CN107324778A - A kind of preparation method of high density, high conductivity ITO target - Google Patents
A kind of preparation method of high density, high conductivity ITO target Download PDFInfo
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- CN107324778A CN107324778A CN201710439323.4A CN201710439323A CN107324778A CN 107324778 A CN107324778 A CN 107324778A CN 201710439323 A CN201710439323 A CN 201710439323A CN 107324778 A CN107324778 A CN 107324778A
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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Abstract
The present invention discloses a kind of high density, the preparation method of high conductivity ITO target, comprises the following steps：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material, hydrofluoric acid nitric acid germanium and hydrofluoric acid bismuth nitrate settled solution are produced, above-mentioned two solution is mixed with the indium oxide containing urea with tin oxide solution respectively, is kept stirring for, 90 DEG C are progressively warming up to, and constant temperature 1h is untill precipitation is completely.Washed to without Cl ions and existed with deionized water and organic mixed solvent；Dry, calcining produces the ito powder of bismuth-containing and germanium；Plus it is compressing after 2%PVA granulations, sintered in the oxygen atmosphere of flowing, obtain ITO target, the present invention adds sintering aid using coprecipitation method, reaches being uniformly distributed for atomic size, significantly decreases sintering temperature, promote densification, while improving the electric conductivity of target.
Description
Technical field
The present invention relates to function ceramics preparing technical field, more particularly to a kind of high density, the system of high conductivity ITO target
Preparation Method.
Background technology
Ito thin film can be prepared by ITO target through magnetron sputtering method, in the industrial production, mostly using magnetron sputtering
Method, ITO target is sputtered on glass very thin layer of transparent conducting film (thickness 100nm or so), film is performed etching,
To prepare the electrode material of flat-panel monitor.
The ito film of high-quality is prepared, must be using the ITO targets that uniformity is good and density is high.Because low density target
Inside there is the uncertain element in many holes, hole also to enter ito film in sputter procedure, so as to influence ito film electric conductivity
Energy.The low oxide that other low-density ITO target surfaces easily produce some melanism in sputter procedure is called dross, therefore
Arcing phenomena (i.e. partial breakdown discharges) occurs in sputter procedure, so as to cause sputtering technology unstable, makes to occur in ito film
Impurity defect.Furthermore low-density ITO target thermal conductivities are low, make target cracking etc. due to there is thermal stress in sputter procedure.
The production of ITO target mainly includes powder and prepares, is molded and three key links of sintering.Using nanoscale ITO powder
End, is conducive to improving ITO target densities.Though using high temperature insostatic pressing (HIP) production technology after isostatic cool pressing, make ITO target relative density
More than 99% is brought up to, but cost height is unfavorable for industrialized production, and the target size size of production is limited.Another technique is
Appropriate agglutinant is added in ito powder to improve the sintered density of target.
The content of the invention
The present invention provides a kind of high density, the preparation method of high conductivity ITO target, in order to be able to which preparing for economy is highly dense
Degree, the ITO target of high conductivity, the present invention prepare the ito powder of doped high-activity using the coprecipitation of improvement, pass through nothing
ITO target is made in pressure sintering, and on the one hand the sintering aid after optimization improves the electric conductivity of ITO targets, on the other hand improves ITO targets
Target density.
