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CN1686923A - Method for preparing corundum bricks composite with Nano alpha-Al2O3 - Google Patents

Method for preparing corundum bricks composite with Nano alpha-Al2O3 Download PDF

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CN1686923A
CN1686923A CN 200510017457 CN200510017457A CN1686923A CN 1686923 A CN1686923 A CN 1686923A CN 200510017457 CN200510017457 CN 200510017457 CN 200510017457 A CN200510017457 A CN 200510017457A CN 1686923 A CN1686923 A CN 1686923A
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corundum
nano
powder
composite
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CN100436369C (en
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钟香崇
贾晓林
叶方保
李素平
梁敏
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Zhengzhou University
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Zhengzhou University
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Abstract

本发明提供了一种纳米α－Al2O3复合刚玉砖的制备方法。该方法以电熔刚玉颗粒，电熔刚玉细粉，α－Al2O3纳米粉和α－Al2O3微粉为原料，采用特殊的分散技术和成型工艺制备纳米α－Al2O3复合刚玉砖。本发明制备的刚玉砖烧结温度比同类技术烧结温度降低200～400℃，同时具有良好的高温性能和物理特性。用本发明制备含α－Al2O3纳米粉的刚玉砖性能优良，可在冶金、石油化工、煤化工等众多领域中广泛应用。The invention provides a method for preparing nano-α-Al 2 O 3 composite corundum bricks. The method uses fused corundum particles, fused corundum fine powder, α-Al 2 O 3 nano powder and α-Al 2 O 3 micro powder as raw materials, and adopts special dispersion technology and molding process to prepare nano α-Al 2 O 3 composite Corundum brick. The sintering temperature of the corundum brick prepared by the invention is 200-400°C lower than that of the similar technology, and has good high-temperature performance and physical properties at the same time. The corundum brick containing α-Al 2 O 3 nano powder prepared by the invention has excellent performance and can be widely used in many fields such as metallurgy, petrochemical industry and coal chemical industry.

Description

Nanometer α-Al 2O 3The preparation method of composite corundum brick
Affiliated field:
The invention belongs to refractory oxide goods manufacturing technology field, be specifically related to a kind of with electro-corundum, α-Al 2O 3Micro mist and α-Al 2O 3Nano powder is the preparation method of the composite corundum brick of primary raw material.
Background technology:
Because Al 2O 3Be the ionic linkage compound, the low (Al of its particle spread coefficient 3+Spread coefficient only is 10 in the time of 1700 ℃ -11Cm 2.s -1), sintering temperature is higher, and the sintering temperature of general corundum products can be up to 1800 ℃.In order to reduce the sintering temperature of corundum products, people once attempted at high temperature to produce liquid phase by sintering aid and come acceleration of sintering (liquid phase sintering mechanism) by adding sintering aid, and regrettably the adding of agglutinant will cause the material at high temperature performance to reduce.Nanometer α-Al 2O 3Powder is because size is little, surface atom accounts for sizable ratio, thereby surface energy height, has high activity, the more conventional powder of its sintering temperature is much lower, be introduced into and both can be used as sintering aids in the corundum products and also in the corundum products sintering process, serving as simultaneously effect in conjunction with phase, thereby be expected when reducing the corundum products sintering temperature, improving microstructure of products, to make goods to keep good high-temperature behavior.
Recent domestic studies show that nano heterogeneous ceramic, introduces nanodispersed phase and carry out compoundly in the micron order matrix, can make the fracture strength of material, fracture toughness improve 2～4 times, and material creep resistance and antifatigue destructive characteristics are improved.Therefore nano-powder is compound in the refractory material, obtains good high-temperature behavior by the control to its microstructure.Along with the nano powder preparation technology improves constantly, preparation cost constantly reduces, and the application and development of nano-powder is extensive day by day, and many traditional materials field is also actively introducing nano material, in the hope of further improving material property.Yet, with regard to nano-powder with regard to the applied research in the material, mainly concentrate on fine ceramics and nano heterogeneous ceramic aspect up to now, applied research in refractory materials still is in the starting stage to nano-powder, to nano-powder introduce refractory materials preparation technology and to the sintering character of material, microstructure and to mechanical behavior under high temperature produce to influence the aspect report very few.
