CN101792179B - Production method of electrically melt yttrium oxide stabilized zirconia granulation powder - Google Patents
Production method of electrically melt yttrium oxide stabilized zirconia granulation powder Download PDFInfo
- Publication number
- CN101792179B CN101792179B CN2010101091601A CN201010109160A CN101792179B CN 101792179 B CN101792179 B CN 101792179B CN 2010101091601 A CN2010101091601 A CN 2010101091601A CN 201010109160 A CN201010109160 A CN 201010109160A CN 101792179 B CN101792179 B CN 101792179B
- Authority
- CN
- China
- Prior art keywords
- powder
- electric smelting
- yttrium
- zirconium
- granulation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention discloses a production method of electrically melt yttrium oxide stabilized zirconia granulation powder which is profitable, green and environmentally friendly. The method comprises the following steps: adding zircon sand and Y-doped cubic zirconia powder (or Y-Zr powder) in reducing agent for mixing and electric smelting or directly adding baddeleyite for mixing and electric smelting, cooling, performing coarse crushing and fine crushing, screening, performing coarse grinding and fine grinding, performing wet grinding to generate pulp, performing surface modification, performing spray granulation, mixing evenly and packaging. The method of the invention uses Y-Zr powder as raw material, the technical process is simple and easy, the method does not discharge waste water, waste gas and waste residue; the equipment investment is less, the product quality meets user requirements, the production process does not adopt secondary electric smelting and high-temperature heat treatment and add stabilizing agent; and under the same conditions, compared with the stabilized Zr and granulation powder thereof which are produced by the current and popular technology, the granulation powder quality is higher, the performance is better and the cost is reduced by 30-40%.
Description
Technical field
The present invention relates to a kind of preparation method of high profit green non-pollution stable zirconium oxide granulation powder, particularly to mix yttrium cubic phase zircite powder (hereinafter to be referred as the yttrium zirconium powder) be the working method of feedstock production environment-friendly type electrically melt yttrium oxide stabilized zirconia granulation powder with a kind of.
Background technology
Electric-melting zirconia is country's " Eighth Five-Year Plan " brainstorm project, and electric smelting stable zirconium oxide granulation powder is the electric-melting zirconia deep processed product; This scientific research project of the development and use of yttrium zirconium powder was stood tackling key problem mutually in 97 years by Ministry of Science and Technology's approval, and the fund project code is: 97-D100.The present invention unites two into one the scientific research project of these two national levels, has opened up the new direction of Chinese synthetic materials aspect.
As everyone knows, zirconium white is a polycrystal, and the zirconium Sauerstoffatom is arranged differently under different critical temperatures, and when critical transformation temperature, ground, microcosmic aspect changes the volume sudden change that causes material macroscopic view aspect, causes the wrinkling or fracture of goods.For the manufacturing that guarantees material is used with normal; Must add certain stablizer; Make it that whole phase transformation not take place under critical temperature, partial phase change causes that the stress that volume change produces can compensation temperature change the stress that produces, and makes be able to prolong the work-ing life of its goods.The kind of stablizer and quantity are to the stable decisive role of zircite product.Electric smelting stabilised zirconia (pyrogenic process) and chemically stable zirconium (wet method) under equal conditions (identical stabilizer type and quantity) their lattice, crystalline phase, hardness, proportion are all different.So the electric smelting stabilised zirconia is different with their performance of chemically stable zirconium, the field of use is also different.
Electric smelting stable zirconium oxide goods with its macrolattice high temperature resistant wash away degrade, good, the wear-resisting resistance to chemical attack of thermal shock resistance monopolizes its synthetic novel material and uses the field; Be the main raw of modern age hi-tech structural ceramics, function ceramics, support the pillar of new material industry such as modern high-temperature electric heat equipment, aerospacecraft member, sensor, metallurgical refractory materials.Be mainly used in aspect the toughening ceramic: mover device and heat-resistant component on aerospacecraft and the automotive industry, like cylinder liner, piston head, valve guide bushing, intake & exhaust valves seat, cylinder rotor, piston-ring, bearing tappet, rocket nozzle and aircraft engine wearing piece; The wear resistant corrosion resistant device is used in machinery, weaving, chemical industry and mining industry, like bearing, pump seal, blade and the pump housing, valve member, wortle, weaving porcelain spare, friction plate, pipe drawing mold, cutter and thermal insulation barriers; The nuclear industry atom is sent out and should be piled the engineering high-temperature structural material, the zirconia ceramics pipeline; The metallurgical industry rolling and casting is with metering nozzle, refractory castable; The modern high performance refractory materials is like load bearing board of zirconia, crucible, ozzle, slide plate, glass-melting furnace wall tile; The grinding materials and grinding tool industry is used high-abrasive material, like high firmness emery wheel, sand paper etc.; Navigation naval vessels shell, water screw, water power engine driven water screw surface spraying etc.The annual speed increase of pressing 10-15% of market demand.