In order to achieve the above object, the technical scheme is that：
The preparation method of a kind of high density, high conductivity ITO target, comprises the following steps：
(1) preparation of bismuth and germanium mixed solution：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material into
The settled solution of hydrofluoric acid bismuth nitrate and germanium；
(2) preparation of the indium oxide containing urea and tin oxide solution：Urea, indium oxide, tin oxide are each dissolved in water
In, remix together；
(3) it is co-precipitated：Bismuth and germanium mixed solution are added in the mixed solution that step (2) is configured, are kept stirring for, by
Step is warming up to 90 DEG C and constant temperature 1 hours, it is to be precipitated completely untill；
(4) wash：The sediment that step (3) is obtained is washed with deionized to without Cl repeatedly-Ion exist, then with mix
Close organic solvent washing three times；
(5) calcining and granulation：By mixed with the indium tin sediment of bismuth and germanium it is spray-dried after, in 900 DEG C, 3h calcinings are obtained
To the ITO powders for mixing bismuth and germanium, after the PVA for plus 2%, granulated with drying process with atomizing；
(6) shaping and dumping：Pelletizing through single shaft press precompressed after, then through isostatic cool pressing 250MPa handle after obtain ITO element
Base, is warming up to 600 DEG C of insulation 2h with 50 DEG C/h, carries out dumping processing；
(7) sinter：ITO base substrates after dumping are placed in the oxygen atmosphere sintering stove of flowing, ITO target is produced after cooling.
Wherein it is preferred to, In in the step (2)2O3:SnO2=90:10, the addition of urea is with precipitation in step (3)
After completely, the pH of solution>It 8.0 is defined.
Wherein it is preferred to, Ge and Bi addition is the 0.5~2% of In and Sn total amounts, wherein Ge in the step (3):
Bi=1:1.
Wherein it is preferred to, the volume ratio of the organic solvent in the step (4) is 1:3:5 cyclohexanol.Ethyl acetate and
Ethanol.
Wherein it is preferred to, pressureless sintering is with 80~120 DEG C/h to be warming up to 1300 under oxygen atmosphere in the step (7)
~1500 DEG C, it is incubated 5~10 hours.
Beneficial effects of the present invention：
The present invention prepares the ito powder of high activity doping using coprecipitation, using compound organic in washing process
Solvent reduces the hard aggregation of powder, improves sintering activity, while optimizing sintering aid, on the one hand, can reduce sintering temperature, promotees
Enter densification, on the other hand, improve the electric conductivity of target.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also
To obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is the middle-high density of the embodiment of the present invention 1, the typical microstructure figure of high conductivity ITO target.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, all other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of high density, the preparation method of high conductivity ITO target, comprises the following steps：
(1) preparation of bismuth and germanium mixed solution：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material into
The settled solution of hydrofluoric acid bismuth nitrate and germanium；
(2) preparation of the indium oxide containing urea and tin oxide solution：Urea, indium oxide, tin oxide are each dissolved in water
In, remix together；In2O3:SnO2=90:10, after the addition of urea in step (3) to precipitate completely, the pH of solution>
It 8.0 is defined；
(3) it is co-precipitated：Bismuth and germanium mixed solution are added in the mixed solution that step (2) is configured, wherein bismuth and germanium
Content is the 0.5% of In and Sn total amounts, and Bi:Ge=1:1, it is kept stirring for, is progressively warming up to 90 DEG C of simultaneously constant temperature 1 hours, waits to sink
Untill forming sediment completely；
(4) wash：The sediment that step (3) is obtained is washed with deionized to without Cl repeatedly-Ion exist, then with mix
Close organic solvent washing three times；Its mixed organic solvents is that volume ratio is 1:3:5 cyclohexanol, ethyl acetate and ethanol；
(5) calcining and granulation：By mixed with the indium tin sediment of bismuth and germanium it is spray-dried after, in 900 DEG C, 3h calcinings are obtained
To the ITO powders for mixing bismuth and germanium, after the PVA for plus 2%, granulated with drying process with atomizing；
(6) shaping and dumping：Pelletizing through single shaft press precompressed after, then through isostatic cool pressing 250MPa handle after obtain ITO element
Base, is warming up to 600 DEG C of insulation 2h with 50 DEG C/h, carries out dumping processing；
(7) sinter：Base substrate after above-mentioned dumping is placed in the oxygen atmosphere sintering stove of flowing, 1300 are warming up to 80 DEG C/h
DEG C, and it is incubated 10h.
The relative density of ITO targets made from the present embodiment is 99.5%, and target resistivity is 2.1 × 10-4Ω·cm.This implementation
The obtained high density of example, high conductivity ITO target typical microstructure figure are as shown in Figure 1.
