invention relates to a low-cost preparation method of ceramic powder, which belongs to the field of inorganic non-metal materials. The present invention uses a liquid-solid gelling reaction method for synthesizing ceramic powder and has the technical steps of material preparation, ball-milling mixture, slurry gelling drying and thermal processing. The present invention solves the low-cost rapid preparation technology of single-phase ceramic powder, complex-phase ceramic powder and composite function ceramic powder and has the advantages of sufficient source of raw materials, mature and reliable technology, convenient manufacture and high production efficiency.
Description
Technical field: the invention belongs to field of inorganic nonmetallic material, relate to the low-cost preparation method of ceramic powder.
Background technology: common ceramic powder preparation method mainly contains sol-gel method and coprecipitation method etc.People such as domestic Chen Wei [University of Science ﹠ Technology, Beijing's journal, 1995, Vol (5)] and Ma Yalu [inorganic chemicals industry, 1998, Vol (1)] utilize coprecipitation method to prepare multiple ceramic powder.The coprecipitation method raw materials cost is low, is easy to prepare the multicomponent system powder, but its coagulation process and filtration procedure repeatedly are quite time-consuming, loaded down with trivial details.And for the polycomponent compound system, because of different metal ion in the solution generates sedimentary condition difference, it almost is impossible allowing the different kinds of ions of composition material precipitate simultaneously.Simultaneously, different throw out solubility product differences may generating unit in the water washing process be divided the loss of component, cause the inaccurate of composition, influence the performance of powder.People [XI AN JIAOTONG UNIVERSITY Subject Index, 1996, Vol (12)] such as people such as Wang Yuhua [Lanzhou University's journal, 1994, Vol (3)] and Yao Kui have prepared multiple ultra micro ceramic powder with sol-gel method respectively.
Sol-gel method is utilized good dispersed and suitable dehydration, the drying process of colloidal particle, can obtain the nanometer superfine powder body.But it is a raw material with the more expensive metal alkoxide of price all generally, and cost height, cycle are long, and the control of sol-gel process also has certain difficulty, if dewatering was not at that time, polycondensation, caking phenomenon occur, cause the hard aggregation between the particle, so its industrialization generation has been subjected to very big restriction.
Summary of the invention: the present invention proposes a kind of new powder synthetic method-liquid-solid gel reaction synthesis method, to overcome shortcoming such as the loaded down with trivial details and cost height of washing, filter operation that polycomponent that traditional solid reaction process exists disperses inhomogeneous problem of bringing and conventional liquid phase method to exist, simultaneously, also can avoid the generation and the problem of environment pollution caused of obnoxious flavour.
Technical scheme of the present invention is: a kind of method of utilizing the liquid-solid gel reaction synthesizing ceramic powder, it is characterized in that,
1, batching, composition requirement according to prepared ceramic powder, calculate and various required solid-state ceramic raw material powders of weighing and soluble compound raw material, measure required deionized water or distilled water by solid volume fraction 40～55vol%, soluble compound is dissolved in the water, then the soluble compound aqueous solution and solid-state ceramic raw material powder are added in the ball grinder, add neutral ceramic slurry dispersion agent-ZD282 simultaneously, the add-on of dispersion agent is 0.2%～0.8% of a solid-state ceramic raw material powder weight, take by weighing organic monomer and linking agent again, organic monomer is water soluble propene's acid amides or Methacrylamide, linking agent is N, N '-methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the ratio of organic monomer and linking agent can be chosen between 10: 1～30: 1, and total add-on is 10～30% of a water weight;
2, ball milling mixes, after various raw materials prepare, ball grinder is placed on carries out ball milling on the ball mill and mix, the ball milling time decides according to the initial size of ceramic powder, be generally 5～30h, before discharging, add organic monomer and linking agent during 2h, continue ball milling, discharging behind the 2h finally forms the mixed uniformly ceramic slurry of each component;
3, slurry gel, adding initiator in through the mixed ceramic slurry of ball milling is ammonium persulfate aqueous solution, stirs, the add-on of initiator is 0.2～0.6% of an organic monomer weight; Heat then and make its gelation, can be placed in the thermostat container or put into water bath and heat, Heating temperature is 30～100 ℃;
4, drying after solution gelization is finished, is taken out gelinite, is cut into small pieces, and dehydrates then, and drying mode can adopt seasoning, blowing drying or heat drying;
5, thermal treatment is placed on dried gelinite in the air furnace and heat-treats, and temperature rise rate is controlled at 5～20 ℃, at first is raised to 500～700 ℃ of insulation 0.5～5h, is warmed up to 800～1600 ℃ of insulation 2～8h then, and cooling is come out of the stove then.
