CN102424592A - Zirconia slide plate and preparation method thereof - Google Patents
Zirconia slide plate and preparation method thereof Download PDFInfo
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- CN102424592A CN102424592A CN2011102696358A CN201110269635A CN102424592A CN 102424592 A CN102424592 A CN 102424592A CN 2011102696358 A CN2011102696358 A CN 2011102696358A CN 201110269635 A CN201110269635 A CN 201110269635A CN 102424592 A CN102424592 A CN 102424592A
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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 zirconium white matter 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 inflow and effusive molten steel reach balance, thereby makes continuous casting operation control more easily.The slide gate nozzle system is made up of filling pipe end, slide plate and the following mouth of a river.Slide plate is the parts of directly controlling molten steel flow and flow velocity, determining the slide gate nozzle system function, is considered to most important parts in the slide gate nozzle system.
The main effect of calcium in molten steel is to carry out deoxidation, desulfurization and inclusion is carried out denaturing treatment, thereby improves molten steel flow property and the quality that improves steel.The calcium of molten steel is handled the technology as a kind of refined molten steel, is used widely at present.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 that the magnesia slide plate that main raw material makes can satisfy the continuous casting operation of 100～400 tons of big-and-middle-sized steel ladle pouring calcium treated steels, but is merely its work-ing life 1～2 time.ZIRCONIUM DIOXIDE 99.5 at high temperature chemical property is very stable, when contacting with quicklime, still can keep high melt point, is the ideal material of casting calcium treated steel slide plate." 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 kiln uses, but its SiO
2Content is higher, is not suitable for the cast calcium treated steel." zirconium white slide plate " (Jin Congjin, Li Zeya, zirconium white slide plate preparation technology be to its performance and microstructural influence, 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 bigger, is unfavorable for following process; And the zirconium white slide plate thermal shock resistance that makes is still good inadequately, 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 height, good thermal shock stability, erosion-resisting characteristics are good, the zirconium white matter slide plate of long service life and preparation method thereof.
For realizing above-mentioned purpose, the technical scheme that the present invention takes is: the zirconium white micro mist granulation material of 100 parts of quality and the zirconium nitrate-resin-alcohol mixed solution of 15～25 parts of quality 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 after immersion oil, destructive distillation, punch and grind processing, promptly get zirconium white matter 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 nitrate-resin-alcohol mixed solution is: 15～25 parts of zirconium nitrate powders, 12～18 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 60～70 parts of absolute ethyl 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; Reduce to 1250 ℃ with 0.8～1.2 ℃/minute speed from firing temperature, reduce to 1050 ℃ from 1250 ℃ with 0.2～0.5 ℃/minute speed; Reduce 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 nitrate-resin-alcohol mixed solution, has guaranteed zirconium nitrate and the liquid phenolic resin dispersing uniformity in raw material.In sintering process, zirconium nitrate can be decomposed to form primary particle size and be merely 20～100nm zirconium white, and its activity is very high, and the sintering of promotes oxidn 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 suppressed growing up unusually of in sintering process zirconium white crystal grain effectively, helps improving the breaking tenacity of material; Meanwhile, a part of resin carbon gets in the zirconia crystal lattice and makes monoclinic zirconia be transformed into stable tetragonal zircite, has improved the volume stability of material in the high temperature use.The increase of breaking tenacity and volume stability all helps improving the thermal shock resistance of material.
Therefore, zirconium white matter slide plate of the present invention has breaking tenacity height, 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
Below in conjunction with embodiment the present invention being done further description, is not the restriction to its protection domain.
For avoiding repetition; Earlier the said process system unification of burning till of this embodiment is described below: rise to 1050 ℃ from room temperature with 1.0～1.6 ℃/minute speed; 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; Reduce to 1250 ℃ with 0.8～1.2 ℃/minute speed from firing temperature, reduce to 1050 ℃ from 1250 ℃ with 0.2～0.5 ℃/minute speed; Reduce to room temperature with≤1.0 ℃/minute speed from 1050 ℃.Repeat no more among the embodiment.
