CN113387682A - ITO target waste target recycling method - Google Patents

ITO target waste target recycling method Download PDF

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CN113387682A
CN113387682A CN202110564896.6A CN202110564896A CN113387682A CN 113387682 A CN113387682 A CN 113387682A CN 202110564896 A CN202110564896 A CN 202110564896A CN 113387682 A CN113387682 A CN 113387682A
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ito
target
waste
temperature
steps
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曾墩风
王志强
石煜
陶成
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Wuhu Yingri Technology Co ltd
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Wuhu Yingri Technology Co ltd
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62204Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62645Thermal treatment of powders or mixtures thereof other than sintering
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3286Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3293Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]

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Abstract

The invention provides a recycling method of an ITO target waste target, which comprises the steps of putting the ITO waste target into a vaporization furnace, raising the temperature in the vaporization furnace to 4000-5000 ℃ in a gradient manner, raising the temperature to 500 ℃ in 0-30min, putting the ITO waste target at the temperature, then preserving the heat, raising the temperature to 3000 ℃ in 30-40min, raising the temperature to 4000-5000 ℃ in 40-60min, then preserving the heat until the ITO waste target is completely vaporized, finally cooling in a nitrogen atmosphere to obtain ITO powder with the purity of 4N and the specific surface of 6-8, carrying out ball milling, cold isostatic pressing, sintering, machining and binding to finally obtain the ITO target, thus adopting the gradient temperature rise, putting the waste target when the temperature is raised to 500 ℃, raising the temperature to 4000-5000 ℃ again, completely vaporizing the waste target, well controlling the complete vaporization of the waste target, and obtaining the ITO powder with high purity and good utilization effect of the waste target.

