CN102863210A - Preparation method of high-density high-conductivity tin antimony oxide ceramic - Google Patents
Preparation method of high-density high-conductivity tin antimony oxide ceramic Download PDFInfo
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- CN102863210A CN102863210A CN2012103859287A CN201210385928A CN102863210A CN 102863210 A CN102863210 A CN 102863210A CN 2012103859287 A CN2012103859287 A CN 2012103859287A CN 201210385928 A CN201210385928 A CN 201210385928A CN 102863210 A CN102863210 A CN 102863210A
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Abstract
The invention discloses a preparation method of high-density high-conductivity tin antimony oxide ceramic. The method comprises the steps of 1), preparing tin antimony oxide nano powder with different antimony (Sb) doping content, enabling tin antimony oxide with a Sb doping content of 20at.% and SnO2 nano powder to serve as raw materials, and obtaining tin antimony oxide nano powder with a Sb doping content of 1-20at.% by using a ball-milling method; 2), dandifying an electrical field auxiliary low temperature of the tin antimony oxide nano powder rapidly, placing the powder into a die, and preparing the high-density tin antimony oxide ceramic at a low temperature rapidly through an electrical field auxiliary condition; and 3), subjecting the tin antimony oxide ceramic to low-temperature homogenization process, placing the obtained ceramic into a heating furnace, and conducting low-temperature homogenization process in the air, so that the resistance of the ceramic can be reduced remarkably, and the density is not affected. The tin antimony oxide ceramic has the advantages of being low in cost, good in electrical conductivity, sufficient in raw material, simple in process, low in densifying and homogenizing temperature and capable of reducing energy consumption substantially.
Description
Technical field
The present invention relates to ceramic field, particularly introduced the preparation method of a kind of high densification, high conductive tin oxide antimony pottery, can prepare high tin-antiomony oxide pottery fine and close, high conduction with this method and be used as electrode materials and sputtering target material.
Background technology
Current, photovoltaic industry and optoelectronic information industry are in the develop rapidly stage, and the demand of the transparent conductive material that photosensitive and electric field-sensitive is had both also highlights day by day.Transparent conductive film is a kind of novel energy material that development in recent years is got up, because it has both high conductivity and high visible light permeability is widely used in solar cell, flat-panel monitor, specific function window coating and other field of photoelectric devices simultaneously.At present, the transparent conductive film that is most widely used mainly is the indium tin oxide target (In of Sn element doping
2O
3, be called for short ITO), its share of market and demand are and increase progressively fast year by year situation, and output market value in 2010 is up to 1,500,000,000 dollars.But very rare as the resource of the In of main ingredient among the ITO, only about 1.6 ten thousand tons of its geologic reserve only have 1/6 of gold geology reserves, and In is a kind of toxic substance, can bring serious problem of environmental pollution.Therefore, need a kind of environmental protection of searching, cheap transparent conductive film to have ITO now to substitute.Tin-antiomony oxide (the SnO of Sb element doping
2Be called for short tin-antiomony oxide) be exactly a kind of novel transparent conductive film that development in recent years is got up, its aboundresources, low price, nontoxic pollution-free, and have the large (〉 3.6eV of energy gap), the excellent properties such as good conductivity, visible light transmissivity height, radioprotective, Heat stability is good, be one of material that is hopeful most alternative ITO.And in order to realize its commercial application, the sputter coating technology is topmost industrial production technology, and high-quality sputtering target material is most important industrial raw materials, therefore must prepare high-quality tin-antiomony oxide ceramic target, requires its density height, good conductivity and foreign matter content low.
