CN107130217A - A kind of low cost, the preparation method of high-density ITO targe material - Google Patents

A kind of low cost, the preparation method of high-density ITO targe material Download PDF

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CN107130217A
CN107130217A CN201710405569.XA CN201710405569A CN107130217A CN 107130217 A CN107130217 A CN 107130217A CN 201710405569 A CN201710405569 A CN 201710405569A CN 107130217 A CN107130217 A CN 107130217A
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ito
preparation
addition
powders
low cost
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CN107130217B (en
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张天舒
宋晓超
蒋卫国
钱邦正
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ANHUI TUOJITAI NOVEL CERAMIC TECHNOLOGY Co Ltd
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ANHUI TUOJITAI NOVEL CERAMIC TECHNOLOGY Co Ltd
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Abstract

The present invention discloses a kind of low cost, the preparation method of high-density ITO targe material, comprises the following steps：Take dispersant and bonding agent to be added to the water, stir, adjust pH value to 8~11 with ammoniacal liquor, obtain premixed liquid；The dispersant weight ratio is 1~2：1 citric acid and the mixture of poly amic acid；The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, carries out obtaining mixed slurry after ball milling, ball milling in ball mill, is stirred, the bubble removed in slurry is vacuumized；The agglutinant is by rare earth oxide, titanium nitride and nanometer GeO2Composition；Aluminum mould dress on gypsum, gained slurry is injected in aluminum mould；Drying is stripped after midge shaping, ITO base substrates are obtained；Dried ITO base substrates are sintered under the atmosphere of normal pressure purity oxygen, obtain ITO target.Compared with prior art, the product consistency of this method acquisition is high, cost is low, resistivity is low and grain size distribution is uniform.