Document " nanometer Fe 2O 3Impact to magchrome refractory sintering and mechanical property " (refractory material, 2003,37 (5): 256～258) " introduced a kind of nanometer Fe that contains 2O 3The preparation method of magchrome refractory.
Document " nanometer Al 2O 3And SiO 2Impact to corundum based refractory materials sintering and mechanical property " (refractory material, 2002,36 (2): 66～69) introduced a kind of nanometer α-Al that contains 2O 3And SiO 2Corundum brick, this technology makes the sintering temperature of corundum brick reduce by 100～200 ℃, but the high-temperature behavior of the standby material of institute system not.
Summary of the invention:
The objective of the invention is with electro-corundum material, α-Al 2O 3Micro mist and α-Al 2O 3Nano powder is raw material, adopts special dispersion technology and moulding process to prepare nanometer α-Al 2O 3Composite corundum brick had both effectively reduced the firing temperature of corundum refractory brick, improved again its performance simultaneously.
Technical scheme of the present invention is:
With Al 2O 3Content is greater than 99% electro-corundum particle and fine powder, α-Al 2O 3Nano powder and α-Al 2O 3Micro mist is raw material, adopts dispersion technology and moulding process, the steps include:
A. be α-Al of 0.25-3.5% with parts by weight 2O 3Nano powder adds water and is mixed with suspension, and ultrasonic dispersion adds the dispersant of parts by weight 0.05-2.0% and α-Al of 2-15% 2O 3Micro mist is mixed and made into mud;
B. be that the corundum in granules of 84-96% and fine powder and mud mix with parts by weight, add the wedding agent of raw material gross weight 3-6%, be mixed into pug, under the room temperature ageing mixture 22-25 hour, machine was pressed into green compact, 100-120 ℃, 20-24h drying treatment;
C. dried green compact are placed stove, are warming up to 950-1100 ℃, continue to be warming up to 1250-1600 ℃ with 30-100 ℃/hour speed again and burn till, be incubated 3-10 hour with 60-300 ℃/hour speed, be cooled to room temperature after, promptly get product.
Wherein:
α-Al 2O 3The particle diameter of nano powder is 50-120nm.
α-Al 2O 3The D of micro mist 50=1-10 μ m.
In fused corundom particle and the fine powder, coarse grained particle diameter is 5-1mm, and parts by weight are 45-65%; Middle particle grain size is 1-0.088mm, parts by weight 10-20%; The particle diameter of fine powder is less than 0.088mm, parts by weight 15-35%.
Dispersion agent is an ammonium polyacrylate, sodium polyacrylate, polycarboxylate ether, tripoly phosphate sodium STPP, one or both in the Sodium hexametaphosphate 99.
Wedding agent is a kind of in dextrin, polyvinyl alcohol, xylogen, the carboxymethyl cellulose.
The invention has the advantages that:
1, the present invention has added a small amount of α-Al in corundum brick 2O 3Nano powder makes the sintering temperature of corundum brick reduce by 200～400 ℃, is conducive to save energy and reduce the cost, and is easier to make.
2, at nanometer α-Al 2O 3In the preparation process of composite corundum brick, the dispersion technology of employing and mud moulding process can guarantee α-Al 2O 3Nano powder is Uniform Dispersion in matrix.
3, the nanometer α for preparing with the present invention-Al 2O 3Composite corundum brick improves 30-80% than present commodity corundum brick high temperature break resistant intensity, and thermal shock resistance improves 20-50%.
Embodiment:
Below in conjunction with embodiment the present invention is further described, but is not limited to the following example.
Embodiment 1
Raw material:
Select Al 2O 3Content is greater than 99% electro-corundum coarse granule, middle particle, fine powder, α-Al 2O 3Micro mist and α-Al 2O 3Nano powder is raw material, wherein α-Al 2O 3The nano powder average grain diameter is 50-120nm, corundum in granules, fine powder, α-Al 2O 3Granularmetric composition such as the table 1 of micro mist,
Table 1 corundum in granules, fine powder and α-Al 2O 3The granularmetric composition of micro mist
Component Al 2O 3
Coarse granule Middle particle Fine powder α-Al 2O 3Micro mist
Mm 5-1 1-0.088 ＜0.088 0.005 (D 50)
Various raw materials by weight are: α-Al 2O 3Nano powder 1%, α-Al 2O 3Micro mist 6%, corundum coarse granule 45%, corundum fine grained 15%, corundum fine powder 33%.
