CN103342545A - Method for preparing wear-resistant microcrystalline aluminum oxide ceramic at low temperature - Google Patents

Method for preparing wear-resistant microcrystalline aluminum oxide ceramic at low temperature Download PDF

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Publication number
CN103342545A
CN103342545A CN2013102892704A CN201310289270A CN103342545A CN 103342545 A CN103342545 A CN 103342545A CN 2013102892704 A CN2013102892704 A CN 2013102892704A CN 201310289270 A CN201310289270 A CN 201310289270A CN 103342545 A CN103342545 A CN 103342545A
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China
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compound
mineral
aluminum oxide
wear
oxide ceramic
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CN2013102892704A
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胡成
吴伯麟
刘君昌
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Guilin University of Technology
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Guilin University of Technology
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Priority to CN2013102892704A priority Critical patent/CN103342545A/en
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Abstract

The invention discloses a method for preparing wear-resistant microcrystalline aluminum oxide ceramic at low temperature, which comprises the following steps: (1) preparing the following raw materials in percentage by mass: 70-99.7% of aluminum oxide powder, 0.05-15% of calcium compound or mineral, 0.05-15% of magnesium compound or mineral and 0.1-10% of silicon compound or mineral; (2) performing ball milling for 24-72 hours, uniformly mixing, and pulverize; and controlling the particle size of the powder to be 0.3-3 mu m, wherein the mass ratio of added water to the raw materials is (1:3)-(3:1); (3) drying the slurry, and performing isopressing, roll forming or axial compression forming to obtain a green body; and (4) sintering the obtained green body in an air atmosphere or reducing atmosphere (namely CO, H2 or N2) at 1150-1650 DEG C, keeping the temperature for 10-300 minutes, and cooling to room temperature to obtain the wear-resistant aluminum oxide ceramic material. According to the invention, the method is wide in raw material source, simple in process, low in firing temperature and easy to realize industrial production; and by adding a compound additive, and regulating and controlling the sintering temperature and firing time of the aluminum oxide ceramic, the microcrystalline aluminum oxide ceramic having excellent wear resistance is prepared.

