CN104193322B - A kind of preparation method of high-compactness tindioxide one-component ceramic - Google Patents
A kind of preparation method of high-compactness tindioxide one-component ceramic Download PDFInfo
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Abstract
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps: that Polyethylene Glycol-600, tinfoil paper are obtained by reacting the stable mixing solutions containing tin, mn ion by A. under compressed oxygen atmosphere; B. the stable mixing solutions containing tin, mn ion steps A prepared adds oleic oil acid-respons, and reaction product is carried out pulverizing and namely obtained additive Mn tindioxide single phase nano powder; C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, stir and obtain stable slurry; Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding stannic oxide ceramic base substrate, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 5 ~ 7 hours in 900 ~ 1000 DEG C of sintered heat insulatings.Production cost of the present invention is low, powder sintering excellent performance, acquisition stannic oxide ceramic density high.
Description
Technical field
The present invention relates to a kind of preparation method of stannic oxide ceramic.
Background technology
Tin dioxide powder has the characteristics such as acidproof, alkaline-resisting, high temperature resistant, mechanical resistant impact as inorganic oxide material.Tin dioxide powder being sintered into pottery then can utilize above-mentioned characteristic to be made into the refractory materials of glass furnace, substitutes precious metal and is used as crucible, as thermocouple sheath etc.But tin dioxide powder belongs to special hard-to-sinter material, adopt conventional non-pressure sintering technology cannot sinter the pure stannic oxide ceramic of high-compactness.Large quantity research display, cupric oxide etc. can promote that tindioxide sinters (CN8510034, CN101001815B, CN102875142A), it is generally acknowledged that the sintering mechanism of cupric oxide is liquid phase sintering, namely cupric oxide is finally present in the crystal boundary of stannic oxide ceramic in a large number.Because acidproof, alkaline-resisting, high temperature resistant, the mechanical resistant impact characteristics of cupric oxide can not show a candle to tindioxide, therefore the cupric oxide being present in tindioxide crystal boundary has side effect for acidproof, alkaline-resisting, high temperature resistant, the mechanical resistant impact characteristics that tindioxide is intrinsic, should avoid using cupric oxide as sintering aid.
Research shows that mn ion also can promote that tin dioxide powder sinters, and its sintering mechanism is solid state sintering mechanism, namely mn ion can not by promoting the sintering of tindioxide in sintering process to the diffusion of tindioxide crystal boundary, mn ion can not be assembled by crystal boundary in stannic oxide ceramic, thus makes the stannic oxide ceramic obtained maintain acidproof, alkaline-resisting, high temperature resistant, the mechanical resistant impact characteristics of tin dioxide powder.Therefore manganese is good tindioxide sintering aid.
The sintering of usual stannic oxide ceramic all adopts pure tin dioxide powder, sintering aid powder and binding agent, dispersion agent etc. are raw material, first by batch mixing, wet ball grinding, dry, the step such as to sieve obtains raw material for sintering powder, then carries out dry-pressing, cold isostatic compaction, finally sintering obtains stannic oxide ceramic (CN8510034, CN102875142A, CN101001815B, CN101439967A, CN101830694B, CN102234194B, CN102811971A).It is simple that above-mentioned technique has technique, the advantages such as interpolation ion elements addition manner addition is flexible, but also there is shortcomings simultaneously, as raw material tindioxide and sintering aid powder granule are comparatively large, make powder sintering activity lower, be difficult to sintering and obtain high-compactness stannic oxide ceramic, sintering temperature is too high simultaneously, the high temperature of usual needs more than 1400 DEG C, and soaking time is long, this considerably increases sintering energy consumption and agglomerating plant input cost.Domestic industry produces 20 feather weight large size stannic oxide ceramics needs 1500 DEG C to sinter more than 7 days time usually.Sintering aid by solid phase diffusion extremely difficulty enter completely in stannic oxide ceramic, the sintering aid failing to enter then can have a negative impact to the properties of stannic oxide ceramic.In addition, the wet ball grinding process of material powder also can introduce foreign ion, causes sintering some degradation of stannic oxide ceramic obtained.
