CN101973760B - Method for reducing firing temperature of aluminum oxide ceramics - Google Patents
Method for reducing firing temperature of aluminum oxide ceramics Download PDFInfo
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- CN101973760B CN101973760B CN201010298941XA CN201010298941A CN101973760B CN 101973760 B CN101973760 B CN 101973760B CN 201010298941X A CN201010298941X A CN 201010298941XA CN 201010298941 A CN201010298941 A CN 201010298941A CN 101973760 B CN101973760 B CN 101973760B
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Abstract
The invention discloses a method for reducing the firing temperature of aluminum oxide ceramics, which comprises the following steps of: dissolving silica sol, calcium compounds and magnesium compounds into a solvent to form mixed solution, and simultaneously adjusting the pH value of the mixed solution to be 4.5 to 8.0; adding aluminum oxide powder into the mixed solution and ball-milling, drying and performing calcination at 800 to 1,200 DEG C; and adding an adhesive into the calcinated powder, pelleting, tabletting and removing the adhesive, and then sintering at 1,350 to 1,550 DEG C. The method is simple; and as the gelation transformation of the silica sol is controlled by adjusting the pH value to uniformly coat the auxiliaries of silicon, calcium and magnesium onto the surface of the aluminum oxide powder and generate nanoscale particles in the calcination process, and the nanoscale particles with small particle sizes are utilized to fill gaps of the aluminum oxide powder and simultaneously are reacted with aluminum oxides due to high surface activity to produce a glass phase, the firing temperature of the aluminum oxide ceramics is maximally reduced on the basis of adding small amounts of auxiliaries.
Description
Technical field
The present invention relates to a kind of method that reduces the alumina-ceramic firing temperature, belong to materials science field.
Background technology
Alumina-ceramic has the physical strength height, hardness is big, dielectric loss is little, resistivity is big, voltage breakdown is high; And premium properties such as wear-resistant, corrosion-resistant, high temperature resistant, obtained widespread use in industries such as electronic apparatus, machinery, automobile, chemical industry, weaving, metallurgy, aviation, thermoelectricity, building materials, dyestuff, coating at present.But alumina-ceramic has stronger ionic linkage, makes its fusing point up to 2050 ℃, and the liquid phase that when high temperature, produces is few, and the firing temperature that causes alumina-ceramic is up to more than 1750 ℃.So high firing temperature will impel that ceramic crystalline grain is sharply grown, remaining pore assembles and grow up; Thereby the mechanical property that causes material reduces, the resistance to air loss variation; The energy and the high performance fuel that in sintering process, need simultaneously labor; Also need consume refractory materials and high temperature Heating element that a large amount of high temperature burn till, make that thus the production cost of alumina-ceramic is high.Therefore, reducing the infringement to kiln and kiln furnitures of the firing temperature, energy efficient, minimizing of alumina-ceramic, is the important topic that solution is concerned about and is badly in need of to the alumina-ceramic industry.
For reducing the firing temperature of alumina-ceramic, mainly contain following two kinds of approach at present.A kind of is through obtaining to be uniformly dispersed, not have reunion; And the superfine powder with good sintering activity reaches the purpose that reduces the alumina-ceramic firing temperature; (Anhui University of Science and Technology's journal such as Liu Yin for example; 2006,01:41-44) through in coarse-grain is alumina powder jointed the interpolation 40% nano alumina powder jointed, can the firing temperature of alumina-ceramic be reduced to 1550 ℃; Huang etc. (Materials Research Bulletin, 2008,6:1463-1471) with the nano-alumina powder be raw material, at 1450 ℃ of dense sinterings of realizing alumina-ceramic; But the above-mentioned nanometer grade powder that utilizes is higher as the cost of raw material.The another kind of method that reduces the alumina-ceramic firing temperature is an amount of sintering aid of interpolation in alumina powder jointed, for example Li Jiang etc. (Journal of Inorganic Materials, 2003,6:1192-1198) with MgO and SiO
2Be sintering aid, obtain high performance alumina-ceramic at 1450 ℃ of sintering; Kwon (J Am Ceram Soc, 1990,73:275-278), Singh (J Am Ceram Soc, 1981,64:133-136) and Akira (J Am Ceram Soc, 1996,79:3 199-210) etc. in alumina powder jointed, add CaO-MgO-SiO respectively
2, MgO-Al
2O
3-SiO
2, CaO-Al
2O
3-SiO
2Deng glass powder, the firing temperature of alumina-ceramic 1400～1450 ℃ have been reduced to; In addition, TiO
2, B
2O
3, oxide compounds such as MnO, CuO also are used for adding to the alumina powder jointed firing temperature that reduces pottery.
