CN101468397B - Method for preparing ATO conductive powder using nano antimony oxide and tin oxide powder - Google Patents
Method for preparing ATO conductive powder using nano antimony oxide and tin oxide powder Download PDFInfo
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- CN101468397B CN101468397B CN200710304877XA CN200710304877A CN101468397B CN 101468397 B CN101468397 B CN 101468397B CN 200710304877X A CN200710304877X A CN 200710304877XA CN 200710304877 A CN200710304877 A CN 200710304877A CN 101468397 B CN101468397 B CN 101468397B
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Abstract
The invention relates to a method for preparing ATO conductive powder by nano antimony oxide powder and nano tin oxide powder. The method comprises: charging nano tin oxide powder and nano antimony oxide powder in a V-shaped mixing machine according to the proportion of 80-98:20-2, and mixing both powder for 30 to 120min by a dry method to form mixed powder preliminarily; charging the mixed powder and then carnelian ball and solvent in a carnelian tank according to the proportion of 1:0.5-1.5:1-5, and stirring the three substances evenly by a glass rod; then, putting the substances in a ball mill for ball milling, and the ball milling process is that the rotation speed of the ball mill is 200 to 400r/min and the ball milling time is 1 to 8h; putting slurry obtained after ball milling into a drying box for drying, and crushing and sieving the slurry after drying; and finally, calcining the powder in air at a temperature of between 800 and 1,200 DEG C for 2 to 8h so as to obtain top-quality ATO conductive powder. Moreover, the solvent is one or a combination of alcohol, acetone, distilled water and deionized water.
Description
Technical field
The invention belongs to the material technology field, specially refer to the method that a kind of nano oxidized antimony and stannic oxide powder prepare the ATO conducting powder.
Background technology
Stibium doping stannic oxide, English name are Antimony doped tin oxide, are called for short ATO, are a kind of metal oxide composite powders with excellent conductive capability, have characteristics high temperature resistant, corrosion-resistant, good mechanical stability.As the novel conductive filler, can be used for the antistatic of material, be widely used in anti-static plastic, coating, fiber and display with antistatic antiradiation coating material, its effect is better than traditional carbon black and metal-powder.Also can be used for aspects such as INFRARED ABSORPTION heat-barrier material, gas sensor and solar energy electrode material.
At present, the preparation method of ATO powder is mainly coprecipitation.Coprecipitation is with SnCl
45H
2O and SbCl
3Be raw material, add a certain amount of hydrochloric acid solution then, form strongly acidic solution, strongly acidic solution and alkaline solution such as ammoniacal liquor are added fill in the container of a certain amount of distilled water and constant temperature again, keep certain pH value, and continue stirring until reaction and finish, form and precipitate.The mother liquor that will contain precipitation filtered then in still aging a period of time of room temperature, and the gained filter cake is successively with distilled water and alcohol washing several.Washing back gained filter cake is dry at a certain temperature, obtains dry powder.With dry powder a period of time of heat treatment at high temperature, promptly get the ATO powder at last.
Coprecipitation is produced the ATO powder and is had some shortcomings:
1) because Sb
3+And Sn
4+All be very easy to hydrolysis, at SnCl
4And SbCl
3Solution mixed process in to add a large amount of hydrochloric acid and suppress hydrolysis, add a large amount of alkali then and make it hydrolytic precipitation, this not only causes production cost to improve, and also can cause the washing of precipitation extremely difficult, Cl
-Residual Cl is removed in extremely difficult washing
-The hard aggregation that can cause powder.
2) in alkaline solution (as ammoniacal liquor) neutralization precipitation process, because Sb
3+And Sn
4+Hydrolysis is asynchronous, and the ATO presoma that co-precipitation makes is actually Sn (OH)
4And Sb
4O
5Cl
2The ATO powder that the heterogeneous mixture of two kinds of precipitations, co-precipitation make can not be realized real fully evenly doping.
3) in the process of producing, use a large amount of bronsted lowry acids and bases bronsted lowries, store, use very inconvenience, the gas of volatilization has very strong excitant, is detrimental to health, and the acid or the alkali wasteliquid of draining simultaneously pollute the environment.
4) production cycle longer, complex manufacturing process, process procedure is more, is difficult to realize the control that becomes more meticulous of producing in batches, the poor stability of technology.
Summary of the invention
For addressing the above problem; the purpose of this invention is to provide the method that a kind of nano oxidized antimony and stannic oxide powder prepare the ATO conducting powder; this method can be made the ATO conductive powder of different Sb dopings according to required powder components in certain proportion allotment, can realize the large-scale production of ATO conductive powder.Because the granularity of nanometer powder is little, the surface can be bigger, can reduce the calcining heat and the time of ATO powder, reduces production costs.
