CN102268196A - Preparation method of conductive powder with antimony-doped tin oxide (ATO) coated transparent sheet core material - Google Patents
Preparation method of conductive powder with antimony-doped tin oxide (ATO) coated transparent sheet core material Download PDFInfo
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Abstract
Belonging to the chemical field, the invention relates to a preparation method of conductive powder with an antimony-doped tin oxide (ATO) coated transparent sheet core material. In the method, the surface of the sheet material is subjected to mixed coating with an Sb/Sn oxide so as to make Sb doped into SnO2 crystal lattices and make the coating layer become a P-type semiconductor of low resistivity. As the semiconductor layer is on the surface of the sheet material, the specific surface area of the conductive material is increased and the consumption of the semiconductor material is reduced. Furthermore, by means of organic modification on the surface of the powder prepared, the conductive powder of the invention can bring the excellent bonding force and conductive performance into play in an organic system.
Description
Technical field
The present invention relates to the preparation method that a kind of stibium doping stannic oxide coats the conducting powder of transparent sheet-like core, belong to chemical field.
Background technology
Impurity in the semi-conductor is very big to the influence of resistivity.When mixing trace impurity in the semi-conductor, near the cycle potential field the impurity atoms is interfered and forms additional bound state, produces impurity level in the forbidden band.At SnO
2When mixing impurity atomss such as trivalent element Sb in the crystal, impurity atoms forms the covalent attachment fashion with four tin atoms on every side and lacks an electronics, thereby having a room, the corresponding energy state in room is exactly an impurity level therewith, is usually located at the below, forbidden band near the valence band place.Electronics in the valence band is very easy excitated fills up this room on impurity level, make impurity atoms become negative ion.Form a hole carrier owing to lacking an electronics in the valence band.This impurity in hole that can provide is called acceptor impurity.When having acceptor impurity, it is more much smaller than proper semiconductor situation to form a hole carrier institute energy requirement in valence band, and its resistivity descends greatly behind the semiconductor doping.
Semi-conductor can both produce electron-hole pair under any temperature, thermal excitation that heating or illumination produce or optical excitation all can make the free carrier number increase and cause resistivity to reduce.
Along with doping content increases, it is good more that semi-conductive electroconductibility will become within the specific limits, and reason is that the electron amount that can enter the conduction band can improve and increase along with doping content.But after reaching a certain threshold value, continue to improve doped level, electron density is tending towards a saturation value, and this moment, tramp material generated nonconducting second mutually with the oxygen reaction, caused electronic mobility sharply to descend, and resistivity is rising trend.
Stibium doping stannic oxide (ATO) conductive powder body has special photoelectric properties, is a kind of Multifunction transparent conductive material that has development potentiality.Along with the development of electronic industry, and the continuous expansion of macromolecular material Application Areas, this conducting powder physical efficiency is widely used in the antistatic conductive electric material.Its excellent conducting performance makes it can be used for electro-conductive fiber, rubber, pottery, plastics, Antistatic Paint and conductive filler material, can replace platinum or rare metal to be used in glass melting furnace and chemical industry as electrode materials; Also be used for semi-conductor pole plate storage vessel, solar cell material is in the various fields such as semiconductor gas sensor and humidity-sensitive element; And liquid-crystal display (LCD), geseous discharge demonstration, electroluminescent demonstration (ELD), flat teletube, fluorescence demonstration and electricity cause the transparent conducting coating that colour TV shows various display devices such as (ECD).Secondly; the ATO material has good optics light-coloured transparent, high transmitance, good functions such as antireflective, radioprotective and infrared absorption; the shielding protection district that is widely used in low-E glass for building, radar is in the fields such as the transparent window of anti-electromagnetic interference, infrared absorption lagging material.
