CN103113089A - Method for preparing indium tin oxide (ITO) target through hot-press method - Google Patents
Method for preparing indium tin oxide (ITO) target through hot-press method Download PDFInfo
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- CN103113089A CN103113089A CN2012104463111A CN201210446311A CN103113089A CN 103113089 A CN103113089 A CN 103113089A CN 2012104463111 A CN2012104463111 A CN 2012104463111A CN 201210446311 A CN201210446311 A CN 201210446311A CN 103113089 A CN103113089 A CN 103113089A
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Abstract
The invention relates to an indium tin oxide (ITO) target and in particular to a method for preparing the indium tin oxide (ITO) target through a hot-press method. The method comprises the following steps: preparing indium tin hydroxide precipitate solution; performing centrifugal separation on the precipitate solution to obtain precipitate and liquid; washing the precipitate through water, and centrifugally separating the precipitate and water; drying and calcining the precipitate to obtain ITO powder; adding polyvinyl alcohol into the ITO powder, and performing dry pressing on the ITO powder into a formed body by utilizing a die; arranging the formed body in a hot-pressing furnace, and preparing the ITO target. The temperature, PH value and other conditions of the synthetic solution are controlled, so that the ITO powder reaches a nano scale, and conditions are provided for preparing high-density ITO target in the hot-pressing method; and meanwhile, according to the precipitate subjected to repeated centrifugal separation and washing, the impurities on the surface of the precipitate can be effectively removed, and the conductivity of the ITO powder is improved, so that the performance of the ITO target is improved; and moreover, the forming pressure required by the hot-pressing method is low, the sintering temperature is low, the time is short, the production cost is low, grain growth can be inhibited, and the ITO target which has the density close to the theoretical density and has low porosity is obtained.
Description
Technical field
The present invention relates to producing of ITO target, is to utilize pressure sintering to prepare the method for ITO target specifically.
Background technology
ITO(tin indium oxide) main component is that stannic oxide is solid-solubilized in the composite oxides in Indium sesquioxide.ITO has good photoelectric properties, and the film that contains ITO has high electroconductibility and visible light transmission, is widely used in the various fields such as solar cell, liquid crystal indicator, touch-control electroplax.Universal fast along with liquid crystal flat-panel display unit etc., the consumption of ITO target is more and more, and is also more and more higher to the requirement of target.At present, the direction that it is target investigator unremitting effort that the employing nano material prepares low sintering ITO target, prior art method commonly used adopts coprecipitation method to prepare ito powder, then sinters the ITO target into ito powder.But the ito powder sintering character of the method for the employing of prior art preparation is relatively poor, and the density of the ITO target that finally obtains is lower, has limited the application of ITO target.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of pressure sintering of utilizing and prepare the method that ITO target density is higher, production cost is lower.
The technical scheme that the present invention solves the problems of the technologies described above employing is: pressure sintering prepares the method for ITO target, and it comprises the following steps:
(1) at first indium metal is dissolved in hydrochloric acid soln, adds tin tetrachloride in this solution, keeping the indium tin mass ratio in mixing solutions is 9.45:1; Then mixing solutions is imported in trolamine and polyvinylpyrrolidonesolution solution, and add ammoniacal liquor, form resulting solution; Then to the resulting solution heating, obtain the indium tin hydroxide precipitation solution;
(2) throw out and the liquid in the centrifugation precipitation solution;
(3) wash throw out with water, and the centrifugation water and sediment;
(4) repeating step is (3) 3 times-5 times, is precipitated thing;
(5) throw out of drying, calcining step (4), obtain ito powder;
(6) add polyvinyl alcohol in ito powder, utilize mould that the ito powder dry-pressing is become formed body;
(7) formed body is placed in hot pressing furnace, produces the ITO target.
As preferably, keeping the mass ratio of polyvinyl alcohol in described resulting solution is 0.7%-1.0%.
As preferably, described Heating temperature is 80 ℃, and keeping the pH value of resulting solution is 6-7.
As preferably, the calcining temperature of described step (5) is 1100 ℃-1300 ℃.
As preferably, the sintering condition of described step (7) is: 1100 ℃ of temperature, pressure 10MPa, 300 minutes time.
As preferably, described polyvinylpyrrolidone and sedimentary mass ratio are 1:10.