For achieving the above object, the present invention adopts following technical scheme:
Described nano oxidized antimony and stannic oxide powder prepare the method for ATO conducting powder, earlier in nano tin dioxide: nano oxidized antimony=80～98: 20～2 ratio is packed two kinds of powder in the V-type batch mixer, dry method is mixed powder 30～120min, and two kinds of powder tentatively are mixed into mixed-powder; Again in mixed-powder: agate ball: the ratio of solvent=1: 0.5～1.5: 1～5 is packed mixed-powder into earlier in the agate jar, add agate ball and solvent then, three kinds of materials are stirred with glass bar, put into ball mill again and carry out ball milling, ball-milling technology is: drum's speed of rotation 200～400r/min, ball milling time 1～8h; Slurry behind the ball milling is put into drying box dry, with its fragmentation, sieve after the oven dry; At last powder is calcined 2～8h in 800～1200 ℃ air, promptly obtain the ATO conducting powder of high-quality.
Described nano oxidized antimony and stannic oxide powder prepare the method for ATO conducting powder, and its solvent is a kind of or its combination in alcohol, acetone, distilled water, the deionized water.
Described nano oxidized antimony and stannic oxide powder prepare the method for ATO conducting powder, and its made ATO conducting powder specific area is 2～10m
2/ g, resistivity＜30 Ω .cm.
Because adopt aforesaid technical scheme, the present invention has following superiority:
1, compare with wet production ATO powder, this method technology is simple, with short production cycle, has reduced the cost of ATO powder.
2, overcome that traditional liquid phase method powder process raw material corrosivity is strong, complex procedures and the more high shortcoming of cost, and in the process of preparation, can not introduce acid ion, can not cause damage to environment.
3, to adopt nano oxidized antimony and nano tin dioxide be raw material in the present invention, and the granularity of making the ATO conducting powder is little, and specific area is at 2～10m
2/ g, average grain diameter is less than 200nm, and the resistivity of powder is less than 30 Ω .cm.
Description of drawings
Fig. 1 is a process chart of the present invention
The specific embodiment
Embodiment one
With nano oxidized antimony powder end and nano oxidized tin powder is raw material, and the specific area at nano oxidized antimony powder end is 50m
2/ g, the specific area of nano oxidized tin powder is 25m
2The SnO that/g produced
2-B1.
Earlier by nano tin dioxide: the ratio of nano oxidized antimony=85: 15 is packed powder in the V-type batch mixer, and dry method is mixed powder 40min, and two kinds of powder are tentatively mixed, and purpose is to allow the evenly distribution in stannic oxide powder of antimony oxide powder.Powder after the dry mixed and agate ball and alcohol are packed in the ball grinder, powder solution is stirred with glass bar.Mixed-powder: agate ball: alcohol=1: 1: 3.Ball grinder is put into ball mill powder is carried out the mixed powder of ball milling, ball-milling technology is: rotating speed: 200r/min, ball milling time: 4h.After ball milling finishes powder slurries is put into drying box and dry, with the material fragmentation after the oven dry, screening.At last powder is calcined 3h in 900 ℃ air, promptly obtain the uniform blue ATO conducting powder of granularity pattern.
Embodiment two
With nano oxidized antimony powder end and nano oxidized tin powder is raw material, and the specific area at nano oxidized antimony powder end is 50m
2/ g, the specific area of nano oxidized tin powder is 10m
2The SnO that/g produced
2-B2.
Earlier by nano tin dioxide: the ratio of nano oxidized antimony=90: 10 is packed powder in the V-type batch mixer, and dry method is mixed powder 60min, and two kinds of powder are tentatively mixed, and purpose is to allow the evenly distribution in stannic oxide powder of antimony oxide powder.Powder after the dry mixed and agate ball and distilled water are packed in the ball grinder, and mixed-powder: agate ball: distilled water=1: 1: 2.5 stirs powder solution with glass bar.Ball grinder is put into ball mill powder is carried out the mixed powder of ball milling, ball-milling technology is: rotating speed: 300r/min, ball milling time: 5h.After ball milling finishes powder slurries is put into drying box and dry, with the material fragmentation after the oven dry, screening.At last powder is calcined 5h in 1050 ℃ air, promptly obtain the uniform blue ATO conducting powder of granularity pattern.
Embodiment three
With nano oxidized antimony powder end and nano oxidized tin powder is raw material, and the specific area at nano oxidized antimony powder end is 30m
2/ g, the specific area of nano oxidized tin powder is 10m
2The SnO that/g produced
2-B2.
