CN107162590A - A kind of method that electric smelting method produces magnesium stabilised zirconia - Google Patents
A kind of method that electric smelting method produces magnesium stabilised zirconia Download PDFInfo
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- CN107162590A CN107162590A CN201710376681.5A CN201710376681A CN107162590A CN 107162590 A CN107162590 A CN 107162590A CN 201710376681 A CN201710376681 A CN 201710376681A CN 107162590 A CN107162590 A CN 107162590A
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Abstract
The present invention relates to a kind of method that electric smelting method produces magnesium stabilised zirconia, including：Step S1, zirconium oxide and carbon reducing agent refined in electric arc furnaces after desiliconization, then add magnesium stabilizer and reacted；After the completion of step S2, reaction, lifting electrode is at the top of molten bath, then adds into stove and to add magnesium stabilizer after zirconium oxide, zirconium melting to be oxidized and reacted；Step S3, n step S2 is repeated, the safety line with bath surface no more than stove inner top is highly advisable；After the completion of step S4, melting, with the molten surface that sticks together of magnesium stabilizer covering furnace high-temperature, insulation more than 120h comes out of the stove.Magnesium-based stabilised zirconia is produced using the inventive method, single furnace output can be not only lifted, production cost is reduced, and the sufficiently large product of crystal growth can be obtained.Product grains are big, and crystal boundary is few, and the probability that harmful constituent phases are generated between crystal boundary is reduced, and product quality is stable.
Description
Technical field
The present invention relates to technical field of inorganic material, the method that specifically a kind of electric smelting method produces magnesium stabilised zirconia.
Background technology
The preparation method of magnesium-based stabilised zirconia mainly has a sintering process and electric smelting method, and current fire resisting material field is with magnesium stabilised zirconia master
Will be based on the production of two step electric smelting methods.Two step electric smelting methods produce magnesium stabilised zirconia, i.e., first melt out oxidation with desiliconization in zircon sand stove
After zirconium, then stabilizer is added with zirconium oxide to carry out secondary smelting generation stable type zirconium oxide.Because zirconium oxide have monocline, four directions and cube
Three kinds of crystalline phases, zirconium oxide is with the opposite Tetragonal of rise monocline, the cubic phase transition of temperature, with the reduction cubic phase oxygen of temperature
Change zirconium again gradually to Tetragonal and monocline phase in version.Warm change process is accompanied by bulk effect simultaneously, so monocline phase oxidation
Zirconium can not be manufactured into product and use, it is necessary to introduce appropriate stabilizer.The production method of current industry magnesium-based stabilised zirconia it is main with
Based on electric smelting method, its product is used widely in the fields such as structural ceramics, function ceramics, but in some function ceramics neck
Domain, is such as used for the stable Zr refractory material of magnesium of metallurgical continuous casting, and the index such as its corrosion resistance and service life also has larger carry
Between lift-off.The defect of magnesium stabilised zirconia generally existing in the market is that material grains are small, and crystal boundary is more, and impurity is formed between crystal boundary
Evil phase, ultimately results in that product cold strength is poor, consistency is relatively low, and heat endurance fluctuation is big, it is impossible to the industry pair such as satisfaction metallurgy, chemical industry
The requirement of the material index of magnesium-based stabilised zirconia.
The content of the invention
In order to overcome the defect of above-mentioned prior art, the technical problems to be solved by the invention are to provide a kind of electric smelting method life
The method for producing magnesium stabilised zirconia, can be produced using this method and obtain the sufficiently large magnesium-based stabilised zirconia of crystal growth, and product grains are big,
Crystal boundary is few, and the harmful constituent phases generated between crystal boundary are reduced, and the cold strength of product is good, and consistency is effectively lifted, and heat endurance is good, energy
Effectively meet the requirements of the industry to the material index of magnesium-based stabilised zirconia such as metallurgy, chemical industry.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of method that electric smelting method produces magnesium stabilised zirconia, comprises the following steps：
Step S1, zirconium oxide and carbon reducing agent refined in electric arc furnaces after desiliconization, then add magnesium stabilizer
Reacted；
After the completion of step S2, reaction, at the top of lifting electrode to molten bath, then the addition zirconium oxide continuation melting into stove, treat oxygen
Magnesium stabilizer is added after change zirconium melting to be reacted；
Step S3, n step S2 is repeated, n is more than or equal to 1, and the safety of stove inner top is no more than with bath surface
Line is highly advisable；
After the completion of step S4, melting, with the molten surface that sticks together of magnesium stabilizer covering furnace high-temperature, insulation more than 120h comes out of the stove.
