CN103496954A - Process for manufacturing aluminum oxide ceramic nozzle - Google Patents

Process for manufacturing aluminum oxide ceramic nozzle Download PDF

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CN103496954A
CN103496954A CN201310482273.XA CN201310482273A CN103496954A CN 103496954 A CN103496954 A CN 103496954A CN 201310482273 A CN201310482273 A CN 201310482273A CN 103496954 A CN103496954 A CN 103496954A
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gypsum
nozzle
slurry
alumina
preparation technology
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CN103496954B (en
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李爱民
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Shandong University
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Abstract

The invention relates to a process for manufacturing an aluminum oxide ceramic nozzle. The process includes weighing, by mass, 85-95% of alpha-Al<2>O<3>, 1-5% of kaolin, 0.5-2% of light calcium carbonate, 0.5-2% of burned talc, 2-6% of boron carbide or zirconium oxide and 0-2% of other ingredients, adding the alpha-Al<2>O<3>, the kaolin, the light calcium carbonate, the burned talc, the boron carbide or zirconium oxide and the other ingredients into a ball mill, adding purified water into the ball mill, performing ball-milling on the alpha-Al<2>O<3>, the kaolin, the light calcium carbonate, the burned talc, the boron carbide or zirconium oxide and the other ingredients until the median diameters D50 of particles range from 1.8 micrometers to 2.0 micrometers, and performing stirring and vacuum degassing on the particles to form slurry; injecting the slurry into a gypsum mold via a pipeline under the slurry injection pressure ranging from 0.1MPa to 0.2MPa, absorbing water in a body by gypsum, releasing a semi-finished nozzle from the mold after the body has certain strength, and firing the semi-finished nozzle. The other ingredients include one or a plurality of barium carbonate, magnesium oxide, alkali powder and water glass. The process has the advantages that owing to the gypsum pressure slurry injection process, the production efficiency is greatly improved as compared with a thermal die-casting process, the problem of low thermal die-casting forming efficiency can be solved, and the qualified rate of fired products can be greatly increased.

Description

A kind of preparation technology of alumina-ceramic nozzle
Technical field
The present invention relates to a kind of preparation technology of alumina-ceramic nozzle, the preparation technology especially for the nozzle of lime stone slurry atomization in flue gas desulfurization, belong to the nozzle field shaping technique.
Background technology
China's " national economy and social development 11th Five-Year Plan outline " is using the target of total sulfur dioxide reduction 10% as a restrictive target that must complete.The power industry sulfur dioxide emissions account for the over half of national total release, during Eleventh Five-Year Plan (2006-2010), can existing coal-burning power plant sulfurous gas be effectively controlled, and will become and control national sulfur dioxide emissions, the key that can the total amount reduction target be realized as scheduled.Therefore, strengthen when the means of flue gas desulfurization of power plant project construction ensures well existing sweetener safe operation and work as last urgently and difficult task.
Control the technical research and development of sulfur dioxide emissions since the 1950's, the desulfurization technology kind has reached kind more than 200 so far.At present, coal-burning power plant applies fume desulphurization method more widely has: Gypsum Wet, flue gas circulating fluidized bed method, seawater method, semidrying, rotary spraying and drying method, electronic beam method etc.Limestone-gypsum Wet Flue Gas Desulfurization Process technique is to apply in the world at present at most, the most ripe Flue Gas Desulfurization Technology of Power Plant, and the sulfurous gas that the method utilizes the lime stone slurry after atomization to absorb in flue gas generates gypsum, reaches the purpose of desulfurization.At present, the main Limestone-gypsum Wet Flue Gas Desulfurization Process technique that adopts is administered in the flue gas desulfurization of China's firepower electrical plant.
Nozzle for flue gas desulfurization is one of key equipment in the Limestone-gypsum Wet Flue Gas Desulfurization Process system.Due to abradability and the corrodibility of lime stone slurry, alternative nozzle material is very limited.Chinese scholars is developed well through exploration for many years, and the stupalith that finally is summed up as high rigidity, high-wearing feature can meet wear-resisting, the corrosion resistant requirement of desulfurization nozzle.At present, the flue gas desulfurization atomizing nozzle adopts the silicon carbide reaction-sintered material substantially both at home and abroad, and major part is external product.But, due to the free silica that contains 20% left and right in silicon carbide reaction-sintered, its resistance to erosion and corrosion resistance nature are affected.Simultaneously, still there is the problem that price is high, atomizing effect is undesirable in the silicon carbide nozzle at present.
