CN105732006A - Method for preparing IWTO (indium wolfram-tin oxide) target of transparent conductive film - Google Patents

Method for preparing IWTO (indium wolfram-tin oxide) target of transparent conductive film Download PDF

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CN105732006A
CN105732006A CN201610126603.5A CN201610126603A CN105732006A CN 105732006 A CN105732006 A CN 105732006A CN 201610126603 A CN201610126603 A CN 201610126603A CN 105732006 A CN105732006 A CN 105732006A
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iwto
target
powder
transparent conductive
conductive film
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刘玉洁
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Wuxi Nanligong Technology Development Co Ltd
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Wuxi Nanligong Technology Development Co Ltd
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Abstract

The invention relates to a method for preparing an IWTO (indium wolfram-tin oxide) target of a transparent conductive film. The method comprises the following steps: (1) proportioning raw materials, wherein raw materials including In2O3 powder, WO3 powder and SnO2 powder are weighed in a mass ratio; (2) uniformly mixing the raw materials, wherein the raw materials are put into a ball mill for ball milling for 5-10h, the raw materials are evenly mixed, taken out and then prepared into suspension liquid by adopting deionized water, then a magnetic stirrer is used for heating and mixing the suspension liquid till the deionized water is evaporated and the suspension liquid is changed into a sol-like mixture; (3) performing compression molding, wherein the sol-like mixture is put into a mold and subjected to compression molding under the load of 250-300 KN, a primarily molded green body is obtained, then secondary compression molding is performed under the load of 200-250 KN, and a green body is obtained; (4) forging the green body, wherein the obtained green body is put in a muffle furnace for calcination in an air atmosphere at a temperature of 1000-1100 DEG C for 8-18 hours; the IWTO target is obtained after the calcined green body is cooled to the room temperature.