At present more about the relevant report of stibium doping stannic oxide class inorganic composite type conducting powder, for example mention among Du Pont's patent CN1054139 a kind of with white mica as core, the outer conducting powder that coats stibium doping stannic oxide, but this method is at the outer increase one deck hydroxylation silica dioxide coating that needs of mica; Also mention a kind of inorganic composite type conducting powder among the patent CN1847156A of Shanghai Institute Of Technology, but the conducting powder composition relative complex that this method makes, technology is also comparatively loaded down with trivial details, and these have all increased production cost virtually.Mention the method that a kind of skin of making core with kaolin coats the compound-type conducting powder of antimony-doped tin oxide among the patent CN101174485A of Central South University, solved the kaolinic problem of utilizing well.But conducting powder finally is to be applied in the organic system, seldom mention in the conducting powder patent in the past conducting powder is carried out the surface-treated problem, the addition of not surface treated conducting powder in the organic resin system is limited, and obviously can increase the viscosity of compound system.
Summary of the invention
Technical problem to be solved by this invention provide a kind of technological design rationally, low, the constant product quality of strong, the obviously enhancing of product electroconductibility of the bonding force between utilization ratio height, powder and the organism of transparent sheet-like base material, energy-conserving and environment-protective, cost, stibium doping stannic oxide coat the preparation method of the conducting powder of transparent sheet-like core.
It is the preparation method that this stibium doping stannic oxide coats the conducting powder of transparent sheet-like core that the present invention solves the problems of the technologies described above the technical scheme that is adopted, and the step of its preparation is:
A, transparent sheet-like base material 45～65 weight parts that take by weighing median size 1～100 μ m place reactor, add the deionized water that is equivalent to 5～15 times of base material powder weight again in reactor, stir evenly;
B, add inorganic acid for adjusting pH value to 1.0～5.0 then, 30～70 ℃ of controlled temperature are made the core aqeous suspension;
C, with the SnCl of 60～100 weight parts
45H
2The SbCl of O and 3～10 weight parts
3Place container, add concentration and be 32% hydrochloric acid and make it dissolving, be diluted to SnCl with deionized water again
45H
2O and SbCl
3Total mass concentration be the solution of 200～400g/L, make tin antimony mixed solution;
D, tin antimony mixed solution is at the uniform velocity pumped in the core aqeous suspension, 300～600 rev/mins of control stirring velocitys are kept temperature of reaction at 30～70 ℃, and are kept pH value at 1.0～5.0 with alkali lye, continue to stir 1 hour so that its reaction is thorough, obtain mother liquor;
E, the mother liquor vacuum is filtered, with deionized water with compacting after the filter cake flushing 5～10 times;
F, with the filter cake after the compacting in 80～150 ℃ of oven dry, obtain powder, more dried powder is calcined;
G, the powder after will calcining are cooled to room temperature, again be scattered in it in deionized water then, be warming up to 40～80 ℃, 200～500 rev/mins of rotating speeds, regulate pH value to 3.0～10.0, pour the coating materials that is equivalent to powder weight 0.1～3.0% then into, insulated and stirred 10～60 minutes obtains the conducting powder slurry;
H, with the conducting powder slurries filtration, wash 1～3 time, 90～120 ℃ of oven dry in baking oven obtain the conducting powder that loose stibium doping stannic oxide coats the transparent sheet-like core.
As preferably, the calcining among the step f of the present invention is for to calcine according to certain temperature rise rate, and the calcining temperature rise rate is as follows: normal temperature～200 ℃: heat up 25～30 ℃/minute; 200～850 ℃: heat up 10～15 ℃/minute, be incubated 1～3 hour down at 750～850 ℃.
As preferably, transparent sheet-like base material of the present invention is natural mica, synthetic mica, glass flake, tabular alumina or flaky silicon dioxide.
As preferably, the median size of transparent sheet-like base material of the present invention is 1～10 μ m.
As preferably, mineral acid of the present invention is one or more the mixing in hydrochloric acid, nitric acid, sulfuric acid, the phosphoric acid.
As preferably, alkali lye of the present invention is a kind of in sodium hydroxide solution, the ammoniacal liquor or both mixing.