The reduction of powder granularity improves the sintering activity of powder, reduces sintering temperature, improves sintered density, particularly adopt nano-powder effect more obviously (S. J. Park, K. Hirota, H. yamamura, Densification of Nonadditive SnO
2by Hot Isostatic Pressing,
ceram. Inter., 1984,10,115-116; M. Yoshinaka, K. Hirota, M. Ito, H. Takano, O. Yamaguchi, Hot Isostatic Pressing of Reactive SnO 2 powder, J. Am. Ceram. Soc., 1999,82,216-218), simultaneously by just sintering aid ion being added to nano-powder when prepared by nano-powder preparation, then more can promote the sintering of powder, avoiding residual (CN101182096) of unnecessary sintering aid simultaneously.But the preparation of existing tindioxide matrix nano-powder is raw material substantially with tin chloride, adopt the precipitator method, hydrothermal method prepares (CN101182096, CN102976396A, CN103641157A, CN103613123A, CN101941734A), although it is simple that aforesaid method has technique, tindioxide matrix nano-powder can be obtained, but precipitation, containing a large amount of chlorion in intermediate product after hydro-thermal, the existence of chlorion not only produces heavy corrosion to production unit, the abnormal loaded down with trivial details poor efficiency of its washing removing, usually the deionized water wash that one kilogram of tin dioxide powder needs more than 150 kilograms is often produced, even so, the content of the chlorion of final residue in powder also can at more than 500ppm, the reunion that so high residual quantity can cause stannic oxide nano powder serious, also sintering can be hindered in follow-up ceramic post sintering process, and the chlorion that pyroprocess discharges can produce corrosion to agglomerating plant.Tin chloride is adopted to be that raw material is except above-mentioned negative consequence, the cost that tin chloride is relatively high also can cause stannic oxide nano powder high cost, on market, tin chloride is the price of the tin dioxide powder that raw material obtains is more than 3 times that the traditional tin of employing spends the tin dioxide powder price of nitrate method explained hereafter, stannic oxide ceramic is produced with this tin dioxide powder, the market competitiveness is extremely weak, the stannic oxide ceramic also not having enterprise to declare that it is produced at present be adopt tin chloride be raw material tin dioxide powder produce.
In sum, the stannic oxide nano powder doped with solid state sintering auxiliary agent mn ion adopting low cost direct production is raw material, and sintering stannic oxide ceramic is the effective way obtaining high-compactness tindioxide one-component ceramic.
Summary of the invention
In order to overcome the above-mentioned deficiency of the preparation method of existing stannic oxide ceramic, the invention provides that a kind of production cost is low, powder sintering excellent performance, acquisition the preparation method of the high high-compactness tindioxide one-component ceramic of stannic oxide ceramic density.
The technical scheme that the present invention solves its technical problem is: a kind of preparation method of high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 80 DEG C ~ 120 DEG C, mixing speed is 280 revs/min ~ 430 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.6 ~ 0.9 times of tinfoil paper quality, and the quality of compressed oxygen is 0.5 ~ 0.7 times of tinfoil paper quality, and manganese is 1:62.5 ~ 500 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 2 ~ 4:1, reactor is heated to 330 DEG C ~ 340 DEG C, stirring velocity is 70 revs/min ~ 100 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 5 ~ 7 hours in 900 ~ 1000 DEG C of sintered heat insulatings.
Beneficial effect of the present invention is: production cost is low, powder sintering excellent performance, acquisition stannic oxide ceramic density high.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment one
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 100 DEG C, mixing speed is 350 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.7 times of tinfoil paper quality, and the quality of compressed oxygen is 0.6 times of tinfoil paper quality, and manganese is 1:300 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 3:1, reactor is heated to 335 DEG C, stirring velocity is 80 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration (such as ball milling, grinding etc.), carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate (relative density here refers to the density of stannic oxide ceramic base substrate relative to stannic oxide ceramic entity) that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 950 DEG C of sintered heat insulatings 6 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment two
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 95 DEG C, mixing speed is 280 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.9 times of tinfoil paper quality, and the quality of compressed oxygen is 0.58 times of tinfoil paper quality, and manganese is 1:62.5 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 3.5:1, reactor is heated to 340 DEG C, stirring velocity is 85 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 900 DEG C of sintered heat insulatings 5 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment three
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 80 DEG C, mixing speed is 420 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.65 times of tinfoil paper quality, and the quality of compressed oxygen is 0.55 times of tinfoil paper quality, and manganese is 1:100 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 2.1:1, reactor is heated to 330 DEG C, stirring velocity is 100 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 1000 DEG C of sintered heat insulatings 5.2 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment four
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 120 DEG C, mixing speed is 410 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.85 times of tinfoil paper quality, and the quality of compressed oxygen is 0.5 times of tinfoil paper quality, and manganese is 1:70 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 2:1, reactor is heated to 333 DEG C, stirring velocity is 70 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 960 DEG C of sintered heat insulatings 7 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment five