At present, generally all use zircon sand to add stablizer in the current technology and produce various stable zirconium oxides, comprise the zirconium white that high performance yttrium oxide is stable as raw material.Stable zirconium oxide can be divided into according to different stabilizer type: the zirconium white of the zirconium white of stable calcium oxide, the zirconium white of stabilized magnesium hydroxide, stabilized with yttrium oxide.According to different stablizer add-ons, stable zirconium oxide can be divided into: PSZ and fully stabilized zirconia; Ratio according to different production methods and the existence of different crystalline phases; Stable zirconium oxide can be divided into again: the mechanical stability zirconium white; Crystal is main with monocline mutually; Stablizer and zirconium white exist with the form of non-solid solution body, just mechanically mix, and all the other are exactly tetragonal phase zirconium oxide, cubic phase zircite and compound crystalline phase zirconium white; According to different production technology, stable zirconium oxide can be divided into macrolattice pyrogenic process electric smelting stabilised zirconia and microcrystal wet chemistry stabilised zirconia again.
Electric smelting method production stability zirconium white, it is main with the zirconium white kind of stable calcium oxide mainly.Because of quicklime cheap, so absolute production cost is very low.But its goods fragility is big, and work-ing life is short, and relative cost is higher; The gas sensor aspect is because O
2-The moving passage resistance is big, and the response lag sensitivity is poor.The zirconium white of stabilized with yttrium oxide, because yttrium-zirconium intermiscibility is good, goods plasticity is strong, good toughness, long service life, the air-sensitive sensitivity is good, and it covers the zirconic purposes of all stable calcium oxides.Because yttrium oxide costs an arm and a leg, and is 150 times of quicklime cost, absolute cost is higher, in use range, receives price limit, and it is main using the zirconium white of stable calcium oxide with user's inertia on the market.
The yttrium zirconium powder; Be the sub product in the synthetic cubic phase zircite gem processing process, the Guangxi province Wuzhou is cubic zirconia production, processing distribution centre the biggest in the world, has every year the zirconium jewel sub product of many tons of four kilotons to handle; Be equivalent to raw ore more than ten million ton; This material is compared the physics and chemistry composition with zircon sand, rare-earth mineral completely different, and the chemical ingredients of great circle cutting powder is following, zirconium white 79.5%, yttrium oxide 20%; 200 order powder loose densitys are 1.55g/cm3, and tap density is 2.1g/cm
3, true specific gravity is 5.98g/cm
3, specific surface area is 0.9m
2/ g, original spacing of lattice is bigger, and the surface atom intensity is low; The zirconium yttrium is a complete stable cubic phase sosoloid, and the post-production sintering stress is big, has limited its direct use; After the phase transformation disintegration, let it be transformed into other available existence form, could embody its use value.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes existing stable zirconium oxide kind, and providing a kind of is raw material with the yttrium zirconium powder, the method for the electrically melt yttrium oxide stabilized zirconia granulation powder of preparation low-cost and high-performance environment-friendly type.
The working method of electrically melt yttrium oxide stabilized zirconia granulation powder of the present invention, it comprises the following steps:
1) be that main raw material adopts the electric smelting method to prepare partially stabilized yttrium with the yttrium zirconium powder--zirconium cube phase matrix oxide solid solution;
2) after the electric smelting yttrium Zirconium oxide sosoloid cooling with the step 1) preparation, the broken polishing in Hubei Province regathers the fine powder less than the 40um particle diameter;
3) with step 2) the fine powder wet-milling to the 3-5um particle diameter, the micro mist slurry;
4) the micro mist slurry of step 3) is added the dispersion agent of 2-3% weight ratio, stirred 15-20 minute, add the sticker of 2-3% weight ratio then, stirred unlatching heating installation, preparation granulation 10-15 minute;
Through kind, proportioning and the churning time of test of many times preferred dispersants, sticker, obtained guaranteeing solid solution powder macroscopic view physico-chemical property through mist projection granulating, can keep the particulate primary characteristic again.
5) the micro mist slurry is squeezed into the granulation of prilling tower internal spraying;
The slurry of handling through above-mentioned steps is low through the granulation powder soccer fraud rate that spraying, thermal dehydration processing obtain, and controlled, the narrowly distributing of particle diameter has good flowability.
6) the granulation powder that step 5) is prepared sieves with the mixer mixing and packs.