As preferably, coating materials of the present invention is the KH-590(3-mercaptopropyl trimethoxysilane), the KH-570(methacryloxypropyl trimethoxy silane), KH-560(3-glycidyl ether oxygen base propyl trimethoxy silicane), the KH-550(3-aminopropyl triethoxysilane), KH-902(Y-aminopropyl methyldiethoxysilane), KH-792(3-(2-aminoethyl)-aminopropyl trimethoxysilane), KH-602(3-(2-aminoethyl)-aminopropyl methyl dimethoxysilane), the A-171(vinyltrimethoxy silane), the A-151(vinyltriethoxysilane), A-172(vinyl three (2-methoxy ethoxy) silane), A-1130(diethylenetriamine base propyl trimethoxy silicane), the mixing of one or more A-1160(3-urea groups propyl-triethoxysilicane).
The present invention compares with existing technology, have the following advantages and characteristics: the present invention mainly is to be core with ultra-fine mica powder (or other transparent sheet-like material), with chemical precipitation method the tindioxide of antimony dopant evenly is coated on its surface, if after surface treatment, the addition of conducting powder in organic system obviously increases, and make conducting powder and organic system that superior bonding force be arranged, the electroconductibility of compound system obviously strengthens.The present invention simultaneously simplifies the preparation technology of inorganic composite type conducting powder, makes production cost reduce greatly.The conducting powder that the present invention obtains has excellent electroconductibility and good dispersiveness (need not grind), powder outward appearance look more shallow, be easy to toning, and the base material cost is lower, obtain easily (can from the fine mica powder that produces in the wet method mica production process), and this conducting powder and base material have excellent bonding force, are fit to the application of multiple antistatic, electromagnetic shielding occasion.The conducting powder of the present invention's preparation has excellent conductivity, and average resistivity can be widely used in the antistatic material and have good dispersing property reaching more shallow outward appearance look less than 3.0 Ω cm.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1:
Adding the natural mica powder of 50g median size 1～10 μ m in the 1000ml beaker, add deionized water to liquid level 500ml, be stirred into the mica slurry, be warming up to 60 ℃, is 32% hydrochloric acid adjusting pH to 3.0 with concentration.
Accurately take by weighing 105g SnCl
45H
2O and 5g SbCl
3In the 500ml beaker, add 125ml concentration and be 32% hydrochloric acid and make it dissolving, it is stand-by to be diluted to 250ml with deionized water again.
The tin antimony mixing solutions that the prepares speed by 50ml/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 3.0 simultaneously, 60 ℃ of holding temperatures, 400 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 5 times, the filter cake compacting, go into baking oven in 100 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 60 ℃, 200 rev/mins of rotating speeds, regulate slurry pH value to 5.0 with 20%NaOH solution, the silane coupling agent KH-570(γ-methacryloxypropyl trimethoxy silane that will be equivalent to conducting powder weight 2.0% then) directly pours in the conducting powder slurry under the high-speed stirring, insulated and stirred 60 minutes, filter, wash 3 times, 120 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 3.0 Ω cm.
Embodiment 2:
Adding the natural mica powder of 4kg median size 1～10 μ m in the 80L reactor, add deionized water to liquid level 40L, be stirred into the mica slurry, be warming up to 60 ℃, is 32% hydrochloric acid adjusting pH to 3.0 with concentration.
Accurately take by weighing 8.4kg SnCl
45H
2O and 400g SbCl
3In the 20L container, add 10L concentration and be 32% hydrochloric acid and make it dissolving, it is stand-by to be diluted to 20L with deionized water again.
The tin antimony mixing solutions that the prepares speed by 2.8L/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 3.0 simultaneously, 60 ℃ of holding temperatures, 400 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 5 times, the filter cake compacting, go into baking oven in 120 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 70 ℃, 220 rev/mins of rotating speeds, regulate slurry pH value to 8.0 with 20%NaOH solution, the silane coupling agent KH-590(γ-mercaptopropyl trimethoxysilane that will be equivalent to conducting powder weight 1.5% then) directly pours in the conducting powder slurry under the high-speed stirring, insulated and stirred 40 minutes, filter, wash 3 times, 120 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 2.8 Ω cm.