Description

A kind of low cost, the preparation method of high-density ITO targe material
Technical field
The present invention relates to function ceramics preparing technical field, more particularly to a kind of preparation method of high-density ITO targe material.
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 the sintered density of ITO targets.Though using heat and other static pressuring processes after first isostatic cool pressing, make ITO targets relatively close Degree up to more than 99%, but cost is high, is unfavorable for industrialization large-scale production.It is general using in ito powder in industrial production Suitable agglutinant is added, and pressureless sintering makes the density of target bring up to more than 99% under oxygen atmosphere.
The content of the invention
The present invention provides a kind of preparation method of high-density ITO targe material, optimal sintering aid is filtered out first, with reference to slip casting Advantage (low cost production large-size components) pressureless sintering under the oxygen atmosphere of flowing of moulding process, obtains high density ITO target Material.
To reach above-mentioned purpose, the technical scheme is that：
A kind of preparation method of low-cost high-density ITO target, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant and bonding agent to be added to the water, stir, pH value is adjusted to 8~11 with ammoniacal liquor, Obtain premixed liquid；The addition of dispersant is the 0.2~0.3% of ITO powder qualities, and the addition of bonding agent is ITO powder qualities 0.3~2%, the addition of water is the 10~20% of ITO powder qualities；The dispersant is that weight ratio is 1~2：1 lemon The mixture of acid and poly amic acid；
(2) preparation of suspended nitride：The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, Carry out obtaining mixed slurry after ball milling, ball milling in ball mill, stir, vacuumize the bubble removed in slurry；The sintering Agent is by rare earth oxide, titanium nitride and nanometer GeO2Composition；
(3) injection forming：Aluminum mould dress on gypsum, slurry obtained by step (2) is injected in aluminum mould；Midge into Drying is stripped after type, drying temperature is 30~70 DEG C, obtains ITO base substrates；
(4) sinter：Dried ITO base substrates are sintered under the atmosphere of normal pressure purity oxygen, and temperature is 1450~1550 DEG C, is protected The warm time is 4~8 hours, obtains ITO target.
Wherein it is preferred to, the mass content of tin oxide is 5~20% in the ITO powders, and the mass content of indium oxide is 80~95%, powder purity is not less than 99.9%, and the particle diameter of powder is 0.2~1.0 μm.
Wherein it is preferred to, the bonding agent is polyacrylic based adhesives or polyvinyl butyral resin.
Wherein it is preferred to, the rare earth oxide is CeO2、Y2O3Or Dy2O3, the addition of the rare earth oxide is The 1.0~1.5% of ITO powders.
Wherein it is preferred to, the addition of the titanium nitride is ITO powders 0.005~0.05%, the nanometer GeO2Add Dosage is the 0.6~1.0% of ITO powders.
Beneficial effects of the present invention：
Compared with prior art, innovation of the invention is by rare earth doped oxide, titanium nitride and nanometer GeO2, ITO target is sintered under the atmosphere of normal pressure purity oxygen.By adding sintering in the In-Sn oxide powder that coprecipitation method is synthesized Agent, during sintering, occurs the effect of solid solution and liquid-phase sintering in lower temperature.In addition, in the preparation of suspended nitride Cheng Zhong, ITO powder be suspended in dispersant solution formation Newtonian fluid viscosity it is low, stability is good.ITO powders can uniformly be stablized It is scattered.The viscosity of suspended nitride increases with solid content has exponent relation increase.
The relative density of ITO target prepared by the present invention is 99.0~99.8%, and bending strength is 128~156MPa, electricity Resistance rate is 2.2 × 10-4Ω cm to 3.2 × 10-4Between Ω cm.Compared with prior art, the product that this method is obtained is fine and close Degree is high, resistivity is low and grain size distribution is uniform.The present invention is applied to high density, the preparation of large-size ITO target material.
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 typical microstructure figure of the middle-high density ITO target of the embodiment of the present invention 1.
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 low cost, the preparation method of high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant and bonding agent to be added to the water, stir, adjust pH value to 10 with ammoniacal liquor, obtain pre- Mixed liquid；The addition of dispersant is the 0.25% of ITO powder qualities, and the addition of bonding agent is the 1% of ITO powder qualities, water Addition be ITO powder qualities 15%；The dispersant is that weight ratio is 1~2：1 citric acid and poly amic acid Mixture；
(2) preparation of suspended nitride：The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, Carry out obtaining mixed slurry after ball milling, ball milling in ball mill, stir, vacuumize the bubble removed in slurry；The sintering Agent is by rare earth oxide, titanium nitride and nanometer GeO2Composition；The rare earth oxide is CeO2、Y2O3Or Dy2O3, the metal oxygen The addition of compound is the 1.2% of ITO powders.The addition of the titanium nitride is ITO powders 0.02%, the nanometer GeO2's Addition is the 0.8% of ITO powders；
(3) injection forming：Aluminum mould dress on gypsum, slurry obtained by step (2) is injected in aluminum mould；Midge into Drying is stripped after type, drying temperature is 50 DEG C, obtains ITO base substrates；
(4) sinter：Dried ITO base substrates are sintered under the atmosphere of normal pressure purity oxygen, and temperature is 1450~1550 DEG C, is protected The warm time is 6 hours, obtains ITO target (Fig. 1).
Wherein, the mass content of tin oxide is 12% in the ITO powders, and the mass content of indium oxide is 88%, powder Purity is 99.91%, and the particle diameter of powder is 0.2~1.0 μm.
Wherein, the bonding agent is polyacrylic based adhesives.
The relative density of ITO target manufactured in the present embodiment is 99.8%, and bending strength is 152MPa, and resistivity is 2.2 ×10-4Ω·cm。
Embodiment 2
The present embodiment provides a kind of low cost, the preparation method of high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant and bonding agent to be added to the water, stir, adjust pH value to 8 with ammoniacal liquor, obtain pre- Mixed liquid；The addition of dispersant is the 0.3% of ITO powder qualities, and the addition of bonding agent is the 0.3% of ITO powder qualities, water Addition be ITO powder qualities 20%；The dispersant is that weight ratio is 1~2：1 citric acid and poly amic acid Mixture；