Embodiment 2
The present embodiment provides a kind of high density, the preparation method of high conductivity ITO target, comprises the following steps：
(1) preparation of bismuth and germanium mixed solution：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material into
The settled solution of hydrofluoric acid bismuth nitrate and germanium；
(2) preparation of the indium oxide containing urea and tin oxide solution：Urea, indium oxide, tin oxide are each dissolved in water
In, remix together；In2O3:SnO2=90:10, after the addition of urea in step (3) to precipitate completely, the pH of solution>
It 8.0 is defined；
(3) it is co-precipitated：Bismuth and germanium mixed solution are added in the mixed solution that step (2) is configured, wherein bismuth and germanium
Content is the 0.5% of In and Sn total amounts, and Bi:Ge=1:1, it is kept stirring for, is progressively warming up to 90 DEG C of simultaneously constant temperature 1 hours, waits to sink
Untill forming sediment completely；
(4) wash：The sediment that step (3) is obtained is washed with deionized to without Cl repeatedly-Ion exist, then with mix
Close organic solvent washing three times；Its mixed organic solvents is that volume ratio is 1:3:5 cyclohexanol, ethyl acetate and ethanol；
(5) calcining and granulation：By mixed with the indium tin sediment of bismuth and germanium it is spray-dried after, in 900 DEG C, 3h calcinings are obtained
To the ITO powders for mixing bismuth and germanium, after the PVA for plus 2%, granulated with drying process with atomizing；
(6) shaping and dumping：Pelletizing through single shaft press precompressed after, then through isostatic cool pressing 250MPa handle after obtain ITO element
Base, is warming up to 600 DEG C of insulation 2h with 50 DEG C/h, carries out dumping processing；
(7) sinter：Base substrate after above-mentioned dumping is placed in the oxygen atmosphere sintering stove of flowing, is warming up to 110 DEG C/h
1400 DEG C, and it is incubated 8h.
The relative density of ITO targets made from the present embodiment is 99.7%, and target resistivity is 2.2 × 104Ω·cm。
Embodiment 3
The present embodiment provides a kind of high density, the preparation method of high conductivity ITO target, comprises the following steps：
(1) preparation of bismuth and germanium mixed solution：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material into
The settled solution of hydrofluoric acid bismuth nitrate and germanium；
(2) preparation of the indium oxide containing urea and tin oxide solution：Urea, indium oxide, tin oxide are each dissolved in water
In, remix together；In2O3:SnO2=90:10, after the addition of urea in step (3) to precipitate completely, the pH of solution>
It 8.0 is defined；
(3) it is co-precipitated：Bismuth and germanium mixed solution are added in the mixed solution that step (2) is configured, wherein bismuth and germanium
Content is the 0.5% of In and Sn total amounts, and Bi:Ge=1:1, it is kept stirring for, is progressively warming up to 90 DEG C of simultaneously constant temperature 1 hours, waits to sink
Untill forming sediment completely；
(4) wash：The sediment that step (3) is obtained is washed with deionized to without Cl repeatedly-Ion exist, then with mix
Close organic solvent washing three times；Its mixed organic solvents is that volume ratio is 1:3:5 cyclohexanol, ethyl acetate and ethanol；
(5) calcining and granulation：By mixed with the indium tin sediment of bismuth and germanium it is spray-dried after, in 900 DEG C, 3h calcinings are obtained
To the ITO powders for mixing bismuth and germanium, after the PVA for plus 2%, granulated with drying process with atomizing；
(6) shaping and dumping：Pelletizing through single shaft press precompressed after, then through isostatic cool pressing 250MPa handle after obtain ITO element
Base, is warming up to 600 DEG C of insulation 2h with 50 DEG C/h, carries out dumping processing；
(7) sinter：Base substrate after above-mentioned dumping is placed in the oxygen atmosphere sintering stove of flowing, is warming up to 100 DEG C/h