In the method for above-mentioned reduction alumina-ceramic firing temperature, add sintering aid and be the most simply, the most effective, also be the cheapest a kind of method of price.But the introducing of a large amount of low-temperature sintering auxiliary agents will have a negative impact to each item performance of alumina-ceramic; Particularly in alumina powder jointed, add the glass powder and the micron-sized oxides additive of big particle, will be residual behind sintering a large amount of second be distributed in the alumina grain border mutually, worsens ceramic each item performance.Therefore, on the basis of reducing the low-temperature sintering additive dosage, farthest reduce the firing temperature of alumina-ceramic as far as possible, not only help saving the shared material cost of sintering aid, also will help improving each item performance of alumina-ceramic.
Summary of the invention
The purpose of this invention is to provide a kind of effect of farthest bringing into play sintering aid, when a small amount of sintering aid adds, can effectively reduce the method for alumina-ceramic firing temperature.
The method of the reduction alumina-ceramic firing temperature that the present invention proposes may further comprise the steps:
(1) compound of the compound of silicon sol, calcium, magnesium is dissolved in respectively in water or the absolute ethyl alcohol according to 1: 0.01～0.6: 0.01～0.6 mol ratio,, the pH value of mixing solutions is transferred to 4.5～8.0 then with above-mentioned three kinds of solution mixing and stirring;
(2) account for alumina powder jointed 0.2～5% molar content by silicon sol, the mixing solutions that above-mentioned (1) is prepared mixes with alumina powder jointed, carries out ball milling then;
(3) place 80 ℃～120 ℃ to carry out drying in the mixture behind the above-mentioned ball milling, calcine at 800 ℃～1200 ℃ then, obtain the ceramic powder of white;
(4) in above-mentioned ceramic powder, add polyvinyl alcohol water solution as tackiness agent.Carry out granulation, moulding, binder removal then, carry out sintering at 1350 ℃～1550 ℃ again, obtain alumina-ceramic.
In the technique scheme, the compound of said calcium is at least a in nitrocalcite, calcium acetate and the calcium chloride; The compound of said magnesium is at least a in magnesium nitrate, magnesium acetate and the magnesium chloride; Described pH value regulator is nitric acid, acetic acid or ammoniacal liquor.
The present invention compared with prior art has following advantage:
1, through adjusting to mixing solutions pH value; Impel silicon sol generation gelation to change; Make the compound of silicon, calcium, magnesium after the molecular level level is mixed, evenly be coated on alumina powder jointed particulate surface; Thereby can farthest bring into play the effect of sintering aid, effectively reduce the consumption of sintering aid;
2,800 ℃～1200 ℃ calcine after, the compound of silicon, calcium, magnesium will be transformed into nano level SiO
2, CaO, MgO powder, in the forming process of ceramics process, can fill up alumina powder jointed particulate gap, promote the raising of biscuit of ceramics density;
3, in ceramic sintering process, nanometer SiO
2, CaO, MgO will utilize the liquid phase wetting action to reduce the firing temperature of alumina-ceramic at the alumina powder jointed particle surface generation glassy phase that reacts, and utilize the high-ratio surface of its nano-powder can promote ceramic sintering simultaneously.
Embodiment
Below in conjunction with instance the present invention is further described.