Adopt the electric smelting method to prepare partially stabilized yttrium-zirconium cube phase matrix oxide solid solution in the step 1) two kinds of schemes arranged:
A. with yttrium zirconium powder, zircon sand and powdered carbon by 1: 2.28: the refining classification electric smelting of slightly refining, heat up of part by weight mixing (0.24-0.26), the starting the arc, until chemical combination silicon all overflow electric smelting sosoloid.The chemical reaction that this technology relates to is following:
ZrO
2·SiO
2+C——ZrO
2+SiO+CO
SiO+C+O
2——SiO
2+CO
2
Zircon sand electric smelting method is produced zirconium white; It is not the independent invention of technology in modern age; It is the extension of traditional technology; It with traditional literature introduce the zircon sand charing---the charing operation of chlorination production zirconium tetrachloride plays the same tune on different musical instruments, only different on the reductive agent proportioning, add stablizer in addition and form stabilised zirconia sosoloid.
In the current technology because ac arc furnace (what all use like factories such as Shandong, Henan, Liaoning is ac arc furnace) temperature is high in the arc district, thermal radiation is strong, speed of response is fast; The negative-pressure air-flow that the silica flour recovery system is powerful can make the stablizer that adds with the powder form follow SiO, CO to rise altogether together; Make the ratio of stablizer in the melt lose perseverance, cause the stabilization rate of product unstable.So use ac arc furnace production stability zirconium white, generally all be to carry out the secondary electric smelting with adding stablizer again after the zircon sand electric smelting desiliconization earlier; Direct current electric arc furnace heat energy intensity in the arc district is gentle; The SiO that reaction is overflowed, CO gas vol rise and fall very little in whole process; The negative pressure gravitation that silica flour reclaims can be ignored to the degree that feed composition changes, and has the successful experience parameter to contrast, can an electric smelting moulding.
This workshop section is because the density of yttrium zirconium powder is more much bigger than yttrium oxide, quicklime or lime carbonate; Be higher than zircon sand, so, no matter be direct current electric arc furnace or ac arc furnace; Can an electric smelting straight forming; It is heating installation that the present invention selects direct current electric arc furnace for use, and its thermal energy conversion rate is high, and electrical network is not had impact.Middle sub product silica flour is the good additive of rubber, glass industry, the CO of collection
2Be used to do the light calcium carbonate fine powder raw material.
B. yttrium zirconium powder and monoclinic zirconia (or 99.5% technical grade zirconium white) were reacted 1-1.5 hour by 1: 1.50 part by weight mixing electric smelting, get electric smelting sosoloid.
Except that making the raw material of zircon sand, natural baddeleyite or commercially available technical grade monocline zirconium all can disintegrate complete stable cubic zirconium crystalline phase directly with mixing yttrium cube zirconium powder mixing electric smelting, become partially stabilized yttrium--zirconium cubic phase zircite sosoloid.
A, b two workshop sections are different with the formation mechanism of the domestic electric smelting of production stabilised zirconia enterprise, and traditional technology all is that the monocline zirconium is formed partially stabilized zirconium through adding an amount of stablizer electric smelting reaction.And present method is complete stable cubic phase zircite to be added the monocline zirconium form partially stabilized zirconium through electric smelting reaction back, and the former is synthetic, and synthetic ratio is lower than 95%, clips free stablizer in the component, needs through high-temperature heat treatment, makes it fully synthetic; The latter is dilution, and the stabilization rate is complete, need not through bakingout process.The present invention is inclined to and selects the b of workshop section.
Above-mentioned steps 2) step that in electric smelting yttrium Zirconium oxide solid solution powder is broken into powder is: after the melt cooling; Broken machine is broken to below the 25mm through Hubei Province earlier, is broken to below the 2mm through roll crusher again, crosses M1200 and revolves the screening of shaking below the sieve collection 2mm; After the magnetic separator deironing; Material is pulverized through micronizer mill again, through regulating the rotating speed of grading wheel, collects the powder less than 40um.
The electric smelting method is produced the yttrium stabilised zirconia, and the operation of process is main with physical treatment, is crushed to the lumpy material of macroscopical aspect through crusher in crushing at different levels, pulverizing mill the powder of arts demand.
The wet-milling process of step 3) is: fine powder is added pure water to solid-to-liquid ratio 1: 1, puts into and stir the mill staving, with the zirconium ball milling of different diameter to the 3-5um particle diameter, must the micro mist slurry.
This workshop section mill is situated between and replaces the aluminium ball with the zirconium ball, has not only guaranteed quality product but also shortened the ball milling time; Ball milling heating causing slurry temperature raises, and utilizes the outer circulation type of cooling to guarantee the persistence of producing.Outer circulation not only solved temperature of charge too high cause producing be interrupted, repeat to change the position that grinds of particulate aspect macroscopical, make the exterior appearance of particulate be consistent basically.