Because the Application Areas of transparent conductive film is wider, different field is also different to the performance requriements of this material, and wherein surface resistivity can be 10
2~ 10
4Change in Ω/ scope.In order to satisfy the application demand of different field, can prepare by the Sb doping content in the change target tin-antiomony oxide film of different conductivities.And the Sb doping content in the tin-antiomony oxide material powder of present industrial production is mainly 20at.%, and the tin-antiomony oxide power production of other components is less, is difficult for obtaining.Because there are two kinds of valence state (Sb in the Sb in the tin-antiomony oxide
5+And Sb
3+), and Sb
5+Replace Sn
4+The N-shaped current carrier that produces is main electrical conduction mechanism.Tin-antiomony oxide ceramic target electroconductibility mainly is to determine by carrier concentration and mobility.Therefore, adopt a kind of easy method to prepare the tin-antiomony oxide powder of different components, thereby effectively control Sb doping content, Sb
5+Content and the carrier transport ability be control its electrical property size key factor.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of simple high densification, high conductive tin oxide antimony pottery to be used for improving the density of tin-antiomony oxide pottery, reduces its resistivity, thereby prepares the tin-antiomony oxide pottery of high densification, high conduction.
The preparation method of high densification provided by the invention, high conductive tin oxide antimony pottery, as raw material take two kinds of nano-powders, make at low temperatures described tin-antiomony oxide pottery in conjunction with the electric field subsidiary conditions, the low temperature homogenizing in later stage is processed should make its resistivity decreased, and do not affect density, the method adopts the method that may further comprise the steps:
(1) preparation of the tin-antiomony oxide nano-powder of different Sb doping contents:
Be that the ratio of 1～20at.% takes by weighing tin-antiomony oxide powder and the pure SnO that the Sb doping content is 20at.% in the Sb doping content
2Powder joins in the ball grinder mixing nano-powder, agate ball and the dehydrated alcohol mass ratio by 1:2:1, and behind the ball mill ball milling, oven dry, grinding obtain required tin-antiomony oxide nano-powder;
(2) the electric field assisted cryogenic quick densifying of tin-antiomony oxide nano-powder:
Gained tin-antiomony oxide nano-powder in the step (1) is packed in the mould, transfer in the electric field assisted sintering system, under 800～1200 ℃ temperature, carry out sintering, obtain high fine and close tin-antiomony oxide pottery;
(3) the low temperature homogenizing of tin-antiomony oxide pottery is processed:
Place process furnace to carry out the homogenizing processing on the tin-antiomony oxide pottery of gained in the step (2), the homogenizing treatment temp is 500～1000 ℃, and the time is 10～100 hours;
Through above-mentioned steps, obtain described high fine and close, the high tin-antiomony oxide pottery that conducts electricity.
In the above-mentioned steps (1), tin-antiomony oxide powder and SnO that described Sb doping content is 20at.%
2The purity of powder can for 99.9%, particle diameter is 10～50nm.
In the above-mentioned steps (1), be that the ratio of 1～20at.% obtains the tin-antiomony oxide nano-powder in the Sb doping content.
The present invention adopts electric field assisted sintering technology when sintering pressure is 20～100MPa, is warming up to 800～1200 ℃ of insulation tin-antiomony oxide ceramic dense degree that sintering obtains after 1～5 minute with 50～300 ℃/minute and all can reaches 90～99%.
The mold material of described employing can be high-strength graphite or wolfram varbide;
Described ball mill can be planetary ball mill, and 12 hours post-drying slurries of ball milling grind and obtain required tin-antiomony oxide nano-powder, and this diameter of particle is 20 ~ 30nm.
Described mould can be the graphite jig of Φ 20.
Adopt preparation method of the present invention, can obtain density is 90～98%, and resistivity is 1～10 * 10
-3The tin-antiomony oxide pottery of Ω cm.
The present invention compared with prior art has following major advantage:
One. adopt the low temperature homogenizing to process, can significantly lower the resistivity of tin-antiomony oxide pottery, but not affect its density.
They are two years old. because the required raw material of preparation is easy to obtain, have that cost is low, the characteristics of good conductivity, prepare required raw material and be easy to obtain, technique is simple, and the temperature of densification and homogenizing processing is low, but the decrease energy consumption.