The beneficial effects of the present invention are：Magnesium-based stabilised zirconia is produced using the inventive method, single stove production can be not only lifted
Amount, reduces production cost, and can obtain the sufficiently large product of crystal growth.Product grains are big, and crystal boundary is few, between crystal boundary
The probability of the harmful constituent phases of generation is reduced, and example 1 and the legend of example 2 are shown in the detection of product crystalline phase, and product quality is stable.Meanwhile, this
The product that technique productions go out is by detecting that cold conditions compression strength reaches 150-170MPa, and real density is 5.85-6.0g/cm3, cold strong
Spend, consistency is effectively lifted, heat endurance is good, can effectively meet the industries such as metallurgy, chemical industry and the material of magnesium-based stabilised zirconia is referred to
Target requirement, has further promoted electric smelting method to prepare the development of high-quality magnesium-based stabilised zirconia technology.
Brief description of the drawings
Fig. 1 schemes for the magnesium-based stabilised zirconia crystalline phase detection of the embodiment 1 of the specific embodiment of the invention；
Fig. 2 schemes for the magnesium-based stabilised zirconia crystalline phase detection of the embodiment 2 of the specific embodiment of the invention.
Embodiment
To describe technology contents, the objects and the effects of the present invention in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is：Single stove melting in batches is carried out using electrode ascending manner segmentation melting technique,
After the completion of lower floor's melting, zirconium oxide is added at the top of lifting electrode to molten bath and magnesium stabilizer carries out upper strata melting, upper strata is utilized
Stick together molten to lower floor of melt is incubated, and promotes the molten crystal sticked together of lower floor to grow up, reduces the formation of grain boundary impurities phase.After melting terminates
Sticked together surface with the high temperature melting in magnesium stabilizer powder covering stove, is incubated the molten top that sticks together, it is ensured that the crystal at the molten top that sticks together
Have enough growth times, thus produce obtain that coarse grains, crystal boundary be few, magnesium that harmful constituent phases for generating between crystal boundary are few it is stable
Zirconium.
Specifically, the method that the electric smelting method that the present invention is provided produces magnesium stabilised zirconia, comprises the following steps：
Step S1, zirconium oxide and carbon reducing agent refined in electric arc furnaces after desiliconization, then add magnesium stabilizer
Reacted；
After the completion of step S2, reaction, at the top of lifting electrode to molten bath, then the addition zirconium oxide continuation melting into stove, treat oxygen
Magnesium stabilizer is added after change zirconium melting to be reacted；
Step S3, n step S2 is repeated, n is more than or equal to 1, and the safety of stove inner top is no more than with bath surface
Line is highly advisable；
After the completion of step S4, melting, with the molten surface that sticks together of magnesium stabilizer covering furnace high-temperature, insulation more than 120h comes out of the stove.
In aforementioned production method, originally it is incorporated a small amount of carbon reducing agent and carries out desiliconization and refining, can make residual in stove
The oxide impurity such as silicon, aluminium, iron, titanium for staying high temperature reduction is removed, it is to avoid influence of the impurity to product.It is subsequently added magnesium stabilizer
With zirconium oxide react obtaining magnesium stabilised zirconia, take electrode ascending manner to be segmented melting technique and carry out single stove melting in batches, under
After the completion of layer melting, zirconium oxide is added at the top of lifting electrode to molten bath and magnesium stabilizer carries out upper strata melting, upper strata melt pair
Molten stick together of lower floor plays insulation effect, promotes the molten crystal sticked together of lower floor to grow up, and reducing grain boundary impurities, mutually formation is acted on, and is sent while improving
Electrically operated continuity, improves single furnace output, reduces product material consumption.After melting terminates, cover high in stove with magnesium stabilizer powder
Wen Rong sticks together surface, is incubated the molten top that sticks together, the cooling velocity at the molten top that sticks together of reduction, it is ensured that the molten crystal for sticking together top has enough
Growth time.
In aforementioned production method, magnesium stabilizer is added after oxidation zirconium melting, it is possible to prevente effectively from magnesium stabilizer is direct
Contacted with the carbon such as electrode, prevent magnesium stabilizer from being consumed by the element reduction of the charcoals such as electrode.
It was found from foregoing description, the beneficial effects of the present invention are：Magnesium-based stabilised zirconia is produced using the inventive method, not only
Single furnace output can be lifted, production cost is reduced, and the sufficiently large product of crystal growth can be obtained.Product grains
Greatly, crystal boundary is few, and the probability that harmful constituent phases are generated between crystal boundary is reduced, and product quality is stable.Meanwhile, the product that this technique productions goes out
Cold strength is good, and consistency is effectively lifted, and heat endurance is good, can effectively meet material of the industries such as metallurgy, chemical industry to magnesium-based stabilised zirconia
Expect the requirement of index, further promote electric smelting method to prepare the development of high-quality magnesium-based stabilised zirconia technology.