With the surface-treated of step 4) micro mist slurry be: add the dispersion agent of 2-3% weight ratio, stirred 15-20 minute, add the sticker of 2-3% weight ratio again, stirred 10-15 minute, open heating installation then, carry out granulation preparation work.
Kinds of surfactants is a lot, selects pulp surface promoting agent provided by the invention for use, can not cause secondary pollution to slurry, and the granulation powder soccer fraud of preparation is few, and controlled, the narrowly distributing of aggregate particle size has good flowability.
Adopt the stabilised zirconia granulation powder stable physical-chemical indexes property of present method preparation high, instant sample representativeness is strong, the quality The profile.
At present, domestic electrically melt yttrium oxide stabilized zirconia granulation powder standard is the NA report still, and product of the present invention and Shandong like product quality comparing result are listed in table 1:
Table 1
Find out that from table 1 products obtained therefrom quality of the present invention is higher than Shandong colleague enterprise like product.
The present invention compares with existing technology, has following advantage:
1, metal content is high in the raw material yttrium zirconium powder, and price is low; Raw and auxiliary material consumption is few, and cost is low, and metal recovery rate is high.The composition of raw material shows that its total metal content is worth and compares the zirconic content of conversion with the zircon sand price is 120%, is 1.82 times of zircon sand, and price but is 6/7 of a zircon sand.The present invention uses the yttrium zirconium powder to produce the zirconium white of stabilized with yttrium oxide as raw material, and it is lower than the zirconium white cost of stable calcium oxide, and performance is than its height.
2, among the present invention with highly purified yttrium zirconium powder; Cooperate high-grade zircon sand or monocline zirconium, production process need not to carry out the chemical after-treatment reason just can surpass existing like product quality standard, and whole technology realizes not having " three wastes " discharging; Promptly there is not the waste water,waste gas and industrial residue discharging; Technological process is controlled easily, belongs to green non-pollution environment-friendly type project, meets the environmental protection spirit that country advocates energy-saving and emission-reduction.
3, facility investment is few, and quality is higher than domestic like product, The profile.
4, using and mix the yttrium cubic phase zircite and be the stable zirconium white of raw material production electro-melting yttrium oxide, is raw material production electric smelting yttrium stabilised zirconia than traditional technology with zircon sand (monoclinic zirconia) and yttrium oxide, on year-on-year basis (1) electric energy reduce 4,000 respectively, (2,000) KWh/ ton; (2) the high-temperature heat treatment gas 350Kg/ ton (treating processes of the present invention does not need high-temperature heat treatment) that consumes petroleum less; (3) pure profit exceed traditional technology 1-1.5 doubly, remarkable in economical benefits.
5, the present invention uses direct current electric arc furnace, and energy conversion rate is high, and electrical network is not had impact.
6, finished product of the present invention is the granulation powder, is the extension product of stabilised zirconia Physical Processing bottommost layer time, and it is suitable for the technology of isostatic pressing most and makes, and uses simple and conveniently, and this also is an importance of all its product performance of ceramics decision.
7, reaction mechanism of the present invention is equally applicable to yttrium, zirconium is the exploitation and the production of the natural mineral reserve of main body.
Embodiment
Embodiment 1:
(Australia produces, ZrO to get 200Kg yttrium zirconium powder and 60 order 456Kg zircon sands
2>=66% time is together), 50 order 48.0Kg carbon dusts spray 5 liters of mixings of soft water, drop in the direct current electric arc furnace striking carbon piece that furnace bottom place mat 50mm is high in batches; Open hydraulic pressure, water-cooled, end anode cooling system, start air compressor machine and send pulse of compressed air to swat the cloth bag dust collector, open cyclonic separator, start silica flour recovery system induced draft fan; After treating that all are normally, the submerged arc electric smelting that feeds intake, 100 volts of striking voltages, 2000 amperes in electric current; Controlled temperature adds clout more than 1700 ℃ through oscillating batch charger, melting 4.0-4.5 hour desiliconization, 50 volts of regulating voltages; 9000 amperes in electric current, 2800 ℃ of temperature are about refining half a hour, till chemical combination silicon is all overflowed.Promote electrode, cover bell, driving hangs out table, cooling; Melt is smashed in the graphite pond, frit is crushed to below the 25mm, be broken to below the 2mm through roll crusher again with the broken machine in Hubei Province; Cross vibratory screening apparatus and collect the screening below the 1mm, after the electromagnetic separator deironing, ball milling is to 0.1mm; Pulverize through micronizer mill again,, collect powder less than 40um through regulating the rotating speed of grading wheel; Above-mentioned powder is put into the surface in the polyamine lipid steel drum; Use diameter to add the water solid-to-liquid ratio and be milled to 3um at 1: 1 as the cubic zirconium ball of 80mm; Add SD00 dispersion agent (production unit: nanometer ceramic technology development corporation, Ltd. of Nanjing clouds section; Address: in No. 5 Nanjing University of Technology's Materials Academies of the new exemplary road in Nanjing, down together.) weight ratio 3%, stirred 20 minutes, add 1788 then (buy the place: Shanghai City Ji Tuo trade Co., Ltd, No. 355, the good peace of Shanghai City Jiading District highway 1735 lanes, hereinafter mention 2088 too.) sticker, weight ratio 3% stirred 10 minutes; Open the prilling tower heating system, be warming up to 300 ℃, slip is delivered in the prilling tower with surge pump; The impulse air-atomizing granulation of contracting; The granulation powder is delivered in the V-type mixer mixed 30 minutes blowings sieves, collect 180-200 purpose powder packing, the powder of remaining particle diameter turns back to the wet-milling operation.