The invention solves the low-cost technology of preparing fast of single-phase, complex phase and composite function ceramics powder, and proposed a whole set of technical scheme, make it to be adapted to the suitability for industrialized production requirement.Its advantage mainly shows as:
The first, compare with domestic and international at present general ceramic powder preparation method, adopting general ceramics powder and inorganic salt is raw material, and the starting material source is sufficient.
The second, this technical maturity is reliable, and is easily manufactured, the production efficiency height.
Three, this technology part raw material adopts inorganic salt solution, become the mixing between the liquid-solid phase, utilize the polymer principle to realize the uniform mixing of various raw materials by high molecular instaneous polymerization, help fully carrying out fast of late phase reaction transformation, also can guarantee the uniformity consistency on the last powder composition.
Four, synthesis temperature can reduce by 200～300 ℃, has saved the energy greatly.
Description of drawings.
Description of drawings: Fig. 1 is the process flow sheet that utilizes solid-liquid gel reaction synthesizing ceramic powder.
Embodiment: the present invention is described in further details below in conjunction with accompanying drawing.The present invention is very simple to the requirement of raw material, and major ingredient is a ceramics powder, and auxiliary material is that inorganic salt solution gets final product, if can't divide main ingredient the time, a kind of ceramics powder of using another kind ofly gets final product with inorganic salt solution.Prepared powder diameter is relevant with the initial particle diameter of ceramic powder stock.Main technique step of the present invention is as follows:
1, batching.
Composition requirement according to prepared ceramic powder, calculate and according to predetermined various required ceramic raw materials of proportioning weighing and inorganic salt raw material, measure required deionized water or distilled water by solid volume fraction 40～55vol%, soluble compound is dissolved in the water, then the soluble compound aqueous solution is added and be equipped with in the ball grinder of ceramic powder, add neutral ceramic slurry dispersion agent simultaneously, the add-on of dispersion agent is 0.2%～0.8% of a pressed powder content; Take by weighing organic monomer and linking agent.Organic monomer is water soluble propene's acid amides or Methacrylamide, linking agent is N, N '-methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the ratio of organic monomer and linking agent can be chosen between 10: 1～30: 1, and total add-on is 10～30% of a water weight;
2, ball milling mixes.
After various raw materials prepare, ball grinder is placed on carries out ball milling on the ball mill and mix, the ball milling time decide according to the initial size of ceramic powder, initial size hour, the ball milling time is short, opposite initial size is greatly the time, ball milling time length.Be generally 5～30h, add organic monomer and linking agent during 2h before discharging, continue ball milling, discharging behind the 2h finally forms the mixed uniformly ceramic slurry of each component.
3, slurry gel.
Add the initiator ammonium persulfate aqueous solution in the mixed above-mentioned solution of abundant ball milling, stir, the add-on of initiator is 0.2～0.6% of an organic monomer weight; Heat then, can be placed directly in the thermostat container or put into water bath and heat, Heating temperature is 30～100 ℃.
4, drying.
After solution gelization is finished, gelinite is taken out, be cut into small pieces, dehydrate then, drying mode can adopt seasoning, blowing drying or heat drying.
5, thermal treatment.
Dried gelinite is placed in the air furnace heat-treats, stove can be sintering ovens such as box-type furnace, bell jar stove, tunnel furnace, and temperature rise rate is controlled at 5～20 ℃, at first is raised to 500～700 ℃ of insulation 0.5～5h, be warmed up to 800～1600 ℃ of insulation 2～8h then, cooling is come out of the stove then.
The preparation of embodiment 1 yttria-stabilized zirconia (2.5mol%) powder.