Dispersion agent is an ammonium polyacrylate, and consumption is 0.2% of a raw material weight.
Preparation:
With α-Al 2O 3Nano-powder adds water (amount of water be total amount of water about 50%) and is mixed with suspension, and ultrasonic dispersion adds ammonium polyacrylate and α-Al 2O 3Micro mist is mixed and made into mud; Successively corundum coarse granule, middle particle, fine powder and mud are added mixer, take the dextrin of batch mixing weight 3% as bond, adding mixes, and ageing mixture is 24 hours under the room temperature, and machine is pressed into green compact under the pressure of 150MPa, green compact through 120 ℃, 24h is dry processes.
Above-mentioned green compact are placed stove, be warming up to 1000 ℃ with 120 ℃/hour speed; Continue to be warming up to 1350 ℃ with 60 ℃/hour speed again, be incubated 9 hours; Treat that furnace temperature reduces to room temperature and take out, promptly make nanometer α-Al 2O 3Composite corundum brick.
After testing, prepared nanometer α-Al 2O 3The bulk density of composite corundum brick is 3.21g/cm 3, apparent porosity is 17.9%, strength at normal temperature is 18MPa, cold crushing strength is 93MPa, the high temperature break resistant intensity under 1400 ℃ is 9Mpa, 1100 ℃ of water-cooleds once after thermal shock residual strength conservation rate be 38%.
Embodiment 2
Raw materials used and granularity is with embodiment 1.
Various raw materials by weight are: α-Al 2O 3Nano powder 1%, α-Al 2O 3Micro mist 4%, corundum coarse granule 50%, corundum fine grained 10%, corundum fine powder 35%.
Dispersion agent is that polycarboxylate ether and ammonium polyacrylate are composite, and consumption is 0.78% and 0.1% of a raw material weight.
Preparation α-Al 2O 3Nano-powder suspension and ultrasonic dispersion add polycarboxylate ether and α-Al 2O 3Micro mist is mixed and made into mud; Successively corundum coarse granule, middle particle, fine powder and mud are added mixer, take the dextrin of batch mixing weight 3% as bond, ageing mixture is 22 hours under the room temperature, and machine is pressed into green compact under the pressure of 150MPa, the dry 24h that processes about 110 ℃.
Above-mentioned green compact are warming up to 1000 ℃ with 160 ℃/hour speed; Continue to be warming up to 1500 ℃ with 65 ℃/hour speed again, be incubated 5 hours; Treat that furnace temperature reduces to room temperature and take out, promptly make nanometer α-Al 2O 3Composite corundum brick.
After testing, prepared nanometer α-Al 2O 3The bulk density of composite corundum brick is 3.25g/cm 3, apparent porosity is 17.5%, and strength at normal temperature is 20MPa, and cold crushing strength is 102MPa, and the high temperature break resistant intensity under 1400 ℃ is 10MPa; 1100 ℃ of water-cooleds once after thermal shock residual strength conservation rate be 37%.
Embodiment 3
Raw materials used and granularity is with embodiment 1.
Various raw materials by weight are: α-Al 2O 3Nano powder 0.5%, α-Al 2O 3Micro mist 12%, corundum coarse granule 45%, corundum fine grained 15%, corundum fine powder 27.5%.
Dispersion agent is a Sodium hexametaphosphate 99, and consumption is 0.08% of a raw material weight.
Preparation α-Al 2O 3Nano-powder suspension and ultrasonic dispersion add calgon and α-Al 2O 3Micro mist is mixed and made into mud; Successively corundum coarse granule, middle particle, fine powder and mud are added mixer, take the carboxymethyl cellulose of batch mixing weight 2.5% as bond, adding mixes, and ageing mixture is about 23 hours under the room temperature, machine is pressed into green compact under the pressure of 120MPa, 110 ℃ of dry 24h that process.
Above-mentioned green compact are placed stove, be warming up to 1000 ℃ with 180 ℃/hour speed; Continue to be warming up to 1250 ℃ with 80 ℃/hour speed again, be incubated 4 hours; Treat that furnace temperature reduces to room temperature and take out, promptly make nanometer α-Al 2O 3Composite corundum brick.