They are three years old. and excellent performance: prepared tin-antiomony oxide ceramic dense degree all reaches more than 90%, and resistivity can be down to 5 * 10
-3Ω cm.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Fig. 2 is density and the resistivity curve figure of the tin-antiomony oxide pottery of the embodiment of the invention 1 gained.
Fig. 3 is fracture scanning electronic microscope (SEM) photo before the tin-antiomony oxide pottery homogenizing of the embodiment of the invention 3 gained is processed.
Fig. 4 is fracture scanning electronic microscope (SEM) photo after the tin-antiomony oxide pottery homogenizing of the embodiment of the invention 3 gained is processed.
Fig. 5 is density and the resistivity curve figure of the tin-antiomony oxide pottery of the gained of the embodiment of the invention 4 under the technique that different homogenizing is processed.
Fig. 6 is the fracture SEM photo before the tin-antiomony oxide pottery homogenizing of the embodiment of the invention 5 gained is processed.
Fig. 7 is the fracture SEM photo after the tin-antiomony oxide pottery homogenizing of the embodiment of the invention 5 gained is processed.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but be not limited to following described embodiment.
Embodiment 1
(1) taking by weighing tin-antiomony oxide nano-powder, 120 gram agate balls and the 60 gram dehydrated alcohols that the commercially available Sb doping content of 60 grams is 20at.% joins in the nylon ball grinder, in planetary ball mill, mix, rotating speed is 180 rev/mins, Ball-milling Time is 12 hours, with the oven dry of the slurry of gained, grind and obtain the tin-antiomony oxide powder that the Sb doping content is 20at.%.
(2) packing in the mould, transfer in the electric field assisted sintering system, is under the 40MPa at 900 ~ 1050 ℃ sintering temperatures, sintering pressure, and with 100 ℃ of/minute sintering 3 minutes, the density that obtains and resistivity were as shown in Figure 2.
(3) the Sb doping content that sintering in the step (2) is obtained is that the high fine and close tin-antiomony oxide pottery of 20at.% places process furnace, and 800 ℃ of lower annealing 100 hours, considerable change did not occur for the tin-antiomony oxide ceramic dense degree and the resistivity that obtain.
By test result as can be known, when the tin-antiomony oxide nano-powder take pure Sb doping content as 20at.% during as raw material, density and electrical property are all more excellent before the annealing, and it is little on the impact of structure and performance to anneal.
Embodiment 2
(1) preparation of tin-antiomony oxide nano-powder: take by weighing tin-antiomony oxide powder, 53.5 gram SnO that 6.5 gram Sb doping contents are 20at.%
2Powder, 120 gram agate balls and 60 gram dehydrated alcohols, join in the nylon ball grinder, mix in planetary ball mill, rotating speed is 180 rev/mins, Ball-milling Time is 12 hours, with the oven dry of the slurry of gained, grind and obtain the tin-antiomony oxide powder that the Sb doping content is 4at.%.
(2) the electric field assisted cryogenic quick densifying of tin-antiomony oxide nano-powder: take by weighing the above-mentioned gained powder of 8 grams, pack in the mould, transfer in the electric field assisted sintering system, when pressure is 30MPa, be warming up to 1000 ℃ of sintering 3 minutes with 100 ℃/minute speed, obtain density and be 97.0%, resistivity is the tin-antiomony oxide pottery of 3.898 Ω cm.
(3) the low temperature homogenizing of tin-antiomony oxide pottery is processed: the tin-antiomony oxide ceramic block behind the sintering is put into process furnace carrying out the homogenizing processing under 800 ℃ after 100 hours, obtaining density has slight downward trend, and resistivity becomes large, reaches 17 Ω cm.
By test result as can be known, when the Sb doping content was 4at.%, resistivity was higher, and annealing is unfavorable for that its electrical property improves.
