CN103304247A - Zirconium oxide fire-resistant material and preparation process thereof - Google Patents
Zirconium oxide fire-resistant material and preparation process thereof Download PDFInfo
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Abstract
The invention relates to a fire-resistant material, and particularly relates to a zirconium oxide fire-resistant material and a preparation process thereof. The zirconium oxide fire-resistant material provided by the invention has good heat shock stability because electric-smelting monoclinic zirconium oxide has better fracture toughness and strength, and can further play a stabilizing role on the electric-smelting monoclinic zirconium oxide, improve the heat expansion coefficient of the electric-smelting monoclinic zirconium oxide, enhance the toughness of the electric-smelting monoclinic zirconium oxide, outstandingly enhance the heat shock stability of a product and reduce the firing temperature of the electric-smelting monoclinic zirconium oxide through the addition of yttrium oxide or yttrium nitrate and barium oxide or barium carbonate or barium phosphate, thereby reducing the energy consumption and enlarging the firing range. The preparation process of the zirconium oxide fire-resistant material, which is provided by the invention, has the advantage that the fire-resistant material has the characteristic of crack-growth stability because a pre-burned material has very excellent heat shock property and compactness by being subjected to activated treatment at a temperature lower than burning temperature, and the compactness, heat shock property and the mechanical property of the fire-resistant material are enhanced.
Description
Technical field
The present invention relates to a kind of refractory materials, relate in particular to zirconia refractory and preparation technology thereof.
Background technology
Zirconium white physicochemical property excellence has very high fusing point, and the high-purity compact zircite product has that use temperature height, refractory melt corroded by liquid, antiscour, are not easy precipitation, good chemical stability, is a kind of broad-spectrum high-performance refractory goods.
When making zircite product, generally use semi-stability or complete stable zirconium white raw material in the market, by granulation, compacting, technology such as burn till and make related products, because the higher hard-to-sinter of zirconium white fusing point, firing temperature needs more than 1700 ℃, the firing temperature high energy consumption is big, and firing range is narrow again, cause the goods cracking easily, distortion, for burn till require high, and there are a large amount of thick pores in the goods part tight section that this handicraft forms, cause thermal shock resistance poor, in use occur easily bursting, cracking, phenomenons such as precipitation, the performance of material are difficult to stable and guarantee.
Summary of the invention
Zirconia refractory provided by the invention is intended to overcome and burns till difficulty in the prior art, the deficiency that material character is difficult to guarantee.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme: zirconia refractory, comprise the electric smelting monoclinic zirconia, quality is the pre-burned material of electric smelting monoclinic zirconia 10～50%, and quality is that the magnesium oxide of electric smelting monoclinic zirconia 2.5～4% or magnesiumcarbonate or magnesium hydroxide, quality are that the yttrium oxide of electric smelting monoclinic zirconia 0.1～0.5% or Yttrium trinitrate, quality are that the barium oxide of electric smelting monoclinic zirconia 0.1～0.2% or barium carbonate or barium phosphate, quality are the wedding agent of electric smelting monoclinic zirconia 6～8%;
Described pre-burned material package is drawn together: electric smelting monoclinic zirconia, quality are magnesium oxide or magnesiumcarbonate or the magnesium hydroxide of electric smelting monoclinic zirconia 2.5～4% in the pre-burned material;
Described wedding agent comprises: 3～5% glycerine, 3～5% ethanol, 9～10% polyvinyl alcohol, all the other are water.
As preferably, zirconia content requires greater than 99% in the electric smelting monoclinic zirconia, and granularity requirements D50 because zirconium white has higher purity and thinner granularity, makes the product of making have better properties at 3～6 microns.
As preferably, described glycerine is industry glycerol, and described ethanol is industrial alcohol, the material of this purity be easy to make and price relatively low, reduced the manufacturing cost of product.