After testing, prepared nanometer α-Al 2O 3The bulk density of composite corundum brick is 3.31g/cm 3, apparent porosity is 16.3%, and strength at normal temperature is 21MPa, and cold crushing strength is 121MPa, and the high temperature break resistant intensity under 1400 ℃ is 14MPa; 1100 ℃ of water-cooleds once after thermal shock residual strength conservation rate be 28%.
Embodiment 4
Select for use raw material with embodiment 1.
α-Al wherein 2O 3The nano powder average grain diameter is 50-120nm, corundum in granules, fine powder, α-Al 2O 3The granularmetric composition of micro mist is as shown in table 2.
Table 2 corundum in granules, fine powder and α-Al 2O 3The granularmetric composition of micro mist
Component Al 2O 3
Coarse granule Middle particle Fine powder α-Al 2O 3Micro mist
Mm 4-1 1-0.088 ＜0.044 0.01 (D 50)
Various raw materials by weight are: α-Al 2O 3Nano powder 1%, α-Al 2O 3Micro mist 8%, corundum coarse granule 50%, corundum fine grained 10%, corundum fine powder 31%.
Dispersion agent is that polycarboxylate ether and Sodium hexametaphosphate 99 are composite, and consumption is respectively 0.2% and 0.05% of raw material weight.
Preparation α-Al 2O 3Nano-powder suspension and ultrasonic dispersion add polycarboxylate ether and calgon and α-Al 2O 3Micro mist is mixed and made into mud; Successively corundum coarse granule, middle particle, fine powder and mud are added mixer, take the carboxymethyl cellulose of batch mixing weight 2% as bond, adding mixes, and ageing mixture is 24 hours under the room temperature, and machine is pressed into green compact under the pressure of 180MPa, 120 ℃ of dry 24h that process.
Above-mentioned green compact are placed stove, be warming up to 950 ℃ with 100 ℃/hour speed; Continue to be warming up to 1450 ℃ with 60 ℃/hour speed again, be incubated 6 hours; Treat that furnace temperature reduces to room temperature and take out, promptly make nanometer α-Al 2O 3Composite corundum brick.
After testing, prepared nanometer α-Al 2O 3The bulk density of composite corundum brick is 3.29g/cm 3, apparent porosity is 16.0%, and strength at normal temperature is 18MPa, and cold crushing strength is 141MPa, and the high temperature break resistant intensity under 1400 ℃ is 16MPa; 1100 ℃ of water-cooleds once after thermal shock residual strength conservation rate be 32%.
Embodiment 5
Raw materials used and granularity is with embodiment 4.
Various raw materials by weight are: α-Al 2O 3Nano powder 3%, α-Al 2O 3Micro mist 10%, corundum coarse granule 60%, corundum fine grained 10%, corundum fine powder 17%.
Dispersion agent is a sodium polyacrylate, and consumption is 0.3% of a raw material weight.
Preparation α-Al 2O 3Nano-powder suspension and ultrasonic dispersion add Sodium Polyacrylate and α-Al 2O 3Micro mist is mixed and made into mud; Successively corundum coarse granule, middle particle, fine powder and mud are added mixer, take the polyvinyl alcohol of batch mixing weight 3% as bond, adding mixes, and ageing mixture is 22 hours under the room temperature, and machine is pressed into green compact under the pressure of 150MPa, 120 ℃ of dry 22h that process.
Above-mentioned green compact are placed stove, be warming up to 1100 ℃ with 120 ℃/hour speed; Continue to be warming up to 1600 ℃ with 90 ℃/hour speed again, be incubated 3 hours; Treat that furnace temperature reduces to room temperature and take out, obtain nanometer α-Al 2O 3Composite corundum brick.
After testing, prepared nanometer α-Al 2O 3The bulk density of composite corundum brick is 3.24g/cm 3, apparent porosity is 17.0%, and strength at normal temperature is 16MPa, and cold crushing strength is 132MPa, and high temperature break resistant intensity is 12MPa in the time of 1400 ℃; 1100 ℃ of water-cooleds once after thermal shock residual strength conservation rate be 33%.
Embodiment 6
Institute's raw material is with embodiment 1.