Earlier by nano tin dioxide: the ratio of nano oxidized antimony=95: 5 is packed powder in the V-type batch mixer, and dry method is mixed powder 80min, and two kinds of powder are tentatively mixed, and purpose is to allow the evenly distribution in stannic oxide powder of antimony oxide powder.Powder after the dry mixed and agate ball and distilled water are packed in the ball grinder, and mixed-powder: agate ball: distilled water=1: 1.2: 3 stirs powder solution with glass bar.Ball grinder is put into ball mill powder is carried out the mixed powder of ball milling, ball-milling technology is: rotating speed: 300r/min, ball milling time: 7h.After ball milling finishes powder slurries is put into drying box and dry, with the material fragmentation after the oven dry, screening.At last powder is calcined 6h in 1150 ℃ air, promptly obtain the uniform blue ATO conducting powder of granularity pattern.
Claims (2)
1. nano oxidized antimony and stannic oxide powder prepare the method for ATO conducting powder, it is characterized in that: earlier in nano tin dioxide: nano oxidized antimony=80～98: 20～2 ratio is packed two kinds of powder in the V-type batch mixer, dry method is mixed powder 30～120min, and two kinds of powder tentatively are mixed into mixed-powder; Again in mixed-powder: agate ball: the ratio of solvent=1: 0.5～1.5: 1～5 is packed mixed-powder into earlier in the agate jar, add agate ball and solvent then, three kinds of materials are stirred with glass bar, put into ball mill again and carry out ball milling, ball-milling technology is: drum's speed of rotation 200～400r/min, ball milling time 1～8h; Slurry behind the ball milling is put into drying box dry, with its fragmentation, sieve after the oven dry; At last powder is calcined 2～8h in 800～1200 ℃ air, promptly obtain the ATO conducting powder, the specific area of described ATO conducting powder is 2～10m
2/ g, resistivity＜30 Ω .cm.
2. nano oxidized antimony as claimed in claim 1 and stannic oxide powder prepare the method for ATO conducting powder, it is characterized in that: its solvent is a kind of or its combination in alcohol, acetone, distilled water, the deionized water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102013279B (en) * | 2010-09-03 | 2012-02-22 | 大连博众应用材料有限公司 | Method for preparing indium tin oxide target material slurry |
| CN102010197B (en) * | 2010-09-29 | 2013-02-13 | 大连交通大学 | Method for preparing antimony-doped tin oxide (ATO) nano powder |
| CN104496198A (en) * | 2014-12-09 | 2015-04-08 | 成都摩卡科技有限责任公司 | High-definition high-transmittance ultraviolet-resistant film and manufacturing method thereof |
| CN104827022A (en) * | 2015-04-27 | 2015-08-12 | 苏州统明机械有限公司 | Nickel-chrome alloy coating for ceramic and preparation method thereof |
| CN106205766A (en) * | 2016-08-31 | 2016-12-07 | 安徽斯迈尔电子科技有限公司 | A kind of preparation method of resistance slurry conductive phase |
| CN108251801A (en) * | 2016-12-29 | 2018-07-06 | 宁波江丰电子材料股份有限公司 | The preparation method of magnesia, zinc oxide mixed-powder |
| CN106967384A (en) * | 2017-01-22 | 2017-07-21 | 上海师范大学 | A kind of infrared absorbing material and its preparation and application |
| CN107142081A (en) * | 2017-06-22 | 2017-09-08 | 上海科润光电技术有限公司 | A kind of preparation of colour inorganic infrared absorbing material |
| CN117410010A (en) * | 2023-10-16 | 2024-01-16 | 上海银浆科技有限公司 | Low-temperature conductive silver paste for HJT battery and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062780A (en) * | 2006-04-26 | 2007-10-31 | 四川大学 | Nano titanium oxide and mechanical force chemical reaction preparation method for its composite powder |
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|---|---|---|---|---|
| CN101062780A (en) * | 2006-04-26 | 2007-10-31 | 四川大学 | Nano titanium oxide and mechanical force chemical reaction preparation method for its composite powder |
Non-Patent Citations (2)
| Title |
|---|
| M.I.B.Bernardi ETAL..Comparison of blue pigments prepared by two different methods.《Journal of the European Ceramic Society》.2002,第22卷2911-2919. * |
| 张建荣等.纳米Sb掺杂SnO2(ATO)导电粉体合成与应用研究.《2003年钠微粉体制备与技术应用研讨会.2003,第266页2.ATO材料的现有合成方法1)固相法,第267页第22-23行. * |
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