A kind of preparation technology of above-mentioned zirconia refractory may further comprise the steps:
A, preparation pre-burned material: be earlier that the magnesium oxide of electric smelting monoclinic zirconia 2.5～4% or magnesiumcarbonate or magnesium hydroxide mix with electric smelting monoclinic zirconia, quality, fire by 1300～1500 ℃ then, be incubated 1～10 hour, be broken into powder at last and obtain the pre-burned material;
B, be that the yttrium oxide of electric smelting monoclinic zirconia 0.1～0.5% or Yttrium trinitrate, quality are that the barium oxide of electric smelting monoclinic zirconia 0.1～0.2% or barium carbonate or barium phosphate mix with electric smelting monoclinic zirconia, quality are the pre-burned material that made by step a of electric smelting monoclinic zirconia 10～50%, quality is electric smelting monoclinic zirconia 2.5～4% magnesium oxide or magnesiumcarbonate or magnesium hydroxide, quality;
C, to add quality in the compound of step b again be the wedding agent of electric smelting monoclinic zirconia 6～8% among the step b, mixes;
D, the material that step c is mixed sieve;
E, carry out processed, degree of dehydration is that moisture content is 2% to 3%;
F, granulation;
G, moulding;
H, seasoning were burnt till by following condition after 24 hours:
Naturally temperature～250 ℃ of 30 ℃/hour intensification;
250 ℃～500 ℃ 25 ℃/hour intensification;
500～1630 ℃ or 1650 ℃ of 50 ℃/hour intensification;
Be incubated 12 hours;
Naturally slowly cool to the nature temperature.
As preferably, the degree of crushing of prefabricated material is 5 to 10 microns in a step, makes prefabricated material have granularity preferably, has improved the quality of product.
As preferably, the mixing time in the b step is 2 to 10 minutes, and prefabricated material and granulation material mix, and have improved the quality of product.
As preferably, the mixing time in the c step is 30 to 50 minutes, and prefabricated material and granulation material and wedding agent mix the further quality that improves product.
As preferably, sieving in the d step requires to being at least 16 mesh sieves, makes material have better fineness, improved the amount processed of product.
As preferably, in the f step granulation be shaped as sphere because sphere has better properties, further improved the quality of product.
As preferably, forming pressure is 20 to 25MPa in the g step, and this pressure range has good processability and pressure obtains easily, has reduced the manufacturing cost of product and has improved the quality of product.
Zirconia refractory provided by the invention, have following advantage: the electric smelting monoclinic zirconia has fracture toughness property and intensity preferably, mainly be owing to the different thermal mismatchings that produce with cubic phase thermal expansivity of monocline phase, thereby in microstructure, form tiny crack, so good thermal shock stability, the adding of yttrium oxide or Yttrium trinitrate and barium oxide or barium carbonate or barium phosphate, not only can further play stabilization to the electric smelting monoclinic zirconia, and improved the thermal expansivity of electric smelting monoclinic zirconia, strengthen the toughness of electric smelting monoclinic zirconia, the significant thermal shock resistance that improves goods, can also reduce by 50～100 ℃ of the firing temperatures of electric smelting monoclinic zirconia in addition, the firing range amplitude reaches about 80 ℃, has reduced energy consumption, enlarged firing range.
The preparation technology of zirconia refractory provided by the invention, have following advantage: firing temperature is active to be handled the pre-burned material through being lower than, has very outstanding thermal shock performance and compactness, through scanning electron microscope analysis, have 60～80% average grain size in the goods and be approximately 30 microns, wherein 20～40% grain-sizes are 1～2 micron crystallite, be evenly distributed in the goods, make material have the feature of stable crack propagation, make compactness and the thermal shock performance of product be improved, mechanical property also is improved.
Embodiment
Embodiment one
Zirconia refractory, comprise the electric smelting monoclinic zirconia, quality is the pre-burned material of electric smelting monoclinic zirconia 30%, quality is that magnesium oxide, the quality of electric smelting monoclinic zirconia 2.5% is the yttrium oxide of electric smelting monoclinic zirconia 0.2%, quality is the barium oxide of electric smelting monoclinic zirconia 0.15%, and quality is the wedding agent of electric smelting monoclinic zirconia 6%;
The prescription of described pre-burned material is: electric smelting monoclinic zirconia, quality are the magnesium oxide of electric smelting monoclinic zirconia 2.5% in the pre-burned material;
The prescription of described wedding agent is: 4% industry glycerol, 3% industrial alcohol, 10% polyvinyl alcohol, all the other are water;
The requirement of electric smelting monoclinic zirconia is in the above-mentioned prescription: zirconia content requires greater than 99% in the electric smelting monoclinic zirconia, and granularity requirements D50 is at 6 microns.