α-Al wherein 2O 3The nano powder average grain diameter is 50-120nm, corundum in granules, fine powder, α-Al 2O 3The granularmetric composition of micro mist is as shown in table 3.
Table 3 corundum in granules, fine powder, α-Al 2O 3The granularmetric composition of micro mist
Component Al 2O 3
Coarse granule Middle particle Fine powder α-Al 2O 3Micro mist
Mm 5-1 1-0.088 ＜0.088 0.008 (D 50)
Various raw materials by weight are: α-Al 2O 3Nano powder 2%, α-Al 2O 3Micro mist 5%, corundum coarse granule 47%, corundum fine grained 18%, corundum fine powder 28%.
Dispersion agent is a tripoly phosphate sodium STPP, and consumption is 0.08% of a raw material weight.
Preparation α-Al 2O 3Nano-powder suspension and ultrasonic dispersion add ammonium polyacrylate and α-Al 2O 3Micro mist is mixed and made into mud, successively corundum coarse granule, middle particle, fine powder and mud is added mixer, take the lignin of batch mixing weight 6% as bond, adding mixes, ageing mixture is 24 hours under the room temperature, and machine is pressed into green compact under the pressure of 250MPa, 120 ℃ of dry 24h that process.
Above-mentioned green compact are placed stove, under oxidizing atmosphere, be warming up to 1000 ℃ with 200 ℃/hour speed; Continue to be warming up to 1550 ℃ with 60 ℃/hour speed again, be incubated 5 hours; Treat that furnace temperature reduces to room temperature and take out, obtain nanometer α-Al 2O 3Composite corundum brick.
After testing, prepared nanometer α-Al 2O 3The bulk density of composite corundum brick is 3.26g/cm 3, apparent porosity is 16.8%, and strength at normal temperature is 21MPa, and cold crushing strength is 126MPa, and the high temperature break resistant intensity under 1400 ℃ is 15MPa; 1100 ℃ of water-cooleds once after thermal shock residual strength conservation rate be 34%.

Claims (7)

1、纳米α-Al2O3复合刚玉砖的制备方法，以Al2O3含量大于99％的电熔刚玉颗粒和细粉、α-Al2O3纳米粉和α-Al2O3微粉为原料，采用分散技术和成型工艺，其特征在于：1. The preparation method of nanometer α-Al 2 O 3 composite corundum brick, using fused corundum particles and fine powder with Al 2 O 3 content greater than 99%, α-Al 2 O 3 nano powder and α-Al 2 O 3 micro powder As a raw material, using dispersion technology and molding process, it is characterized in that: a.将重量份数为0.25-3.5％的α-Al2O3纳米粉加水配制成悬浮液，超声分散，加入重量份数0.05-2.0％的分散剂和2-15％的α-Al2O3微粉混合制成泥浆；a. Add 0.25-3.5% by weight of α-Al 2 O 3 nano powder to prepare a suspension, ultrasonically disperse, add 0.05-2.0% by weight of dispersant and 2-15% of α-Al 2 O3 micropowder is mixed to make mud; b.将重量份数为84-96％的刚玉颗粒及细粉与泥浆混合均匀，加入原料总重量3-6％的结合剂，混合均匀成泥料，室温下困料22-24小时，机压成生坯，100-120℃、20-24h干燥处理；b. Mix 84-96% corundum particles and fine powder with the mud evenly, add 3-6% of the total weight of the raw materials as a binder, mix evenly to form a mud, store the material at room temperature for 22-24 hours, and machine Press into a green body, dry at 100-120°C for 20-24h; c.将干燥后的生坯置于炉中，以60-300℃/小时的速率升温至950-1100℃，再以30-100℃/小时的速率继续升温至1250-1600℃烧成，保温3-10小时，冷却至室温后，即得产物。c. Put the dried green body in the furnace, heat up to 950-1100°C at a rate of 60-300°C/hour, and then continue to heat up to 1250-1600°C at a rate of 30-100°C/hour for firing, and keep warm After 3-10 hours, after cooling to room temperature, the product is obtained. 2 依照权利要求1述的纳米α-Al2O3复合刚玉砖的制备方法，其特征在于α-Al2O3纳米粉的粒径为50-120nm。