Embodiment 3:
Adding the natural mica powder of 400kg median size 1～10 μ m in the 8000L reactor, add deionized water to liquid level 4000L, be stirred into the mica slurry, be warming up to 60 ℃, is 32% hydrochloric acid adjusting pH to 3.0 with concentration.
Accurately take by weighing 840kg SnCl
45H
2O and 40kg SbCl
3In the 2000L container, add 1000L concentration and be 32% hydrochloric acid and make it dissolving, it is stand-by to be diluted to 2000L with deionized water again.
The tin antimony mixing solutions that the prepares speed by 200L/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 3.0 simultaneously, 60 ℃ of holding temperatures, 400 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 5 times, the filter cake compacting, go into baking oven in 140 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 50 ℃, 260 rev/mins of rotating speeds, regulate slurry pH value to 7.5 with 20%NaOH solution, the silane coupling agent KH-560(3-(2 that will be equivalent to conducting powder weight 2.0% then, 3-epoxy third oxygen) propyl trimethoxy silicane) directly pour in the conducting powder slurry under the high-speed stirring, insulated and stirred 60 minutes, filter, wash 3 times, 120 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 2.6 Ω cm.
Embodiment 4:
Adding the compound mica of 40g median size 1～10 μ m in the 1000ml beaker, add deionized water to liquid level 600ml, be stirred into the mica slurry, be warming up to 70 ℃, is 32% hydrochloric acid adjusting pH to 1.5 with concentration.
Accurately take by weighing 80g SnCl
45H
2O and 8g SbCl
3In the 500ml beaker, add 100ml concentration and be 32% hydrochloric acid and make it dissolving, it is stand-by to be diluted to 300ml with deionized water again.
The tin antimony mixing solutions that the prepares speed by 40ml/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 3.0 simultaneously, 50 ℃ of holding temperatures, 350 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 5 times, the filter cake compacting, go into baking oven in 100 ℃ of oven dry, more dried powder was calcined 60 minutes in 800 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 80 ℃, 200 rev/mins of rotating speeds, regulate slurry pH value to 4.0 with 20%NaOH solution, the silane resin acceptor kh-550 (vinyltriethoxysilane) that will be equivalent to conducting powder weight 1.0% is then directly poured in the conducting powder slurry under the high-speed stirring, insulated and stirred 30 minutes, filter, wash 3 times, 110 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 3.1 Ω cm.
Embodiment 5:
Add the synthetic mica powder of 50g median size 1～10 μ m in the 1000ml beaker, add deionized water to liquid level 400ml, the form slurry that stirs is warming up to 65 ℃, is 32% hydrochloric acid adjusting pH to 2.5 with concentration.
Accurately take by weighing 95 SnCl
45H
2O and 18g SbCl
3In the 500ml beaker, add 200ml concentration and be 32% hydrochloric acid and make it dissolving, it is stand-by to be diluted to 400ml with deionized water again.
The tin antimony mixing solutions that the prepares speed by 50ml/ hour is at the uniform velocity pumped in the above-mentioned tabular alumina slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 2.5 simultaneously, 65 ℃ of holding temperatures, 450 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 5 times, the filter cake compacting, go into baking oven in 150 ℃ of oven dry, more dried powder was calcined 70 minutes in 750 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 75 ℃, 300 rev/mins of rotating speeds, regulate slurry pH value to 9.5 with 20%NaOH solution, the silane coupling agent KH-570(γ-methacryloxypropyl trimethoxy silane that will be equivalent to conducting powder weight 1.5% then) directly pours in the conducting powder slurry under the high-speed stirring, insulated and stirred 45 minutes, filter, wash 3 times, 120 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 2.7 Ω cm.
Embodiment 6:
Adding the natural mica powder of 45g median size 1～10 μ m in the 1000ml beaker, add deionized water 225ml, be stirred into the mica slurry, be warming up to 30 ℃, is 32% hydrochloric acid adjusting pH to 4.0 with concentration.