(2) preparation of suspended nitride：The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, Carry out obtaining mixed slurry after ball milling, ball milling in ball mill, stir, vacuumize the bubble removed in slurry；The sintering Agent is by rare earth oxide, titanium nitride and nanometer GeO2Composition；The rare earth oxide is CeO2、Y2O3Or Dy2O3, the rare earth oxygen The addition of compound is the 1.0% of ITO powders.The addition of the titanium nitride is ITO powders 0.05%, the nanometer GeO2's Addition is the 0.6% of ITO powders；
(3) injection forming：Aluminum mould dress on gypsum, slurry obtained by step (2) is injected in aluminum mould；Midge into Drying is stripped after type, drying temperature is 70 DEG C, obtains ITO base substrates；
(4) sinter：Dried ITO base substrates are sintered under the atmosphere of normal pressure purity oxygen, and temperature is 1450~1550 DEG C, is protected The warm time is 4 hours, obtains ITO target.
Wherein, the mass content of tin oxide is 20% in the ITO powders, and the mass content of indium oxide is 80%, powder Purity is 99.95%, and the particle diameter of powder is 0.2~1.0 μm.
Wherein, the bonding agent is polyacrylic based adhesives.
The relative density of ITO target manufactured in the present embodiment is 99.3%, and bending strength is 128MPa, and resistivity is 3.2 ×10-4Ω·cm。
Embodiment 3
The present embodiment provides a kind of low cost, the preparation method of high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant and bonding agent to be added to the water, stir, adjust pH value to 11 with ammoniacal liquor, obtain pre- Mixed liquid；The addition of dispersant is the 0.2% of ITO powder qualities, and the addition of bonding agent is the 2% of ITO powder qualities, water Addition is the 10% of ITO powder qualities；The dispersant is that weight ratio is 1~2：1 citric acid and poly amic acid it is mixed Compound；
(2) preparation of suspended nitride：The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, Carry out obtaining mixed slurry after ball milling, ball milling in ball mill, stir, vacuumize the bubble removed in slurry；The sintering Agent is by rare earth oxide, titanium nitride and nanometer GeO2Composition；The rare earth oxide is CeO2、Y2O3Or Dy2O3, the rare earth oxygen The addition of compound is the 1.5% of ITO powders.The addition of the titanium nitride is ITO powders 0.005%, the nanometer GeO2 Addition be ITO powders 1.0%；
(3) injection forming：Aluminum mould dress on gypsum, slurry obtained by step (2) is injected in aluminum mould；Midge into Drying is stripped after type, drying temperature is 30 DEG C, obtains ITO base substrates；
(4) sinter：Dried ITO base substrates are sintered under the atmosphere of normal pressure purity oxygen, and temperature is 1450~1550 DEG C, is protected The warm time is 8 hours, obtains ITO target.
Wherein, the mass content of tin oxide is 5% in the ITO powders, and the mass content of indium oxide is 95%, and powder is pure Spend for 99.94%, the particle diameter of powder is 0.2~1.0 μm.
Wherein, the bonding agent is polyacrylic based adhesives.
The relative density of ITO target manufactured in the present embodiment is 99.6%, and bending strength is 156MPa, and resistivity is 2.4 ×10-4Ω·cm。
Embodiment 4
The present embodiment provides a kind of low cost, the preparation method of high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant and bonding agent to be added to the water, stir, adjust pH value to 9 with ammoniacal liquor, obtain pre- Mixed liquid；The addition of dispersant is the 0.29% of ITO powder qualities, and the addition of bonding agent is the 0.75% of ITO powder qualities, The addition of water is the 12% of ITO powder qualities；The dispersant is that weight ratio is 1~2：1 citric acid and poly amic acid Mixture；
(2) preparation of suspended nitride：The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, Carry out obtaining mixed slurry after ball milling, ball milling in ball mill, stir, vacuumize the bubble removed in slurry；The sintering Agent is by metal oxide, titanium nitride and nanometer GeO2
Composition；The rare earth oxide is CeO2、Y2O3Or Dy2O3, the addition of the rare earth oxide is ITO powders 1.4%.
The addition of the silicon nitride is ITO powders 0.03%, the nanometer GeO2Addition for ITO powders 0.9%；
(3) injection forming：Aluminum mould dress on gypsum, slurry obtained by step (2) is injected in aluminum mould；Midge into Drying is stripped after type, drying temperature is 50 DEG C, obtains ITO base substrates；
(4) sinter：Dried ITO bodies are sintered under the atmosphere of normal pressure purity oxygen, and temperature is 1450~1550 DEG C, insulation Time is 7 hours, obtains ITO target.
Wherein, the mass content of tin oxide is 14% in the ITO powders, and the mass content of indium oxide is 86%, powder Purity is 99.92%, and the particle diameter of powder is 0.2~1.0 μm.
Wherein, the bonding agent is polyvinyl butyral resin.
The relative density of ITO target manufactured in the present embodiment is 99.5%, and bending strength is 145MPa, and resistivity is 2.8 ×10-4Ω·cm。
Embodiment 5
The present embodiment provides a kind of low cost, the preparation method of high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant and bonding agent to be added to the water, stir, adjust pH value to 10 with ammoniacal liquor, obtain pre- Mixed liquid；The addition of dispersant is the 0.28% of ITO powder qualities, and the addition of bonding agent is the 1.5% of ITO powder qualities, The addition of water is the 19% of ITO powder qualities；The dispersant is that weight ratio is 1~2：1 citric acid and poly amic acid Mixture；
(2) preparation of suspended nitride：The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, Carry out obtaining mixed slurry after ball milling, ball milling in ball mill, stir, vacuumize the bubble removed in slurry；The sintering Agent is by metal oxide, silicon nitride and nanometer GeO2Composition；The rare earth oxide is CeO2、Y2O3Or Dy2O3, the rare earth oxygen The addition of compound is the 1.4% of ITO powders.
The addition of the titanium nitride is ITO powders 0.01%, the nanometer GeO2Addition for ITO powders 0.7%；
(3) injection forming：Aluminum mould dress on gypsum, slurry obtained by step (2) is injected in aluminum mould；Midge into Drying is stripped after type, drying temperature is 50 DEG C, obtains ITO base substrates；
(4) sinter：Dried ITO base substrates are sintered under the atmosphere of normal pressure purity oxygen, and temperature is 1450~1550 DEG C, is protected The warm time is 7 hours, obtains ITO target.
Wherein, the mass content of tin oxide is 8% in the ITO powders, and the mass content of indium oxide is 92%, and powder is pure Spend for 99.93%, the particle diameter of powder is 0.2~1.0 μm.
Wherein, the bonding agent polyvinyl butyral resin.
The relative density of ITO target manufactured in the present embodiment is 99.4%, and bending strength is 135MPa, and resistivity is 2.7 ×10-4Ω·cm。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.