Embodiment 3
(1) preparation of tin-antiomony oxide nano-powder: take by weighing tin-antiomony oxide powder, 34.7 gram SnO that 25.3 gram Sb doping contents are 20at.%
2Powder, 120 gram agate ball and an amount of dehydrated alcohols, join in the nylon ball grinder, mix in planetary ball mill, rotating speed is 180 rev/mins, Ball-milling Time is 12 hours, with the oven dry of the slurry of gained, grind and obtain the tin-antiomony oxide powder that the Sb doping content is 8at.%.
(2) the electric field assisted cryogenic quick densifying of tin-antiomony oxide nano-powder: take by weighing the above-mentioned gained powder of 8 grams, in the mould of packing into, transfer in the electric field assisted sintering system, when pressure is 30MPa, with 100
oC/ minute speed is warming up to 1000 ℃ of sintering 3 minutes, obtains density and be 97.1%, resistivity is the tin-antiomony oxide pottery of 5.78 Ω cm.
(3) the low temperature homogenizing of tin-antiomony oxide pottery is processed: the tin-antiomony oxide ceramic block behind the sintering is put into process furnace carrying out the homogenizing processing under 800 ℃ after 100 hours, obtaining density has slight downward trend, and resistivity is 4 * 10
-2Ω cm.
The Sb doping content that obtains is to reach before the tin-antiomony oxide pottery of 8 at. % is annealed in the section SEM photo difference of 800 ℃ of lower annealing after 100 hours as shown in Figure 3 and Figure 4.
Embodiment 4
(1) preparation of tin-antiomony oxide nano-powder: take by weighing tin-antiomony oxide powder, 22.7 gram SnO that 33.3 gram Sb doping contents are 20 at. %
2Powder, 120 gram agate ball and an amount of dehydrated alcohols, join in the nylon ball grinder, mix in planetary ball mill, rotating speed is 180 rev/mins, Ball-milling Time is 12 hours, with the oven dry of the slurry of gained, grind and obtain the tin-antiomony oxide powder that the Sb doping content is 12at.%.
(2) the low temperature quick densifying of tin-antiomony oxide nano-powder: take by weighing the above-mentioned gained powder of 8 grams, in the mould of packing into, transfer in the electric field assisted sintering system, when pressure is 40MPa, with 100
oC/ minute speed is warming up to 1000 ℃ of sintering 3 minutes, obtains density and be 94.2%, resistivity is 8 * 10
-3The tin-antiomony oxide pottery of Ω cm.
(3) the low temperature homogenizing of tin-antiomony oxide pottery is processed: with the tin-antiomony oxide ceramic block behind the sintering put into process furnace 700～900 ℃ lower respectively after homogenizing are processed 20 hours, 50 hours, 100 hours, obtain the density of tin-antiomony oxide pottery of density and resistivity as shown in Figure 5.
Embodiment 5
(1) preparation of tin-antiomony oxide nano-powder: take by weighing tin-antiomony oxide powder, 11.2 gram SnO that 48.8 gram Sb doping contents are 20at.%
2Powder, 120 gram agate ball and an amount of dehydrated alcohols, join in the nylon ball grinder, mix in planetary ball mill, rotating speed is 180 rev/mins, Ball-milling Time is 12 hours, with the oven dry of the slurry of gained, grind and obtain the tin-antiomony oxide powder that the Sb doping content is 16at.%.
(2) the low temperature quick densifying of tin-antiomony oxide nano-powder: take by weighing the above-mentioned gained powder of 8 grams, pack in the mould, transfer in the electric field assisted sintering system, when pressure is 50MPa, speed with 100 ℃/min is warming up to 1000 ℃ of sintering 3 minutes, obtains density and be 95.2%, resistivity is the tin-antiomony oxide pottery of 1.808 Ω cm.
(3) the low temperature homogenizing of tin-antiomony oxide pottery is processed: the tin-antiomony oxide ceramic block behind the sintering is put into process furnace after 800 ℃ of lower homogenizing are processed 100 hours, and resistivity is 6.275 * 10
-2Ω cm.
