CN103979980A - Preparation method of zirconia metering nozzle - Google Patents
Preparation method of zirconia metering nozzle Download PDFInfo
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- CN103979980A CN103979980A CN201410190638.6A CN201410190638A CN103979980A CN 103979980 A CN103979980 A CN 103979980A CN 201410190638 A CN201410190638 A CN 201410190638A CN 103979980 A CN103979980 A CN 103979980A
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Abstract
The invention discloses a making method of a zirconia metering nozzle. The method comprises the following steps: mixing magnesium oxide partially-stabilized zirconia aggregates with co-milled fine powder composed of monoclinic zirconia and magnesium oxide, adding a zirconia gel binder, mixing, ageing, molding, sintering in an electrical kiln, controlling the concentration of magnesium oxide in the co-milled fine powder to make the concentration of magnesium oxide 0.2-0.5% higher than the content of magnesium oxide in the aggregates, and reacting in the sintering process of the monoclinic zirconia in the co-milled fine powder to partially form stable zirconia; controlling the precipitation of magnesium oxide in the aggregates by utilizing a concentration difference; and mixing the aggregates with the co-milled powder according to a certain ratio, adding a proper amount of the zirconia gel binder, carrying out compression molding, drying at 100-110DEG C for 24h, and sintering at 1710-1720DEG C to make the zirconia metering nozzle with the service life reaching above 34h. A result of microscopic structure analysis of a used residual sample shows that the stabilizer precipitation quantity is extremely small, and the phase transition rupture of zirconia particles does not appear basically.
Description
Technical field
The present invention relates to about casting tundish in ferrous metallurgical industry continuously with controlling the preparation of functional refractory for the device of molten steel flow, specifically a kind of preparation method of zirconium oxide metering nozzle.
Background technology
Metering nozzle refers to the functional device of a kind of high-temperature structural ceramics making that is arranged on continuous casting tundish bottom.Its Main Function is that Metal in Tundish static pressure remains unchanged substantially, and molten steel flows into crystallizer by metering nozzle, and crystallizer is by large flow water-cooled, and liberated heat while taking away solidification of molten steel, makes molten steel solidification become base.Because the heat that crystallizer water-cooled is taken away is limited, thereby the molten steel quantity that flows into crystallizer in the unit time must be within limits.The aperture of metering nozzle is larger, and the unit time flows into crystallizer molten steel quantity the more, selects suitable aperture to make tundish water nozzle, is metering nozzle.The major cause that metering nozzle lost efficacy is owing to reacting with the stablizer in zirconium white in MOLTEN STEEL FLOW process, stablizer precipitation, and then cause zirconium white unstability, particle is made an exception, intensity significantly reduces, scour resistance declines and causes hole enlargement, and the molten steel solidification liberated heat that makes to flow into crystallizer is greater than the heat that crystallizer water coolant can take away and exits use.
In zirconium oxide metering nozzle, zirconic content (wt%) is generally 95% left and right, and be about 10 hours actual service life.Work-ing life, short major cause was Zirconia-stabilized dose of precipitation, other elements in stablizer and steel, slag form low melting point eutectic, eutectic runs off, zirconium white unstability, breakage of particles, intensity significantly reduces, and scour resistance declines and causes hole enlargement, thereby causes zirconium oxide metering nozzle short work-ing life.
