CN106673626B - Low-cost alumina powder material for producing self-toughening alumina wear-resistant ceramic - Google Patents
Low-cost alumina powder material for producing self-toughening alumina wear-resistant ceramic Download PDFInfo
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Abstract
The invention discloses a low-cost alumina powder material for producing self-toughening alumina wear-resistant ceramics, which is prepared by the steps of firstly putting industrial gamma-alumina, an additive, oleic acid and the like into a ball mill, carrying out dry grinding to obtain fine particle powder with the particle size D50 of less than 3 mu m, calcining at the temperature of 1200 ℃ and ~ 1400 ℃ for 2 ~ 10 hours to obtain alumina powder A with sodium impurities removed for later use, then putting industrial aluminum hydroxide, the additive, the oleic acid and the like into the ball mill, carrying out dry grinding to obtain fine particle powder with the particle size D50 of less than 3 mu m, calcining at the temperature of 900 ℃ and ~ 1200 ℃ for 2 ~ 10 hours to obtain alumina powder B with the sodium impurities removed for later use, mixing the alumina powder A and the alumina powder B according to a proportion, adding the additive according to the types of the wear-resistant ceramics, carrying out sanding and carrying out spray granulation to obtain the alumina powder material with the mass fraction of less than 0.2 percent and the median particle size D50 of less than 2 mu m, which is suitable for dry pressing or isostatic pressing molding.
Description
Technical Field
The invention relates to a raw material for producing alumina wear-resistant ceramics, in particular to a low-cost alumina powder material for producing self-toughening alumina wear-resistant ceramics.
Background
At present, the raw material for producing the domestic alumina wear-resistant ceramic is mainly industrial gamma-alumina or aluminum hydroxide, the defect is mainly that the content of sodium is high, and when the ceramic is directly formed and sintered, the ceramic is difficult to densify due to worm-shaped holes existing after phase change, so that the gamma-alumina or the aluminum hydroxide is generally calcined at high temperature to be converted into alpha-alumina before preparing the block ceramic, and a mineralizer such as boride, chloride or fluoride is added in the calcining process to form a volatile low-melting-point compound with sodium so as to remove sodium impurities in the alumina. In order to ensure that the sodium content is sufficiently low, the calcination temperature is generally more than 1400 ℃, so that the primary crystal size of the calcined alpha-alumina is generally more than 3 μm, the microstructure of the ceramic prepared by molding and sintering the raw material is isometric crystal, and the crystal grain size is more than 5 μm. The alumina wear-resistant ceramic product with the microstructure has lower bending strength, hardness and fracture toughness. Because the application of high-speed and high-load grinding equipment is wider and wider in the field of wear resistance at present, the traditional wear-resistant alumina ceramic cannot meet the requirements due to high wear and easy breakage, and the strength, hardness and toughness of the alumina wear-resistant ceramic need to be improved.
The performance of alumina ceramics is generally improved by two methods, one method is to add a second phase, for example, Chinese patent publication No. CN101508562B discloses a toughened alumina structural ceramic material, which adopts raw materials consisting of 78-85 wt% of alumina, 13-20 wt% of yttrium-stabilized zirconia and 0.5-2 wt% of titanium dioxide, wherein the yttrium-stabilized zirconia consists of 97 mol% of zirconia and 3 mol% of yttria. The toughened alumina structural ceramic material takes alumina as a matrix and adopts yttrium-stabilized zirconia as a toughening agent, not only has excellent performance of the traditional alumina structural ceramic material, but also has good toughness, and compared with a self-toughened zirconia ceramic material, the toughened alumina structural ceramic material has lower material cost, but also has higher cost compared with an alumina material. Another method for improving the performance of the alumina ceramic is self-toughening, and Chinese patent publication No. CN101182193 discloses a preparation method of in-situ self-toughening alumina ceramic, which adopts nano aluminum powder and high-purity alumina powder as initial raw materials and uniformly mixes the raw materials; drying and grinding the mixed slurry into powder; forming the obtained powder into a blank; the blank is directly sintered in a common air sintering furnace to obtain the alumina ceramic with in-situ grown long columnar and plate-shaped crystals, and the alumina product has the advantages of high density, high purity and high toughness, but has the defects that the raw material adopts nano aluminum powder, the cost is high, and the large-scale production is difficult.