Summary of the invention
The preparation technology who the objective of the invention is to overcome the deficiencies in the prior art and a kind of alumina-ceramic nozzle is provided, improved quality and the efficiency of product.
The technical scheme that the present invention takes is:
A kind of preparation technology of alumina-ceramic nozzle comprises that step is as follows:
(1) make the gypsum mold of nozzle;
(2) example takes α-Al in mass ratio 2o 385~95%, kaolin 1~5%, light calcium carbonate 0.5~2%, ripe talcum 0.5~2%, norbide or zirconium white 2~6%, other compositions 0~2%, other compositions are selected from one or more in barium carbonate, magnesium oxide, ground caustic, water glass, add in ball mill, then the pure water that adds institute's materials opaque amount 50%~60%, be milled to granularity meso-position radius D50:1.8~2.0 μ m, D90<3.0 μ m, the degassed pulping of stirring vacuum;
(3) slurries are passed through to pipeline pressure slip casting in gypsum mold, grouting pressure 0.1-0.2MPa, gypsum absorbs the moisture in base substrate, and after base substrate has intensity, but the nozzle work in-process are taken out in the demoulding;
(4) the nozzle work in-process are fired to 1550 ℃~1580 ℃ of firing temperatures, soaking time 4~5h, cooling finished product.
The described gypsum mold of step in above-mentioned preparation method (1) adopts high strength β-terra alba or α-terra alba to make, and the cream quality ratio of α-gypsum slurry is 1.5~1.8:1,801 glue of additional gypsum quality mark 5~10%, 901 glue or thermoplastic resin; The cream quality ratio of β-gypsum slurry is 1.5~1.9:1,801 glue of additional gypsum quality mark 5~10%, 901 glue or thermoplastic resin.
In above-mentioned steps (2), vacuum outgas vacuum tightness requires 0.7~0.9mPa.The preferred barium carbonate of described other compositions, magnesium oxide, ground caustic mix with the water glass arbitrary proportion.
Slip casing by pressure described in above-mentioned steps (3), preferably 100~200 small transfer lines inject 100~200 cover gypsum molds, the preferred 0.1MPa of grouting pressure simultaneously.
The invention has the advantages that:
(1) adopt the premium high-alumina raw material, additional 2~6% titanium carbides or zirconium white raw material, the good abrasion-resistance of hardness of raising alumina-ceramic, prepare the flue gas desulfurization glue size atomizing nozzle, substitutes existing import reaction sintering silicon carbide ceramic product.
(2) flue gas desulfurization glue size atomizing and oxidizing aluminium ceramic nozzle adopts slip casing by pressure technique, and use equipment is few, simple to operate, but disposal molding produces that to have solved in the injection moulding process use equipment many in enormous quantities, the problem yielded poorly; The pure water as medium of slurry, the suspension of slurry, good fluidity, cost is low; The pressure product is seen once-firing, and hot die-casting molding, product must be through dewaxing technique, twice firing, and energy consumption is large; Thereby guarantee compactness, the precision of nozzle, improve the good slurry spraying effect of finished product rate.
The present invention adopts gypsum slip casing by pressure technique, than injection moulding explained hereafter efficiency, is improved largely, and solved the inefficient problem of hot die-casting molding, and the product qualification rate of burning till has also had large increase.With respect to the reaction sintering silicon carbide ceramic nozzle, the alumina-ceramic nozzle has very strong price advantage, 1/4th of the not enough silicon carbide of its raw materials cost.In addition, the sintering temperature of alumina-ceramic, far below silicon carbide ceramics, is produced the aluminum oxide nozzle and is had energy-saving effect preferably.Wear-resisting, resistance to erosion, the corrosion resistance nature of alumina-ceramic nozzle are better than the silicon carbide nozzle, and the pressure of Chinese firepower electrical plant dependence on import silicon carbide nozzle will be greatly alleviated in the application of flue gas desulfurization oxidation aluminium nozzle.
Embodiment
Below in conjunction with specific embodiment, further illustrate.
Embodiment 1
A kind of preparation technology of alumina-ceramic nozzle comprises that step is as follows:
1, the preparation of gypsum mold
(1) gypsum mold adopts high strength α-terra alba to make.