1500 DEG C, and it is incubated 5h.
The relative density of ITO targets made from the present embodiment is 99.8%, and target resistivity is 3.0 × 10-4Ω·cm。
Embodiment 4
The present embodiment provides a kind of high density, the preparation method of high conductivity ITO target, comprises the following steps：
(1) preparation of bismuth and germanium mixed solution：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material into
The settled solution of hydrofluoric acid bismuth nitrate and germanium；
(2) preparation of the indium oxide containing urea and tin oxide solution：Urea, indium oxide, tin oxide are each dissolved in water
In, remix together；In2O3:SnO2=90:10, after the addition of urea in step (3) to precipitate completely, the pH of solution>
It 8.0 is defined；
(3) it is co-precipitated：Bismuth and germanium mixed solution are added in the mixed solution that step (2) is configured, wherein bismuth and germanium
Content is the 1% of In and Sn total amounts, and Bi:Ge=1:1, it is kept stirring for, is progressively warming up to 90 DEG C of simultaneously constant temperature 1 hours, it is to be precipitated
Untill completely；
(4) wash：The sediment that step (3) is obtained is washed with deionized to without Cl repeatedly-Ion exist, then with mix
Close organic solvent washing three times；Its mixed organic solvents is that volume ratio is 1:3:5 cyclohexanol, ethyl acetate and ethanol；
(5) calcining and granulation：By mixed with the indium tin sediment of bismuth and germanium it is spray-dried after, in 900 DEG C, 3h calcinings are obtained
To the ITO powders for mixing bismuth and germanium, after the PVA for plus 2%, granulated with drying process with atomizing；
(6) shaping and dumping：Pelletizing through single shaft press precompressed after, then through isostatic cool pressing 250MPa handle after obtain ITO element
Base, is warming up to 600 DEG C of insulation 2h with 50 DEG C/h, carries out dumping processing；
(7) sinter：Base substrate after above-mentioned dumping is placed in the oxygen atmosphere sintering stove of flowing, 1400 are warming up to 90 DEG C/h
DEG C, and it is incubated 8h.
The relative density of ITO targets made from the present embodiment is 99.6%, and target resistivity is 2.8 × 10-4Ω·cm。
Embodiment 5
The present embodiment provides a kind of high density, the preparation method of high conductivity ITO target, comprises the following steps：
(1) preparation of bismuth and germanium mixed solution：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material into
The settled solution of hydrofluoric acid bismuth nitrate and germanium；
(2) preparation of the indium oxide containing urea and tin oxide solution：Urea, indium oxide, tin oxide are each dissolved in water
In, remix together；In2O3:SnO2=90:10, after the addition of urea in step (3) to precipitate completely, the pH of solution>
It 8.0 is defined；
(3) it is co-precipitated：Bismuth and germanium mixed solution are added in the mixed solution that step (2) is configured, wherein bismuth and germanium
Content is the 2.0% of In and Sn total amounts, and Bi:Ge=1:1, it is kept stirring for, is progressively warming up to 90 DEG C of simultaneously constant temperature 1 hours, waits to sink
Untill forming sediment completely；
(4) wash：The sediment that step (3) is obtained is washed with deionized to without Cl repeatedly-Ion exist, then with mix
Close organic solvent washing three times；Its mixed organic solvents is that volume ratio is 1:3:5 cyclohexanol, ethyl acetate and ethanol；
(5) calcining and granulation：By mixed with the indium tin sediment of bismuth and germanium it is spray-dried after, in 900 DEG C, 3h calcinings are obtained
To the ITO powders for mixing bismuth and germanium, after the PVA for plus 2%, granulated with drying process with atomizing；
(6) shaping and dumping：Pelletizing through single shaft press precompressed after, then through isostatic cool pressing 250MPa handle after obtain ITO element
Base, is warming up to 600 DEG C of insulation 2h with 50 DEG C/h, carries out dumping processing；
(7) sinter：Base substrate after above-mentioned dumping is placed in the oxygen atmosphere sintering stove of flowing, is warming up to 120 DEG C/h