From technique scheme as can be known, temperature and the condition such as pH value of the present invention by controlling resulting solution can make ito powder reach nano level, provides condition for pressure sintering prepares highdensity ITO target; The present invention simultaneously adopts the throw out of repeatedly centrifugation washing, can effectively remove the impurity on throw out, helps to improve the electroconductibility of ito powder, thereby improves the performance with the ITO target of its preparation; And the required forming pressure of pressure sintering of the present invention is less, and sintering temperature is low, the time is short, and production cost is low, but inhibiting grain growth obtains near theoretical density with than the ITO target of low porosity.
Embodiment
The below is described in further detail the present invention:
The present invention includes following steps:
(1) at first indium metal is dissolved in hydrochloric acid soln, adds tin tetrachloride in this solution, keeping the indium tin mass ratio in mixing solutions is 9.45:1; Then mixing solutions is imported in trolamine and polyvinylpyrrolidonesolution solution, and add ammoniacal liquor, ammoniacal liquor should add according to about 25% mass ratio, thereby forms resulting solution; Then to synthetic solution stirring and heating, obtain the indium tin hydroxide precipitation solution.In implementation process, should control the Heating temperature of solution, generally to be advisable with 80 ℃ of left and right, heating should make solution cooling later, and standing for some time, makes reaction more abundant.In resulting solution, the acidity of reaction soln also can affect the size of producing ito powder, and the present invention can add the pH value of hydrochloric acid conditioning solution in resulting solution, and making pH value is 6-7, and keeps constant, can make like this particle diameter minimum of the ito powder of preparation.Add polyvinylpyrrolidone as protective material, it has good network and ability and provide protection, but the ito powder particle of synthesizing spherical, and particle is comparatively even, and usually, adopting ITO and polyvinylpyrrolidone mass ratio is 10%, can reach better effect.
(2) the indium tin hydroxide precipitation solution is carried out need throw out and liquid are carried out centrifugation after standing precipitation processes, make solid-liquid separation more thorough.
(3) after solid-liquid separation, use the distilled water wash solid sediment, the foreign ion on disgorging, and centrifugation water and sediment.
(4) repeating step is (3) 3 times-5 times, and thoroughly the impurity on the scavenger precipitation thing, improve the purity of precipitation, thereby obtains comparatively clean throw out, improves the purity of calcined powder.
(5) throw out removal of impurities, clean after, need be dried, the further liquid on disgorging, drying can adopt spraying or the method such as freezing; Dried throw out can be calcined, and preferably, calcining furnace adopts the temperature of 1100 ℃-1300 ℃ to calcine, and obtains ito powder.Utilize the mean diameter of the powder that aforesaid method produces between 10nm-100nm.
(6) add polyvinyl alcohol in ito powder, utilize mould that the ito powder dry-pressing is become formed body; As preferably, the mass ratio of polyvinyl alcohol is 0.7%-1.0%, and polyvinyl alcohol is conducive to the ITO powder granule to be reset, and reduces intergranular hole, and then improves density and the intensity of the formed body of preparation; And polyvinyl alcohol also can reduce between the ITO powder and powder and mold wall between friction, make the density distribution of forming pressure and formed body more even, be conducive to the demoulding.But polyvinyl alcohol content is difficult for too high, is guaranteeing that formed body everywhere under the prerequisite of even density, should reduce its consumption, and the present invention most preferably is 0.8%.
(7) formed body is placed in hot pressing furnace and carries out sintering, thereby produce the ITO target.General keep sintering temperature 1100 ℃ of left and right, pressure 10MPa left and right, 300 minutes time to be advisable.The density of the ITO target that can make by aforesaid method reaches more than 99%, satisfies the user demand of most products.
Embodiment
At first indium metal is dissolved in appropriate hydrochloric acid soln, adds tin tetrachloride in this solution, it is 9.45:1 that the indium in the maintenance mixing solutions, the mass conversion of tin ion become Indium sesquioxide and stannic oxide mass ratio; Then mixing solutions is imported trolamine and mass ratio and be in 10% polyvinylpyrrolidonesolution solution, and add the ammoniacal liquor of 25% mass ratio, the violent stirring precipitation solution is 6-7 by the pH value that adds hydrochloric acid to regulate precipitation solution simultaneously; Simultaneously, the Heating temperature of controlling solution is 80 ℃, heats after 120 minutes, makes its naturally cooling, standing precipitation 8 hours; Then throw out is filtered, carry out centrifugal treating, then throw out is placed in distilled water and stirs, centrifugation distilled water and throw out, with distilled water wash throw out 3 times, then the throw out oven dry is placed in calcining furnace, adopts 1200 ℃ of temperature to be sintered into the ito powder particle.Measure the particle diameter of ito powder, its median size is 36nm.Add 1% polyvinyl alcohol in the ito powder particle, be pressed into formed body with mould, after the formed body demoulding, be placed in vacuum sintering furnace, adopt 1100 ℃ of sintering temperatures, pressure 10MPa, 300 minutes time to carry out hot pressing, subsequently sintered compact is made the ITO target.The relative density that sampling records target is 99%.