Description

ITO target waste target recycling method
Technical Field
The invention relates to the field of ITO target materials, in particular to a method for recycling waste ITO target materials.
Background
When the ITO target is used by a customer, the ITO target cannot be used up completely, the utilization rate of the rotary ITO target is 75 percent, the utilization rate of the plane ITO target is 35 percent, and the principles of energy regeneration and environmental protection are relied on, so that a large amount of waste targets need to be recovered. The conventional industry practice is to recover 2N indium from the ITO waste target by dry or wet reduction and refine the indium into 4N indium ingots by a refining mode, and the method has high cost, only utilizes In the ITO waste target and has low recovery value of tin. The prior art patent CN102367519B discloses an efficient recovery method of an ITO waste target, which adopts a plasma gasification method production device to directly gasify an ITO target material to generate ITO powder, the whole recovery process is completed in a plasma gasification device, a stable plasma arc is generated in the device, and the ITO waste target is instantaneously gasified, cooled and collected under the action of the high temperature of the arc. However, the temperature of the arc vaporization of the patent is not limited, only the high temperature of the arc is 3000-6000 ℃, but the vaporization is carried out only by the high temperature of the temperature, the vaporization effect is uncontrollable, and the quality of the recovery effect of the target material is uncontrollable. Therefore, it is necessary to solve this problem.
Disclosure of Invention
In order to solve the problems, the invention provides a recycling method of an ITO target waste target, which comprises the steps of putting the ITO waste target into a vaporization furnace, raising the temperature in the vaporization furnace to 4000-, the problems occurring in the background art are solved.
The invention aims to provide a recycling method of an ITO target waste target, which comprises the steps of putting the ITO waste target into a vaporization furnace, raising the temperature in the vaporization furnace to 4000-;
the temperature rise of the gasification furnace is in gradient rising: heating to 500 ℃ in 0-30min, putting the ITO waste target at the temperature, then preserving heat, heating to 3000 ℃ in 30-40min, heating to 4000-;
and performing ball milling on the ITO powder to obtain nanoscale ITO powder, performing cold isostatic pressing to prepare an ITO blank, sintering to prepare a high-density ITO target intermediate, machining, and binding to finally obtain the ITO target.
The further improvement lies in that: the filling rate of the nitrogen gas is 6L/min after 0-3min, and the filling rate is 2L/min later.
The further improvement lies in that: the ball milling is specifically as follows: and putting the obtained ITO powder into a ball mill for ball milling, sanding and spray granulation in sequence to obtain the nanoscale ITO powder.
The further improvement lies in that: the cold isostatic pressing is specifically as follows: and (3) filling the nano-grade ITO powder prepared by ball milling into a polyurethane mold, and molding by using a cold isostatic pressing device to prepare an ITO blank.
The further improvement lies in that: the sintering specifically comprises the following steps: and sintering the ITO blank prepared by cold isostatic pressing in a high-temperature oxygen sintering furnace to prepare the high-density ITO target intermediate.
The further improvement lies in that: the machining specifically comprises: and (4) carrying out internal and external circular grinding and edge grinding machining on the high-density ITO target intermediate obtained by sintering.
The further improvement lies in that: the binding specifically comprises: binding the high-density ITO target intermediate after machining on the outer surface of the titanium tube.
The invention has the beneficial effects that: the method comprises the steps of putting an ITO waste target into a vaporization furnace, raising the temperature in the vaporization furnace to 4000-; the waste target is placed when the temperature is raised to 500 ℃ by adopting gradient temperature rise, and then the temperature is raised to 4000-; the cooling is carried out in the nitrogen atmosphere, the cooling efficiency is high, the effect is good, the filling rate of nitrogen is 6L/min after 0-3min, and the filling rate is 2L/min, so that the cooling effect is better enhanced; and performing ball milling, sanding, spraying and granulating on the prepared ITO powder to obtain nano ITO powder, preparing an ITO blank, and finally processing and binding by a sintering machine to well utilize the ITO waste target, realize recycling of the ITO waste target and protect the environment.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
The embodiment provides a method for recycling waste ITO target, which comprises the following steps:
the method comprises the following steps: putting the ITO waste target into a vaporizing furnace, and raising the temperature of the vaporizing furnace in a gradient way: heating to 500 ℃ in 0-30min, then preserving heat, heating to 3000 ℃ in 30-40min, putting an ITO waste target at the temperature, heating to 4000-;
step two: putting the obtained ITO powder into a ball mill for ball milling, sanding and spray granulation in sequence to obtain nanoscale ITO powder;
step three: loading the nanoscale ITO powder into a polyurethane mold, and molding by using a cold isostatic pressing device to prepare an ITO blank;
step four: placing the ITO blank in a high-temperature oxygen sintering furnace for sintering to prepare a high-density ITO target intermediate;
step five: carrying out internal and external circular grinding and edge grinding machine processing on the high-density ITO target intermediate;
step six: binding the high-density ITO target intermediate after machining on the outer surface of the titanium tube.
The temperature rise of the vaporizing furnace was analyzed:
Figure DEST_PATH_IMAGE002
therefore, gradient temperature rise is adopted, the temperature is raised to 500 ℃ firstly, the waste target is placed, the temperature is raised to 3000 ℃, the waste target is placed, the temperature is raised to 4000-.
Analysis of nitrogen cooling rate:
Figure DEST_PATH_IMAGE004
therefore, the filling rate is 6L/min after 0-3min, and then the filling rate is 2L/min, so that the cooling effect is better enhanced, and the recovery rate of the ITO powder is high.

Claims (7)