Summary of the invention
The object of the invention is to, a kind of zirconium oxide metering nozzle novel preparation method is provided, stop the zirconia particles stablizer precipitation of preconditioning by additive, metering nozzle sintering process mesostroma part additive and monoclinic zirconia form new stable phase, performance has exceeded all by the performance of the prepared metering nozzle of PSZ, and can reach more than 30 hours work-ing life.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of preparation method of zirconia metering nozzle, it is characterized in that, the method is taking magnesia partial stabilized zirconia as aggregate, be equipped with the common pulverized powder of monoclinic zirconia and magnesium oxide composition, add zirconium white gel bonding agent, through mixing, ageing mixture aftershaping, then in electrical kiln, burn till, specifically carry out according to the following step:
1) the common abrasive dust preparation of monoclinic zirconia micro mist and fine magnesium oxide micro-powder
Pulverized powder adopts monoclinic zirconia and fine magnesium oxide micro-powder altogether, wherein:
The size composition of monoclinic zirconia is: d
50=0.8～0.9 μ m, d
90< 4.0 μ m;
The size composition of fine magnesium oxide micro-powder is: d
50=0.3～0.5 μ m, d
90< 2.0 μ m;
In the weight percent composition of monoclinic zirconia micro mist chemistry, ZrO
2+ HfO
2> 99%, SiO
2< 0.1%;
In the chemical weight percent composition of fine magnesium oxide micro-powder, MgO > 99%, SiO
2< 0.2%;
According to monoclinic zirconia micro mist: fine magnesium oxide micro-powder=(97.1～96.8): (2.9～3.2) are made into common pulverized powder, monoclinic zirconia and magnesian ratio must ensure that in common abrasive dust, magnesian content is greater than content of magnesia in aggregate, are controlled at magnesian content in common abrasive dust and are greater than content of magnesia 0.2～0.5% in aggregate; Pulverized powder packs in polyurethane ball-milling pot altogether, adopts zirconium oxide porcelain ball, grinds altogether 24 hours, and monoclinic zirconia and magnesium oxide are fully mixed;
2) press aggregate: pulverized powder=45:55 prepares burden altogether, add the zirconium white gel bonding agent of the total amount 8% of preparing burden, mixing 45 minutes, the pug ageing mixture mixing 24 hours, then adopted the moulding of 150t hydropress;
3) the base substrate seasoning after moulding is after 24 hours, then in 105 ± 5 DEG C of baking ovens dry 24 hours again; Dry rear qualified base substrate is incubated 6 hours and burns till in the electrical kiln of 1710～1720 DEG C, makes zirconium oxide metering nozzle.
Zirconium oxide metering nozzle performance prepared by the present invention has exceeded all by the performance of the prepared metering nozzle of PSZ, and can reach more than 34 hours work-ing life.Show that by rear residual sample microstructure analysis stablizer precipitation quantity is few, zirconia particles breaks without phase transformation substantially.
Brief description of the drawings
Fig. 1 is preparation technology's schema of metering nozzle of the present invention.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment
2003, applicant (Xi'an University of Architecture and Technology) has born industry in Shaanxi province brainstorm project " exploitation of baddeleyite corundum eutectoid fine crystallization pyroceramic " (item number 2003K07-G9), and the Xi'an City, Shanxi Province of bearing industry brainstorm project " the compound disperse corundum of zirconium white phase Special high-temperature pottery (numbering GG200347) "; Within 2010, bear Jinan Quan Cheng scholar's construction project " ZrO
2/ Al
2o
3the research of composite diphase material and the application in continuous casting functional material ", applicant's contriver obtains Jinan " spring city scholar " honorary title; 2013, on previous research work basis, bear state natural sciences fund general project " zirconia metering nozzle stablizer precipitation breakage of particles mechanism and life-span are improved research " (item number 51372193).Damage mechanism and improve work-ing life according to born project research zirconium oxide metering nozzle, achievement in research shows, the main process of zirconium oxide metering nozzle damage is that stabilizer magnesium oxide in semi-stability zirconium white is because its activity is high, in use first react with the composition in molten steel or slag and form eutectic loss, after stabilized magnesium hydroxide agent precipitation in zirconium white, zirconium white undergoes phase transition, crack, zirconia particles breaks, macrobead division becomes many small-particles, zirconia metering nozzle intensity significantly declines, the performance of flushing of anti-molten steel and slag declines, small-particle washes away loss, cause metering nozzle hole enlargement to roll off the production line, therefore designed inhibition stabilizing zirconia stablizer New technology for desolventizing hot.