Embodiment 1
A kind of zirconium white matter 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 nitrate-resin-alcohol mixed solution of 15～20 parts of quality 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 after immersion oil, destructive distillation, punch and grind processing, promptly get zirconium white matter 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 nitrate-resin-alcohol mixed solution is: 15～20 parts of zirconium nitrate powders, 12～14 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 65～70 parts of absolute ethyl alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density>=the 4.72g/cm of the prepared zirconium white matter of present embodiment slide plate
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 zirconium white matter 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 nitrate-resin-alcohol mixed solution of 18～23 parts of quality 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, is 1580～1620 ℃ at firing temperature and burns till.Burn till after immersion oil, destructive distillation, punch and grind processing, promptly get zirconium white matter 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 nitrate-resin-alcohol mixed solution is: 17～22 parts of zirconium nitrate powders, 14～16 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 63～68 parts of absolute ethyl alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density>=the 4.65g/cm of the prepared zirconium white matter of present embodiment slide plate
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 zirconium white matter 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 nitrate-resin-alcohol mixed solution of 16～21 parts of quality 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, is 1570～1610 ℃ at firing temperature and burns till.Burn till after immersion oil, destructive distillation, punch and grind processing, promptly get zirconium white matter 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 nitrate-resin-alcohol mixed solution is: 16～21 parts of zirconium nitrate powders, 13～15 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 60～65 parts of absolute ethyl alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density>=the 4.67g/cm of the prepared zirconium white matter of present embodiment slide plate
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 zirconium white matter 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 nitrate-resin-alcohol mixed solution of 20～25 parts of quality 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, is 1600～1650 ℃ at firing temperature and burns till.Burn till after immersion oil, destructive distillation, punch and grind processing, promptly get zirconium white matter 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 by mass ratio, processes through wet ball grinding and mist projection granulating; The preparation method of zirconium nitrate-resin-alcohol mixed solution is: 18～23 parts of zirconium nitrate powders, 15～17 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 65～70 parts of absolute ethyl alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density>=the 4.68g/cm of the prepared zirconium white matter of present embodiment slide plate
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 zirconium white matter 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 nitrate-resin-alcohol mixed solution of 17～22 parts of quality 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, is 1550～1600 ℃ at firing temperature and burns till.Burn till after immersion oil, destructive distillation, punch and grind processing, promptly get zirconium white matter 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 by mass ratio, processes through wet ball grinding and mist projection granulating; The preparation method of zirconium nitrate-resin-alcohol mixed solution is: 20～25 parts of zirconium nitrate powders, 16～18 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 62～67 parts of absolute ethyl alcohols successively, stirred 2～4 hours at 40～60 ℃.
Volume density>=the 4.65g/cm of the prepared zirconium white matter of present embodiment slide plate
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 nitrate-resin-alcohol mixed solution, has guaranteed zirconium nitrate and the liquid phenolic resin dispersing uniformity in raw material.In sintering process, zirconium nitrate can be decomposed to form primary particle size and be merely 20～100nm zirconium white, and its activity is very high, and the sintering of promotes oxidn 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 suppressed growing up unusually of in sintering process zirconium white crystal grain effectively, helps improving the breaking tenacity of material; Meanwhile, a part of resin carbon gets in the zirconia crystal lattice and makes monoclinic zirconia be transformed into stable tetragonal zircite, has improved the volume stability of material in the high temperature use.The increase of breaking tenacity and volume stability all helps improving the thermal shock resistance of material.
Therefore, zirconium white matter slide plate of the present invention has breaking tenacity height, 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 (6)
1. the preparation method of a zirconium white matter slide plate is characterized in that: the zirconium white micro mist granulation material of 100 parts of quality and the zirconium nitrate-resin-alcohol mixed solution of 15～25 parts of quality 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 after immersion oil, destructive distillation, punch and grind processing, promptly get zirconium white matter slide plate.
2. the preparation method of zirconium white matter 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 zirconium white matter slide plate according to claim 1; The preparation method who it is characterized in that described zirconium nitrate-resin-alcohol mixed solution is: 15～25 parts of zirconium nitrate powders, 12～18 parts of heat-reactive phenolic resins and 1～2 part of hexamethylenetetramine are joined in 60～70 parts of absolute ethyl alcohols successively, stirred 2～4 hours at 40～60 ℃.
4. the preparation method of zirconium white matter slide plate according to claim 1 is characterized in that the described isostatic pressing that is shaped to.
5. the preparation method of zirconium white matter slide plate according to claim 1; It is characterized in that the described process system that burns till is: rise to 1050 ℃ from room temperature with 1.0～1.6 ℃/minute speed; 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; Reduce to 1250 ℃ with 0.8～1.2 ℃/minute speed from firing temperature, reduce to 1050 ℃ from 1250 ℃ with 0.2～0.5 ℃/minute speed; Reduce to room temperature with≤1.0 ℃/minute speed from 1050 ℃.
6. according to the prepared zirconium white matter slide plate of preparation method of each described zirconium white matter slide plate in the claim 1～5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643099A (en) * | 2012-05-15 | 2012-08-22 | 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 |
| CN113698202A (en) * | 2021-08-30 | 2021-11-26 | 中科南京绿色制造产业创新研究院 | Water gap and preparation method and application thereof |
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|---|---|---|---|---|
| JPH06219829A (en) * | 1993-01-28 | 1994-08-09 | Shinagawa Refract Co Ltd | Carbon-containing refractory |
| 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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2011
- 2011-09-13 CN CN 201110269635 patent/CN102424592B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06219829A (en) * | 1993-01-28 | 1994-08-09 | Shinagawa Refract Co Ltd | Carbon-containing refractory |
| 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 (1)
| Title |
|---|
| 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》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643099A (en) * | 2012-05-15 | 2012-08-22 | 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 |
| CN113698202A (en) * | 2021-08-30 | 2021-11-26 | 中科南京绿色制造产业创新研究院 | Water gap and preparation method and application thereof |
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| CN102424592B (en) | 2013-03-06 |
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