Embodiment 2:
Get 200Kg yttrium zirconium powder and 60 order 456Kg zircon sands, 5 liters of mixings of 50 order 52Kg carbon dusts sprinkling soft water, drop in the direct current electric arc furnace in batches, the striking carbon piece that furnace bottom place mat 50mm is high is opened hydraulic pressure, water-cooled, end anode cooling system; Start air compressor machine and send pulse of compressed air to swat the cloth bag dust collector, open cyclonic separator, start silica flour recovery system induced draft fan; After treating that all are normally, the submerged arc electric smelting that feeds intake, 100 volts of striking voltages; 2000 amperes in electric current, controlled temperature adds clout more than 1700 ℃ through oscillating batch charger; Melting 4.0-4.5 hour desiliconization, 50 volts of regulating voltages, 9000 amperes in electric current; 2800 ℃ of temperature are about refining half a hour, till chemical combination silicon is all overflowed.Promote electrode, cover bell, driving hangs out table, cooling; Melt is smashed in the graphite pond, frit is crushed to below the 25mm, be broken to below the 2mm through roll crusher again with the broken machine in Hubei Province; Cross vibratory screening apparatus and collect the screening below the 1mm, after the electromagnetic separator deironing, ball milling is to 0.1mm; Pulverize through micronizer mill again,, collect powder less than 40um through regulating the rotating speed of grading wheel; Above-mentioned powder is put into the surface in the polyamine lipid steel drum, uses diameter to add the water solid-to-liquid ratio and be milled to 3um at 1: 1, adding SD00 dispersion agent weight ratio 2% as the cubic zirconium ball of 50mm; Stirred 15 minutes, and added 2088 stickers then, weight ratio 3%; Stirred 15 minutes, and opened the prilling tower heating system, be warming up to 300 ℃; With surge pump slip is delivered in the prilling tower, the impulse air-atomizing granulation of contracting is delivered to the granulation powder that mixed 30 minutes blowings sieve in the V-type mixer; Collect 180-200 purpose powder packing, the powder of remaining particle diameter turns back to the wet-milling operation.
Embodiment 3:
250Kg yttrium zirconium powder and 325 order 375Kg monoclinic zirconias are comprised electric smelting monoclinic zirconia mixing, drop in the direct current electric arc furnace in batches, the striking carbon piece that furnace bottom place mat 50mm is high.Open hydraulic pressure, water-cooled, end anode cooling system, treat all normal after, the submerged arc electric smelting that feeds intake, 100 volts of striking voltages; 2000 amperes in electric current, controlled temperature adds clout more than 1700 ℃ through oscillating batch charger, melting 1 hour; 50 volts of regulating voltages, 9000 amperes in electric current, 2800 ℃ of temperature, refining 10--20 minute; Promote electrode, hang out table with driving, cooling is smashed melt in the graphite pond, with the broken machine in Hubei Province frit is crushed to below the 25mm; Be broken to below the 2mm through roll crusher, cross vibratory screening apparatus and collect the screening below the 1mm, after the electromagnetic separator deironing, ball milling is to 0.1mm; Pulverize through micronizer mill again,, collect powder less than 40um through regulating the rotating speed of grading wheel; Above-mentioned powder is put into the surface in the polyamine lipid steel drum, uses diameter to add the water solid-to-liquid ratio and be milled to 4um at 1: 1, adding SD00 dispersion agent weight ratio 2.5% as the cubic zirconium ball of 50mm; Stirred 15 minutes, and added 2088 stickers then, weight ratio 2%; Stirred 15 minutes, and opened the prilling tower heating system, be warming up to 300 ℃; With surge pump slip is delivered in the prilling tower, the impulse air-atomizing granulation of contracting is delivered to the granulation powder that mixed 30 minutes blowings sieve in the V-type mixer; Collect 180-200 purpose powder packing, the powder of remaining particle diameter turns back to the wet-milling operation.