The preparation method of zirconia metering nozzle of the present invention, taking magnesia partial stabilized zirconia as aggregate, is equipped with the common pulverized powder of monoclinic zirconia and magnesium oxide composition, add zirconium white gel bonding agent, through mixing, ageing mixture aftershaping, then in electrical kiln, burn till, specifically carry out according to the following step:
1) choosing of PSZ aggregate
Available PSZ has the yttrium partially stabilized zirconium white of oxidation, magnesia partial stabilized zirconia, calcium oxide PSZ and magnesium oxide calcium oxide composite portion stabilizing zirconia in the market.In the present embodiment, aggregate adopts magnesia partial stabilized zirconia, and the chemical constitution of the magnesia partial stabilized zirconia aggregate of purchasing is (wt%): ZrO
2=95.12, HfO
2=2.14, MgO=2.69, CaO=0.02, Al
2o
3=0.03.
2) the common pulverized powder preparation of monoclinic zirconia micro mist and fine magnesium oxide micro-powder
Pulverized powder adopts monoclinic zirconia and fine magnesium oxide micro-powder altogether, wherein:
The size composition of monoclinic zirconia is: d
50=0.8～0.9 μ m, d
90< 4.0 μ m;
The size composition of fine magnesium oxide micro-powder is: d
50=0.3～0.5 μ m, d
90< 2.0 μ m;
Monoclinic zirconia micro mist chemical constitution (wt%): ZrO
2+ HfO
2> 99, SiO
2< 0.1;
The chemical constitution (wt%) of fine magnesium oxide micro-powder: MgO > 99, SiO
2< 0.2.
According to monoclinic zirconia micro mist: fine magnesium oxide micro-powder=(97.1～96.8): (2.9～3.2) (mass ratio) carries out accurate weighing and be made into common pulverized powder, pulverized powder packs in polyurethane ball-milling pot altogether, adopt zirconium oxide porcelain ball, grind altogether 24 hours, ensure that monoclinic zirconia micro mist and fine magnesium oxide micro-powder fully mix.
Monoclinic zirconia and magnesian ratio must ensure that in common abrasive dust, magnesian content is greater than content of magnesia in aggregate, general control magnesian content in common abrasive dust be greater than aggregate in content of magnesia 0.2～0.5%.By this composition configuration, at the initial stage of burning till, in pulverized powder, magnesium oxide does not also form sosoloid with monoclinic zirconia altogether, and the magnesium oxide concentration in pulverized powder is much larger than the magnesium oxide concentration of aggregate altogether, and the magnesium oxide in aggregate can precipitation.Along with firing temperature raising and the prolongation of time, in pulverized powder, the solid solution of part magnesium oxide is in monoclinic zirconia altogether, and part forms stabilizing zirconia.Reach after firing temperature, the stabilizing zirconia quantity forming in pulverized powder altogether reaches maximum value.
In process of cooling, precipitation is wanted in stabilized magnesium hydroxide agent theoretically, but altogether the magnesium oxide concentration in pulverized powder is greater than the magnesium oxide concentration of aggregate, and therefore, the magnesium oxide in aggregate can precipitation.In the stabilizing zirconia process of cooling forming in pulverized powder altogether, owing to there being free magnesium, magnesian precipitation is difficult to carry out.Do not form the monoclinic zirconia of sosoloid, change tetragonal zircite when high temperature into, in process of cooling, undergo phase transition, change monoclinic zirconia into, produce volume effect, matrix part produces the tiny crack that can control the size; Tiny crack have a raising that is beneficial to metering nozzle toughness and thermal shock resistance, can prevent that the problem of bursting of watering from appearring opening in metering nozzle.
3) preparation of zirconium white gel bonding agent
Get by weight percentage ZrOCl
2.8H
2o prepares mother liquor, in mother liquor, and ZrOCl
2.8H
2the concentration of O is 0.5～2.0Mol/L, adds the dispersion agent PEG of mother liquor gross weight 1.2%, NH
4(OH) positive titration, is stirred to pH=7～10, makes gel, gel ageing 9h～16h, and-0.095MPa vacuum suction filter, deionized water wash to Silver Nitrate can't detect Cl
-till, as zirconium white gel bonding agent.
