CN102424592B - Zirconia slide plate and preparation method thereof - Google Patents
Zirconia slide plate and preparation method thereof Download PDFInfo
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- CN102424592B CN102424592B CN 201110269635 CN201110269635A CN102424592B CN 102424592 B CN102424592 B CN 102424592B CN 201110269635 CN201110269635 CN 201110269635 CN 201110269635 A CN201110269635 A CN 201110269635A CN 102424592 B CN102424592 B CN 102424592B
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Abstract
The invention especially relates to a zirconia slide plate and a preparation method thereof, belonging to the field of refractory materials. A technical scheme provided in the invention is as follows: 100 parts by mass of a zirconia micropowder granulation material and 15 to 25 parts by mass of a zirconium hydroxide-resin-ethanol mixed solution are uniformly mixed; an obtained mixture is aged for 20 to 24 hours; molding is carried out; a molded green body is dried at a temperature of 50 to 60 DEG C for 8 to 16 hours, insulated at a temperature of 180 to 240 DEG C for 20 to 24 hours and sintered at a temperature of 1550 to 1650 DEG C; and the sintered green body is subjected to oil immersion, dry distillation, punching and grinding processing so as to obtain the zirconia slide plate. The zirconia slide plate provided in the invention has the characteristics of high rapture strength, good thermal shock stability and excellent anti-erosion performance, has a long service life and can meet demands for casting of Ca-treated steel.
Description
Technical field
The invention belongs to fire resisting material field, especially relate to a kind of Zirconia slide plate and preparation method thereof.
Background technology
In continuous casting production process, the slide gate nozzle system is the important control device of molten steel in the continuous caster casting cycle, can accurately regulate the flow of molten steel from the ladle to the tundish, makes the molten steel that flows into and flow out reach balance, thereby makes more easily control of continuous casting operation.The slide gate nozzle system is comprised of filling pipe end, slide plate and the lower mouth of a river.Slide plate is the parts of directly controlling molten steel flow and flow velocity, decision slide gate nozzle system function, is considered to most important part in the slide gate nozzle system.
The Main Function of calcium in molten steel is to carry out deoxidation, desulfurization and inclusion is carried out denaturing treatment, thereby improves the flowability of molten steel and improve the quality of steel.The calcium of molten steel is processed the technique as a kind of refined molten steel, now is used widely.But the Al in [Ca] in the calcium treated steel water and aluminium carbon commonly used or the aluminum-zirconium-carbon slide
2O
3, SiO
2Reaction generates eutectic, causes that slide plate damage speed is multiplied when the casting calcium treated steel.
" a kind of prescription of magnesia slide brick and production technique " be patented technology (ZL200410010211.X), adopting highly-purity magnesite and alumina powder is the continuous casting operation that magnesia slide plate that main raw material makes can satisfy 100～400 tons of big-and-middle-sized steel ladle pouring calcium treated steels, but only be 1～2 its work-ing life.Zirconium dioxide at high temperature chemical property is very stable, still can keep higher fusing point when contacting with calcium oxide, is the ideal material of casting Slide Nozzle Plate for Calcium-Treated." preparation method of Higly oxidized zirconia refractory " be patented technology (CN200510044209.9), and a kind of Higly oxidized zirconia refractory is provided, and its homogeneous microstructure is fine and close, flawless, and void content is low, and solidity to corrosion is good, and suitable glass furnace uses, but its SiO
2Content is higher, is not suitable for for the cast calcium treated steel." zirconium white slide plate " (Jin Congjin, Li Zeya, zirconium white slide plate preparation technology be on its performance and microstructural impact, refractory materials, 2008,42 (4): 288-290) disclosed technology, adopt MgO-Y
2O
3The zirconium white skateboard of PSZ micro mist granulation material preparation is fine and close, have higher intensity and lower apparent porosity, but its fragility is larger, is unfavorable for following process, and the zirconium white slide plate thermal shock resistance that makes is still good not, has limited its work-ing life.
Summary of the invention
The present invention is intended to overcome the prior art defective, and purpose is to provide that a kind of breaking tenacity is high, good thermal shock stability, erosion-resisting characteristics are good, the Zirconia slide plate of long service life and preparation method thereof.
For achieving the above object, the technical scheme that the present invention takes is: the zirconium white micro mist granulation material of 100 parts of quality and the zirconium hydroxide-resin of 15～25 parts of quality-alcohol mixed solution are mixed ageing mixture 20～24 hours, moulding; Base substrate after the moulding under 50～60 ℃ of conditions dry 8～16 hours 180～240 ℃ of insulations 20～24 hours, is 1550～1650 ℃ at firing temperature and burns till; Burn till by immersion oil, destructive distillation, punch and grind processing, namely get Zirconia slide plate.
