CN107226680A - A kind of preparation method of injection forming high-density ITO targe material - Google Patents

A kind of preparation method of injection forming high-density ITO targe material Download PDF

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CN107226680A
CN107226680A CN201710385688.3A CN201710385688A CN107226680A CN 107226680 A CN107226680 A CN 107226680A CN 201710385688 A CN201710385688 A CN 201710385688A CN 107226680 A CN107226680 A CN 107226680A
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ito
preparation
injection forming
density
forming high
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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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Priority to CN201710385688.3A priority Critical patent/CN107226680A/en
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    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
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Abstract

The present invention discloses a kind of preparation method of injection forming high-density ITO targe material, comprises the following steps：Take dispersant to be added to the water, stir, adjust pH value to 8~11 with ammoniacal liquor, obtain premixed liquid；ITO powders are added into premixed liquid, after ball mill wet-milling；Obtained slurry is subjected to vacuum degassing, slurry after degasification is injected in gypsum mold；It is stripped after being molded through midge, green compact is dried into more than 72h, ITO biscuit bodies are obtained；Plain blank sintering obtains ITO target.It is of the invention to use injection forming with sintering ITO target process route without pressure oxygen atmosphere, can the inexpensive high-end ITO target for producing high densification.

Description

A kind of preparation method of injection forming high-density ITO targe material
Technical field
The present invention relates to tin indium oxide target material preparing technical field, more particularly to a kind of injection forming high-density ITO targe material Preparation method.
Background technology
ITO (tin indium oxide) main component is the composite oxides that tin oxide is solid-solubilized in indium oxide.ITO has very Good photoelectric properties, ITO film has high electric conductivity and visible light transmission, is widely used in solar cell, liquid The various fields such as crystal device, touch-control electroplax.With the quick popularization of liquid crystal flat-panel display device etc., the consumption of ITO target It is more and more, requirement to target also more and more higher.At present, it is target to prepare low sintering ITO target using nano material The direction of researcher's unremitting effort, although conventional method is to prepare nano-ITO powder, but prior art system using coprecipitation Standby ito powder sintering character is poor, and the density of the ITO target finally given is relatively low, limits ITO target in high-end display etc. The application in field.
ITO target blank forming technology is divided into dry-press process and the major class of wet moulding two.Dry method generally uses first precompressed again The method of isostatic cool pressing (CIP)；Wet method is using methods such as injection forming, press filtration injection formings.
Dry-pressing formed technology is that ITO powders are placed directly within mould, carries out axial pressure by press and is molded.It is made Journey is short, simple to operate, but molding blank Density inhomogeneity, mold process easily occur layering, mould and pressing precision are required it is high, It is difficult to suppress big specification base substrate.Injection forming technology is typically by previously prepared ITO slurry casts into plaster mold, using many Face, two-sided or one side midge, make ITO blank formings.Big specification, high density, uniform plane tabular base substrate are can obtain with the method, And cost is relatively low.The difficult point of injection forming is how to develop the technology of preparing for the slurry for being suitable for cast, the technology used at present Prepared slurry has that solid content is low, viscosity big, poor fluidity the shortcomings of, the base substrate prepared is easily cracking, layering, Uneven, deformation etc., causes percent defective to increase, and ITO target relative density is made relatively low.
The content of the invention
The present invention provides one kind using double dispersant slip castings to produce high-density ITO targe material, solves existing ITO Base substrate percent defective is high in the preparation process of the wet moulding of target, obtain the problem of target relative density is relatively low.
In order to solve the above technical problems, the technical scheme is that：
A kind of preparation method of injection forming high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant to be added to the water, stir, adjust pH value to 8~11 with ammoniacal liquor, obtain premixed liquid； The addition of dispersant is the 1.5~3.0% of ITO powder qualities, and the addition of water is the 10~20% of ITO powder qualities；
(2) preparation of suspended nitride：ITO powders are added into premixed liquid, wet-milling is carried out through ball mill；
(3) blank forming：Slurry after ball milling is subjected to vacuum degassing, slurry after vacuum degassing is injected gypsum mold In；It is stripped after midge shaping, green compact is dried into more than 72h, ITO base substrates are obtained；
(4) degreasing：Dry ITO base substrates are placed into debinding furnace and are warming up to 600 DEG C with 0.5 DEG C/min, and are incubated 3h；
(5) sinter：ITO base substrates after degreasing are placed into sintering furnace, under the oxygen atmosphere of flowing, with 50~120 DEG C/ H is warming up to 1450~1650 DEG C, and is incubated 5~10h, by being naturally cooling to temperature less than 200 DEG C, and obtains high density ITO target Material.