4) press aggregate: pulverized powder=45:55 prepares burden altogether, add the zirconium white gel bonding agent of the total amount 8% of preparing burden, mixing 45 minutes.The pug ageing mixture mixing 24 hours, then adopts the moulding of 150t hydropress;
Base substrate seasoning after moulding is after 24 hours, in the baking oven of 105 ± 5 DEG C dry 24 hours, dry after qualified base substrate in electrical kiln, at 1710 DEG C～1720 DEG C temperature, be incubated to burn till for 6 hours and make zirconium oxide metering nozzle.
Below the embodiment that contriver provides.
Embodiment 1:
Step 1, the chemical constitution of choosing magnesia partial stabilized zirconia aggregate is (wt%): ZrO
2=95.12, HfO
2=2.14, MgO=2.69, CaO=0.02, Al
2o
3=0.03; Size composition is 0～0.5mm.
Monoclinic zirconia micro mist chemical constitution (wt%): ZrO
2+ HfO
2=99.5, SiO
2=0.07, Fe
2o
3=0.01, surplus is impurity;
The chemical constitution (wt%) of fine magnesium oxide micro-powder: MgO=99.0, SiO
2=0.17, CaO=0.21, Al
2o
3=0.13, surplus is impurity.
The size composition of monoclinic zirconia is: d
50=0.845 μ m, d
90=3.89 μ m;
The size composition of fine magnesium oxide micro-powder is: d
50=0.337 μ m, d
90< 1.975 μ m.
Monoclinic zirconia micro mist by mass percentage: fine magnesium oxide micro-powder=96.8:3.2 batching, batching packs in polyurethane ball-milling pot, adopts zirconium oxide porcelain ball, grinds altogether 24 hours, makes common pulverized powder.
Step 2, gets ZrOCl by weight percentage
2.8H
2o prepares mother liquor, ZrOCl in mother liquor
2.8H
2o concentration is 0.5Mol/L, adds the dispersion agent PEG of mother liquor gross weight 1.2%, NH
4(OH) positive titration, is stirred to PH=7～10, makes gel.Gel ageing 12h ,-0.095MPa vacuum suction filter, deionized water wash to Silver Nitrate can't detect Cl
-till, make zirconium white gel bonding agent.
Step 3, according to mass ratio, aggregate: pulverized powder altogether=45:55 batching.
Get batching 5kg, additional zirconium white gel bonding agent 8%, i.e. 0.40kg, mixing 45 minutes, mixes and makes blank.The blank ageing mixture mixing 24 hours.
Step 4, the blank making packs mould into, and with 150t hydropress, in 150MPa moulding, molding blank seasoning, after 24 hours, is dried 24h under 105 ± 5 DEG C of conditions again, then sintering at 1710 DEG C of temperature, the metering nozzle making can reach 34h its work-ing life.Show that by rear residual sample microstructure analysis stablizer precipitation quantity is few, zirconia particles breaks without phase transformation substantially.
Embodiment 2:
The present embodiment and embodiment 1 difference are: the micro mist of monoclinic zirconia by mass percentage in step 1: fine magnesium oxide micro-powder=97.1:2.9, in the common abrasive dust of i.e. control, in content of magnesia and magnesia partial stabilized zirconia aggregate, magnesian concentration difference is lower value 0.2%, and all the other steps are identical.More than the metering nozzle making can reach 34h its work-ing life.
Embodiment 3:
The present embodiment and embodiment 1 difference are: in step 3, use 150t hydropress after 150MPa mechanical pressing, under 230MPa pressure, adopt again isostatic cool pressing post forming, sintering temperature is adjusted into 1720 DEG C, and the zirconium oxide metering nozzle making can reach 38h its work-ing life.