Embodiment 1:
Take by weighing the 1mol silicon sol and be dissolved in the 400ml deionized water, take by weighing 0.3mol nitrocalcite and be dissolved in the 400ml deionized water, take by weighing the 0.2mol magnesium nitrate and be dissolved in the 300ml absolute ethyl alcohol; With above-mentioned three kinds of solution mixing and stirring, add 100ml acetic acid then the pH value of mixing solutions is transferred to 6.7.In above-mentioned mixing solutions, add 50mol alumina powder jointed (5098 gram), put into the ball grinder mixing and ball milling; Place 90 ℃ baking oven to carry out drying in the mixture behind the above-mentioned ball milling,, obtain the ceramic powder of white then 1100 ℃ of calcinings.
In above-mentioned ceramic powder, add the 400g polyvinyl alcohol water solution, carry out granulation behind the thorough mixing, at the forming under the pressure of 120Mpa, be incubated 2 hours at 1500 ℃ behind the binder removal pottery is carried out sintering then.Adopt the volume density of drainage test alumina-ceramic, the result shows that its density has reached 96.2% of alumina-ceramic theoretical density.
Embodiment 2:
Take by weighing the 1mol silicon sol and be dissolved in the 400ml absolute ethyl alcohol, take by weighing the 0.2mol calcium acetate and be dissolved in the 250ml absolute ethyl alcohol, take by weighing the 0.4mol magnesium nitrate and be dissolved in the 450ml deionized water; With above-mentioned three kinds of solution mixing and stirring, add 30ml concentration then and be 10% nitric acid the pH value of mixing solutions is transferred to 4.8.In above-mentioned mixing solutions, add 20mol alumina powder jointed (2039 gram), put into the ball grinder mixing and ball milling; Place 85 ℃ baking oven to carry out drying in the mixture behind the above-mentioned ball milling,, obtain the ceramic powder of white then 1150 ℃ of calcinings.
In above-mentioned ceramic powder, add the 180g polyvinyl alcohol water solution, carry out granulation behind the thorough mixing, at the forming under the pressure of 120Mpa, be incubated 2 hours at 1450 ℃ behind the binder removal pottery is carried out sintering then.Adopt the volume density of drainage test alumina-ceramic, the result shows that its density has reached 95.8% of alumina-ceramic theoretical density.
Embodiment 3:
Take by weighing the 1mol silicon sol and be dissolved in the 450ml deionized water, take by weighing 0.5mol nitrocalcite and be dissolved in the 500ml absolute ethyl alcohol, take by weighing the 0.3mol magnesium acetate and be dissolved in the 300ml absolute ethyl alcohol; With above-mentioned three kinds of solution mixing and stirring, add 23ml ammoniacal liquor then the pH value of mixing solutions is transferred to 6.0.In above-mentioned mixing solutions, add 30mol alumina powder jointed (3059 gram), put into the ball grinder mixing and ball milling; Place 90 ℃ baking oven to carry out drying in the mixture behind the above-mentioned ball milling,, obtain the ceramic powder of white then 1200 ℃ of calcinings.
In above-mentioned ceramic powder, add the 250g polyvinyl alcohol water solution, carry out granulation behind the thorough mixing, at the forming under the pressure of 120Mpa, be incubated 2 hours at 1450 ℃ behind the binder removal pottery is carried out sintering then.Adopt the volume density of drainage test alumina-ceramic, the result shows that its density has reached 95.6% of alumina-ceramic theoretical density.
Embodiment 4:
Take by weighing the 1mol silicon sol and be dissolved in the 450ml deionized water, take by weighing 0.1mol calcium chloride and 0.4mol nitrocalcite is dissolved in the 500ml absolute ethyl alcohol, take by weighing 0.1mol magnesium chloride and 0.2mol magnesium acetate and be dissolved in the 300ml absolute ethyl alcohol; With above-mentioned three kinds of solution mixing and stirring, add 22ml ammoniacal liquor then the pH value of mixing solutions is transferred to 6.0.In above-mentioned mixing solutions, add 30mol alumina powder jointed (3059 gram), put into the ball grinder mixing and ball milling; Place 90 ℃ baking oven to carry out drying in the mixture behind the above-mentioned ball milling,, obtain the ceramic powder of white then 1150 ℃ of calcinings.