Further, in step sl, voltage of the electric arc furnaces in refining is 160~260V, and electric current is 5~13KA.
Further, in step sl, refining time is 10~40min, to control in stove melt as micro-oxygenation atmosphere,
Then magnesium stabilizer is added to be reacted.
It was found from foregoing description, the beneficial effects of the present invention are：Regulate and control stove in melt be micro-oxygenation atmosphere after again plus
Enter magnesium stabilizer and carry out stabilization reactions, can effectively reduce the loss of the charcoals such as magnesium stabilizer and electrode element reaction.
Further, the reaction time of magnesium stabilizer and zirconium oxide is 5~15min.
Further, the zirconium oxide is grade >=99wt% high-purity electric-melting zirconia, and the carbon reducing agent is selected from
The weight ratio of one or more in graphite electrode, petroleum coke, pitch coke and charcoal, zirconium oxide and carbon reducing agent is zirconium oxide
: carbon reducing agent=45~90: 1.
Further, the amount of allocating of the magnesium stabilizer is the 2.75%~3.75% of zirconium oxide weight.
Further, in step s 2, after at the top of slow lifting electrode to molten bath, the power of reduction electrode makes the top in molten bath
Portion maintains melting zone, and zirconium to be oxidized is promoted to former power and carries out melting again after adding.
It was found from foregoing description, the beneficial effects of the present invention are：After at the top of slow lifting electrode to molten bath, electrode is reduced
Power molten bath is only maintained melting zone at top, on the one hand can make molten bath other parts carry out Slow cooling crystallization, prolong
The growth time of long crystal, promotes crystal to grow up, and the melting zone kept at the top of another aspect molten bath, which can also be prevented effectively from, to be occurred
Stream, break equal problem and the secondary starting the arc.
Further, one or more of the magnesium stabilizer in electrically molten magnesia, magnesium hydroxide and magnesite.
Embodiment 1
1st, by zirconium oxide and graphite electrode in mass ratio 86:1 ratio is added in electric arc furnaces after mixing and carried out after desilication reaction,
Booster tension refines 11min to 220V, to regulate and control in stove melt as oxidizing atmosphere；
2 and then percent mass ratio is added into furnace high-temperature melt proceed high temperature for 3.2% electrically molten magnesia
Melting 6min, makes electrically molten magnesia fully fuse stabilization with zirconium oxide；
3rd, at the top of slow lifting electrode to molten bath, zonule melting at the top of molten bath is kept with small-power, thing is added into stove
The zirconia material first got ready, hoisting power carries out high melt；
4th, the electrically molten magnesia for adding 3.2% ratio after zirconium melting to be oxidized into furnace high-temperature melt proceeds high temperature
Melting 8min；
5th, repeated as described in step 3, until bath surface is close to stove inner top safety line height, power-off stops molten
Refining；
6th, upgrade after electrode, rapidly spread preprepared electrically molten magnesia powder into the molten surface that sticks together of furnace high-temperature,
Sticked together with being incubated to allow melt in stove with stove Slow cooling；
7th, come out of the stove after furnace cooling 150h, obtain magnesium-based stabilised zirconia product, detection product cold conditions compression strength reaches
164MPa, real density is 5.93g/cm3Product crystalline phase detects See Figure 1.
Embodiment 2
1st, by zirconium oxide and graphite electrode in mass ratio 78:1 ratio is added in electric arc furnaces after mixing and carried out after desilication reaction,
Booster tension refines 20min to 240V, to regulate and control in stove melt as oxidizing atmosphere；
2 and then percent mass ratio is added into furnace high-temperature melt proceed high temperature melting for 3.6% magnesium hydroxide
5min is refined, magnesium hydroxide is fully fused stabilization with zirconium oxide；
3rd, at the top of slow lifting electrode to molten bath, molten bath top section melting zone is kept with small-power, is added into stove prior
The zirconium dioxide raw material got ready, hoisting power carries out high melt；
4th, the magnesium hydroxide for adding 3.5% ratio after zirconium melting to be oxidized into furnace high-temperature melt proceeds high temperature melting
Refine 6.5min；
5th, repeated as described in step 3, until bath surface is close to stove inner top safety line height, power-off stops molten
Refining；
6th, upgrade after electrode, rapidly spread preprepared magnesium hydroxide powder into the molten surface that sticks together of furnace high-temperature, with
Insulation allows melt and sticked together in stove with stove Slow cooling；
7th, come out of the stove after furnace cooling 130h, obtain magnesium-based stabilised zirconia product.Detection product cold conditions compression strength reaches
158MPa, real density is 5.86g/cm3Fig. 2 is shown in the detection of product crystalline phase.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalents that bright specification and accompanying drawing content are made, or the technical field of correlation is directly or indirectly used in, similarly include
In the scope of patent protection of the present invention.