Wherein it is preferred to, the ITO powder purities are more than 99.99%, and average particle size range is 0.10~0.3 μm.
Wherein it is preferred to, the dispersant is that weight ratio is 1:1~2 citric acid and the mixture of poly amic acid.
Wherein it is preferred to, the dispersant is that weight ratio is 1:1~2 citric acid and the mixture of polyethylene glycol.
Wherein it is preferred to, the dispersant is that weight ratio is 1:1~2 citric acid and the mixture of gum arabic.
Wherein it is preferred to, the ball-milling medium of ball mill is a diameter of 5mm zirconia ball, ratio of grinding media to material in the step (2) For 2~4：1.
Wherein it is preferred to, nylon tank rotating speed is 120rpm in the step (2), and milling time is 35~45h.
Beneficial effects of the present invention：
The present invention, due to combining regulation solution ph using double dispersants, makes Gao Gu in the preparation process of suspended nitride Content ITO powders suspend, and formation Newtonian fluid viscosity in aqueous is low, and stability is good.The viscosity of suspended substance increases with solid content Plus have exponent relation increase.The present invention prepares its viscosity number of high solids content ITO slurries for 140~265mPas (room temperature, rotating speed 20s-1), its good mobility can be smoothed out casting process.
Particle micro-structural is obtained in ITO base substrates using the slurry injection forming of optimization uniform and fine and close, it is scarce without substantially macroscopic view Fall into.Add after dispersant, green compact radial crushing strength increases to 13.5MPa, be conducive to the processes such as follow-up biscuit carrying, processing. After oversintering, almost fully dense sintered body is obtained, relative density is more than 99.0%.Its uniform microstructure, it is not different Normal crystal grain is grown up and abnormal defect.
Using injection forming and the pressureless sintering ITO target technique in oxygen atmosphere low cost, height can be made fine and close in the present invention The ITO target of change.
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.
The base substrate typical microstructure obtained in Fig. 1 present invention using the injection forming technology after optimization；
The ITO target typical microstructure of high densification is made in Fig. 2 present invention.
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 preparation method of injection forming high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant to be added to the water, stir, adjust pH value to 9 with ammoniacal liquor, obtain premixed liquid；It is scattered The addition of agent is the 2.2% of ITO powder qualities, and the addition of water is the 15% of ITO powder qualities；
(2) preparation of suspended nitride：ITO powders are added into premixed liquid, then wet-milling is carried out through ball mill；Prepare ITO slurries It is 195mPas (room temperature, rotating speed 20s to expect its viscosity number-1)
(3) blank forming：Slurry after ball milling is subjected to vacuum degassing, slurry after degasification is injected in gypsum mold；Inhale Be stripped after slurry shaping, green compact are dried into 72h, ITO base substrates are obtained (see Fig. 1)；
(4) degreasing：Dry ITO base substrates are placed into debinding furnace and are warming up to 600 DEG C with 0.5 DEG C/min, and are incubated 3h；
(5) sinter：ITO base substrates after degreasing are placed into sintering furnace, under the oxygen atmosphere of flowing, heated up with 75 DEG C/h To 1500 DEG C, and 8h is incubated, by being naturally cooling to temperature less than 200 DEG C, and obtains high-density ITO targe material.
Wherein, the ITO powder purities are more than 99.99%, and average particle size range is 0.10~0.3 μm.
Wherein, the dispersant is that weight ratio is 1:1 citric acid and the mixture of poly amic acid.
Wherein, the zirconia ball that the ball-milling medium of ball mill is a diameter of 5mm in the step (2), ratio of grinding media to material is 3：1.
Wherein, nylon tank rotating speed is 120rpm in the step (2), and milling time is 40h.
The relative density that sampling measures ITO target made from the present embodiment is 99.6%.Its typical micro-structural is shown in Fig. 2.
Embodiment 2
The present embodiment provides a kind of preparation method of injection forming high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant to be added to the water, stir, adjust pH value to 8 with ammoniacal liquor, obtain premixed liquid；It is scattered The addition of agent is the 3.0% of ITO powder qualities, and the addition of water is the 10% of ITO powder qualities；
(2) preparation of suspended nitride：ITO powders are added into premixed liquid, then wet-milling is carried out through ball mill；Prepare ITO slurries It is 240mPas (room temperature, rotating speed 20s to expect its viscosity number-1)
(3) blank forming：Slurry after ball milling is subjected to vacuum degassing, slurry after degasification is injected in gypsum mold；Inhale It is stripped after slurry shaping, green compact is dried into 80h, ITO base substrates are obtained；
(4) degreasing：Dry ITO base substrates are placed into debinding furnace and are warming up to 600 DEG C with 0.5 DEG C/min, and are incubated 3h；
(5) sinter：ITO base substrates after degreasing are placed into sintering furnace, under the oxygen atmosphere of flowing, heated up with 50 DEG C/h To 1450 DEG C, and 10h is incubated, by being naturally cooling to temperature less than 200 DEG C, and obtains high-density ITO targe material.
Wherein, the ITO powder purities are more than 99.99%, and average particle size range is 0.10~0.3 μm.
Wherein, the dispersant is that weight ratio is 1:2 citric acid and the mixture of polyethylene glycol.