1. A method for recycling waste ITO target is characterized by comprising the following steps: placing the ITO waste target into a vaporization furnace, raising the temperature in the vaporization furnace to 4000-;
the temperature rise of the gasification furnace is in gradient rising: heating to 500 ℃ in 0-30min, putting the ITO waste target at the temperature, then preserving heat, heating to 3000 ℃ in 30-40min, heating to 4000-;
and performing ball milling on the ITO powder to obtain nanoscale ITO powder, performing cold isostatic pressing to prepare an ITO blank, sintering to prepare a high-density ITO target intermediate, machining, and binding to finally obtain the ITO target.
2. The method for recycling the waste ITO target as claimed in claim 1, wherein the method comprises the following steps: the filling rate of the nitrogen gas is 6L/min after 0-3min, and the filling rate is 2L/min later.
3. The method for recycling the waste ITO target as claimed in claim 1, wherein the method comprises the following steps: the ball milling is specifically as follows: and putting the obtained ITO powder into a ball mill for ball milling, sanding and spray granulation in sequence to obtain the nanoscale ITO powder.
4. The method for recycling the waste ITO target as claimed in claim 1, wherein the method comprises the following steps: the cold isostatic pressing is specifically as follows: and (3) filling the nano-grade ITO powder prepared by ball milling into a polyurethane mold, and molding by using a cold isostatic pressing device to prepare an ITO blank.
5. The method for recycling the waste ITO target as claimed in claim 1, wherein the method comprises the following steps: the sintering specifically comprises the following steps: and sintering the ITO blank prepared by cold isostatic pressing in a high-temperature oxygen sintering furnace to prepare the high-density ITO target intermediate.
6. The method for recycling the waste ITO target as claimed in claim 1, wherein the method comprises the following steps: the machining specifically comprises: and (4) carrying out internal and external circular grinding and edge grinding machining on the high-density ITO target intermediate obtained by sintering.
7. The method for recycling the waste ITO target as claimed in claim 1, wherein the method comprises the following steps: the binding specifically comprises: binding the high-density ITO target intermediate after machining on the outer surface of the titanium tube.
CN202110564896.6A 2021-05-24 2021-05-24 ITO target waste target recycling method Pending CN113387682A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114804853A (en) * 2022-05-10 2022-07-29 芜湖映日科技股份有限公司 Method for recycling IGZO waste target

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Publication number Priority date Publication date Assignee Title
JP2004323877A (en) * 2003-04-22 2004-11-18 Sumitomo Metal Mining Co Ltd Ito thin film manufacturing target, and method for manufacturing the same
US20080073819A1 (en) * 2006-09-25 2008-03-27 Cheng Loong Corporation Method of manufacturing sputtering targets
CN101269834A (en) * 2008-05-19 2008-09-24 昆明理工大学 Method for producing nano-ITO powder with plasma electrical arc one-step method
CN102367519A (en) * 2011-09-16 2012-03-07 中国船舶重工集团公司第七二五研究所 Efficient recovering method for waste indium tin oxide (ITO) targets
CN104843771A (en) * 2015-04-24 2015-08-19 柳州百韧特先进材料有限公司 Method for recovering and preparing nanometer TIO powder from ITO target wastes
CN112079627A (en) * 2020-09-16 2020-12-15 韶关市欧莱高新材料有限公司 Preparation method for directly crushing ITO waste target to prepare powder and producing ITO target

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JP2004323877A (en) * 2003-04-22 2004-11-18 Sumitomo Metal Mining Co Ltd Ito thin film manufacturing target, and method for manufacturing the same
US20080073819A1 (en) * 2006-09-25 2008-03-27 Cheng Loong Corporation Method of manufacturing sputtering targets
CN101269834A (en) * 2008-05-19 2008-09-24 昆明理工大学 Method for producing nano-ITO powder with plasma electrical arc one-step method
CN102367519A (en) * 2011-09-16 2012-03-07 中国船舶重工集团公司第七二五研究所 Efficient recovering method for waste indium tin oxide (ITO) targets
CN104843771A (en) * 2015-04-24 2015-08-19 柳州百韧特先进材料有限公司 Method for recovering and preparing nanometer TIO powder from ITO target wastes
CN112079627A (en) * 2020-09-16 2020-12-15 韶关市欧莱高新材料有限公司 Preparation method for directly crushing ITO waste target to prepare powder and producing ITO target

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114804853A (en) * 2022-05-10 2022-07-29 芜湖映日科技股份有限公司 Method for recycling IGZO waste target

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