Disclosure of Invention
The invention aims to provide a low-cost alumina powder material for producing self-toughening alumina wear-resistant ceramics.
In order to achieve the purpose, the invention can adopt the following technical scheme:
the low-cost alumina powder material for producing the self-toughening alumina wear-resistant ceramic comprises the following preparation steps:
firstly, industrial gamma-alumina is selected to be put into a ball mill, an additive with the total mass fraction of the gamma-alumina being 0.1 ~ 3% and oleic acid, stearic acid or sodium stearate with the total mass fraction of 0.2 ~ 2% are added to be dry-milled, mixed and crushed with the gamma-alumina to obtain fine particle mixed powder with the median particle diameter D50 being less than 3 mu m, wherein the additive is one or a mixture of two or more of boric acid, calcium fluoride, ammonium chloride and aluminum fluoride, the additive can play a role in removing impurities and inhibiting the growth of crystal grains, and the oleic acid, the stearic acid or the sodium stearate can play a role in grinding aid and avoiding the agglomeration of fine particles;
secondly, calcining the fine particle mixed powder prepared in the first step at the temperature of 1200 ℃ ~ 1400 ℃ for 2 ~ 10 hours to obtain aluminum oxide powder A without sodium impurities for later use;
thirdly, putting industrial-grade aluminum hydroxide into a ball mill, adding an additive with the total mass fraction of 0.1 ~ 3% of aluminum hydroxide and 0.2 ~ 2% of oleic acid, stearic acid or sodium stearate, mixing the mixture with the aluminum hydroxide by dry grinding, and crushing aggregates to obtain fine particle mixed powder with the median particle size D50 less than 3 mu m, wherein the additive is one or a mixture of two or more of boric acid, calcium fluoride, ammonium chloride, aluminum fluoride, magnesium chloride and magnesium fluoride;
fourthly, calcining the fine particle mixed powder prepared in the third step at the temperature of 900 ℃ and ~ 1200 ℃ and 1200 ℃ for 2 ~ 10 hours to obtain aluminum oxide powder B with sodium impurities removed for later use;
fifthly, mixing the alumina powder A prepared in the second step and the alumina powder B prepared in the fourth step according to the weight part of 1:0.5 ~ 3, adding different additives (aiming at reducing the sintering temperature and improving the ceramic performance) according to the type of the wear-resistant ceramic, sanding and spraying for granulation to obtain the alumina powder material which has the sodium mass fraction of less than 0.2 percent, the median particle diameter D50 of less than 2 mu m and is suitable for dry pressing or isostatic pressing for preparing fine ceramic(ii) a The Vickers hardness HV5 of 95 alumina ceramics obtained by sintering the powder material is more than 13GPa, and the fracture toughness is higher than 3.8 MPa.m1/2。
The additive added in the fifth step is CaO, MgO and SiO2、TiO2、La2O3、CAS(CaO-Al2O3-SiO2) One or a mixture of two or more of the glass, so that the glass forms a glass phase in the subsequent sintering process to reduce the sintering temperature.
The total mass fraction of impurities of the industrial grade gamma-alumina is less than 2 percent; the total mass fraction of impurities of the industrial-grade aluminum hydroxide is less than 2 percent.
When the aluminum oxide powder A and the aluminum oxide powder B are actually prepared, the same effect is achieved when oleic acid, stearic acid or sodium stearate is added;
when the alumina powder A is prepared, the adopted additive can be any one or a mixture of two or more of boric acid, calcium fluoride, ammonium chloride and aluminum fluoride, and the effect is the same;
when the alumina powder B is prepared, the adopted additive can be one or a mixture of two or more of boric acid, calcium fluoride, ammonium chloride, aluminum fluoride, magnesium chloride and magnesium fluoride, and the effect is the same.