Wherein, the zirconia ball that the ball-milling medium of ball mill is a diameter of 5mm in the step (2), ratio of grinding media to material is 2：1.
Wherein it is preferred to, nylon tank rotating speed is 120rpm in the step (2), and milling time is 35h.
The relative density that sampling measures ITO target made from the present embodiment is 99.5%.
Embodiment 3
The present embodiment provides a kind of preparation method of injection forming high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant to be added to the water, stir, adjust pH value to 11 with ammoniacal liquor, obtain premixed liquid；Point The addition of powder is the 1.5% of ITO powder qualities, and the addition of water is the 20% of ITO powder qualities；
(2) preparation of suspended nitride：ITO powders are added into premixed liquid, then wet-milling is carried out through ball mill；Prepare ITO slurries It is 140mPas (room temperature, rotating speed 20s to expect its viscosity number-1)
(3) blank forming：Slurry after ball milling is subjected to vacuum degassing, slurry after degasification is injected in gypsum mold；Inhale It is stripped after slurry shaping, green compact is dried into 84h, ITO base substrates are obtained；
(4) degreasing：Dry ITO base substrates are placed into debinding furnace and are warming up to 600 DEG C with 0.5 DEG C/min, and are incubated 3h；
(5) sinter：ITO base substrates after degreasing are placed into sintering furnace, under the oxygen atmosphere of flowing, with 120 DEG C/h liters Temperature is incubated 5h to 1650 DEG C, by being naturally cooling to temperature less than 200 DEG C, and obtains high-density ITO targe material.
Wherein, the ITO powder purities are more than 99.99%, and average particle size range is 0.10~0.3 μm.
Wherein, the dispersant is that weight ratio is 1:2 citric acid and the mixture of gum arabic.
Wherein, the zirconia ball that the ball-milling medium of ball mill is a diameter of 5mm in the step (2), ratio of grinding media to material is 4：1.
Wherein, nylon tank rotating speed is 120rpm in the step (2), and milling time is 45h.
The relative density that sampling measures ITO target made from the present embodiment is 99.6%.
Embodiment 4
The present embodiment provides a kind of preparation method of injection forming high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant to be added to the water, stir, adjust pH value to 10 with ammoniacal liquor, obtain premixed liquid；Point The addition of powder is the 2.4% of ITO powder qualities, and the addition of water is the 12% of ITO powder qualities；
(2) preparation of suspended nitride：ITO powders are added into premixed liquid, then wet-milling is carried out through ball mill；Prepare ITO slurries It is 265mPas (room temperature, rotating speed 20s to expect its viscosity number-1)
(3) blank forming：Slurry after ball milling is subjected to vacuum degassing, slurry after degasification is injected in gypsum mold；Inhale It is stripped after slurry shaping, green compact is dried into 72h, ITO base substrates are obtained；
(4) degreasing：Dry ITO base substrates are placed into debinding furnace and are warming up to 600 DEG C with 0.5 DEG C/min, and are incubated 3h；
(5) sinter：ITO base substrates after degreasing are placed into sintering furnace, under the oxygen atmosphere of flowing, heated up with 60 DEG C/h To 1600 DEG C, and 6h is incubated, by being naturally cooling to temperature less than 200 DEG C, and obtains high-density ITO targe material.
Wherein, the ITO powder purities are more than 99.99%, and average particle size range is 0.1~0.3 μm.
Wherein, the dispersant is that weight ratio is 1:1 citric acid and the mixture of gum arabic.
Wherein, the zirconia ball that the ball-milling medium of ball mill is a diameter of 5mm in the step (2), ratio of grinding media to material is 3：1.
Wherein, nylon tank rotating speed is 120rpm in the step (2), and milling time is 40h.
The relative density that sampling measures ITO target made from the present embodiment is 99.7%.
Embodiment 5
The present embodiment provides a kind of preparation method of injection forming high-density ITO targe material, comprises the following steps：
(1) prepared by premixed liquid：Take dispersant to be added to the water, stir, adjust pH value to 9 with ammoniacal liquor, obtain premixed liquid；It is scattered The addition of agent is the 1.8% of ITO powder qualities, and the addition of water is the 12% of ITO powder qualities；
(2) preparation of suspended nitride：ITO powders are added into premixed liquid, wet-milling is carried out in ball mill；Prepare ITO Its viscosity number of slurry is 212mPas (room temperature, rotating speed 20s-1)
(3) blank forming：Slurry after ball milling is subjected to vacuum degassing, slurry after degasification is injected in gypsum mold；Inhale It is stripped after slurry shaping, green compact is dried into 72h, ITO base substrates are obtained；
(4) degreasing：Dry ITO base substrates are placed into debinding furnace and are warming up to 600 DEG C with 0.5 DEG C/min, and are incubated 3h；
(5) sinter：ITO base substrates after degreasing are placed into sintering furnace, under the oxygen atmosphere of flowing, heated up with 80 DEG C/h To 1550 DEG C, and 7h is incubated, by being naturally cooling to temperature less than 200 DEG C, and obtains high-density ITO targe material.
Wherein, the ITO powder purities are more than 99.99%, and average particle size range is 0.10~0.3 μm.
Wherein, the dispersant is that weight ratio is 1:2 citric acid and the mixture of polyethylene glycol.
Wherein, the zirconia ball that the ball-milling medium of ball mill is a diameter of 5mm in the step (2), ratio of grinding media to material is 3：1.
Wherein, nylon tank rotating speed is 120rpm in the step (2), and milling time is 40h.
The relative density that sampling measures ITO target made from the present embodiment is 99.8%.
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 (7)