Embodiment 4:
400Kg yttrium zirconium powder and 80 order 912Kg zircon sands, 50 order 100Kg carbon dusts spray 10 liters of mixings of soft water, drop in the direct current electric arc furnace for several times, and the striking carbon piece that furnace bottom place mat 50mm is high is opened hydraulic pressure, water-cooled, end anode cooling system; Start air compressor machine and send pulse of compressed air to swat the cloth bag dust collector, open cyclonic separator, start silica flour recovery system induced draft fan, regulate air-valve; After treating that all are normally, the submerged arc electric smelting that feeds intake, 100 volts of striking voltages; 2000 amperes in electric current, controlled temperature adds clout more than 1700 ℃ through oscillating batch charger; Melting 4.0-4.5 hour desiliconization, 50 volts of regulating voltages, 9000 amperes in electric current; 2800 ℃ of temperature, refining are about 30 minutes, till chemical combination silicon is all overflowed.Promote electrode, cover bell, driving hangs out table; Cooling is smashed melt in the graphite pond, with the broken machine in Hubei Province frit is crushed to below the 25mm, is broken to below the 2mm through roll crusher again; Cross vibratory screening apparatus and collect the screening below the 1mm, after the electromagnetic separator deironing, ball milling is to 0.1mm; Pulverize through micronizer mill again,, collect powder less than 40um through regulating the rotating speed of grading wheel; Above-mentioned powder is put into the surface in the polyamine lipid steel drum, uses diameter to add the water solid-to-liquid ratio and be milled to 5um at 1: 1, adding SD00 dispersion agent weight ratio 2% as the cubic zirconium ball of 70mm; Stirred 20 minutes, and added 2088 stickers then, weight ratio 2.5%; Stirred 10 minutes, and opened the prilling tower heating system, be warming up to 300 ℃; With surge pump slip is delivered in the prilling tower, the impulse air-atomizing granulation of contracting is delivered to the granulation powder that mixed 30 minutes blowings sieve in the V-type mixer; Collect 180-200 purpose powder packing, the powder of remaining particle diameter turns back to the wet-milling operation.
Embodiment 5:
250Kg yttrium zirconium powder and 100 order 375Kg monoclinic zirconias are comprised electric smelting monoclinic zirconia mixing, drop in the direct current electric arc furnace in batches, the striking carbon piece that furnace bottom place mat 50mm is high.Open hydraulic pressure, water-cooled, end anode cooling system, treat all normal after, the submerged arc electric smelting that feeds intake, 100 volts of striking voltages; 2000 amperes in electric current, controlled temperature adds clout more than 1700 ℃ through oscillating batch charger, melting 40-50 minute; 50 volts of regulating voltages, 9000 amperes in electric current, 2800 ℃ of temperature, refining 10--20 minute; Promote electrode, cover bell, driving hangs out table, and cooling is smashed melt in the graphite pond; With the broken machine in Hubei Province frit is crushed to below the 25mm, is broken to below the 2mm through roll crusher again, cross vibratory screening apparatus and collect the screening below the 1mm, after the electromagnetic separator deironing; Ball milling is pulverized through micronizer mill to 0.1mm again, through regulating the rotating speed of grading wheel, collects the powder less than 40um; Above-mentioned powder is put into the surface in the polyamine lipid steel drum, uses diameter to add the water solid-to-liquid ratio and be milled to 5um at 1: 1.5, adding SD00 dispersion agent weight ratio 2% as the cubic zirconium ball of 60mm; Stirred 20 minutes, and added 1788 stickers then, weight ratio 2.5%; Stirred 15 minutes, and opened the prilling tower heating system, be warming up to 300 ℃; With surge pump slip is delivered in the prilling tower, the impulse air-atomizing granulation of contracting is delivered to the granulation powder that mixed 30 minutes blowings sieve in the V-type mixer; Collect 180-200 purpose powder packing, the powder of remaining particle diameter turns back to the wet-milling operation.