The preparation technology of zirconia refractory may further comprise the steps:
A, preparation pre-burned material: the magnesium oxide that with electric smelting monoclinic zirconia, quality is electric smelting monoclinic zirconia 2.5% earlier mixes, and fires by 1400 ℃ then, is incubated 10 hours, is broken into 10 microns pre-burned material at last;
B, be that the pre-burned material that made by a step of electric smelting monoclinic zirconia 30%, the magnesium oxide that quality is electric smelting monoclinic zirconia 2.5%, the yttrium oxide that quality is electric smelting monoclinic zirconia 0.2%, the barium oxide that quality is electric smelting monoclinic zirconia 0.15% mix with electric smelting monoclinic zirconia, quality, mixing time is 2 minutes;
C, to add quality in the compound of step b again be the wedding agent of electric smelting monoclinic zirconia 6% among the step b, mixes, and mixing time is 30 minutes;
D, the material that step c is mixed sieve with 16 order vibratory screening apparatuss;
E, carry out processed, degree of dehydration is that moisture content is 3%;
F, granulation, being shaped as of granulation is spherical;
G, be the equipment compression molding of 25Mpa with pressure;
H, seasoning are after 24 hours, and the condition of clicking is burnt till:
Naturally temperature～250 ℃ is by 30 ℃ of/hour intensifications;
250 ℃～500 ℃ by 25 ℃ of/hour intensifications;
500～1630 ℃ by 50 ℃ of/hour intensifications;
Be incubated 12 hours;
Naturally slowly cool to the nature temperature.
The zirconium white slide plate performance index of making by above-mentioned prescription and technology are: apparent porosity 6.3%, volume density 5.28g/cm
3, compressive strength 285Mpa carries out water-cooled thermal shock test number of times under 1100 ℃ and obviously cracking occurs 12 times.
Embodiment two
Zirconia refractory, comprise the electric smelting monoclinic zirconia, quality is the pre-burned material of electric smelting monoclinic zirconia 50%, quality is that magnesiumcarbonate, the quality of electric smelting monoclinic zirconia 4% is the Yttrium trinitrate of electric smelting monoclinic zirconia 0.5%, quality is the barium carbonate of electric smelting monoclinic zirconia 0.2%, and quality is the wedding agent of electric smelting monoclinic zirconia 7%;
Described pre-burned material package is drawn together: electric smelting monoclinic zirconia, quality are the magnesiumcarbonate of electric smelting monoclinic zirconia 4% in the pre-burned material;
Described wedding agent comprises: 3% industry glycerol, 4% industrial alcohol, 9% polyvinyl alcohol, all the other are water;
The requirement of electric smelting monoclinic zirconia is in the above-mentioned prescription: zirconia content requires greater than 99% in the electric smelting monoclinic zirconia, and granularity requirements D50 is at 3 microns.
The preparation technology of zirconia refractory may further comprise the steps:
A, be that the magnesiumcarbonate of electric smelting monoclinic zirconia 4% mixes with electric smelting monoclinic zirconia, quality, fire by 1500 ℃, be incubated 5 hours, be broken into 5 microns pre-burned material;
B, be that the pre-burned material that made by a step of electric smelting monoclinic zirconia 50%, the magnesiumcarbonate that quality is electric smelting monoclinic zirconia 4%, the Yttrium trinitrate that quality is electric smelting monoclinic zirconia 0.5%, the barium carbonate that quality is electric smelting monoclinic zirconia 0.2% mix with electric smelting monoclinic zirconia, quality, mixing time is 10 minutes;
C, to add quality in the compound of step b again be the wedding agent of electric smelting monoclinic zirconia 7% among the step b, mixes, and mixing time is 50 minutes;
D, the material that step c is mixed sieve with 20 order vibratory screening apparatuss;
E, carry out processed, degree of dehydration is that moisture content is 2%;
F, granulation, being shaped as of granulation is spherical;
G, be the equipment compression molding of 20Mpa with pressure;
H, seasoning are after 24 hours, and the condition of clicking is burnt till:
Naturally temperature～250 ℃ is by 30 ℃ of/hour intensifications;
250 ℃～500 ℃ by 25 ℃ of/hour intensifications;
500～1650 ℃ by 50 ℃ of/hour intensifications;
Be incubated 12 hours;
Naturally slowly cool to the nature temperature.
The zirconium white slide plate performance index of making by above-mentioned prescription and technology are: apparent porosity 3.55%, volume density 5.33g/cm
3, compressive strength 323Mpa carries out water-cooled thermal shock test number of times under 1100 ℃ and obviously cracking occurs 10 times.
Embodiment three
Zirconia refractory, comprise the electric smelting monoclinic zirconia, quality is the pre-burned material of electric smelting monoclinic zirconia 40%, quality is that magnesium hydroxide, the quality of electric smelting monoclinic zirconia 3% is the yttrium oxide of electric smelting monoclinic zirconia 0.4%, quality is the barium phosphate of electric smelting monoclinic zirconia 0.1%, and quality is the wedding agent of electric smelting monoclinic zirconia 8%;
The prescription of described pre-burned material is: electric smelting monoclinic zirconia, quality are the magnesium hydroxide of electric smelting monoclinic zirconia 3% in the pre-burned material;
The prescription of described wedding agent is: 5% industry glycerol, 5% industrial alcohol, 10% polyvinyl alcohol, all the other are water;
The requirement of electric smelting monoclinic zirconia is in the above-mentioned prescription: zirconia content requires greater than 99% in the electric smelting monoclinic zirconia, and granularity requirements D50 is at 5 microns.