Claims (8)
1. a kind of method that electric smelting method produces magnesium stabilised zirconia, it is characterised in that comprise the following steps：
Step S1, zirconium oxide and carbon reducing agent refined in electric arc furnaces after desiliconization, then add magnesium stabilizer and carry out
Reaction；
After the completion of step S2, reaction, at the top of lifting electrode to molten bath, then the continuation melting of addition zirconium oxide, zirconium to be oxidized into stove
Magnesium stabilizer is added after fusing to be reacted；
Step S3, n step S2 is repeated, n is more than or equal to 1, high no more than the safety line of stove inner top with bath surface
Degree is advisable；
After the completion of step S4, melting, with the molten surface that sticks together of magnesium stabilizer covering furnace high-temperature, insulation more than 120h comes out of the stove.
2. the method that electric smelting method according to claim 1 produces magnesium stabilised zirconia, it is characterised in that：In step sl, electric arc
Voltage of the stove in refining is 160~260V, and electric current is 5~13KA.
3. the method that electric smelting method according to claim 1 produces magnesium stabilised zirconia, it is characterised in that：In step sl, refine
Time is 10~40min, to control melt in stove as micro-oxygenation atmosphere, then to add magnesium stabilizer and reacted.
4. the method that electric smelting method according to claim 1 produces magnesium stabilised zirconia, it is characterised in that：Magnesium stabilizer and zirconium oxide
Reaction time be 5~15min.
5. the method that electric smelting method according to claim 1 produces magnesium stabilised zirconia, it is characterised in that：The zirconium oxide is grade
>=99wt% high-purity electric-melting zirconia, the carbon reducing agent in graphite electrode, petroleum coke, pitch coke and charcoal one
Plant or a variety of, the weight ratio of zirconium oxide and carbon reducing agent is zirconium oxide: carbon reducing agent=45~90: 1.
6. the method that electric smelting method according to claim 1 produces magnesium stabilised zirconia, it is characterised in that：The magnesium stabilizer is matched somebody with somebody
It is the 2.75%~3.75% of zirconium oxide weight to enter amount.
7. the method that electric smelting method according to claim 1 produces magnesium stabilised zirconia, it is characterised in that：In step s 2, lifted
After at the top of electrode to molten bath, the power of reduction electrode makes to maintain melting zone at the top of molten bath, and zirconium to be oxidized is promoted to again after adding
Former power carries out melting.
8. the method that electric smelting method according to claim 1 produces magnesium stabilised zirconia, it is characterised in that：The magnesium stabilizer is selected from
One or more in electrically molten magnesia, magnesium hydroxide and magnesite.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110961570A (en) * | 2019-12-31 | 2020-04-07 | 三祥新材股份有限公司 | Preparation method of zirconium oxide composite spray coating for metal mold casting |
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| CN1456532A (en) * | 2002-09-28 | 2003-11-19 | 郑州振中电熔锆业有限公司 | Calcium stabilizing zircon alba and electric melting producing method thereof |
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2017
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|---|---|---|---|---|
| CN1456532A (en) * | 2002-09-28 | 2003-11-19 | 郑州振中电熔锆业有限公司 | Calcium stabilizing zircon alba and electric melting producing method thereof |
| CN101622209A (en) * | 2007-02-28 | 2010-01-06 | 耐火材料知识产权有限两合公司 | Fireproof fusion-cast goods |
Non-Patent Citations (3)
| Title |
|---|
| XU JIAYUE等: "Industrial growth of yttria-stabilized cubic zirconia crystals by skull melting process", 《JOURNAL OF RARE EARTHS》 * |
| 林振汉: "电熔氧化锆的发展、技术、应用和展望", 《钛工业进展》 * |
| 郭海珠等: "《实用耐火材料手册》", 30 September 2000, 中国建材工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110961570A (en) * | 2019-12-31 | 2020-04-07 | 三祥新材股份有限公司 | Preparation method of zirconium oxide composite spray coating for metal mold casting |
| CN110961570B (en) * | 2019-12-31 | 2021-05-25 | 三祥新材股份有限公司 | Preparation method of zirconium oxide composite spray coating for metal mold casting |
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Application publication date: 20170915 |