Claims (5)

1. a kind of low cost, the preparation method of high-density ITO targe material, it is characterised in that comprise the following steps：
(1) prepared by premixed liquid：Take dispersant and bonding agent to be added to the water, stir, adjust pH value to 8~11 with ammoniacal liquor, obtain pre- Mixed liquid；The addition of dispersant is the 0.2~0.3% of ITO powder qualities, and the addition of bonding agent is the 0.3 of ITO powder qualities ~2%, the addition of water is the 10~20% of ITO powder qualities；The dispersant is that weight ratio is 1~2：1 citric acid and The mixture of poly amic acid；
(2) preparation of suspended nitride：The ITO powders and agglutinant prepared with chemical coprecipitation is added into premixed liquid, then at Carry out obtaining mixed slurry after ball milling, ball milling in ball mill, stir, vacuumize the bubble removed in slurry；The agglutinant by Rare earth oxide, titanium nitride and nanometer GeO2Composition；
(3) blank forming after slip casting：Aluminum mould dress on gypsum, slurry obtained by step (2) is injected in aluminum mould；Midge Drying is stripped after shaping, drying temperature is 30~70 DEG C, obtains ITO base substrates；
(4) sinter：Dried ITO base substrates are sintered under the atmosphere of normal pressure purity oxygen, and temperature is 1450~1550 DEG C, during insulation Between be 4~8 hours, obtain ITO target.
2. a kind of low cost according to claim 1, the preparation method of high-density ITO targe material, it is characterised in that：It is described The mass content of tin oxide is 5~20% in ITO powders, and the mass content of indium oxide is 80~95%, and powder purity is not less than 99.9%, the particle diameter of powder is 0.2~1.0 μm.
3. a kind of low cost according to claim 1, the preparation method of high-density ITO targe material, it is characterised in that：It is described viscous Agent is connect for polyacrylic based adhesives or polyvinyl butyral resin.
4. a kind of low cost according to claim 1, the preparation method of high-density ITO targe material, it is characterised in that：It is described dilute Native oxide is CeO2、Y2O3Or Dy2O3, the addition of the rare earth oxide is the 1.0~1.5% of ITO powders.
5. a kind of low cost according to claim 1, the preparation method of high-density ITO targe material, it is characterised in that：The nitrogen The addition for changing titanium is ITO powders 0.005~0.05%, the nanometer GeO2Addition be ITO powders 0.6~1.0%.
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CN114032517A (en) * 2021-10-22 2022-02-11 芜湖映日科技股份有限公司 Preparation method of rare earth ion doped ITO target material
CN116715516A (en) * 2023-05-19 2023-09-08 芜湖映日科技股份有限公司 Rare earth doped ITO target and preparation method thereof

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