2. The method for preparing nano-α-Al 2 O 3 composite corundum bricks according to claim 1, characterized in that the particle size of the α-Al 2 O 3 nano-powder is 50-120nm. 3、依照权利要求1的纳米α-Al2O3复合刚玉砖的制备方法，其特征在于α-Al2O3微粉的D50＝1-10μm。3. The method for preparing nanometer α-Al 2 O 3 composite corundum bricks according to claim 1, characterized in that D 50 of the α-Al 2 O 3 micropowder is 1-10 μm. 4 依照权利要求1所述的纳米α-Al2O3复合刚玉砖的制备方法，其特征在于所说电熔刚玉颗粒和细粉中，粗颗粒的粒径为5-1mm，重量份数为45-65％；中颗粒的粒径为1-0.088mm，重量份数10-20％；细粉的粒径小于0.088mm，重量份数15-35％。4. The method for preparing nano-α-Al 2 O 3 composite corundum bricks according to claim 1, characterized in that in the fused corundum particles and fine powder, the particle size of the coarse particles is 5-1 mm, and the parts by weight are 45-65%; the particle size of the medium particle is 1-0.088mm, and the weight part is 10-20%; the particle size of the fine powder is less than 0.088mm, and the weight part is 15-35%. 5、依照权利要求1-4所述任一纳米α-Al2O3复合刚玉砖的制备方法，其特征在于分散剂为聚丙烯酸铵，聚丙烯酸钠，聚羧酸酯醚，三聚磷酸钠，六偏磷酸钠中的一种或两种。5. According to the preparation method of any nanometer α-Al 2 O 3 composite corundum brick according to claims 1-4, it is characterized in that the dispersant is ammonium polyacrylate, sodium polyacrylate, polycarboxylate ether, sodium tripolyphosphate , one or two of sodium hexametaphosphate. 6、依照权利要求1-5所述任一纳米α-Al2O3复合刚玉砖的制备方法，其特征在于结合剂为糊精、聚乙烯醇、木质素、羧甲基纤维素中的一种。6. According to the preparation method of any nanometer α-Al 2 O 3 composite corundum brick according to claims 1-5, it is characterized in that the binder is one of dextrin, polyvinyl alcohol, lignin, and carboxymethyl cellulose kind. 7、依照权利要求1所述的纳米α-Al2O3复合刚玉砖的制备方法，其特征在于：机压成型的压力为100-250MPa。7. The method for preparing nanometer α-Al 2 O 3 composite corundum bricks according to claim 1, characterized in that: the pressure of machine pressing is 100-250 MPa.
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CN101955361A (en) * 2010-09-29 2011-01-26 河南省伯马股份有限公司 Method for producing high-chrome bricks containing nano composite particles
CN103183516A (en) * 2013-04-10 2013-07-03 济南钢铁集团耐火材料有限责任公司 Machine pressing carbon-free lining brick for steel ladles
CN103183516B (en) * 2013-04-10 2015-01-14 济南钢铁集团耐火材料有限责任公司 Machine pressing carbon-free lining brick for steel ladles
CN105237003A (en) * 2015-10-20 2016-01-13 长兴宏泰耐火器材有限公司 Method for producing environmentally friendly high-temperature fold-resistant high-strength high purity corundum bricks
CN106468086A (en) * 2016-08-31 2017-03-01 长兴科特碳化硅有限公司 Combined type disperse air brick and preparation method thereof
CN108658621A (en) * 2018-05-18 2018-10-16 宜兴市东山新型材料有限公司 A kind of high purity aluminium oxide lightweight load bearing board and preparation method thereof
CN108610027A (en) * 2018-07-16 2018-10-02 武汉科技大学 A kind of high-performance cement combination castable and preparation method thereof
CN108947500A (en) * 2018-08-16 2018-12-07 中钢集团洛阳耐火材料研究院有限公司 A kind of low sodium abrasion-resistant corundum product and preparation method
CN111099883A (en) * 2019-12-27 2020-05-05 江苏国窑科技有限公司 Corundum brick for hazardous waste rotary kiln and preparation method thereof
CN113880563A (en) * 2021-09-16 2022-01-04 山东工业陶瓷研究设计院有限公司 High-temperature creep-resistant ceramic material and preparation method thereof
CN113880563B (en) * 2021-09-16 2023-02-17 山东工业陶瓷研究设计院有限公司 High-temperature creep-resistant ceramic material and preparation method thereof

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