Description

A kind of preparation method of the target of transparent conductive film IWTO
Technical field
The present invention relates to a kind of technical field of new energies, particularly to the preparation method of photoelectric material, the preparation method namely relating to the target of a kind of transparent conductive film IWTO.
Background technology
Transparent conductive film (TCO) is widely used in flat pannel display, OLED, touch pad and solaode due to its high conductance and light transmission.In solar cells, it is typically used as Window layer, and common TCO thin film has In2O3: SnO2(being called ITO), ZnO:Al(is called AZO), SnO2: F(is called FTO) and In2O3: WO3It is called IWO) etc..Wherein, ito thin film has good conductivity, it is seen that the advantage that optical band light transmission is high, and shortcoming is that near infrared band transmitance sharply declines；IWO then has the advantage that mobility is big, near infrared band permeability is high, but electric conductivity is not as ITO；AZO has the advantage that cost is low, stable in hydrogen plasma, and shortcoming is that electric conductivity and light transmission are not as ITO and IWO；FTO film preparing technology is ripe, but its electric conductivity and light transmission are general.Accordingly, it would be desirable to a kind of, both there is good electric conductivity and the high light transmission of visible light wave range, needed again the TCO material also near infrared band with high light transmission.IWTO(mixes the Indium sesquioxide. composite oxides of tungsten and stannum) main component be the Indium sesquioxide. composite oxides of tungsten oxide and doped sno_2；ITO and IWO is mixed to form IWTO(and mixes the Indium sesquioxide. composite oxides of tungsten and stannum) then can form high mobility and the high composite oxides of near infrared band permeability.
At present, adopting nano material to prepare the direction that low sintering IWTO target is target researcher unremitting effort, the density of the target obtained by most of low-temperature sinterings is on the low side, limits its application.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of cost is low, density is high and technique is simply suitable for the low temperature preparation method of IWTO target of electron beam evaporation or reactive plasma deposition thin film.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is, the preparation method of the target of this transparent conductive film IWTO, comprises the following steps,
(1) proportioning raw material: example weighs raw material In in mass ratio2O3Powder, WO3Powder and SnO2Powder；
(2) uniformly mixing raw material: the raw material in step (1) is put into ball mill, ball milling 5 ~ 10h, is made into suspension with deionized water again after taking out after mix homogeneously, then by magnetic stirring apparatus heated and stirred until becoming molten colloidal mixture after deionized water evaporation；
(3) compressing: the molten colloidal mixture in step (2) to be loaded in mould compressing under the load of 250 ~ 300KN, obtain the green compact of first time molding, then it is compressing to carry out secondary by the load of 200 ~ 250KN, obtains green compact；
(4) calcining green compact: being placed in Muffle furnace by the green compact prepared in step (3) and calcine in air atmosphere, calcining heat is 1000 ~ 1100 DEG C, and calcination time is 8 ~ 18h；It is cooled to room temperature, obtains IWTO target.
Further improvement is that, the raw material In in described step (1)2O3Powder, WO3Powder and SnO2The quality proportioning of powder is 90:0.5 ~ 2.5:6 ~ 9.5.
Further improvement is that, in described step (2), the temperature of magnetic agitation is 60 ~ 80 DEG C；The speed of stirring is 500 ~ 800r/min.
Further improvement is that, green compact compressing in described step (3) are cylindrical.
Further improvement is that, the diameter of described cylinder is 100mm.
Further improvement is that, the IWTO target prepared by the method is applicable to electron-beam vapor deposition method or reaction and plasma sedimentation prepares IWTO thin film.
Compared with prior art, the invention has the beneficial effects as follows: the present invention is by simple technique, mixing is suppressed low temperature calcination again and is prepared applicable electron beam evaporation or the target of reactive plasma deposition, such preparation method technique is simply controlled, cost is low, and the density of obtained IWTO target is high, is conducive to industrial large-scale promotion application, it is possible to reduce the preparation cost of IWTO thin film.
Detailed description of the invention
Embodiment one: the preparation method of the target of transparent conductive film IWTO, it is characterised in that comprise the following steps,
(1) proportioning raw material: example weighs raw material In in mass ratio2O3Powder, WO3Powder and SnO2Powder；In2O3Powder, WO3Powder and SnO2The quality proportioning of powder is 90:0.5:9.5；
(2) uniformly mixing raw material: the raw material in step (1) is put into ball mill, ball milling 5h, is made into suspension with deionized water again after taking out after mix homogeneously, then by magnetic stirring apparatus heated and stirred until becoming molten colloidal mixture after deionized water evaporation；The temperature of magnetic agitation is 60 DEG C；The speed of stirring is 800r/min；
(3) compressing: the molten colloidal mixture in step (2) to be loaded in mould compressing under the load of 250KN, obtain the green compact of first time molding, then it is compressing to carry out secondary by the load of 250KN, obtains green compact；Compressing green compact be cylindrical；The diameter of described cylinder is 100mm；
(4) calcining green compact: being placed in Muffle furnace by the green compact prepared in step (3) and calcine in air atmosphere, calcining heat is 1000 DEG C, and calcination time is 18h；It is cooled to room temperature, obtains IWTO target；IWTO target prepared by the method is applicable to electron-beam vapor deposition method or reaction and plasma sedimentation prepares IWTO thin film.
The preparation method of embodiment two: IWTO target, it is characterised in that comprise the following steps,
(1) proportioning raw material: example weighs raw material In in mass ratio2O3Powder, WO3Powder and SnO2Powder；In2O3Powder, WO3Powder and SnO2The quality proportioning of powder is 90:1.5:8.5；
(2) uniformly mixing raw material: the raw material in step (1) is put into ball mill, ball milling 8h, is made into suspension with deionized water again after taking out after mix homogeneously, then by magnetic stirring apparatus heated and stirred until becoming molten colloidal mixture after deionized water evaporation；The temperature of magnetic agitation is 70 DEG C；The speed of stirring is 650r/min；
(3) compressing: the molten colloidal mixture in step (2) to be loaded in mould compressing under the load of 280KN, obtain the green compact of first time molding, then it is compressing to carry out secondary by the load of 220KN, obtains green compact；Compressing green compact be cylindrical；The diameter of described cylinder is 100mm；
(4) calcining green compact: being placed in Muffle furnace by the green compact prepared in step (3) and calcine in air atmosphere, calcining heat is 1050 DEG C, and calcination time is 13h；It is cooled to room temperature, obtains IWTO target；IWTO target prepared by the method is applicable to electron-beam vapor deposition method or reaction and plasma sedimentation prepares IWTO thin film.
The preparation method of embodiment three: IWTO target, it is characterised in that comprise the following steps,
(1) proportioning raw material: example weighs raw material In in mass ratio2O3Powder, WO3Powder and SnO2Powder；In2O3Powder, WO3Powder and SnO2The quality proportioning of powder is 90:2.5:7.5；
(2) uniformly mixing raw material: the raw material in step (1) is put into ball mill, ball milling 10h, is made into suspension with deionized water again after taking out after mix homogeneously, then by magnetic stirring apparatus heated and stirred until becoming molten colloidal mixture after deionized water evaporation；The temperature of magnetic agitation is 80 DEG C；The speed of stirring is 800r/min；
(3) compressing: the molten colloidal mixture in step (2) to be loaded in mould compressing under the load of 300KN, obtain the green compact of first time molding, then it is compressing to carry out secondary by the load of 200KN, obtains green compact；Compressing green compact be cylindrical；The diameter of described cylinder is 100mm；
(4) calcining green compact: being placed in Muffle furnace by the green compact prepared in step (3) and calcine in air atmosphere, calcining heat is 1100 DEG C, and calcination time is 9h；It is cooled to room temperature, obtains IWTO target；IWTO target prepared by the method is applicable to electron-beam vapor deposition method or reaction and plasma sedimentation prepares IWTO thin film.
Particular embodiments described above; the purpose of the present invention, technical scheme and beneficial effect have been further described; it is it should be understood that; the foregoing is only specific embodiments of the invention; it is not limited to the present invention; all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.