1. a kind of preparation method of injection forming high-density ITO targe material, it is characterised in that comprise the following steps：
(1) prepared by premixed liquid：Take dispersant to be added to the water, stir, adjust pH value to 8~11 with ammoniacal liquor, obtain premixed liquid；It is scattered The addition of agent is the 1.5~3.0% of ITO powder qualities, and the addition of water is the 10~20% of ITO powder qualities；
(2) preparation of suspended nitride：ITO powders are added into premixed liquid, wet-milling is carried out through ball mill；
(3) blank forming：Slurry after ball milling is subjected to vacuum degassing, slurry after vacuum degassing is injected in gypsum mold；Inhale It is stripped after slurry shaping, green compact is dried into more than 72h, ITO base substrates are obtained；
(4) degreasing：Dry ITO base substrates are placed into debinding furnace and are warming up to 600 DEG C with 0.5 DEG C/min, and are incubated 3h；
(5) sinter：ITO base substrates after degreasing are placed into sintering furnace, under the oxygen atmosphere of flowing, with 50~120 DEG C/h liters Temperature is incubated 5~10h to 1450~1650 DEG C, by being naturally cooling to temperature less than 200 DEG C, and obtains high-density ITO targe material.
2. a kind of preparation method of injection forming high-density ITO targe material according to claim 1, it is characterised in that：It is described ITO powder purities are more than 99.99%, and average particle size range is 0.10~0.3 μm.
3. a kind of preparation method of injection forming high-density ITO targe material according to claim 1, it is characterised in that：It is described Dispersant is that weight ratio is 1:1~2 citric acid and the mixture of poly amic acid.
4. a kind of preparation method of injection forming high-density ITO targe material according to claim 1, it is characterised in that：It is described Dispersant is that weight ratio is 1:1~2 citric acid and the mixture of polyethylene glycol.
5. a kind of preparation method of injection forming high-density ITO targe material according to claim 1, it is characterised in that：It is described Dispersant is that weight ratio is 1:1~2 citric acid and the mixture of gum arabic.
6. a kind of preparation method of injection forming high-density ITO targe material according to claim 1, it is characterised in that：It is described The ball-milling medium of ball mill is a diameter of 5mm zirconia ball in step (2), and ratio of grinding media to material is 2~4：1.
7. a kind of preparation method of injection forming high-density ITO targe material according to claim 6, it is characterised in that：It is described Nylon tank rotating speed is 120rpm in step (2), and milling time is 35~45h.
CN201710385688.3A 2017-05-26 2017-05-26 A kind of preparation method of injection forming high-density ITO targe material Pending CN107226680A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863343A (en) * 2018-06-22 2018-11-23 广东凯盛光伏技术研究院有限公司 A kind of method of the sintering integrated formula production ITO target of degreasing-
CN112592172A (en) * 2020-12-15 2021-04-02 株洲火炬安泰新材料有限公司 Method for preparing ITO sintered body
CN113461420A (en) * 2021-06-21 2021-10-01 桂林电子科技大学 Preparation method of high-density ITO target material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1801400A (en) * 2005-01-07 2006-07-12 中南大学 In203-Sn02 nano film coating material and its preparing method
CN102718499A (en) * 2012-07-10 2012-10-10 国家钽铌特种金属材料工程技术研究中心 Manufacturing method of ITO (Indium Tin Oxide) sputtering target comprising In4Sn3O12 phases
CN103044021A (en) * 2012-12-28 2013-04-17 中国船舶重工集团公司第七二五研究所 Preparation method of slip-casting high-density and high-strength ITO target green body