Adopt Y (NO
3)
36H
2O and Zirconium oxide powder (d
50=2 μ m) as raw material, account for the ratio batching of 2.5mol% in yttrium oxide, add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide, fully mix, the initiator (5% ammonium persulfate aqueous solution for preparing in advance) that adds slip weight 0.5% again after stirring, is put into (also can put into thermostat container is incubated) in 100 ℃ of water baths, all gelations after about 5 minutes, take out gelinite, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h under 900 ℃ of conditions promptly obtains yttria-stabilized zirconia (2.5mol%) powder.
The preparation of embodiment 2 magnesium-aluminium spinel powder.
Adopt Mg (NO
3)
26H
2O and Al
2O
3(d
50=2.5 μ m) be raw material, press MgO: Al
2O
3=1: 1 (mol ratio) batching, add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide fully mixes, and adds the initiator (5% ammonium persulfate aqueous solution for preparing in advance) of slip weight 0.5% again, after stirring, put into (also can put into thermostat container is incubated) in 100 ℃ of water baths, gelinite is taken out in all gelations after about 8 minutes, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h under 1100 ℃ of conditions promptly obtains the magnesium-aluminum spinel ceramic powder.The XRD spectrum of powder as shown in Figure 2.
The preparation of embodiment 3 magnesium-aluminium spinel powder.
Adopt Mg (OH)
24MgCO
36H
2O and Al
2(SO
4)
312H
2O is a raw material, presses MgO: Al
2O
3=1: 1 (mol ratio) batching, add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide fully mixes, and adds the initiator (5% ammonium persulfate aqueous solution for preparing in advance) of slip weight 0.5% again, after stirring, put into (also can put into thermostat container is incubated) in 100 ℃ of water baths, gelinite is taken out in all gelations after about 8 minutes, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h under 1100 ℃ of conditions promptly obtains the magnesium-aluminum spinel ceramic powder.
The preparation of embodiment 4 yttrium aluminum garnets (YAG) powder.
Adopt Y (NO
3)
36H
2O and Al
2O
3(d
50=2.5 μ m) be raw material, press yttrium oxide: Al
2O
3The ratio batching of=2: 5 (mol ratios), add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide fully mixes, and adds the initiator (5% ammonium persulfate aqueous solution for preparing in advance) of slip weight 0.5% again, after stirring, put into (also can put into thermostat container is incubated) in 100 ℃ of water baths, gelinite is taken out in all gelations after about 8 minutes, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h can obtain yttrium aluminum garnet (YAG) ceramic powder under 1250 ℃ of conditions.
The preparation of embodiment 5 yttrium aluminum garnets (YAG) powder.
Adopt Y
2O
3And Al
2(SO
4)
312H
2O is a raw material, presses yttrium oxide: Al
2O
3The ratio batching of=2: 5 (mol ratios), add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide fully mixes, and adds the initiator (5% ammonium persulfate aqueous solution for preparing in advance) of slip weight 0.5% again, after stirring, put into (also can put into thermostat container is incubated) in 100 ℃ of water baths, gelinite is taken out in all gelations after about 8 minutes, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h can obtain yttrium aluminum garnet (YAG) ceramic powder under 1250 ℃ of conditions.
Embodiment 6MgTiO
3The preparation of powder
Adopt Mg (NO
3)
26H
2O and TiO
2(d
50=2.0 μ m) be raw material, press MgO: TiO
2=1: 1 (mol ratio) batching, add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide fully mixes, and adds the initiator (5% ammonium persulfate aqueous solution for preparing in advance) of slip weight 0.5% again, after stirring, put in 100 ℃ of water baths, gelinite is taken out in all gelations after about 8 minutes, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h under 1200 ℃ of conditions promptly obtains the magnesium titanate ceramics powder.
Embodiment 7SrTiO
3The preparation of powder
Adopt Sr (NO
3)
26H
2O and TiO
2(d
50=2.0 μ m) be raw material, press SrO: TiO
2=1: 1 (mol ratio) batching, add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide fully mixes, and adds the initiator (5% ammonium persulfate aqueous solution for preparing in advance) of slip weight 0.5% again, after stirring, put into (also can put into thermostat container is incubated) in 100 ℃ of water baths, gelinite is taken out in all gelations after about 8 minutes, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h under 1200 ℃ of conditions promptly obtains the strontium titanate ceramics powder.