The Sb doping content that obtains is before the tin-antiomony oxide pottery homogenizing of 12at.% is processed and 800
oThe section SEM photo of homogenizing processing after 100 hours respectively as shown in Figure 6 and Figure 7 under the C.
Embodiment 6
(1) preparation of tin-antiomony oxide nano-powder: take by weighing tin-antiomony oxide powder, 22.7 gram SnO that 33.3 gram Sb doping contents are 20 at. %
2Powder, 120 gram agate ball and an amount of dehydrated alcohols, join in the nylon ball grinder, mix in planetary ball mill, rotating speed is 180 rev/mins, Ball-milling Time is 12 hours, with the oven dry of the slurry of gained, grind and obtain the tin-antiomony oxide powder that the Sb doping content is 12at.%.
(2) the low temperature quick densifying of tin-antiomony oxide nano-powder: take by weighing the above-mentioned gained powder of 8 grams, pack in the mould, transfer in the electric field assisted sintering system, when pressure is 100MPa, be warming up to 1000 ℃ of sintering 3 minutes with 100 ℃/minute speed, obtain density and be 98%, resistivity is 5 * 10
-3The tin-antiomony oxide pottery of Ω cm.
(3) the low temperature homogenizing of tin-antiomony oxide pottery is processed: the tin-antiomony oxide ceramic block behind the sintering is put into process furnace after 900 ℃ of lower difference homogenizing are processed 100 hours, and the density of the tin-antiomony oxide pottery that obtains is 98.2%, and resistivity is 1 * 10
-3Ω cm.
In above-described embodiment, the diameter of described mould is Φ 20, perhaps decides according to practical situation.The material of this mould can be high-strength graphite or wolfram varbide.
Described Ball-milling Time also can be decided according to practical situation.
Claims (8)
1. the preparation method of a high densification, high conductive tin oxide antimony pottery, it is characterized in that the method is take two kinds of nano-powders as raw material, make at low temperatures described tin-antiomony oxide pottery in conjunction with the electric field subsidiary conditions, the low temperature homogenizing in later stage is processed should make its resistivity decreased, and do not affect density, the method adopts the method that may further comprise the steps:
(1) preparation of the tin-antiomony oxide nano-powder of different Sb doping contents:
Be that the ratio of 1～20at.% takes by weighing tin-antiomony oxide powder and the pure SnO that the Sb doping content is 20at.% in the Sb doping content
2Powder joins in the ball grinder mixing nano-powder, agate ball and the dehydrated alcohol mass ratio by 1:2:1, and behind the ball mill ball milling, oven dry, grinding obtain required tin-antiomony oxide nano-powder;
(2) the electric field assisted cryogenic quick densifying of tin-antiomony oxide nano-powder:
Gained tin-antiomony oxide nano-powder in the step (1) is packed in the mould, transfer in the electric field assisted sintering system, under 800～1200 ℃ temperature, carry out sintering, obtain high fine and close tin-antiomony oxide pottery;
(3) the low temperature homogenizing of tin-antiomony oxide pottery is processed:
Place process furnace to carry out the homogenizing processing on the tin-antiomony oxide pottery of gained in the step (2), the homogenizing treatment temp is 500～1000 ℃, and the time is 10～100 hours;
Through above-mentioned steps, obtain described high fine and close, the high tin-antiomony oxide pottery that conducts electricity.
2. the preparation method of high densification according to claim 1, high conductive tin oxide antimony pottery is characterized in that: Sb doping content described in the step (1) is tin-antiomony oxide powder and the SnO of 20at.%
2The purity of powder is〉99.9%, particle diameter is 10～50nm.
3. the preparation method of high densification according to claim 1, high conductive tin oxide antimony pottery is characterized in that: in the step (1), be that the ratio of 1～20at.% obtains the tin-antiomony oxide nano-powder in the Sb doping content.