The preparation technology of zirconia refractory may further comprise the steps:
A, preparation pre-burned material: be that the magnesium hydroxide of electric smelting monoclinic zirconia 3% mixes with electric smelting monoclinic zirconia, quality, fire by 1300 ℃, be incubated 7 hours, be broken into 8 microns pre-burned material;
B, be that the pre-burned material that made by a step of electric smelting monoclinic zirconia 40%, the magnesium hydroxide that quality is electric smelting monoclinic zirconia 3%, the yttrium oxide that quality is electric smelting monoclinic zirconia 0.4%, the barium phosphate that quality is electric smelting monoclinic zirconia 0.1% mix with electric smelting monoclinic zirconia, quality, mixing time is 7 minutes;
C, to add quality in the compound of step b again be the wedding agent of electric smelting monoclinic zirconia 8% among the step b, mixes, and mixing time is 40 minutes;
D, the material that step c is mixed sieve with 25 order vibratory screening apparatuss;
E, carry out processed, degree of dehydration is that moisture content is 2.5%;
F, granulation, being shaped as of granulation is spherical;
G, be the equipment compression molding of 27Mpa with pressure;
H, seasoning are after 24 hours, and the condition of clicking is burnt till:
Naturally temperature～250 ℃ is by 30 ℃ of/hour intensifications;
250 ℃～500 ℃ by 25 ℃ of/hour intensifications;
500～1640 ℃ by 50 ℃ of/hour intensifications;
Be incubated 12 hours;
Naturally slowly cool to the nature temperature.
The zirconium white slide plate performance index of making by above-mentioned prescription and technology are: apparent porosity 3.53%, volume density 5.35g/cm
3, compressive strength 325Mpa carries out water-cooled thermal shock test number of times under 1100 ℃ and obviously cracking occurs 14 times.
Being preferred implementation of the present invention only below, being intended to embody outstanding technique effect of the present invention and advantage, is not to be restriction to technical scheme of the present invention.This area the skill personnel it should be understood that, all modifications of making based on the technology of the present invention content, variation or substitute technology feature all should be covered by in the technology category of claims opinion of the present invention.
Claims (10)
1. zirconia refractory is characterized in that: comprise that electric smelting monoclinic zirconia, quality are that the pre-burned material of electric smelting monoclinic zirconia 10～50%, magnesium oxide that quality is electric smelting monoclinic zirconia 2.5～4% or magnesiumcarbonate or magnesium hydroxide, quality are that the yttrium oxide of electric smelting monoclinic zirconia 0.1～0.5% or Yttrium trinitrate, quality are that the barium oxide of electric smelting monoclinic zirconia 0.1～0.2% or barium carbonate or barium phosphate, quality are the wedding agent of electric smelting monoclinic zirconia 6～8%;
Described pre-burned material package is drawn together: electric smelting monoclinic zirconia, quality are magnesium oxide or magnesiumcarbonate or the magnesium hydroxide of electric smelting monoclinic zirconia 2.5～4% in the pre-burned material;
Described wedding agent comprises: 3～5% glycerine, 3～5% ethanol, 9～10% polyvinyl alcohol, all the other are water.
2. zirconia refractory according to claim 1 is characterized in that: zirconia content requires greater than 99% in the electric smelting monoclinic zirconia, and granularity requirements D50 is at 3～6 microns.
3. zirconia refractory according to claim 1, it is characterized in that: described glycerine is industry glycerol, described ethanol is industrial alcohol.