Accurately take by weighing 60g SnCl
45H
2O and 4g SbCl
3In the 500ml beaker, add 125ml concentration and be 32% hydrochloric acid and make it dissolving, be diluted to SnCl with deionized water again
45H2O and SbCl
3Total mass concentration be the solution of 200g/L.
The tin antimony mixing solutions that the prepares speed by 50ml/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 1.0 simultaneously, 70 ℃ of holding temperatures, 500 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 6 times, the filter cake compacting, go into baking oven in 120 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 40 ℃, 400 rev/mins of rotating speeds, regulate slurry pH value to 3.0 with 20%NaOH solution, the KH-590(3-mercaptopropyl trimethoxysilane that will be equivalent to conducting powder weight 3.0% then) directly pours in the conducting powder slurry under the high-speed stirring, insulated and stirred 50 minutes, filter, wash 2 times, 110 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 2.8 Ω cm.
Embodiment 7:
Adding the natural mica powder of 47g median size 1～10 μ m in the 1000ml beaker, add deionized water 280ml, be stirred into the mica slurry, be warming up to 40 ℃, is 32% hydrochloric acid adjusting pH to 5.0 with concentration.
Accurately take by weighing 75g SnCl
45H
2O and 3g SbCl
3In the 500ml beaker, add 125ml concentration and be 32% hydrochloric acid and make it dissolving, be diluted to SnCl with deionized water again
45H2O and SbCl
3Total mass concentration be the solution of 400g/L.
The tin antimony mixing solutions that the prepares speed by 50ml/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 4.0 simultaneously, 50 ℃ of holding temperatures, 600 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 8 times, the filter cake compacting, go into baking oven in 150 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 80 ℃, 500 rev/mins of rotating speeds, regulate slurry pH value to 10.0 with 20%NaOH solution, A-172(vinyl three (2-methoxy ethoxy) silane that will be equivalent to conducting powder weight 1.0% then), the A-1130(diethylenetriamine base propyl trimethoxy silicane that is equivalent to conducting powder weight 1.0%), the A-1160(3-urea groups propyl-triethoxysilicane that is equivalent to conducting powder weight 1.0%) directly pours in the conducting powder slurry under the high-speed stirring, insulated and stirred 20 minutes, filter, wash 1 time, 90 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 2.8 Ω cm.
Embodiment 8:
Adding the natural mica powder of 65g median size 1～10 μ m in the 1000ml beaker, add deionized water 975ml, be stirred into the mica slurry, be warming up to 50 ℃, is 32% hydrochloric acid adjusting pH to 1.0 with concentration.
Accurately take by weighing 100g SnCl
45H
2O and 8g SbCl
3In the 500ml beaker, add 125ml concentration and be 32% hydrochloric acid and make it dissolving, be diluted to SnCl with deionized water again
45H2O and SbCl
3Total mass concentration be the solution of 250g/L.
The tin antimony mixing solutions that the prepares speed by 50ml/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 2.0 simultaneously, 60 ℃ of holding temperatures, 250 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 9 times, the filter cake compacting, go into baking oven in 140 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 50 ℃, 350 rev/mins of rotating speeds, regulate slurry pH value to 8.0 with 20%NaOH solution, the KH-560(3-glycidyl ether oxygen base propyl trimethoxy silicane that will be equivalent to conducting powder weight 1.0% then), the KH-550(3-aminopropyl triethoxysilane that is equivalent to conducting powder weight 1.0%), the KH-902(Y-aminopropyl methyldiethoxysilane that is equivalent to conducting powder weight 1.0%) directly pours in the conducting powder slurry under the high-speed stirring, insulated and stirred 40 minutes, filter, wash 2 times, 100 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 2.9 Ω cm.
Embodiment 9:
Adding the natural mica powder of 63g median size 1～10 μ m in the 1000ml beaker, add deionized water 880ml, be stirred into the mica slurry, be warming up to 35 ℃, is 32% hydrochloric acid adjusting pH to 2.0 with concentration.
