CN102367519A - Efficient recovering method for waste indium tin oxide (ITO) targets - Google Patents
Efficient recovering method for waste indium tin oxide (ITO) targets Download PDFInfo
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- CN102367519A CN102367519A CN2011102739546A CN201110273954A CN102367519A CN 102367519 A CN102367519 A CN 102367519A CN 2011102739546 A CN2011102739546 A CN 2011102739546A CN 201110273954 A CN201110273954 A CN 201110273954A CN 102367519 A CN102367519 A CN 102367519A
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Abstract
The invention provides an efficient recovering method for waste indium tin oxide (ITO) targets. A plasma gasification method production device is adopted so that the ITO targets are directly gasified to generate ITO powder, the whole recovery process is completed in a plasma gasification device, the stable plasma electric arch is generated in the device, and the waste ITO targets can be instantaneously gasified, cooled and collected under the effect of high temperature of the electric arc. The plasma gasification method production device is applied to the field of waste ceramic target recovery, the efficiency recovery of waste ITO targets is successfully realized, the recovery efficiency can reach 99 percent, the average particle diameter of the prepared ITO powder particles is smaller than 100nm, the appearances of particles are most in a spherical shape and a square shape, the powder conglobation is little, and the powder can be directly used for producing ITO targets. The method has the obvious advantages that the work procedure is simple, the automation degree is high, the cyclic reutilization period is short, the recovery rate is high, the cost is low, the energy is saved, the environment is protected, and the like.
Description
Technical field
The present invention relates to a kind of indium tin composite oxides technology, the efficient recycling method of the useless target of particularly a kind of ITO.
Background technology
ITO (Tin-doped Indium Oxide) target is a kind of indium tin compound oxidate ceramic material; The ITO film has characteristics such as printing opacity, conduction and heat reflection; Being widely used in the aspects such as antifrost antifogging glass, sun power cumulative device and lighting of transparency electrode, top-grade building curtain wall, aircraft and the vehicle of flat panel display device, is a kind of important photovaltaic material.In the industrial application, the utilization ratio of ITO target as sputter plated film generally is merely 30% ~ 40%, and rest parts becomes waste target, adds the scrap stock, cutting, the waste product that produce in the target material moulding process.Present global ITO amount of target material surpasses 1000 tons, and the annual waste target that produces is about about 400 tons.Indium is a rare precious metal, and explored in the world total reserves has only 1.6 ten thousand tons, and China is the maximum product indium state in the whole world, also is maximum export State, and primary indium output accounts for more than 60% of global primary indium total amount.Therefore, the recycle of indium is very important, and the recovery of the useless target of ITO is to account for more than 85% of indium recycle.
ITO is useless, and target master composition is: indium 70% ~ 75%, and tin 7% ~ 8%, other are oxygen, the impurity trace.The core of the useless target recovery technology of conventional I TO is effective separation of indium, tin, and with the quality of thick indium and the yield criterion as state of the art, disclosed at present recovery technology has methods such as electrolysis, hydrolytic precipitation, alkaline process separation, displacement.Open application number CN1487102A proposes a kind of method that from the useless target of indium tin oxide, reclaims indium: the useless target cracker of ITO is milled to granularity <behind the 149 μ m; Adopt leaching, removal of impurities, displacement, electrolytic full wet process from useless ITO target, to reclaim indium, obtain containing indium and reach 99.99% high purity indium.What open application number CN101701292A adopted is oxidation style reclaims indium tin from the ITO waste target method: ITO is given up target behind fragmentation, ball milling; The enriching dissolving with hydrochloric acid leaches; Obtain leached mud through adding NaOH oxidation leach liquor and regulating pH value, realize after washing, roasting, oxidation that again tin separates, obtain thick indium; Behind once electrolytic, obtain the 4N indium, the recovery of indium can be stabilized in more than 97%.What openly application number CN101701291A adopted is distillation method reclaims indium tin from the useless target of ITO method, and the useless target of ITO behind fragmentation, ball milling, is leached hydrochloric acid; Add proper amount of oxidant; Process distillation stoste, separate indium, tin, reach the purpose of useless target recycle by certain distil process.