(2) while making gypsum mold, the plaster-water ratio of α-gypsum slurry is 1.5:1, simultaneously additional gypsum quality mark 10%, 801 glue.
(3), while making gypsum mold, must there is the sulphur tire to do subsidiary material.
(4) feature of gypsum nozzle mould: external mold is two die sinkings, three-part pattern or four die sinkings, and internal mold is the loose piece structure, and base is the gypsum cover plate, and mould central authorities, for taper gypsum plug, are wrapped up by the loose piece product.
2, the preparation of grout material and processing
(1) slurry preparation
(A) formula takes the raw material (α-Al such as alpha-aluminium oxide powder, plastic clay, fine particle calcium carbonate, ripe talcum, barium carbonate, magnesium oxide, ground caustic, water glass in mass ratio 2o 3: 85%; Kaolin: 4%; Light calcium carbonate: 2%; Ripe talcum: 2%; Other compositions: 1%, barium carbonate 0.2%, magnesium oxide 0.3%, ground caustic 0.2%, water glass 0.3%) add in ball mill additional norbide: 6%; Then the pure water that adds pan feeding opaque amount 50%, ball milling 30h, stop getting sample after mill, surveys the fineness of slurry with the infrared rays particle size analyzer, requires to be ground to former grain fineness number.
(B) granularity requirements: meso-position radius D50:1.8~2.0 μ m, D90<3.0 μ m.
(C) slurry moisture: 33~45%.
(D) the pH value of slurry: 9~10.5.
(E) viscosity of slurry: 27~31mPaS.
The rotary viscosity instrumentation: 17 * 10(2 rotor, 30r/min)~11 * 10(2 rotor, 30r/min)
(2) slurry is processed: must use stirring vacuum degassed, vacuum tightness requires 0.7mPa.
3, slip casing by pressure pattern
(1) put 100~200 cover gypsum molds on the slip casting frame, the stopping property of mould is strong, and mould leaves grouting hole.
(2) in the eminence higher than 5~8 meters of gypsum molds, pulp injection tank is installed, pulp injection tank has vacuum stirring device.
(3) draw main pipeline from pulp injection tank, from pipeline, 100~200 small transfer lines are drawn by branch later, and the plastics tubing that small transfer line is diameter Ф 14mm left and right inserts in the grouting hole of gypsum mold, open the slip casting valve, but slip casting in 60~90 minutes is complete.
(4) after slip casting, then etc. 60~90 minutes, gypsum further absorbs the moisture in base substrate, after base substrate has intensity, but the nozzle work in-process are taken out in the demoulding.
4, the nozzle work in-process are fired to 1550 ℃ of firing temperatures, soaking time 4h, cooling finished product.
Embodiment 2
A kind of preparation technology of alumina-ceramic nozzle comprises that step is as follows:
1, the preparation of gypsum mold
(1) gypsum mold adopts high strength α-terra alba to make.
(2) while making gypsum mold, the plaster-water ratio of α-gypsum slurry is 1.8:1, simultaneously additional gypsum quality mark 5%, 901 glue.
(3), while making gypsum mold, must there is the sulphur tire to do subsidiary material.
(4) feature of gypsum nozzle mould: external mold is two die sinkings, three-part pattern or four die sinkings, and internal mold is the loose piece structure, and base is the gypsum cover plate, and mould central authorities, for taper gypsum plug, are wrapped up by the loose piece product.
2, the preparation of grout material and processing
(1) slurry preparation
(A) formula takes the raw material (α-Al such as alpha-aluminium oxide powder, plastic clay, fine particle calcium carbonate, ripe talcum, barium carbonate, magnesium oxide, ground caustic, water glass in mass ratio 2o 3: 90%; Kaolin: 3%; Light calcium carbonate: 1%; Ripe talcum: 1%; Other compositions: 1%) add in ball mill additional norbide 4%; Then the pure water that adds pan feeding opaque amount mark 50%, ball milling 30h, stop getting sample after mill, surveys the fineness of slurry with the infrared rays particle size analyzer, requires to be ground to former grain fineness number.
(B) granularity requirements: meso-position radius D50:1.8~2.0 μ m, D90<3.0 μ m.
(C) slurry moisture: 33~45%.