Embodiment 6:
With 300Kg yttrium zirconium powder and 100 order 450Kg monoclinic zirconia mixings, drop in the direct current electric arc furnace in batches, the striking carbon piece that furnace bottom place mat 50mm is high is opened hydraulic pressure, water-cooled, end anode cooling system; After treating that all are normally, the submerged arc electric smelting that feeds intake, 100 volts of striking voltages, 2000 amperes in electric current; Controlled temperature adds clout more than 1700 ℃ through oscillating batch charger, and melting 50-60 minute, 50 volts of regulating voltages; 9000 amperes in electric current, 2800 ℃ of temperature refining 20--30 minute, promote electrode; Driving hangs out table, and cooling is smashed melt in the brick fuel pond, with the broken machine in Hubei Province frit is crushed to below the 25mm, is broken to below the 2mm through roll crusher again; Cross vibratory screening apparatus and collect the screening below the 1mm, after the electromagnetic separator deironing, ball milling is to 0.1mm; Pulverize through micronizer mill again,, collect powder less than 40um through regulating the rotating speed of grading wheel; Above-mentioned powder is put into the surface in the polyamine lipid steel drum, uses diameter to add the water solid-to-liquid ratio and be milled to 4um at 1: 1, adding SD00 dispersion agent weight ratio 3% as the cubic zirconium ball of 80mm; Stirred 15 minutes, and added 1788 stickers then, weight ratio 3%; Stirred 10 minutes, and opened the prilling tower heating system, be warming up to 300 ℃; With surge pump slip is delivered in the prilling tower, the impulse air-atomizing granulation of contracting is delivered to the granulation powder that mixed 30 minutes blowings sieve in the V-type mixer; Collect 180-200 purpose powder packing, the powder of remaining particle diameter turns back to the wet-milling operation.
Claims (3)
1. the working method of an electrically melt yttrium oxide stabilized zirconia granulation powder is characterized in that comprising the following steps:
1) be that main raw material adopts the electric smelting method to prepare partially stabilized yttrium with the yttrium zirconium powder--zirconium cube phase matrix oxide solid solution; This electric smelting method has two kinds of schemes:
A. with yttrium zirconium powder, zircon sand and powdered carbon by 1: 2.28: the refining classification electric smelting of slightly refining, heat up of part by weight mixing (0.24-0.26), the starting the arc, until chemical combination silicon all overflow electric smelting yttrium Zirconium oxide sosoloid;
B. yttrium zirconium powder and monoclinic zirconia are pressed 1: 1.50 part by weight mixing, electric smelting reaction 1-1.5 hour gets electric smelting yttrium Zirconium oxide sosoloid;
2) after the electric smelting yttrium Zirconium oxide sosoloid cooling with the step 1) preparation, the broken polishing in Hubei Province regathers the fine powder less than the 40um particle diameter;
3) with step 2) the fine powder wet-milling to the 3-5um particle diameter, the micro mist slurry;
4) with the dispersion agent of micro mist slurry adding 2-3% weight ratio, stirred 15-20 minute, add the sticker of 2-3% weight ratio then, stirred 10-15 minute, open heating installation, prepare granulation;
5) the micro mist slurry is squeezed into the granulation of prilling tower internal spraying;
6) the granulation powder that step 5) is prepared sieves with the mixer mixing and packs.
2. the working method of electrically melt yttrium oxide stabilized zirconia granulation powder according to claim 1; It is characterized in that step 2) in electric smelting yttrium Zirconium oxide solid solution powder is broken into powder process be: broken machine is broken to below the 25mm particle diameter electric smelting sosoloid through Hubei Province earlier, is broken to below the 2mm particle diameter through roll crusher again, crosses vibratory screening apparatus and collects the screening below the 2mm particle diameter; After the electromagnetic separator deironing; Pulverize through micronizer mill again,, collect fine powder less than the 40um particle diameter through regulating the rotating speed of grading wheel.