Claims (6)

1. the preparation method of the target of a transparent conductive film IWTO, it is characterised in that comprise the following steps,
(1) proportioning raw material: example weighs raw material In in mass ratio2O3Powder, WO3Powder and SnO2Powder；
(2) uniformly mixing raw material: the raw material in step (1) is put into ball mill, ball milling 5 ~ 10h, is made into suspension with deionized water again after taking out after mix homogeneously, then by magnetic stirring apparatus heated and stirred until becoming molten colloidal mixture after deionized water evaporation；
(3) compressing: the molten colloidal mixture in step (2) to be loaded in mould compressing under the load of 250 ~ 300KN, obtain the green compact of first time molding, then it is compressing to carry out secondary by the load of 200 ~ 250KN, obtains green compact；
(4) calcining green compact: being placed in Muffle furnace by the green compact prepared in step (3) and calcine in air atmosphere, calcining heat is 1000 ~ 1100 DEG C, and calcination time is 8 ~ 18h；It is cooled to room temperature, obtains IWTO target.
2. the preparation method of the target of transparent conductive film IWTO according to claim 1, it is characterised in that the raw material In in described step (1)2O3Powder, WO3Powder and SnO2The quality proportioning of powder is 90:0.5 ~ 2.5:6 ~ 9.5.
3. the preparation method of the target of transparent conductive film IWTO according to claim 2, it is characterised in that in described step (2), the temperature of magnetic agitation is 60 ~ 80 DEG C；The speed of stirring is 500 ~ 800r/min.
4. the preparation method of the target of transparent conductive film IWTO according to claim 2, it is characterised in that green compact compressing in described step (3) are cylindrical.
5. the preparation method of the target of transparent conductive film IWTO according to claim 4, it is characterised in that the diameter of described cylinder is 100mm.
6. the preparation method of the target of transparent conductive film IWTO according to claim 5, it is characterised in that the IWTO target prepared by the method is applicable to electron-beam vapor deposition method or reaction and plasma sedimentation prepares IWTO thin film.
CN201610126603.5A 2016-03-07 2016-03-07 Method for preparing IWTO (indium wolfram-tin oxide) target of transparent conductive film Pending CN105732006A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108914064A (en) * 2018-08-01 2018-11-30 研创应用材料（赣州）股份有限公司 A kind of novel RPD polynary conductive oxide material and preparation method thereof
CN113149613A (en) * 2021-05-24 2021-07-23 先导薄膜材料（广东）有限公司 ITWO target material and preparation method thereof
CN114086135A (en) * 2021-11-08 2022-02-25 苏州瑞纳新材料科技有限公司 Electro-dimming film and preparation method thereof
CN116730710A (en) * 2023-02-07 2023-09-12 中山智隆新材料科技有限公司 High-valence element doped indium tin oxide material and preparation method and application thereof
CN117263671A (en) * 2023-10-23 2023-12-22 深圳众诚达应用材料股份有限公司 IWSO target material, preparation method thereof and film prepared from IWSO target material