4. preparation technology of zirconia refractory according to claim 1 is characterized in that: may further comprise the steps:
A, preparation pre-burned material: be earlier that the magnesium oxide of electric smelting monoclinic zirconia 2.5～4% or magnesiumcarbonate or magnesium hydroxide mix with electric smelting monoclinic zirconia, quality, fire by 1300～1500 ℃ then, be incubated 1～10 hour, be broken into powder at last and obtain the pre-burned material;
B, be that the yttrium oxide of electric smelting monoclinic zirconia 0.1～0.5% or Yttrium trinitrate, quality are that the barium oxide of electric smelting monoclinic zirconia 0.1～0.2% or barium carbonate or barium phosphate mix with electric smelting monoclinic zirconia, quality are the pre-burned material that made by step a of electric smelting monoclinic zirconia 10～50%, quality is electric smelting monoclinic zirconia 2.5～4% magnesium oxide or magnesiumcarbonate or magnesium hydroxide, quality;
C, to add quality in the compound of step b again be the wedding agent of electric smelting monoclinic zirconia 6～8% among the step b, mixes;
D, the material that step c is mixed sieve;
E, carry out processed, degree of dehydration is that moisture content is 2% to 3%;
F, granulation;
G, moulding;
H, seasoning were burnt till by following condition after 24 hours:
Naturally temperature～250 ℃ of 30 ℃/hour intensification;
250 ℃～500 ℃ 25 ℃/hour intensification;
500～1630 ℃ or 1650 ℃ of 50 ℃/hour intensification;
Be incubated 12 hours;
Naturally slowly cool to the nature temperature.
5. according to the preparation technology of the described zirconia refractory of claim 4, it is characterized in that: the degree of crushing of prefabricated material is 5 to 10 microns in a step.
6. according to the preparation technology of the described zirconia refractory of claim 4, it is characterized in that: the mixing time in the b step is 2 to 10 minutes.
7. according to the preparation technology of the described zirconia refractory of claim 4, it is characterized in that: the mixing time in the c step is 30 to 50 minutes.
8. according to the preparation technology of the described zirconia refractory of claim 4, it is characterized in that: sieving in the d step requires to being at least 16 mesh sieves.
9. according to the preparation technology of the described zirconia refractory of claim 4, it is characterized in that: granulation is shaped as sphere in the f step.
10. according to the preparation technology of the described zirconia refractory of claim 4, it is characterized in that: forming pressure is 20 to 25MPa in the g step.
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| CN107936364A (en) * | 2016-10-13 | 2018-04-20 | 利萨·德雷克塞迈尔有限责任公司 | The stabilized zirconium dioxide of transition metal oxide in the plastics of auto industry |
| CN111606721A (en) * | 2020-06-01 | 2020-09-01 | 海城市方宏耐火材料有限公司 | Environment-friendly bonding agent for refractory material and preparation method thereof |
| CN112341218A (en) * | 2020-11-05 | 2021-02-09 | 中民驰远实业有限公司 | Method for preparing high-performance magnesium-zirconium composite ceramic tile by spark plasma sintering |
| CN112408979A (en) * | 2020-11-13 | 2021-02-26 | 浙江自立控股有限公司 | Zirconia ceramic for converter slag stopping sliding plate and preparation method thereof |
| CN112777980A (en) * | 2021-01-08 | 2021-05-11 | 湖北工业大学 | Preparation method of waste glass fire-resistant high-strength concrete |
| CN113430330A (en) * | 2021-06-23 | 2021-09-24 | 北京浩德楚业新材料科技有限公司 | Preparation method of zirconia solid electrolyte tube and oxygen determination probe |
| CN115959914A (en) * | 2022-08-04 | 2023-04-14 | 广州飞淘科技发展有限公司 | Refractory material for blast furnace tapping channel by adopting waste refractory material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107936364A (en) * | 2016-10-13 | 2018-04-20 | 利萨·德雷克塞迈尔有限责任公司 | The stabilized zirconium dioxide of transition metal oxide in the plastics of auto industry |
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| CN112341218A (en) * | 2020-11-05 | 2021-02-09 | 中民驰远实业有限公司 | Method for preparing high-performance magnesium-zirconium composite ceramic tile by spark plasma sintering |
| CN112341218B (en) * | 2020-11-05 | 2022-04-12 | 中民驰远实业有限公司 | Method for preparing high-performance magnesium-zirconium composite ceramic tile by spark plasma sintering |
| CN112408979A (en) * | 2020-11-13 | 2021-02-26 | 浙江自立控股有限公司 | Zirconia ceramic for converter slag stopping sliding plate and preparation method thereof |
| CN112777980A (en) * | 2021-01-08 | 2021-05-11 | 湖北工业大学 | Preparation method of waste glass fire-resistant high-strength concrete |
| CN113430330A (en) * | 2021-06-23 | 2021-09-24 | 北京浩德楚业新材料科技有限公司 | Preparation method of zirconia solid electrolyte tube and oxygen determination probe |
| CN115959914A (en) * | 2022-08-04 | 2023-04-14 | 广州飞淘科技发展有限公司 | Refractory material for blast furnace tapping channel by adopting waste refractory material |
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| CN103304247B (en) | 2014-10-22 |
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