3. the working method of electrically melt yttrium oxide stabilized zirconia granulation powder according to claim 1; The wet-milling process that it is characterized in that step 3) is: fine powder is added pure water to solid-to-liquid ratio 1: 1; Put into and stir the mill staving, with the zirconium ball milling of different diameter to the 3-5um particle diameter, must the micro mist slurry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101091601A CN101792179B (en) | 2010-02-11 | 2010-02-11 | Production method of electrically melt yttrium oxide stabilized zirconia granulation powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101091601A CN101792179B (en) | 2010-02-11 | 2010-02-11 | Production method of electrically melt yttrium oxide stabilized zirconia granulation powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101792179A CN101792179A (en) | 2010-08-04 |
| CN101792179B true CN101792179B (en) | 2012-01-25 |
Family
ID=42585137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101091601A Expired - Fee Related CN101792179B (en) | 2010-02-11 | 2010-02-11 | Production method of electrically melt yttrium oxide stabilized zirconia granulation powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101792179B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950977A (en) * | 2014-05-15 | 2014-07-30 | 李树昌 | Method for extracting zirconium oxide from zirconium-containing solid solution substance |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653417B (en) * | 2012-03-26 | 2014-05-14 | 三祥新材股份有限公司 | Method for preparing stable-type zirconium dioxide by electric smelting method |
| CN104129989B (en) * | 2014-07-11 | 2016-05-25 | 东莞信柏结构陶瓷股份有限公司 | The preparation method of yttria-stabilized zirconia pelletizing |
| CN105753510B (en) * | 2014-12-05 | 2018-05-01 | 三祥新材股份有限公司 | A kind of preparation method of heat resist modification electric-melting zirconia and pr-yellow material |
| CN115159980A (en) * | 2022-07-07 | 2022-10-11 | 郑州振中电熔新材料有限公司 | Method for manufacturing fused yttrium stabilized zirconia by using zirconium gem processing waste |
| CN115124073B (en) * | 2022-07-07 | 2023-06-27 | 郑州振中电熔新材料有限公司 | Method for preparing electric smelting yttrium stabilized zirconium by using waste zirconia material |
| CN115010484A (en) * | 2022-07-07 | 2022-09-06 | 郑州振中电熔新材料有限公司 | Method for manufacturing fused calcium stabilized zirconia by using waste zirconia nozzle and sliding plate |
| CN116082036A (en) * | 2022-07-19 | 2023-05-09 | 广东爱斯库生物材料有限公司 | Zirconia recovery method and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1093105C (en) * | 2000-12-12 | 2002-10-23 | 田维 | Kiln aparatus and method for preparing zirconium oxide used in electronic industry |
| CN100463862C (en) * | 2006-12-19 | 2009-02-25 | 王必庆 | Process of preparing zirconia and yttria with Y-doped cubic zirconia powder |
-
2010
- 2010-02-11 CN CN2010101091601A patent/CN101792179B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950977A (en) * | 2014-05-15 | 2014-07-30 | 李树昌 | Method for extracting zirconium oxide from zirconium-containing solid solution substance |
| CN103950977B (en) * | 2014-05-15 | 2015-10-21 | 李树昌 | Zirconic method is extracted from containing zirconium solid solution material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101792179A (en) | 2010-08-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101792179B (en) | Production method of electrically melt yttrium oxide stabilized zirconia granulation powder | |
| CN102583411B (en) | Method for producing mullite by using fly ash | |
| AU2020103188A4 (en) | Concrete Containing Coal-to-liquids Coarse Slag and Preparation Method thereof | |
| CN1415567A (en) | binary mixed coagulated stones and wet cement and method for production, deposit, transportation use and application | |
| CN102976641A (en) | Micro-expansive moderate-heat Portland cement and production method thereof | |
| CN106278324A (en) | A kind of modified high-purity magnesium-aluminum spinel composite brick and preparation method thereof | |
| CN102600939B (en) | Method for manufacturing nanometer zirconia ceramic reinforced wear-resisting steel ball | |
| CN109987892A (en) | One kind is based on flyash-iron tailings geo-polymer fibre reinforced materials and preparation method thereof | |
| CN103848618B (en) | A kind of synthesizing ferrum-aluminium spinelle and production method thereof | |
| JP2010100442A (en) | Method for producing cordierite | |
| CN110436907A (en) | A method of utilizing preparing mullite from gangue | |
| CN101531523A (en) | Method for synthesizing mullite through utilization of waste | |
| CN102976642B (en) | Special silicate cement for nuclear power and production method thereof | |
| CN113860780B (en) | Preparation method of high-activity spherical calcined coal gangue powder | |
| CN105385848A (en) | Preparation method of iron ore powder pelletized magnesian binding agent | |
| CN102304750A (en) | Method for synthesizing mullite whiskers | |
| CN113754451B (en) | Refractory brick prepared from industrial solid waste and preparation method thereof | |
| CN101643359A (en) | Method for preparing porzite powder by fly ash | |
| CN110436908A (en) | A method of cordierite is prepared using gangue | |
| CN103951451B (en) | The manufacture method of high-strength wearable lining brick | |
| CN107445614A (en) | A kind of compound zirconium oxide powder and preparation method thereof | |
| CN103641125B (en) | Method for synthesizing wollastonite with high length-diameter ratio by using industrial waste residue resource | |
| CN113697821A (en) | Magnesium silicate powder and preparation method and application thereof | |
| CN106977181A (en) | A kind of BOF Hood magnesium-aluminum-calcium titanium carbon brick and preparation method thereof | |
| CN107265868B (en) | Microcrystalline glass prepared from Qing mountain flour and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120125 Termination date: 20130211 |