4. the preparation method of high densification according to claim 1, high conductive tin oxide antimony pottery, it is characterized in that: adopt electric field assisted sintering technology when sintering pressure is 20～100MPa, be warming up to 800～1200 ℃ of insulation tin-antiomony oxide ceramic dense degree that sintering obtains after 1～5 minute with 50～300 ℃/minute and all can reach 90～99%.
5. the preparation method of high densification according to claim 1, high conductive tin oxide antimony pottery is characterized in that: the mold material of described employing is high-strength graphite or wolfram varbide.
6. the preparation method of high densification according to claim 1, high conductive tin oxide antimony pottery, it is characterized in that: described ball mill is planetary ball mill, 12 hours post-drying slurries of ball milling grind and obtain required tin-antiomony oxide nano-powder, and this diameter of particle is 20 ~ 30nm.
7. the preparation method of high densification according to claim 1, high conductive tin oxide antimony pottery is characterized in that: obtaining density is 90～98%, and resistivity is 1～10 * 10
-3The tin-antiomony oxide pottery of Ω cm.
8. the preparation method of high densification according to claim 1, high conductive tin oxide antimony pottery is characterized in that: described mould is the graphite jig of Φ 20.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193322A (en) * | 2014-08-27 | 2014-12-10 | 宁波今心新材料科技有限公司 | Preparation method of high-density tin dioxide single-phase ceramic |
| CN106505248A (en) * | 2016-10-26 | 2017-03-15 | 中国地质大学（武汉） | A kind of glass ceramics type method for preparing solid electrolyte |
| CN109216500A (en) * | 2017-06-26 | 2019-01-15 | 苏州科技大学 | Terahertz wave detector substrate and preparation method thereof |
| CN109678498A (en) * | 2019-01-22 | 2019-04-26 | 陕西科技大学 | A kind of method of low temperature Fast Sintering NBT piezoelectric ceramics |
| CN114773053A (en) * | 2022-05-05 | 2022-07-22 | 安徽工业大学 | Al/Ga/In+Ta codoped with TiO2Mesozoelectric dielectric ceramic, preparation method and application thereof |
-
2012
- 2012-10-12 CN CN2012103859287A patent/CN102863210A/en active Pending
Non-Patent Citations (2)
| Title |
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| XUEPING LI ET AL: "Densification of ATO Nanoceramics by Spark Plasma Sintering", 《KEY ENGINEERING MATERIALS》 * |
| 李雪萍 等: "高致密高导电氧化锡锑(ATO)陶瓷的制备", 《第十七届全国高技术陶瓷学术年会摘要集》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193322A (en) * | 2014-08-27 | 2014-12-10 | 宁波今心新材料科技有限公司 | Preparation method of high-density tin dioxide single-phase ceramic |
| CN104193322B (en) * | 2014-08-27 | 2015-09-23 | 宁波今心新材料科技有限公司 | A kind of preparation method of high-compactness tindioxide one-component ceramic |
| CN106505248A (en) * | 2016-10-26 | 2017-03-15 | 中国地质大学（武汉） | A kind of glass ceramics type method for preparing solid electrolyte |
| CN109216500A (en) * | 2017-06-26 | 2019-01-15 | 苏州科技大学 | Terahertz wave detector substrate and preparation method thereof |
| CN109216500B (en) * | 2017-06-26 | 2021-08-17 | 苏州科技大学 | Substrate for terahertz wave detector and preparation method thereof |
| CN109678498A (en) * | 2019-01-22 | 2019-04-26 | 陕西科技大学 | A kind of method of low temperature Fast Sintering NBT piezoelectric ceramics |
| CN114773053A (en) * | 2022-05-05 | 2022-07-22 | 安徽工业大学 | Al/Ga/In+Ta codoped with TiO2Mesozoelectric dielectric ceramic, preparation method and application thereof |
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Application publication date: 20130109 |