(D) the pH value of slurry: 9~10.5.
(E) viscosity of slurry: 27~31mPaS.
The rotary viscosity instrumentation: 17 * 10(2 rotor, 30r/min)~11 * 10(2 rotor, 30r/min)
(2) slurry is processed: must use stirring vacuum degassed, vacuum tightness requires 0.9mPa.
3, slip casing by pressure pattern
(1) put 100~200 cover gypsum molds on the slip casting frame, the stopping property of mould is strong, and mould leaves grouting hole.
(2) in the eminence higher than 5~8 meters of gypsum molds, pulp injection tank is installed, pulp injection tank has vacuum stirring device.
(3) draw main pipeline from pulp injection tank, from pipeline, 100~200 small transfer lines are drawn by branch later, and the plastics tubing that small transfer line is diameter Ф 14mm left and right inserts in the grouting hole of gypsum mold, open the slip casting valve, but slip casting in 60~90 minutes is complete.
(4) after slip casting, then etc. 60~90 minutes, gypsum further absorbs the moisture in base substrate, after base substrate has intensity, but the nozzle work in-process are taken out in the demoulding.
4, the nozzle work in-process are fired to 1560 ℃ of firing temperatures, soaking time 4, cooling finished product.
Embodiment 3
A kind of preparation technology of alumina-ceramic nozzle comprises that step is as follows:
1, the feature of gypsum mold
(1) gypsum mold adopts high strength β-terra alba to make.
(2) while making gypsum mold, the plaster-water ratio of β-gypsum slurry is 1.5:1, additional gypsum quality mark 10% of while, thermoplastic resin.
(3), while making gypsum mold, must there is the sulphur tire to do subsidiary material.
(4) feature of gypsum nozzle mould: external mold is two die sinkings, three-part pattern or four die sinkings, and internal mold is the loose piece structure, and base is the gypsum cover plate, and mould central authorities, for taper gypsum plug, are wrapped up by the loose piece product.
2, the feature of grout material
(1) slurry preparation
(A) formula takes the raw material (α-Al such as alpha-aluminium oxide powder, plastic clay, fine particle calcium carbonate, ripe talcum, barium carbonate, magnesium oxide, ground caustic, water glass in mass ratio 2o 3: 95%; Kaolin: 1%; Light calcium carbonate: 0.5%; Ripe talcum: 0.5%; Other compositions: 1%) add in ball mill additional norbide 2%; Then the pure water that adds pan feeding opaque amount mark 50%, ball milling 30h, stop getting sample after mill, surveys the fineness of slurry with the infrared rays particle size analyzer, requires to be ground to former grain fineness number.(B) granularity requirements: meso-position radius D50:1.8~2.0 μ m, D90<3.0 μ m.
(C) slurry moisture: 33~45%.
(D) the pH value of slurry: 9~10.5.
(E) viscosity of slurry: 27~31mPaS.
The rotary viscosity instrumentation: 17 * 10(2 rotor, 30r/min)~11 * 10(2 rotor, 30r/min)
(2) slurry is processed: must use stirring vacuum degassed, vacuum tightness requires 0.7mPa.
3, slip casing by pressure pattern
(1) put 100~200 cover gypsum molds on the slip casting frame, the stopping property of mould is strong, and mould leaves grouting hole.
(2) in the eminence higher than 5~8 meters of gypsum molds, pulp injection tank is installed, pulp injection tank has vacuum stirring device.
(3) draw main pipeline from pulp injection tank, from pipeline, 100~200 small transfer lines are drawn by branch later, and the plastics tubing that small transfer line is diameter Ф 14mm left and right inserts in the grouting hole of gypsum mold, open the slip casting valve, but slip casting in 60~90 minutes is complete.
(4) after slip casting, then etc. 60~90 minutes, gypsum further absorbs the moisture in base substrate, after base substrate has intensity, but the nozzle work in-process are taken out in the demoulding.
4, the nozzle work in-process are fired to 1580 ℃ of firing temperatures, soaking time 4h, cooling finished product.
The product appearance feature:
Flue gas desulfurization glue size atomizing and oxidizing aluminium ceramic nozzle profile is the cone-type spiral shape.