Claims (3)
1. the preparation method of a zirconia metering nozzle, it is characterized in that, the method is with magnesia partial stabilized zirconia aggregate, be equipped with the common pulverized powder of monoclinic zirconia and magnesium oxide composition, add zirconium white gel bonding agent, through mixing, ageing mixture aftershaping, then in electrical kiln, burn till, specifically carry out according to the following step:
1) the common abrasive dust preparation of monoclinic zirconia micro mist and fine magnesium oxide micro-powder
Pulverized powder adopts monoclinic zirconia and fine magnesium oxide micro-powder altogether, wherein:
The size composition of monoclinic zirconia is: d
50=0.8～0.9 μ m, d
90< 4.0 μ m;
The size composition of fine magnesium oxide micro-powder is: d
50=0.3～0.5 μ m, d
90< 2.0 μ m;
In the weight percent composition of monoclinic zirconia micro mist chemistry, ZrO
2+ HfO
2> 99%, SiO
2< 0.1%;
In the chemical weight percent composition of fine magnesium oxide micro-powder, MgO > 99%, SiO
2< 0.2%;
According to monoclinic zirconia micro mist: fine magnesium oxide micro-powder=(97.1～96.8): (2.9～3.2) are made into common pulverized powder, monoclinic zirconia and magnesian mass ratio will ensure that in common abrasive dust, magnesian content is greater than content of magnesia in aggregate, are controlled at magnesian content in common abrasive dust and are greater than content of magnesia 0.2～0.5% in aggregate; Pulverized powder packs in polyurethane ball-milling pot altogether, adopts zirconium oxide porcelain ball, grinds altogether 24 hours, and monoclinic zirconia and magnesium oxide are fully mixed;
2) press aggregate: pulverized powder=45:55 prepares burden altogether, add the zirconium white gel bonding agent of the total amount 8% of preparing burden, mixing 45 minutes, the pug ageing mixture mixing 24 hours, then adopted the moulding of 150t hydropress;
3) the base substrate seasoning after moulding is after 24 hours, then in 105 ± 5 DEG C of baking ovens dry 24 hours again; After dry, qualified base substrate is incubated 6 hours and burns till and makes zirconium oxide metering nozzle in the electrical kiln of 1710～1720 DEG C.
2. the method for claim 1, is characterized in that, the chemical constitution weight percent of described magnesia partial stabilized zirconia aggregate is: ZrO
2: 95.12%, HfO
2: 2.14%, MgO:2.69%, CaO:0.02%, Al
2o
3: 0.03%.
3. the method for claim 1, is characterized in that, the preparation method of described zirconium white gel bonding agent is:
Get by weight percentage ZrOCl
2.8H
2o prepares mother liquor, the ZrOCl in mother liquor
2.8H
2o concentration is 0.5～2.0Mol/L, adds the dispersion agent PEG of mother liquor gross weight 1.2%, NH
4(OH) positive titration, is stirred to pH=7～10, makes gel; Gel ageing 9h～16h ,-0.095MPa vacuum suction filter, deionized water wash to Silver Nitrate can't detect Cl
-till, obtain zirconium white gel bonding agent.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936442A (en) * | 2014-04-02 | 2014-07-23 | 上海宝威陶瓷新材料有限公司 | Composition and preparation method of magnesium-yttrium-calcium compound stabilized zirconia nozzle brick |
| CN104446560A (en) * | 2014-12-05 | 2015-03-25 | 三祥新材股份有限公司 | Preparation method of zirconium oxide nozzle brick |
| CN104671808A (en) * | 2015-01-27 | 2015-06-03 | 江苏泰瑞耐火有限公司 | ZrO2 metering nozzle and preparation method thereof |