The present invention is when hot pressing, because powder is in the thermoplasticity state, the deformation resistance is little, is easy to plastic flow and densification, so required forming pressure is less; And in preparation process, heat simultaneously, pressurize, the mass transfer process such as help the contact, diffusion of ito powder particle and flow, can reduce sintering temperature and shorten sintering time, suppressed growing up of crystal grain, not only production cost is lower, and the density of the ITO target of preparation is higher.
Above-mentioned embodiment is only for explanation the present invention's, and be not to be limitation of the present invention, the those of ordinary skill in relevant technologies field, without departing from the spirit and scope of the present invention, can also make various variations and modification, so all technical schemes that are equal to also should belong to category of the present invention.
Claims (6)
1. pressure sintering prepares the method for ITO target, and it comprises the following steps:
(1) at first indium metal is dissolved in hydrochloric acid soln, adds tin tetrachloride in this solution, keeping the indium tin mass ratio in mixing solutions is 9.45:1; Then mixing solutions is imported in trolamine and polyvinylpyrrolidonesolution solution, and add ammoniacal liquor, form resulting solution; Then to the resulting solution heating, obtain the indium tin hydroxide precipitation solution;
(2) throw out and the liquid in the centrifugation precipitation solution;
(3) wash throw out with water, and the centrifugation water and sediment;
(4) repeating step is (3) 3 times-5 times, is precipitated thing;
(5) throw out of drying, calcining step (4), obtain ito powder;
(6) add polyvinyl alcohol in ito powder, utilize mould that the ito powder dry-pressing is become formed body;
(7) formed body is placed in hot pressing furnace, produces the ITO target.
2. pressure sintering according to claim 1 prepares the method for ITO target, it is characterized in that: the mass ratio of described polyvinyl alcohol is 0.7%-1.0%.
3. pressure sintering according to claim 1 prepares the method for ITO target, it is characterized in that: described dissolving Heating temperature is 80 ℃, and keeping the pH value of resulting solution is 6-7.
4. pressure sintering according to claim 1 prepares the method for ITO target, it is characterized in that: the calcining temperature of described step (5) is 1100 ℃-1300 ℃.
5. pressure sintering according to claim 1 prepares the method for ITO target, it is characterized in that: the sintering condition of described step (7) is: 1100 ℃ of temperature, pressure 10MPa, 300 minutes time.
6. pressure sintering according to claim 1 prepares the method for ITO target, it is characterized in that: described polyvinylpyrrolidone and sedimentary mass ratio are 1:10.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669186A (en) * | 2016-01-11 | 2016-06-15 | 北京化工大学 | Preparation method of high-relative density and low-resistivity indium tin oxide target material |
Citations (2)
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| CN101575203A (en) * | 2009-06-19 | 2009-11-11 | 西北稀有金属材料研究院 | Preparation method of ITO sputtering target material |
| CN101580379A (en) * | 2009-06-29 | 2009-11-18 | 北京航空航天大学 | Nb-doped nano indium tin oxide powder and method for preparing high density sputtering coating target thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575203A (en) * | 2009-06-19 | 2009-11-11 | 西北稀有金属材料研究院 | Preparation method of ITO sputtering target material |
| CN101580379A (en) * | 2009-06-29 | 2009-11-18 | 北京航空航天大学 | Nb-doped nano indium tin oxide powder and method for preparing high density sputtering coating target thereof |
Non-Patent Citations (1)
| Title |
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| 张楠等: "分散剂对ITO前驱物浆料稳定性的影响", 《稀有金属材料与工程》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105669186A (en) * | 2016-01-11 | 2016-06-15 | 北京化工大学 | Preparation method of high-relative density and low-resistivity indium tin oxide target material |
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Application publication date: 20130522 |