Product burns till feature:
Alumina slurry work in-process dry body flat board is put into silicon carbide sagger, dull and stereotyped material is the same with the material of aluminum oxide nozzle product, flat board is formed by slip casting, then aluminum oxide nozzle work in-process (dry body) is put on the silicon carbide sagger flat board, then with aluminum oxide powder, the roasting of nozzle product is obtained.Perhaps in the middle of nozzle is half-finished, insert conic mandrel bar, the material of plug is consistent with the nozzle product, and plug wants consistent with the bonding surface of nozzle product.
Embodiment 4
A kind of preparation technology of alumina-ceramic nozzle comprises that step is as follows:
1, the feature of gypsum mold
(1) gypsum mold adopts high strength β-terra alba to make.
(2) while making gypsum mold, the plaster-water ratio of β-gypsum slurry is 1.9:1, simultaneously additional gypsum quality mark 7%, 901 glue.
(3), while making gypsum mold, must there is the sulphur tire to do subsidiary material.
(4) feature of gypsum nozzle mould: external mold is two die sinkings, three-part pattern or four die sinkings, and internal mold is the loose piece structure, and base is the gypsum cover plate, and mould central authorities, for taper gypsum plug, are wrapped up by the loose piece product.
2, the feature of grout material
(1) slurry preparation
(A) formula takes the raw material (α-Al such as alpha-aluminium oxide powder, plastic clay, fine particle calcium carbonate, ripe talcum, barium carbonate, magnesium oxide, ground caustic, water glass in mass ratio 2o 3: 90%; Kaolin: 3%; Light calcium carbonate: 1%; Ripe talcum: 1%; Other compositions: 1%, barium carbonate 0.3%, magnesium oxide 0.3%, ground caustic 0.2%, water glass 0.2%) add in ball mill additional zirconium white 4%; Then the pure water that adds pan feeding opaque amount mark 55%, ball milling 30h, stop getting sample after mill, surveys the fineness of slurry with the infrared rays particle size analyzer, requires to be ground to former grain fineness number.(B) granularity requirements: meso-position radius D50:1.8~2.0 μ m, D90<3.0 μ m.
(C) slurry moisture: 33~45%.
(D) the pH value of slurry: 9~10.5.
(E) viscosity of slurry: 27~31mPaS.
The rotary viscosity instrumentation: 17 * 10(2 rotor, 30r/min)~11 * 10(2 rotor, 30r/min)
(2) slurry is processed: must use stirring vacuum degassed, vacuum tightness requires 0.9mPa.
3, slip casing by pressure pattern
(1) put 100~200 cover gypsum molds on the slip casting frame, the stopping property of mould is strong, and mould leaves grouting hole.
(2) in the eminence higher than 5~8 meters of gypsum molds, pulp injection tank is installed, pulp injection tank has vacuum stirring device.
(3) draw main pipeline from pulp injection tank, from pipeline, 100~200 small transfer lines are drawn by branch later, and the plastics tubing that small transfer line is diameter Ф 14mm left and right inserts in the grouting hole of gypsum mold, open the slip casting valve, but slip casting in 60~90 minutes is complete.
(4) after slip casting, then etc. 60~90 minutes, gypsum further absorbs the moisture in base substrate, after base substrate has intensity, but the nozzle work in-process are taken out in the demoulding.
4, the nozzle work in-process are fired to 1570 ℃ of firing temperatures, soaking time 5h, cooling finished product.
The product appearance feature:
Flue gas desulfurization glue size atomizing and oxidizing aluminium ceramic nozzle profile is the cone-type spiral shape.
Product burns till feature:
Alumina slurry work in-process dry body flat board is put into silicon carbide sagger, dull and stereotyped material is the same with the material of aluminum oxide nozzle product, flat board is formed by slip casting, then aluminum oxide nozzle work in-process (dry body) is put on the silicon carbide sagger flat board, then with aluminum oxide powder, the roasting of nozzle product is obtained.Perhaps in the middle of nozzle is half-finished, insert conic mandrel bar, the material of plug is consistent with the nozzle product, and plug wants consistent with the bonding surface of nozzle product.