Accurately take by weighing 65g SnCl
45H
2O and 9g SbCl
3In the 500ml beaker, add 125ml concentration and be 32% hydrochloric acid and make it dissolving, be diluted to SnCl with deionized water again
45H2O and SbCl
3Total mass concentration be the solution of 350g/L.
The tin antimony mixing solutions that the prepares speed by 50ml/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 2.0 simultaneously, 40 ℃ of holding temperatures, 400 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 6 times, the filter cake compacting, go into baking oven in 130 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 70 ℃, 300 rev/mins of rotating speeds, regulate slurry pH value to 9.0 with 20%NaOH solution, A-172 KH-792(3-(2-the aminoethyl)-aminopropyl trimethoxysilane that will be equivalent to conducting powder weight 1.0% then), KH-602(3-(2-the aminoethyl)-aminopropyl methyl dimethoxysilane that is equivalent to conducting powder weight 1.0%), the A-171(vinyltrimethoxy silane that is equivalent to conducting powder weight 1.0%) directly pours in the conducting powder slurry under the high-speed stirring, insulated and stirred 50 minutes, filter, wash 2 times, 100 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 2.9 Ω cm.
Embodiment 10:
Adding the natural mica powder of 55g median size 1～10 μ m in the 1000ml beaker, add deionized water 660ml, be stirred into the mica slurry, be warming up to 55 ℃, is 32% hydrochloric acid adjusting pH to 2.0 with concentration.
Accurately take by weighing 70g SnCl
45H
2O and 7g SbCl
3In the 500ml beaker, add 125ml concentration and be 32% hydrochloric acid and make it dissolving, be diluted to SnCl with deionized water again
45H2O and SbCl
3Total mass concentration be the solution of 200g/L.
The tin antimony mixing solutions that the prepares speed by 50ml/ hour is at the uniform velocity pumped in the above-mentioned mica slurry of high-speed stirring, use the solution-stabilized slurry pH of 20% NaOH 4.0 simultaneously, 70 ℃ of holding temperatures, 300 rev/mins of rotating speeds, the reinforced back of finishing continues to stir 1 hour, the slurry vacuum is filtered again and adds deionized water rinsing 5 times, the filter cake compacting, go into baking oven in 110 ℃ of oven dry, more dried powder was calcined 90 minutes in 850 ℃ of insulations; After treating that burnt powder is cooled to room temperature, again be scattered in it in deionized water, be warming up to 60 ℃, 400 rev/mins of rotating speeds, regulate slurry pH value to 8.0 with 20%NaOH solution, the A-151(vinyltriethoxysilane that will be equivalent to conducting powder weight 1.0% then), A-172(vinyl three (2-methoxy ethoxy) silane that is equivalent to conducting powder weight 1.0%) directly pour in the conducting powder slurry under the high-speed stirring, insulated and stirred 60 minutes, filter, wash 3 times, 110 ℃ of oven dry promptly get loose light green conducting powder in baking oven, and the powder average resistivity is less than 3.0 Ω cm.
In addition, need to prove, the specific embodiment described in this specification sheets, its prescription, title that technology is named etc. can be different.Allly conceive equivalence or the simple change that described structure, feature and principle are done, be included in the protection domain of patent of the present invention according to patent of the present invention.The technician of the technical field of the invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment; only otherwise depart from structure of the present invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.
Though the present invention with embodiment openly as above; but it is not in order to limit protection scope of the present invention; any technician who is familiar with this technology, change and the retouching done in not breaking away from design of the present invention and scope all should belong to protection scope of the present invention.