The invention has the advantages that the phase inversion impurity removal additive is added into the low-cost industrial raw material, the agglomeration is destroyed by ball milling and grinding, the pre-sintering temperature is controlled, the sodium impurities remained in the gamma-alumina and the aluminum hydroxide are removed, and the alpha-alumina with different sintering activities is obtained; and then mixing the prepared alumina powder according to a required proportion, adding a specific additive, and controlling long columnar crystals formed in the microstructure of the powder so that the sintered finished alumina wear-resistant ceramic has a self-toughening effect. The invention has the advantages of low cost of raw materials, simple preparation process, easy control of process generation, easy stabilization and batch production.
In order to ensure that the quality of the finished product alumina powder material meets the requirements, the total mass fraction of impurities of the selected gamma-alumina is less than 2 percent; the total mass fraction of impurities of the selected industrial-grade aluminum hydroxide is less than 2 percent.
Detailed Description
The following will describe in detail the preparation method of the low-cost alumina powder material for producing self-toughened alumina wear-resistant ceramics according to the present invention by using specific examples.
Example 1
1) Putting 800kg of industrial grade gamma-alumina (the total mass fraction of impurities is 0.6%), boric acid accounting for 0.4% of the total alumina mass fraction and sodium stearate accounting for 0.5% of the total alumina mass fraction into a ball mill, carrying out dry grinding and mixing for 8 hours, and crushing aggregates to obtain gamma-alumina fine particle mixed powder with the median particle diameter D50 of 2.8 mu m;
2) calcining the prepared gamma-alumina mixed powder for 4 hours at the temperature of 1400 ℃ to obtain alumina powder A with the mass fraction of sodium impurities less than 0.1%;
3) putting 200kg of industrial-grade aluminum hydroxide (the total mass fraction of impurities is less than 0.6%), calcium fluoride accounting for 0.1% of the mass fraction of the aluminum hydroxide, 0.2% of ammonium chloride and oleic acid accounting for 0.5% of the mass fraction of the aluminum hydroxide into a ball mill, carrying out dry-milling mixing for 8 hours, and crushing aggregates to obtain aluminum hydroxide fine particle mixed powder with the median particle size D50 of 2.6 mu m;
4) calcining the prepared aluminum hydroxide fine particle mixed powder at 1150 ℃ for 6 hours to obtain aluminum oxide powder B with the mass fraction of sodium impurities less than 0.1% for later use;
5) mixing alumina powder A and alumina powder B, adding CaO + MgO + 2% SiO in the amount of 1 wt%2The mixed additive is subjected to sand grinding and spray granulation to obtain an alumina powder material with the median particle diameter D50 of 1.6 mu m, which is tested by a laser particle sizer;
6) sintering the powder material by a conventionally adopted dry pressing or isostatic pressing method to obtain the powder material with high hardness (HV 513 GPa) and high toughness (3.8 MPa.m)1/2) The 95 porcelain alumina wear-resistant ceramic.
Example 2
1) Putting 700kg of industrial grade gamma-alumina (the total mass fraction of impurities is 0.6%), boric acid accounting for 0.3% of the total alumina mass fraction and sodium stearate accounting for 0.6% of the total alumina mass fraction into a ball mill, carrying out dry grinding and mixing for 12 hours, and crushing aggregates to obtain gamma-alumina fine particle mixed powder with the median particle diameter D50 of 2.8 mu m;
2) calcining the prepared gamma-alumina mixed powder at 1380 ℃ for 6 hours to obtain alumina powder A with the mass fraction of sodium impurities less than 0.1%;
3) putting 300kg of industrial-grade aluminum hydroxide (the total mass fraction of impurities is less than 0.6%), magnesium fluoride accounting for 0.3% of the mass fraction of the aluminum hydroxide, 0.1% of ammonium chloride and stearic acid accounting for 0.6% of the mass fraction of the aluminum hydroxide into a ball mill, and carrying out dry grinding, mixing and crushing aggregate to obtain aluminum hydroxide fine particle mixed powder with the median particle size D50 of 2.6 mu m;
4) calcining the prepared aluminum hydroxide fine particle mixed powder for 4 hours at 1100 ℃ to obtain aluminum oxide powder B with the mass fraction of sodium impurities being less than 0.1% for later use;
5) mixing alumina powder A and alumina powder B, adding MgO + 1% SiO 2 wt% of the total powder2The mixed additive is subjected to sand grinding and spray granulation to obtain an alumina powder material with the median particle diameter D50 of 1.4 mu m, which is tested by a laser particle sizer;
6) sintering the powder material by a conventionally adopted dry pressing or isostatic pressing method to obtain the powder material with high hardness (HV 514.5 GPa) and high toughness (4.6 MPa.m)1/2) The 97 ceramic alumina wear-resistant ceramic.