Described zirconium white micro mist granulation material is to process through wet ball grinding and mist projection granulating with the PSZ micro mist; The PSZ micro mist is Y
2O
3PSZ micro mist, MgO PSZ micro mist, MgO-Y
2O
3In the PSZ micro mist more than one.
The preparation method of described zirconium hydroxide-resin-alcohol mixed solution is: 15～25 parts of zirconium hydroxide powders, 12～18 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 60～70 parts of dehydrated alcohols successively, stirred 2～4 hours at 40～60 ℃.
The described isostatic pressing that is shaped to.
The described process system that burns till is: rise to 1050 ℃ with 1.0～1.6 ℃/minute speed from room temperature, rise to 1250 ℃ with 0.2～0.5 ℃/minute speed from 1050 ℃ again, rise to firing temperature with 0.8～1.2 ℃/minute speed from 1050 ℃, under the condition of firing temperature, be incubated 3～6 hours; Be down to 1250 ℃ with 0.8～1.2 ℃/minute speed from firing temperature, be down to 1050 ℃ with 0.2～0.5 ℃/minute speed from 1250 ℃; Be down to room temperature with≤1.0 ℃/minute speed from 1050 ℃.
Because adopt technique scheme, the present invention joins in the zirconium white micro mist granulation material with the form of zirconium hydroxide-resin-alcohol mixed solution, has guaranteed zirconium hydroxide and the liquid phenolic resin dispersing uniformity in raw material.In sintering process, it only is 20～100nm zirconium white that zirconium hydroxide can be decomposed to form primary particle size, and its activity is very high, and the sintering of accelerating oxidation zirconium sliding material has improved the intensity of material; On the other hand, the resin carbon that a part is free on around the zirconium white plays sterically hindered effect, has effectively suppressed the abnormal growth of zirconium white crystal grain in sintering process, is conducive to improve the breaking tenacity of material; Meanwhile, a part of resin carbon enters and makes monoclinic zirconia be transformed into stable tetragonal zircite in the zirconia crystal lattice, has improved the volume stability of material in the applied at elevated temperature process.The increase of breaking tenacity and volume stability all is conducive to improve the thermal shock resistance of material.
Therefore, Zirconia slide plate of the present invention has that breaking tenacity is high, good thermal shock stability, characteristics that erosion-resisting characteristics is good, and long service life can satisfy the needs of cast calcium treated steel.
Embodiment
The invention will be further described below in conjunction with embodiment, is not the restriction to its protection domain.
For avoiding repetition, first the described process system unification of burning till of this embodiment is described below: rise to 1050 ℃ with 1.0～1.6 ℃/minute speed from room temperature, rise to 1250 ℃ with 0.2～0.5 ℃/minute speed from 1050 ℃ again, rise to firing temperature with 0.8～1.2 ℃/minute speed from 1050 ℃, under the condition of firing temperature, be incubated 3～6 hours; Be down to 1250 ℃ with 0.8～1.2 ℃/minute speed from firing temperature, be down to 1050 ℃ with 0.2～0.5 ℃/minute speed from 1250 ℃; Be down to room temperature with≤1.0 ℃/minute speed from 1050 ℃.Repeat no more among the embodiment.
Embodiment 1
A kind of Zirconia slide plate and preparation method thereof, its technological process is:
The zirconium white micro mist granulation material of 100 parts of quality and the zirconium hydroxide-resin of 15～20 parts of quality-alcohol mixed solution are mixed ageing mixture 20～24 hours, isostatic pressing; Base substrate after the moulding under 50～60 ℃ of conditions dry 8～12 hours 180～220 ℃ of insulations 20～24 hours, is 1550～1600 ℃ at firing temperature and burns till; Burn till by immersion oil, destructive distillation, punch and grind processing, namely get Zirconia slide plate.
In the present embodiment: zirconium white micro mist granulation material is with Y
2O
3The PSZ micro mist processes through wet ball grinding and mist projection granulating; The preparation method of zirconium hydroxide-resin-alcohol mixed solution is: 15～20 parts of zirconium hydroxide powders, 12～14 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 65～70 parts of dehydrated alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density 〉=the 4.72g/cm of the prepared Zirconia slide plate of the present embodiment
3, apparent porosity≤19%, folding strength 〉=20MPa, 1100 ℃ of air-cooled number of times 〉=8 of not destroying, erosion-resisting characteristics is good.