| CN104876596A (en) * | 2015-04-21 | 2015-09-02 | 西安建筑科技大学 | Preparation method and equipment of zirconia metering nozzle |
| CN105418096A (en) * | 2015-12-01 | 2016-03-23 | 浙江铁狮高温材料有限公司 | Self-adaptive zirconium oxide tundish nozzle |
| CN105503208A (en) * | 2015-12-15 | 2016-04-20 | 西安建筑科技大学 | Method for preparing sizing nozzle with compound gel stabilizing zirconium oxide as matrix |
| CN106007743A (en) * | 2016-05-13 | 2016-10-12 | 西安建筑科技大学 | Method for preparing zirconium oxide metering nozzle |
| CN109160819A (en) * | 2018-08-07 | 2019-01-08 | 北京中冶设备研究设计总院有限公司 | A kind of preparation method of weakly acidic pH elevated-temperature seal binder |
| CN109503180A (en) * | 2018-12-07 | 2019-03-22 | 深圳市万泽中南研究院有限公司 | A kind of composite ceramic powder, flow-guiding mouth and preparation method thereof |
| CN111482589A (en) * | 2020-04-28 | 2020-08-04 | 宋振亚 | Manufacturing method of long-life fixed diameter water gap |
| CN115010486A (en) * | 2022-07-14 | 2022-09-06 | 中钢集团洛阳耐火材料研究院有限公司 | Near-net-shape preparation method of high-purity zirconia refractory ceramic |
| CN115231931A (en) * | 2022-07-20 | 2022-10-25 | 郑州振中电熔新材料有限公司 | Method for manufacturing high-quality zirconia water gap by using magnesium-zirconium eutectic material and monoclinic zirconia |
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| CN103936442A (en) * | 2014-04-02 | 2014-07-23 | 上海宝威陶瓷新材料有限公司 | Composition and preparation method of magnesium-yttrium-calcium compound stabilized zirconia nozzle brick |
| CN104446560A (en) * | 2014-12-05 | 2015-03-25 | 三祥新材股份有限公司 | Preparation method of zirconium oxide nozzle brick |
| CN104671808A (en) * | 2015-01-27 | 2015-06-03 | 江苏泰瑞耐火有限公司 | ZrO2 metering nozzle and preparation method thereof |
| CN104876596A (en) * | 2015-04-21 | 2015-09-02 | 西安建筑科技大学 | Preparation method and equipment of zirconia metering nozzle |
| CN105418096A (en) * | 2015-12-01 | 2016-03-23 | 浙江铁狮高温材料有限公司 | Self-adaptive zirconium oxide tundish nozzle |
| CN105503208B (en) * | 2015-12-15 | 2018-04-17 | 西安建筑科技大学 | A kind of method that metering nozzle is prepared using plural gel stabilizing zirconia as matrix |
| CN105503208A (en) * | 2015-12-15 | 2016-04-20 | 西安建筑科技大学 | Method for preparing sizing nozzle with compound gel stabilizing zirconium oxide as matrix |
| CN106007743A (en) * | 2016-05-13 | 2016-10-12 | 西安建筑科技大学 | Method for preparing zirconium oxide metering nozzle |
| CN106007743B (en) * | 2016-05-13 | 2019-01-29 | 西安建筑科技大学 | A kind of preparation method of zirconium oxide metering nozzle |
| CN109160819A (en) * | 2018-08-07 | 2019-01-08 | 北京中冶设备研究设计总院有限公司 | A kind of preparation method of weakly acidic pH elevated-temperature seal binder |
| CN109503180A (en) * | 2018-12-07 | 2019-03-22 | 深圳市万泽中南研究院有限公司 | A kind of composite ceramic powder, flow-guiding mouth and preparation method thereof |
| CN111482589A (en) * | 2020-04-28 | 2020-08-04 | 宋振亚 | Manufacturing method of long-life fixed diameter water gap |
| CN115010486A (en) * | 2022-07-14 | 2022-09-06 | 中钢集团洛阳耐火材料研究院有限公司 | Near-net-shape preparation method of high-purity zirconia refractory ceramic |
| CN115231931A (en) * | 2022-07-20 | 2022-10-25 | 郑州振中电熔新材料有限公司 | Method for manufacturing high-quality zirconia water gap by using magnesium-zirconium eutectic material and monoclinic zirconia |
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