It is not thorough that above-mentioned these methods all exist indium, tin to separate, and flow process is loaded down with trivial details, and efficient is lower, the high deficiency of cost recovery.The while traditional method need add strong acid reacts, and can produce a large amount of spent acid solutions, serious environment pollution.
Summary of the invention
Technical problem to be solved by this invention provides the efficient recycling method of the useless target of a kind of ITO, to the deficiency of the useless target recovery technology of conventional I TO, realizes simple, the purposes such as the recovery is high, industrialization degree is high, cost recovery is low, energy-conserving and environment-protective of technical process.
For the purpose that realizes solving the problems of the technologies described above, the present invention has adopted following technical scheme:
The efficient recycling method of the useless target of a kind of ITO of the present invention adopts plasma gasification method production equipment, makes ITO target direct gasification generate ito powder; The whole recovery process is accomplished in the plasma gasification installation, produces stabilized plasma electric arc in this device, and the moment gasification of the useless target of ITO, cooling are collected under the high arc temperature effect.
Concrete technology is:
(1) the useless target cleaning surfaces of ITO: after the obvious foreign material in the target top layer of will giving up are earlier removed; Be placed on and soak 10 ~ 15min in the organic solvent; Taking out the wipe surfaces organic solvent or treat that the organic solvent volatilization finishes, is after scavenging solution carries out ultrasonic cleaning in order to pure water again, dried for standby;
(2) plasma gasification method reclaims the useless target of ITO: removal process is accomplished in plasma gasification production equipment, and dried ITO target is placed in the plasma gasification production equipment reactor drum as negative electrode, and plasma gun is as anode; The ITO target is to be again electrical conductor by the gasification body, between negative electrode and anode, feeds big electric current, resistance heat that this electric current produces and high-intensity magnetic field to the effusive compression under; Produce electric arc; Make the ITO target become steam, under the oxygen atmosphere protection, quenching forms ito powder.
Preferred organic is hydro carbons, ethers, ketone, the unary alcohol organic solvent of boiling point below 200 ℃.Preferred organic solvent is the mixture of any or its arbitrary proportion of ethanol, ether, acetone, hexanaphthene, gasoline, sherwood oil, toluene, ethylbenzene, benzene, YLENE.
Described plasma gasification method reclaims the useless target technology of ITO, its more specifically technical scheme be: the useless target of the ITO after will cleaning is inserted in the plasma gasification production equipment reactor drum, is positioned at below the plasma gun; Reactor drum feeds filtrated air or purity oxygen, forms the oxygen atmosphere protection; Between useless target of ITO and plasma gun, feed electric current, the strength of current scope is 50A ~ 2000A, and the distance between the useless target of adjustment plasma gun and ITO produces continuous electric arc; Under the high-temperature electric arc effect, the gasification of ITO waste target becomes oxide compound steam, and oxide compound steam forms ito powder after cooling off.
Because the temperature of filtrated air or purity oxygen is about 20～30 ℃ under the normal temperature; The temperature of high-temperature electric arc then is about 3000～6000 ℃; Make and have great condensate depression between ITO steam and air or the purity oxygen; Quenching has taken place in the moment that contacts with air or purity oxygen in ITO steam, effectively retrains growing up of oxide particle, the final ito powder median size < 100nm that collects.
Through adopting technique scheme, the present invention has following beneficial effect:
The present invention is applied to the plasma method production equipment that gasifies in the useless target recovery field of pottery, has successfully realized the high efficiente callback of the useless target of ITO, and organic efficiency can reach 99%; The present invention can directly be prepared into ito powder with the useless target of ITO, and < 100nm, granule-morphology are near-spherical and cubic shape to the median size of powder particle mostly, and powder agglomeration is few; Prepared ito powder can directly be used to produce the ITO target, has shortened the cycling and reutilization cycle of useless target greatly; The present invention compares tangible advantages such as having operation is simple, level of automation is high, the cycling and reutilization cycle is short, the recovery is high, cost is low, energy-conserving and environment-protective with traditional recovery technology.