Claims (7)
1. a stibium doping stannic oxide coats the preparation method of the conducting powder of transparent sheet-like core, and the step of its preparation is:
A, transparent sheet-like base material 45～65 weight parts that take by weighing median size 1～100 μ m place reactor, add the deionized water that is equivalent to 5～15 times of base material powder weight again in reactor, stir evenly;
B, add inorganic acid for adjusting pH value to 1.0～5.0 then, 30～70 ℃ of controlled temperature are made the core aqeous suspension;
C, with the SnCl of 60～100 weight parts
45H
2The SbCl of O and 3～10 weight parts
3Place container, add concentration and be 32% hydrochloric acid and make it dissolving, be diluted to SnCl with deionized water again
45H
2O and SbCl
3Total mass concentration be the solution of 200～400g/L, make tin antimony mixed solution;
D, tin antimony mixed solution is at the uniform velocity pumped in the core aqeous suspension, 300～600 rev/mins of control stirring velocitys are kept temperature of reaction at 30～70 ℃, and are kept pH value at 1.0～5.0 with alkali lye, continue to stir 1 hour so that its reaction is thorough, obtain mother liquor;
E, the mother liquor vacuum is filtered, with deionized water with compacting after the filter cake flushing 5～10 times;
F, with the filter cake after the compacting in 80～150 ℃ of oven dry, obtain powder, more dried powder is calcined;
G, the powder after will calcining are cooled to room temperature, again be scattered in it in deionized water then, be warming up to 40～80 ℃, 200～500 rev/mins of rotating speeds, regulate pH value to 3.0～10.0, pour the coating materials that is equivalent to powder weight 0.1～3.0% then into, insulated and stirred 10～60 minutes obtains the conducting powder slurry;
H, with the conducting powder slurries filtration, wash 1～3 time, 90～120 ℃ of oven dry in baking oven obtain the conducting powder that loose stibium doping stannic oxide coats the transparent sheet-like core.
2. stibium doping stannic oxide according to claim 1 coats the preparation method of the conducting powder of transparent sheet-like core, it is characterized in that: the calcining among the described step f is for to calcine according to certain temperature rise rate, and the calcining temperature rise rate is as follows: normal temperature～200 ℃: heat up 25～30 ℃/minute; 200～850 ℃: heat up 10～15 ℃/minute, be incubated 1～3 hour down at 750～850 ℃.
3. stibium doping stannic oxide according to claim 1 coats the preparation method of the conducting powder of transparent sheet-like core, and it is characterized in that: described transparent sheet-like base material is natural mica, synthetic mica, glass flake, tabular alumina or flaky silicon dioxide.
4. coat the preparation method of the conducting powder of transparent sheet-like cores according to claim 1 or 3 described stibium doping stannic oxides, it is characterized in that: the median size of described transparent sheet-like base material is 1～10 μ m.
5. stibium doping stannic oxide according to claim 1 coats the preparation method of the conducting powder of transparent sheet-like core, it is characterized in that: described mineral acid is one or more the mixing in hydrochloric acid, nitric acid, sulfuric acid, the phosphoric acid.
6. stibium doping stannic oxide according to claim 1 coats the preparation method of the conducting powder of transparent sheet-like core, it is characterized in that: described alkali lye is a kind of in sodium hydroxide solution, the ammoniacal liquor or both mixing.
7. stibium doping stannic oxide according to claim 1 coats the preparation method of the conducting powder of transparent sheet-like core, it is characterized in that: described coating materials is one or more the mixing among KH-590, KH-570, KH-560, KH-550, KH-902, KH-792, KH-602, A-171, A-151, A-172, A-1130, the A-1160.
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| CN111205738A (en) * | 2020-03-06 | 2020-05-29 | 涂创时代(苏州)科技开发有限公司 | Low-zinc anticorrosive composition compounded by graphene and flaky conductive material and application thereof |
| CN111205738B (en) * | 2020-03-06 | 2021-08-17 | 涂创时代(苏州)科技开发有限公司 | Low-zinc anticorrosive composition compounded by graphene and flaky conductive material and application thereof |
| CN114685861A (en) * | 2022-03-14 | 2022-07-01 | 太原理工大学 | A kind of fly ash loaded nano antimony doped tin oxide composite material and preparation method thereof |
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