Embodiment 2
A kind of Zirconia slide plate and preparation method thereof, its technological process is:
The zirconium white micro mist granulation material of 100 parts of quality and the zirconium hydroxide-resin of 18～23 parts of quality-alcohol mixed solution are mixed, ageing mixture 20～24 hours, isostatic pressing, base substrate after the moulding under 50～60 ℃ of conditions dry 10～14 hours, 200～240 ℃ of insulations 20～24 hours, be 1580～1620 ℃ at firing temperature and burn till.Burn till by immersion oil, destructive distillation, punch and grind processing, namely get Zirconia slide plate.
In the present embodiment: zirconium white micro mist granulation material is to process through wet ball grinding and mist projection granulating with MgO PSZ micro mist; The preparation method of zirconium hydroxide-resin-alcohol mixed solution is: 17～22 parts of zirconium hydroxide powders, 14～16 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 63～68 parts of dehydrated alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density 〉=the 4.65g/cm of the prepared Zirconia slide plate of the present embodiment
3, apparent porosity≤18%, folding strength 〉=18MPa, 1100 ℃ of air-cooled number of times 〉=6 of not destroying, erosion-resisting characteristics is good.
Embodiment 3
A kind of Zirconia slide plate and preparation method thereof, its technological process is:
The zirconium white micro mist granulation material of 100 parts of quality and the zirconium hydroxide-resin of 16～21 parts of quality-alcohol mixed solution are mixed, ageing mixture 20～24 hours, isostatic pressing, base substrate after the moulding under 50～60 ℃ of conditions dry 11～15 hours, 190～230 ℃ of insulations 20～24 hours, be 1570～1610 ℃ at firing temperature and burn till.Burn till by immersion oil, destructive distillation, punch and grind processing, namely get Zirconia slide plate.
In the present embodiment: zirconium white micro mist granulation material is with MgO-Y
2O
3The PSZ micro mist processes through wet ball grinding and mist projection granulating; The preparation method of zirconium hydroxide-resin-alcohol mixed solution is: 16～21 parts of zirconium hydroxide powders, 13～15 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 60～65 parts of dehydrated alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density 〉=the 4.67g/cm of the prepared Zirconia slide plate of the present embodiment
3, apparent porosity≤17%, folding strength 〉=20MPa, 1100 ℃ of air-cooled number of times 〉=8 of not destroying, erosion-resisting characteristics is good.
Embodiment 4
A kind of Zirconia slide plate and preparation method thereof, its technological process is:
The zirconium white micro mist granulation material of 100 parts of quality and the zirconium hydroxide-resin of 20～25 parts of quality-alcohol mixed solution are mixed, ageing mixture 20～24 hours, isostatic pressing, base substrate after the moulding under 50～60 ℃ of conditions dry 12～16 hours, 200～240 ℃ of insulations 20～24 hours, be 1600～1650 ℃ at firing temperature and burn till.Burn till by immersion oil, destructive distillation, punch and grind processing, namely get Zirconia slide plate.
In the present embodiment: zirconium white micro mist granulation material is with Y
2O
3PSZ micro mist and MgO-Y
2O
3The PSZ micro mist is mixing in 1: 2 in mass ratio, processes through wet ball grinding and mist projection granulating; The preparation method of zirconium hydroxide-resin-alcohol mixed solution is: 18～23 parts of zirconium hydroxide powders, 15～17 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 65～70 parts of dehydrated alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density 〉=the 4.68g/cm of the prepared Zirconia slide plate of the present embodiment
3, apparent porosity≤18%, folding strength 〉=21MPa, 1100 ℃ of air-cooled number of times 〉=9 of not destroying, erosion-resisting characteristics is good.
Embodiment 5
A kind of Zirconia slide plate and preparation method thereof, its technological process is:
The zirconium white micro mist granulation material of 100 parts of quality and the zirconium hydroxide-resin of 17～22 parts of quality-alcohol mixed solution are mixed, ageing mixture 20～24 hours, isostatic pressing, base substrate after the moulding under 50～60 ℃ of conditions dry 9～13 hours, 180～220 ℃ of insulations 20～24 hours, be 1550～1600 ℃ at firing temperature and burn till.Burn till by immersion oil, destructive distillation, punch and grind processing, namely get Zirconia slide plate.
In the present embodiment: zirconium white micro mist granulation material is to be with Y with zirconium white micro mist granulation material
2O
3PSZ micro mist, MgO PSZ micro mist and MgO-Y
2O
3The PSZ micro mist is mixing in 1: 1: 1 in mass ratio, processes through wet ball grinding and mist projection granulating; The preparation method of zirconium hydroxide-resin-alcohol mixed solution is: 20～25 parts of zirconium hydroxide powders, 16～18 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 62～67 parts of dehydrated alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density 〉=the 4.65g/cm of the prepared Zirconia slide plate of the present embodiment
3, apparent porosity≤19%, folding strength 〉=19MPa, 1100 ℃ of air-cooled number of times 〉=10 of not destroying, erosion-resisting characteristics is good.