Claims (1)
1. A low-cost alumina powder material for producing self-toughening alumina wear-resistant ceramics is characterized in that: the preparation method comprises the following steps:
firstly, industrial-grade gamma-alumina is selected and put into a ball mill, an additive with the total mass fraction of 0.1 ~ 3% of gamma-alumina and oleic acid, stearic acid or sodium stearate with the total mass fraction of 0.2 ~ 2% of gamma-alumina are added and mixed with the gamma-alumina in a dry grinding way, aggregates are crushed, and fine particle mixed powder with the median particle size D50 smaller than 3 mu m is obtained, wherein the additive is any one or a mixture of two or more of boric acid, calcium fluoride, ammonium chloride and aluminum fluoride;
secondly, calcining the fine particle mixed powder prepared in the first step at the temperature of 1200 ℃ ~ 1400 ℃ for 2 ~ 10 hours to obtain aluminum oxide powder A without sodium impurities for later use;
thirdly, putting industrial-grade aluminum hydroxide into a ball mill, adding an additive accounting for 0.1 ~ 3% of the total mass fraction of the aluminum hydroxide and 0.2 ~ 2% of oleic acid, stearic acid or sodium stearate which are mixed with the aluminum hydroxide by dry milling, crushing aggregates to obtain fine particle mixed powder with the median particle size D50 being less than 3 mu m, wherein the additive is one or a mixture of two or more of boric acid, calcium fluoride, ammonium chloride, aluminum fluoride, magnesium chloride and magnesium fluoride;
fourthly, calcining the fine particle mixed powder prepared in the third step at the temperature of 900 ℃ and ~ 1200 ℃ and 1200 ℃ for 2 ~ 10 hours to obtain aluminum oxide powder B with sodium impurities removed for later use;
fifthly, mixing the alumina powder A prepared in the second step with the alumina powder B prepared in the fourth step according to the weight part of 1:0.5 ~ 3, adding additives according to the type of the wear-resistant ceramic, sanding and spraying for granulation to obtain the alumina powder material with the median particle size D50 less than 2 mu m;
the additive is CaO, MgO, SiO2、TiO2、La2O3、CaO-Al2O3-SiO2One or a mixture of two or more of glass;
the total mass fraction of impurities of the industrial grade gamma-alumina is less than 2 percent; the total mass fraction of impurities of the industrial-grade aluminum hydroxide is less than 2 percent.
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| CN108298964B (en) * | 2018-04-10 | 2021-03-02 | 淄博启明星新材料股份有限公司 | High-purity fine-grain wear-resistant alumina lining plate and preparation method thereof |
| CN108840668A (en) * | 2018-07-05 | 2018-11-20 | 中国铝业股份有限公司 | A kind of wear-resistant material |
| CN112028098B (en) * | 2019-06-04 | 2022-09-27 | 北京化工大学 | Preparation method of gamma-alumina nano dispersion |
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| CN103145164A (en) * | 2013-04-08 | 2013-06-12 | 郑州玉发精瓷科技有限公司 | Preparation method of aluminum oxide powder for fine ceramics sintered at low temperature |
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