Claims (5)

1. the preparation technology of an alumina-ceramic nozzle, is characterized in that, comprises that step is as follows:
(1) make the gypsum mold of nozzle;
(2) example takes α-Al in mass ratio 2o 385~95%, kaolin 1~5%, light calcium carbonate 0.5~2%, ripe talcum 0.5~2%, norbide or zirconium white 2~6%, other compositions 0~2%, other compositions are selected from one or more in barium carbonate, magnesium oxide, ground caustic, water glass, add in ball mill, then the pure water that adds institute's materials opaque amount 50%~60%, be milled to granularity meso-position radius D50:1.8~2.0 μ m, D90<3.0 μ m, the degassed pulping of stirring vacuum;
(3) slurries are passed through to pipeline pressure slip casting in gypsum mold, grouting pressure 0.1-0.2MPa, gypsum absorbs the moisture in base substrate, and after base substrate has intensity, but the nozzle work in-process are taken out in the demoulding;
(4) the nozzle work in-process are fired to 1550 ℃~1580 ℃ of firing temperatures, soaking time 4~5h, cooling finished product.
2. the preparation technology of a kind of alumina-ceramic nozzle according to claim 1, it is characterized in that, the described gypsum mold of step (1) adopts high strength β-terra alba or α-terra alba to make, the cream quality ratio of α-gypsum slurry is 1.5~1.8:1,801 glue of additional gypsum quality mark 5~10%, 901 glue or thermoplastic resin; The cream quality ratio of β-gypsum slurry is 1.5~1.9:1,801 glue of additional gypsum quality mark 5~10%, 901 glue or thermoplastic resin.
3. the preparation technology of a kind of alumina-ceramic nozzle according to claim 1, is characterized in that, in step (2), vacuum outgas vacuum tightness requires 0.7~0.9mPa.
4. the preparation technology of a kind of alumina-ceramic nozzle according to claim 1, is characterized in that, described other of step (2) become sorting barium carbonate, magnesium oxide, ground caustic to mix with the water glass arbitrary proportion.
5. the preparation technology of a kind of alumina-ceramic nozzle according to claim 1, is characterized in that, the slip casing by pressure described in step (3) selects 100~200 small transfer lines to inject 100~200 cover gypsum molds simultaneously.
CN201310482273.XA 2013-10-15 2013-10-15 Process for manufacturing aluminum oxide ceramic nozzle Expired - Fee Related CN103496954B (en)

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CN104402439A (en) * 2014-10-27 2015-03-11 安徽锐视光电技术有限公司 Boron carbide/alumina compounded ceramic nozzle and making method thereof
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CN104402445A (en) * 2014-10-27 2015-03-11 安徽锐视光电技术有限公司 High strength silicon carbide based ceramic nozzle and making method thereof
CN104402443A (en) * 2014-10-27 2015-03-11 安徽锐视光电技术有限公司 Wear and corrosion resistant silicon carbide based ceramic nozzle and making method thereof
CN104370520B (en) * 2014-10-28 2016-02-17 倪娟形 A kind of oil-burning machine nozzle heat-stable ceramic and preparation method thereof
CN104370520A (en) * 2014-10-28 2015-02-25 倪娟形 Heat-resisting ceramic for nozzle of fuel engine and preparation method of heat-resisting ceramic
CN104387088A (en) * 2014-10-29 2015-03-04 安徽省皖捷液压科技有限公司 Scrap rubber tire particle/silicon nitride composite ceramic nozzle and manufacturing method thereof
CN104387075A (en) * 2014-10-29 2015-03-04 安徽省皖捷液压科技有限公司 Diamond-micropowder-containing ceramic for nozzle and preparation method of diamond-micropowder-containing ceramic
CN104387082A (en) * 2014-10-29 2015-03-04 安徽省皖捷液压科技有限公司 Nano zirconium carbide ceramic nozzle and manufacturing method thereof
CN104355650A (en) * 2014-10-29 2015-02-18 安徽省皖捷液压科技有限公司 Cracking-resistant ceramic for nozzles and preparation method of crack-resisting ceramic
CN104446506A (en) * 2014-10-31 2015-03-25 中国航空工业集团公司基础技术研究院 Improved grouting method for preparing special ceramic
CN107324770A (en) * 2017-08-03 2017-11-07 福建省德化县华晨陶瓷有限公司 A kind of wear-resistant, high-low temperature resistant ceramic pan and its manufacturing process
CN107324770B (en) * 2017-08-03 2021-01-01 福建省德化县华晨陶瓷有限公司 Wear-resistant high-low temperature-resistant ceramic pot and manufacturing process thereof

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