1350 DEG C, and it is incubated 6h.
The relative density of ITO targets made from the present embodiment is 99.7%, and target resistivity is 2.6 × 10-4Ω·cm。
The upper only presently preferred embodiments of the present invention, is not intended to limit the invention, all spirit in the present invention
Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (5)
1. the preparation method of a kind of high density, high conductivity ITO target, it is characterised in that comprise the following steps：
(1) preparation of bismuth and germanium mixed solution：With hydrofluoric acid and nitric acid mixed liquor by high-purity Ge and Bi dissolution of raw material into hydrogen fluorine
The settled solution of acid+nitric acid bismuth and germanium；
(2) preparation of the indium oxide containing urea and tin oxide solution：Urea, indium oxide, tin oxide is each soluble in water, then
It is admixed together；
(3) it is co-precipitated：Bismuth and germanium mixed solution are added in the mixed solution that step (2) is configured, is kept stirring for, progressively rises
Temperature to 90 DEG C and constant temperature 1 hour, it is to be precipitated completely untill；
(4) wash：The sediment that step (3) is obtained is washed with deionized to without Cl repeatedly-Ion is present, then with being mixed with
Machine solvent is washed three times；
(5) calcining and granulation：By mixed with the indium tin sediment of bismuth and germanium it is spray-dried after, in 900 DEG C, 3h calcinings are mixed
After the ITO powders of bismuth and germanium, the PVA for plus 2%, granulated with drying process with atomizing；
(6) shaping and dumping：Pelletizing obtains ITO biscuits after single shaft pressure precompressed, then after isostatic cool pressing 250MPa processing, with
50 DEG C/h is warming up to 600 DEG C of insulation 2h, carries out dumping processing；
(7) sinter：ITO base substrates after dumping are placed in the oxygen atmosphere sintering stove of flowing, ITO target is produced after cooling.
2. a kind of high density according to claim 1, the preparation method of high conductivity ITO target, it is characterised in that：It is described
In in step (2)2O：SnO2=90：10；PH value ＞ 8.0 after the addition of urea is precipitated completely in step (3) is defined.
3. a kind of high density according to claim 1, the preparation method of high conductivity ITO target, it is characterised in that：It is described
Ge and Bi addition total amount is the 0.5~2% of In and Sn total amounts, wherein Ge in step (3):Bi=1:1.
4. a kind of high density according to claim 1, the preparation method of high conductivity ITO target, it is characterised in that：It is described
Organic solvent in step (4) is that volume ratio is 1:3:5 cyclohexanol, ethyl acetate and ethanol.
5. a kind of high density according to claim 1, the preparation method of high conductivity ITO target, it is characterised in that：It is described
Pressureless sintering is that under the oxygen atmosphere of flowing, 1300~1500 DEG C, insulation 5~10 are warming up to 80~120 DEG C/h in step (7)
Hour.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113666736A (en) * | 2021-07-29 | 2021-11-19 | 广州市尤特新材料有限公司 | ITO target material applied to heterojunction and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305957A (en) * | 2001-02-07 | 2001-08-01 | 钟兴文 | Process for preparing powdered mixture of indium oxide and tin oxide |
| CN1868949A (en) * | 2005-05-27 | 2006-11-29 | 北京化工大学 | Preparation method of nanometer grade indium tin oxide composite powder |
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| CN1305957A (en) * | 2001-02-07 | 2001-08-01 | 钟兴文 | Process for preparing powdered mixture of indium oxide and tin oxide |
| CN1868949A (en) * | 2005-05-27 | 2006-11-29 | 北京化工大学 | Preparation method of nanometer grade indium tin oxide composite powder |
| CN102171160A (en) * | 2008-09-25 | 2011-08-31 | Jx日矿日石金属株式会社 | Oxide sintered compact for producing transparent conductive film |
| 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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| CN113666736A (en) * | 2021-07-29 | 2021-11-19 | 广州市尤特新材料有限公司 | ITO target material applied to heterojunction and preparation method thereof |
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