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CN102320824A (en) * 2011-06-01 2012-01-18 内蒙古工业大学 A kind of preparation method of metal ion doped titanium dioxide target and thus obtained target
CN102751341A (en) * 2012-06-20 2012-10-24 常州天合光能有限公司 Transparent conductive film and preparation method thereof
CN104211399A (en) * 2014-07-24 2014-12-17 昆明理工大学 Preparation method of polycrystalline target material with controllable temperature coefficient of resistance (TCR)
CN105374901A (en) * 2015-11-18 2016-03-02 南京迪纳科光电材料有限公司 Preparation method for IWO material used for thin film solar cell transparent electrode

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JP2010070418A (en) * 2008-09-18 2010-04-02 Idemitsu Kosan Co Ltd SnO2-In2O3-BASED OXIDE SINTERED COMPACT AND AMORPHOUS TRANSPARENT CONDUCTIVE FILM
CN102320824A (en) * 2011-06-01 2012-01-18 内蒙古工业大学 A kind of preparation method of metal ion doped titanium dioxide target and thus obtained target
CN102751341A (en) * 2012-06-20 2012-10-24 常州天合光能有限公司 Transparent conductive film and preparation method thereof
CN104211399A (en) * 2014-07-24 2014-12-17 昆明理工大学 Preparation method of polycrystalline target material with controllable temperature coefficient of resistance (TCR)
CN105374901A (en) * 2015-11-18 2016-03-02 南京迪纳科光电材料有限公司 Preparation method for IWO material used for thin film solar cell transparent electrode

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108914064A (en) * 2018-08-01 2018-11-30 研创应用材料（赣州）股份有限公司 A kind of novel RPD polynary conductive oxide material and preparation method thereof
CN108914064B (en) * 2018-08-01 2020-09-29 研创应用材料（赣州）股份有限公司 Multi-element conductive oxide material for RPD and preparation method thereof
CN113149613A (en) * 2021-05-24 2021-07-23 先导薄膜材料（广东）有限公司 ITWO target material and preparation method thereof
CN114086135A (en) * 2021-11-08 2022-02-25 苏州瑞纳新材料科技有限公司 Electro-dimming film and preparation method thereof
CN114086135B (en) * 2021-11-08 2024-05-24 苏州瑞纳新材料科技有限公司 Electroluminescence film and preparation method thereof
CN116730710A (en) * 2023-02-07 2023-09-12 中山智隆新材料科技有限公司 High-valence element doped indium tin oxide material and preparation method and application thereof
CN117263671A (en) * 2023-10-23 2023-12-22 深圳众诚达应用材料股份有限公司 IWSO target material, preparation method thereof and film prepared from IWSO target material
CN117263671B (en) * 2023-10-23 2024-05-14 深圳众诚达应用材料股份有限公司 IWSO target material, preparation method thereof and film prepared from IWSO target material

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Application publication date: 20160706