The present invention joins in the zirconium white micro mist granulation material with the form of zirconium hydroxide-resin-alcohol mixed solution, has guaranteed zirconium hydroxide and the liquid phenolic resin dispersing uniformity in raw material.In sintering process, it only is 20～100nm zirconium white that zirconium hydroxide can be decomposed to form primary particle size, and its activity is very high, and the sintering of accelerating oxidation zirconium sliding material has improved the intensity of material; On the other hand, the resin carbon that a part is free on around the zirconium white plays sterically hindered effect, has effectively suppressed the abnormal growth of zirconium white crystal grain in sintering process, is conducive to improve the breaking tenacity of material; Meanwhile, a part of resin carbon enters and makes monoclinic zirconia be transformed into stable tetragonal zircite in the zirconia crystal lattice, has improved the volume stability of material in the applied at elevated temperature process.The increase of breaking tenacity and volume stability all is conducive to improve the thermal shock resistance of material.
Therefore, Zirconia slide plate of the present invention has that breaking tenacity is high, good thermal shock stability, characteristics that erosion-resisting characteristics is good, and long service life can satisfy the needs of cast calcium treated steel.
Claims (4)
1. the preparation method of a Zirconia slide plate is characterized in that: the zirconium white micro mist granulation material of 100 parts of quality and the zirconium hydroxide-resin of 15 ~ 25 parts of quality-alcohol mixed solution are mixed ageing mixture 20 ~ 24 hours, moulding; Base substrate after the moulding under 50 ~ 60 ℃ of conditions dry 8 ~ 16 hours 180 ~ 240 ℃ of insulations 20 ~ 24 hours, is 1550 ~ 1650 ℃ at firing temperature and burns till; Burn till by immersion oil, destructive distillation, punch and grind processing, namely get Zirconia slide plate;
The preparation method of described zirconium hydroxide-resin-alcohol mixed solution is: 15 ~ 25 parts of zirconium hydroxide powders, 12 ~ 18 parts of heat-reactive phenolic resins and 1 ~ 2 part of hexamethylenetetramine are joined in 60 ~ 70 parts of dehydrated alcohols successively, stirred 2 ~ 4 hours at 40 ~ 60 ℃.
2. the preparation method of Zirconia slide plate according to claim 1 is characterized in that described zirconium white micro mist granulation material is to process through wet ball grinding and mist projection granulating with the PSZ micro mist; The PSZ micro mist is Y
2O
3PSZ micro mist, MgO PSZ micro mist, MgO-Y
2O
3In the PSZ micro mist more than one.
3. the preparation method of Zirconia slide plate according to claim 1 is characterized in that the described isostatic pressing that is shaped to.
4. the prepared Zirconia slide plate of preparation method of each described Zirconia slide plate according to claim 1 ~ 3.
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| CN102643099B (en) * | 2012-05-15 | 2014-02-26 | 武汉科技大学 | Magnesium-zirconium ring of slide plate for calcium-treated steel and preparation method thereof |
| CN112110749A (en) * | 2020-09-24 | 2020-12-22 | 郑州方铭高温陶瓷新材料有限公司 | Preparation method of sintered high-density zirconium dioxide ceramic for slide plate brick |
| CN113698202B (en) * | 2021-08-30 | 2023-07-18 | 中科南京绿色制造产业创新研究院 | Water gap and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774820A (en) * | 2010-02-26 | 2010-07-14 | 卫辉熔金高温材料有限责任公司 | Slide plate refractory with silicon nitride added and production method thereof |
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|---|---|---|---|---|
| JP2575580B2 (en) * | 1993-01-28 | 1997-01-29 | 品川白煉瓦株式会社 | Carbon containing refractories |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774820A (en) * | 2010-02-26 | 2010-07-14 | 卫辉熔金高温材料有限责任公司 | Slide plate refractory with silicon nitride added and production method thereof |
Non-Patent Citations (3)
| Title |
|---|
| JP特开平6-219829A 1994.08.09 |
| 氧化锆滑板制备工艺对其性能和显微结构的影响;金从进等;《耐火材料》;20081231;第42卷(第4期);第288-290页 * |
| 金从进等.氧化锆滑板制备工艺对其性能和显微结构的影响.《耐火材料》.2008,第42卷(第4期),第288-290页摘要. |
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