Description

A kind of low temperature prepares the method for wear-resisting microcrystalline alumina pottery
Technical field
The invention discloses and a kind ofly utilize that additive is compound to mix the method that low temperature prepares wear-resisting microcrystalline alumina pottery.
Background technology
Alumina-ceramic production aspect, what China mainly produced is low and middle-grade wear-resistant ceramics, less to the research of high-grade wear-resistant ceramic, and more to high-grade wear-resistant ceramic research abroad, and alumina porcelain that can mass production wear resisting property excellence.At present, external high-grade wear-resistant ceramic is occupied an leading position in China, but price is generally higher, along with domestic demand to expensive goods increases year by year, press for research and make the technology of the high-grade alumina ceramics of wear resisting property excellence, the technology that the development and use traditional technology can the wear-resisting alumina porcelain of mass production becomes the domestic problem that presses for solution.
Though it is a lot of to wear-resisting alumina porcelain research abroad, but alumina content is that alumina ceramics firing temperature more than 95% is up to 1550 ℃, crystal grain is too grown up, wear resistance and other mechanical properties are not good, and making alumina content and be 95% antiwear alumina ceramic is emphasis and the difficult point that the foreign scholar studies.Therefore, China research and development low temperature prepare wear-resisting alumina porcelain particularly alumina content be that the technology of the antiwear alumina ceramic more than 95% extremely has meaning.
Additive mixes in the alumina ceramics, mainly sintering temperature and the mechanical property of the function influence pottery by solid solution, glassy phase and second phase, and Chinese scholars has been carried out a large amount of research and has been proposed corresponding explanation mechanism to this.Ca-Al-Si system additive mainly is to form glassy phase to the influence of alumina ceramics, the growth of promotes oxidn aluminium grain, and firing temperature is low, but can cause alumina grain partly to be grown up, and the ceramic dense degree is not high, has reduced mechanical property; Mg-Al-Si system additive is incorporated in the alumina-ceramic, mainly is to produce second to suppress grain growth mutually, effectively gets rid of pore, improves mechanical property, but this system alumina-ceramic firing temperature height, and energy consumption is bigger, is not easy for industrial production.There is the investigator to use the compound alumina-ceramic that mixes of Ca-Mg-Si-Al system additive, obtain the alumina-ceramic of mechanical property excellence, but proportioning is remarkable to alumina-ceramic firing temperature and performance impact between this system content of additive and additive, and at present both at home and abroad mix mechanism research and the linear coupling research of alumina ceramics lessly to this system additive is compound, especially the alumina porcelain of alumina content more than 90% studied still less.
We can study aluminium oxide ceramic abrasive resistance and carry out for many years exploring, and have ripe technology circuit and guilding principle, have developed the microcrystalline alumina porcelain before and have reached 200 times of the highest level in the world and putting into production.On this basis, successfully develop by regulation and control composite additive proportioning, the alumina porcelain that low temperature prepares the wear resisting property excellence is the technological method of the antiwear alumina ceramic of alumina content more than 90% especially.
Summary of the invention
The objective of the invention is to increase year by year at the high-grade antiwear alumina ceramic demand of China, and external high-grade antiwear alumina ceramic is expensive, the high-grade antiwear alumina ceramic of domestic production is stranded right present situation relatively, provide a kind of raw material sources extensive, preparation technology is simple, and low temperature produces the method for wear-resisting microcrystalline alumina porcelain.
Concrete steps are:
(1) be that compound or the mineral that the compound of aluminum oxide powder 70%-99.7 %, calcium or compound that mineral are 0.05-15%, magnesium or mineral are 0.05-15% and silicon are that 0.1-10% prepares burden by each constituent mass per-cent of raw material, the mass percent sum of each component of raw material is 100%, and the compound of calcium or mineral, the compound of magnesium or the compound of mineral and silicon or the mass ratio of mineral are 3:1:2-1:3:2.
(2) material that step (1) is prepared adds water, ball milling 24-72 hour, is mixed, pulverizes; The control diameter of particle is 0.3-3 μ m; Wherein amount of water is 1:3-3:1 with the raw materials quality ratio.
(3) behind the slurry drying that step (2) is obtained, static pressure such as employing, roll forming or axial compression moulding make base substrate.
(4) with step (3) gained base substrate at air atmosphere or reducing atmosphere CO, H 2Or N 2Middle sintering, sintering temperature is 1150 ~ 1650 ℃, is incubated 10-300 minute, is cooled to room temperature and makes the wear-resisting alumina ceramic material.
The compound of described calcium be the mass percent of calcium oxide greater than 45% compound, the mineral of calcic are a kind of in limestone, calcite and the chalk rock.
The compound of described magnesium is magnesian mass percent greater than 45% compound, and the mineral that contain magnesium are a kind of in brucite, magnesite, polygorskite and the rhombspar.
The compound of described silicon be the mass percent of silicon oxide greater than 40% compound, siliceous mineral are a kind of in kaolin, diopside, montmorillonite, pyrophyllite, talcum and the serpentine.
Make the wear-resisting alumina ceramic material by standard: 1999 couples of JC/T848.1 – and carry out the wear rate test.
Test result shows: the alumina ceramic material wear rate that the present invention develops reaches 0.000926% h -1
Main characteristic of the present invention is the adding by composite additive, change the proportioning between each additive, sintering temperature and the firing time of regulation and control alumina-ceramic, successfully develop the method that low temperature prepares the microcrystalline alumina pottery of wear resisting property excellence, and raw material sources are extensive, technology is simple, and firing temperature is low, is easy to industrial production.
Embodiment
Embodiment 1:
(1) gets 93% Al by mass percentage 2O 3, 2.3% kaolin, 2.1% calcite and 2.6% magnesite mixes.
(2) material that step (1) is prepared adds deionized water, and ball milling 48 hours is mixed, pulverizes; The control diameter of particle is 0.3-3 μ m, and wherein amount of water is 1:3 with the raw materials quality ratio.
(3) the 105 ℃ of oven dry of slurry that step (2) obtained; Isostatic pressing under 80MP pressure, spherical base substrate is made in pressurize 10 minutes.
(4) with step (3) gained base substrate sintering in air atmosphere, sintering temperature is 1500 ℃, is incubated 100 minutes, is cooled to room temperature and makes the wear-resisting alumina ceramic material.
Test wear-resisting alumina ceramic fret wear rate is 0.00121%h -1
Embodiment 2:
(1) gets 98% Al by mass percentage 2O 3, 0.6% kaolin, 0.6% limestone and 0.6% rhombspar mix.
(2) material that step (1) is prepared adds deionized water, and ball milling 60 hours is mixed, pulverizes; The control diameter of particle is 0.3-3 μ m, and wherein amount of water is 3:1 with the raw materials quality ratio.
(3) the 130 ℃ of oven dry of slurry that step (2) obtained; Isostatic pressing under 80MP pressure, spherical base substrate is made in pressurize 10 minutes.
(4) with step (1) gained base substrate sintering in CO atmosphere, sintering temperature is 1450 ℃, is incubated 60 minutes, is cooled to room temperature and makes the wear-resisting alumina ceramic material.
Test wear-resisting alumina ceramic fret wear rate is 0.000926%h -1

Claims (1)