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 85 DEG C, mixing speed is 430 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.6 times of tinfoil paper quality, and the quality of compressed oxygen is 0.67 times of tinfoil paper quality, and manganese is 1:500 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 2.5:1, reactor is heated to 336 DEG C, stirring velocity is 95 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 920 DEG C of sintered heat insulatings 5.5 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment six
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 110 DEG C, mixing speed is 320 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.8 times of tinfoil paper quality, and the quality of compressed oxygen is 0.65 times of tinfoil paper quality, and manganese is 1:200 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 3.2:1, reactor is heated to 339 DEG C, stirring velocity is 72 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 910 DEG C of sintered heat insulatings 6.7 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment seven
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 90 DEG C, mixing speed is 300 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.62 times of tinfoil paper quality, and the quality of compressed oxygen is 0.53 times of tinfoil paper quality, and manganese is 1:450 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 4:1, reactor is heated to 337 DEG C, stirring velocity is 82 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 970 DEG C of sintered heat insulatings 6.5 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment eight
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 105 DEG C, mixing speed is 400 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.75 times of tinfoil paper quality, and the quality of compressed oxygen is 0.62 times of tinfoil paper quality, and manganese is 1:75 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 2.8:1, reactor is heated to 338 DEG C, stirring velocity is 75 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 930 DEG C of sintered heat insulatings 5.8 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Embodiment nine
A preparation method for high-compactness tindioxide one-component ceramic, comprises the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 115 DEG C, mixing speed is 370 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.83 times of tinfoil paper quality, and the quality of compressed oxygen is 0.7 times of tinfoil paper quality, and manganese is 1:150 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 3.7:1, reactor is heated to 332 DEG C, stirring velocity is 90 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained high-compactness tindioxide one-component ceramic in 980 DEG C of sintered heat insulatings 6.3 hours, and carrying out X-ray diffraction test to pottery, to be shown as tindioxide single-phase.
Claims (1)
1. a preparation method for tindioxide one-component ceramic, is characterized in that comprising the following steps:
A. Polyethylene Glycol-600 is placed in the closed reactor with heating, agitating function, open heating, stir, be heated to confined reaction temperature in the kettle to 80 DEG C ~ 120 DEG C, mixing speed is 280 revs/min ~ 430 revs/min, tinfoil paper is poured in reactor, pass into compressed oxygen to reactor, react to tinfoil paper and all dissolve, stop heating, then manganese acetate is joined in above-mentioned solution the stable mixing solutions obtained containing tin, mn ion;
Wherein, the quality of Polyethylene Glycol-600 is 0.6 ~ 0.9 times of tinfoil paper quality, and the quality of compressed oxygen is 0.5 ~ 0.7 times of tinfoil paper quality, and manganese is 1:62.5 ~ 500 with the ratio of the amount of substance of tin;
What B. steps A prepared contains tin, the stable mixing solutions of mn ion joins with heating, in agitating function reactor, and oleic acid is heated in reactor, the mass ratio of the Polyethylene Glycol-600 in oleic acid quality and steps A is 2 ~ 4:1, reactor is heated to 330 DEG C ~ 340 DEG C, stirring velocity is 70 revs/min ~ 100 revs/min, stirring reaction stops heating after 5 hours, stir, reaction product is pumped in plate-and-frame filter press and carries out solid-liquid separation, and filter cake is placed in deionized water washing by soaking some times, often wash and change a deionized water, the mass percentage of the oleic acid just after washing in deionized water is lower than 0.1%, then filter cake is dried to biodiversity percentage composition lower than 0.5% in 180 DEG C, the filter cake of oven dry is first carried out mechanical disintegration, carry out comminution by gas stream again and namely obtain additive Mn tindioxide single phase nano powder,
C. the additive Mn tindioxide single phase nano powder obtained and polyvinyl alcohol, deionized water are mixed, wherein the mass percentage of additive Mn tindioxide single phase nano powder is 30%, the mass percentage of polyvinyl alcohol is 0.2%, the mass percentage of deionized water is 69.8%, adopts high-shear emulsion machine to carry out stirring and obtains stable slurry;
Slurry is pumped into Pressuresprayingdrier and carries out mist projection granulating, the heat source temperature of Pressuresprayingdrier is 300 DEG C, and the temperature out of Pressuresprayingdrier is 160 DEG C;
The powder obtained through Pressuresprayingdrier mist projection granulating is carried out compression molding and obtain the stannic oxide ceramic base substrate that relative density is 55 ~ 58%, namely this ceramic body is obtained tindioxide one-component ceramic in 5 ~ 7 hours in 900 ~ 1000 DEG C of sintered heat insulatings.
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| CN1357509A (en) * | 2000-12-14 | 2002-07-10 | 成都亿安方博低维材料科技有限公司 | Transparent conductive nano Sb:SnO2 fine powder |
| CN1994965A (en) * | 2006-12-08 | 2007-07-11 | 中南大学 | Process for preparing antimony doped stannic oxide nano powder |
| CN101182188A (en) * | 2007-11-23 | 2008-05-21 | 福州大学 | Method for preparing nano-grade rutile phase RuO2-SnO2 oxide |
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