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1801400A (en) * 2005-01-07 2006-07-12 中南大学 In203-Sn02 nano film coating material and its preparing method
CN102718499A (en) * 2012-07-10 2012-10-10 国家钽铌特种金属材料工程技术研究中心 Manufacturing method of ITO (Indium Tin Oxide) sputtering target comprising In4Sn3O12 phases
CN103044021A (en) * 2012-12-28 2013-04-17 中国船舶重工集团公司第七二五研究所 Preparation method of slip-casting high-density and high-strength ITO target green body

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
钟景明等: "粉浆浇注制备大尺寸 ITO 靶材工艺", 《中国有色金属学报》 *
陈大明: "《先进陶瓷材料的注凝技术与应用》", 30 November 2011, 北京：国防工业出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108863343A (en) * 2018-06-22 2018-11-23 广东凯盛光伏技术研究院有限公司 A kind of method of the sintering integrated formula production ITO target of degreasing-
CN108863343B (en) * 2018-06-22 2021-06-08 广东凯盛光伏技术研究院有限公司 Method for producing ITO target material through integrated degreasing and sintering
CN112592172A (en) * 2020-12-15 2021-04-02 株洲火炬安泰新材料有限公司 Method for preparing ITO sintered body
CN113461420A (en) * 2021-06-21 2021-10-01 桂林电子科技大学 Preparation method of high-density ITO target material

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