In above-mentioned ceramic powder, add the 250g polyvinyl alcohol water solution, carry out granulation behind the thorough mixing, at the forming under the pressure of 120Mpa, be incubated 2 hours at 1450 ℃ behind the binder removal pottery is carried out sintering then.Adopt the volume density of drainage test alumina-ceramic, the result shows that its density has reached 95.9% of alumina-ceramic theoretical density.
Claims (4)
1. method that reduces the alumina-ceramic firing temperature may further comprise the steps:
(1) compound of the compound of silicon sol, calcium, magnesium is dissolved in respectively in water or the absolute ethyl alcohol according to 1: 0.01～0.6: 0.01～0.6 mol ratio,, the pH value of mixing solutions is transferred to 4.5～8.0 then with above-mentioned three kinds of solution mixing and stirring;
(2) account for alumina powder jointed 0.2～5% molar content by silicon sol, the mixing solutions that above-mentioned (1) is prepared mixes with alumina powder jointed, carries out ball milling then;
(3) place 80 ℃～120 ℃ to carry out drying in the mixture behind the above-mentioned ball milling, calcine at 800 ℃～1200 ℃ then, obtain the ceramic powder of white;
(4) in above-mentioned ceramic powder, add polyvinyl alcohol water solution as tackiness agent, carry out granulation, moulding, binder removal then, carry out sintering at 1350 ℃～1550 ℃ again, obtain alumina-ceramic.
2. the method for reduction alumina-ceramic firing temperature according to claim 1, the compound that it is characterized in that said calcium are at least a in nitrocalcite, calcium acetate and the calcium chloride.
3. the method for reduction alumina-ceramic firing temperature according to claim 1, the compound that it is characterized in that said magnesium are at least a in magnesium nitrate, magnesium acetate and the magnesium chloride.
4. the method for reduction alumina-ceramic firing temperature according to claim 1, the regulator that it is characterized in that regulating the pH value is nitric acid, acetic acid or ammoniacal liquor.
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| CN103232226B (en) * | 2013-04-07 | 2014-11-12 | 镇江市江南矿山机电设备有限公司 | Preparation method for alumina ceramic with low thermal conductivity and high compressive strength |
| CN113773060B (en) * | 2021-08-27 | 2022-05-20 | 广东泛瑞新材料有限公司 | high-Q-value ceramic material and preparation method and application thereof |
| CN114656249B (en) * | 2022-03-10 | 2023-02-21 | 蒙娜丽莎集团股份有限公司 | High-strength tawnite-based thin ceramic plate and preparation method thereof |
| CN116161972A (en) * | 2023-03-14 | 2023-05-26 | 广州瑞鑫通科技有限公司 | Preparation method of alumina ceramic sintering aid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164658A (en) * | 2007-08-24 | 2008-04-23 | 晋城市富基新材料有限公司 | Aluminium oxide foam ceramic filter |
| CN101412620A (en) * | 2008-11-14 | 2009-04-22 | 西安交通大学 | Method for preparing porous alumina ceramic supporting body with sol as additive |
| CN101456567A (en) * | 2008-12-25 | 2009-06-17 | 中国计量学院 | Method for synthesizing high temperature stabilizing type alpha-Al2O3 nano powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101164658A (en) * | 2007-08-24 | 2008-04-23 | 晋城市富基新材料有限公司 | Aluminium oxide foam ceramic filter |
| CN101412620A (en) * | 2008-11-14 | 2009-04-22 | 西安交通大学 | Method for preparing porous alumina ceramic supporting body with sol as additive |
| CN101456567A (en) * | 2008-12-25 | 2009-06-17 | 中国计量学院 | Method for synthesizing high temperature stabilizing type alpha-Al2O3 nano powder |
Non-Patent Citations (1)
| Title |
|---|
| 马红萍 等.硅溶胶的凝胶化包覆对氧化铝烧结性能的影响.《稀有金属材料与工程》.2010,第39卷(第增刊2期),第463-466页. * |
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