1. method for preparing alumina-ceramic is characterized in that concrete steps are:
(1) be that compound or the mineral that the compound of aluminum oxide powder 70%-99.7 %, calcium or compound that mineral are 0.05-15%, magnesium or mineral are 0.05-15% and silicon are that 0.1-10% prepares burden by each constituent mass per-cent of raw material, the mass percent sum of each component of raw material is 100%, and the compound of calcium or mineral, the compound of magnesium or the compound of mineral and silicon or the mass ratio of mineral are 3:1:2-1:3:2;
(3) material that step (1) is prepared adds water, ball milling 24-72 hour, is mixed, pulverizes; The control diameter of particle is 0.3-3 μ m; Wherein amount of water is 1:3-3:1 with the raw materials quality ratio;
(4) behind the powder drying that step (3) is obtained, static pressure such as employing, roll forming or axial compression moulding make base substrate;
(5) be CO, H with step (4) gained base substrate at air atmosphere or reducing atmosphere 2Or N 2Middle sintering, sintering temperature is 1150 ~ 1650 ℃, is incubated 10-300 minute, is cooled to room temperature and makes the wear-resisting alumina ceramic material;
The compound of described calcium be the mass percent of calcium oxide greater than 45% compound, the mineral of calcic are a kind of in limestone, calcite and the chalk rock;
The compound of described magnesium is magnesian mass percent greater than 45% compound, and the mineral that contain magnesium are a kind of in brucite, magnesite, polygorskite and the rhombspar;
The compound of described silicon be the mass percent of silicon oxide greater than 40% compound, siliceous mineral are a kind of in kaolin, diopside, montmorillonite, pyrophyllite, talcum and the serpentine.
CN2013102892704A 2013-07-11 2013-07-11 Method for preparing wear-resistant microcrystalline aluminum oxide ceramic at low temperature Pending CN103342545A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN103553577A (en) * 2013-10-22 2014-02-05 襄阳市金控特种陶瓷科技有限公司 Manufacturing method of tube mill ceramic lining for alumina milling
CN103553576A (en) * 2013-10-22 2014-02-05 襄阳市金控特种陶瓷科技有限公司 Method for processing ceramic lining for tube mills
CN104071985A (en) * 2014-07-14 2014-10-01 中国科学院宁波材料技术与工程研究所 Microcrystal glass powder precursor, microcrystal glass powder as well as preparation method and application of microcrystal glass powder precursor and microcrystal glass powder
CN106145906A (en) * 2016-07-04 2016-11-23 浙江工贸职业技术学院 A kind of low-temperature sintering Environment-friendlyceramic ceramic material and preparation technology thereof
CN108726999A (en) * 2018-06-26 2018-11-02 湖南富强特种陶瓷制造有限公司 A kind of technique that low-temperature sintering prepares aluminium oxide ceramic products
CN109896865A (en) * 2017-12-08 2019-06-18 中国科学院上海硅酸盐研究所 A method of improving aluminium oxide ceramics toughness
CN115572151A (en) * 2022-10-10 2023-01-06 淄博和润马科托矿业技术有限公司 Microcrystalline alumina grinding medium and preparation method thereof
CN115677328A (en) * 2022-10-27 2023-02-03 常熟理工学院 Preparation method of alumina structure ceramic material with more than 95 percent

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553577A (en) * 2013-10-22 2014-02-05 襄阳市金控特种陶瓷科技有限公司 Manufacturing method of tube mill ceramic lining for alumina milling
CN103553576A (en) * 2013-10-22 2014-02-05 襄阳市金控特种陶瓷科技有限公司 Method for processing ceramic lining for tube mills
CN104071985A (en) * 2014-07-14 2014-10-01 中国科学院宁波材料技术与工程研究所 Microcrystal glass powder precursor, microcrystal glass powder as well as preparation method and application of microcrystal glass powder precursor and microcrystal glass powder
CN104071985B (en) * 2014-07-14 2016-03-23 中国科学院宁波材料技术与工程研究所 Devitrified glass precursor powder, microcrystalline glass powder, its preparation method and application
CN106145906A (en) * 2016-07-04 2016-11-23 浙江工贸职业技术学院 A kind of low-temperature sintering Environment-friendlyceramic ceramic material and preparation technology thereof
CN109896865A (en) * 2017-12-08 2019-06-18 中国科学院上海硅酸盐研究所 A method of improving aluminium oxide ceramics toughness
CN109896865B (en) * 2017-12-08 2021-05-25 中国科学院上海硅酸盐研究所 Method for improving toughness of aluminum oxide ceramic
CN108726999A (en) * 2018-06-26 2018-11-02 湖南富强特种陶瓷制造有限公司 A kind of technique that low-temperature sintering prepares aluminium oxide ceramic products
CN108726999B (en) * 2018-06-26 2019-04-26 湖南富强特种陶瓷制造有限公司 A kind of technique that low-temperature sintering prepares aluminium oxide ceramic products
CN115572151A (en) * 2022-10-10 2023-01-06 淄博和润马科托矿业技术有限公司 Microcrystalline alumina grinding medium and preparation method thereof
CN115677328A (en) * 2022-10-27 2023-02-03 常熟理工学院 Preparation method of alumina structure ceramic material with more than 95 percent
CN115677328B (en) * 2022-10-27 2023-04-25 常熟理工学院 Preparation method of ceramic material with alumina structure of more than 95 percent

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Application publication date: 20131009