The preparation of embodiment 8 zirconium silicate powder
Adopt Zr (NO
3)
46H
2O and SiO
2(d
50=2.0 μ m) be raw material, press ZrO
2: SiO
2=1: 1 (mol ratio) batching, add deionized water, add neutral ceramic slurry dispersion agent, the add-on of dispersion agent is 0.4% of a pressed powder content, carrying out ball milling then mixes, the ball milling time is the organic monomer acrylamide that adds deionized water weight 15%, 0.8% linking agent methylene-bisacrylamide fully mixes, and adds the initiator (5% ammonium persulfate aqueous solution for preparing in advance) of slip weight 0.5% again, after stirring, put into (also can put into thermostat container is incubated) in 100 ℃ of water baths, gelinite is taken out in all gelations after about 8 minutes, be cut into little, carry out nature then and dehydrate.Put into air furnace after the drying, thermal treatment 2h under 1200 ℃ of conditions promptly obtains the Zirconium silicate ceramic powder.
Claims (1)
1, a kind of method of utilizing the liquid-solid gel reaction synthesizing ceramic powder is characterized in that,
1.1, the batching,
Composition requirement according to prepared ceramic powder, calculate and various required solid-state ceramic raw material powders of weighing and soluble compound raw material, measure required deionized water or distilled water by solid volume fraction 40～55vol%, soluble compound is dissolved in the water, then the soluble compound aqueous solution and solid-state ceramic raw material powder are added in the ball grinder, add neutral ceramic slurry dispersion agent ZD282 simultaneously, the add-on of dispersion agent is 0.2%～0.8% of a solid-state ceramic raw material powder weight, take by weighing organic monomer and linking agent again, organic monomer is water soluble propene's acid amides or Methacrylamide, linking agent is N, N '-methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the ratio of organic monomer and linking agent can be chosen between 10: 1～30: 1, and total add-on is 10～30% of a water weight;
1.2, ball milling mixes,
After various raw materials prepare, ball grinder is placed on carries out ball milling on the ball mill and mix, the ball milling time decides according to the initial size of ceramic powder, be 5～30h, before discharging, add organic monomer and linking agent during 2h, continue ball milling, discharging behind the 2h finally forms the mixed uniformly ceramic slurry of each component;
1.3, slurry gel,
Adding initiator in through the mixed ceramic slurry of ball milling is ammonium persulfate aqueous solution, stirs, and the add-on of initiator is 0.2～0.6% of an organic monomer weight; Heat then and make its gelation, be placed in the thermostat container or put into water bath and heat, Heating temperature is 30～100 ℃;
1.4, drying,
After solution gelization is finished, gelinite is taken out, be cut into small pieces, dehydrate then, drying mode adopts seasoning, blowing drying or heat drying;
1.5, thermal treatment,
Dried gelinite is placed in the air furnace heat-treats, temperature rise rate is controlled at 5～20 ℃, at first is raised to 500～700 ℃ of insulation 0.5～5h, is warmed up to 800～1600 ℃ of insulation 2～8h then, and cooling is come out of the stove then.
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| CN102777214B (en) * | 2012-07-27 | 2014-12-03 | 萍乡市慧成精密机电有限公司 | Nozzle blade of ceramic powder turbocharger and manufacturing method thereof |
| CN103265278B (en) * | 2013-06-20 | 2015-04-22 | 商丘师范学院 | Preparation method of free-agglomeration MgAl2O4 nanometer particle powder |
| CN105418071B (en) * | 2015-07-28 | 2018-01-16 | 山东合创明业精细陶瓷有限公司 | The synthetic method of high pure and ultra-fine ZrC SiC composite granules |
| CN112185642A (en) * | 2020-09-23 | 2021-01-05 | 江西艾特磁材有限公司 | Method for coating magnetic powder core with ball milling modified sol-gel |
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