Description of drawings
Fig. 1 is that embodiment 1 reclaims the ito powder tem observation photo of preparation.
Fig. 2 is that embodiment 2 reclaims the ito powder tem observation photo of preparation.
Embodiment
Embodiment 1
With wipe surfaces behind the acetone solution immersion 15min, water is that scavenging solution is used ultrasonic cleaning 2h to the target that will give up then earlier, puts into plasma gasification method production equipment then, with the direct starting the arc of plasma gun, the continual and steady electric arc of generation, and gasification, and powder is received in quenching.
Parameter is following:
Electric current: ~ 1000A
WV: ~ 50V
Open circuit voltage: ~ 100V
Adopting the phase composite of XRD analysis powder is single cube of In
2O
3Structure does not have the appearance of other diffraction peak, has obtained the ito powder of standard construction.
Adopt the pattern and the grain size of tem analysis powder, employing acetone is dispersion liquid, and ultrasonic dispersing five minutes is dipped in and got upper liquid and drip and on copper mesh, carry out tem observation, result such as Fig. 1.Spherical and the cubic shape of microscopic appearance major part type of being of ito powder, powder median size < 100nm, good dispersibility.
Embodiment 2
Technology is the same, and parameter is following:
Electric current: ~ 2000A
WV: ~ 80V
Open circuit voltage: ~ 200V
Adopting the phase composite of XRD analysis powder is single cube of In
2O
3Structure does not have the appearance of other diffraction peak, has obtained the ito powder of standard construction.
Adopt the pattern and the grain size of tem analysis powder, employing acetone is dispersion liquid, and ultrasonic dispersing five minutes is dipped in and got upper liquid and drip and on copper mesh, carry out tem observation, result such as Fig. 2.Spherical and the cubic shape of microscopic appearance major part type of being of ito powder, powder median size < 100nm, good dispersibility.
Claims (4)
1. the efficient recycling method of the useless target of an ITO is characterized in that concrete technology is:
(1) the useless target cleaning surfaces of ITO: after the obvious foreign material in the target top layer of will giving up are earlier removed; Be placed on and soak 10 ~ 15min in the organic solvent; Taking out the wipe surfaces organic solvent or treat that the organic solvent volatilization finishes, is after scavenging solution carries out ultrasonic cleaning in order to pure water again, dried for standby;
(2) plasma gasification method reclaims the useless target of ITO: removal process is accomplished in plasma gasification production equipment, and dried ITO target is placed in the plasma gasification production equipment reactor drum as negative electrode, and plasma gun is as anode; The ITO target is to be again electrical conductor by the gasification body, between negative electrode and anode, feeds big electric current, resistance heat that this electric current produces and high-intensity magnetic field to the effusive compression under; Produce electric arc; Make the ITO target become steam, under the oxygen atmosphere protection, quenching forms ito powder.
2. according to the efficient recycling method of the useless target of the said ITO of claim 1, it is characterized in that: described organic solvent is hydro carbons, ethers, ketone, the unary alcohol organic solvent of boiling point below 200 ℃.
3. according to the efficient recycling method of the useless target of the said ITO of claim 1, it is characterized in that: described organic solvent is the mixture of any or its arbitrary proportion of ethanol, ether, acetone, hexanaphthene, gasoline, sherwood oil, toluene, ethylbenzene, benzene, YLENE.
4. according to the efficient recycling method of the useless target of the said ITO of claim 1, it is characterized in that: it is that the useless target of the ITO after cleaning is inserted in the plasma gasification production equipment reactor drum that described ion evaporating method reclaims the useless target technology of ITO, is positioned at the plasma gun below; Reactor drum feeds filtrated air or purity oxygen, forms the oxygen atmosphere protection; Between useless target of ITO and plasma gun, feed electric current, the strength of current scope is 50A ~ 2000A, and the distance between the useless target of adjustment plasma gun and ITO produces continuous electric arc; Under the high-temperature electric arc effect, the gasification of ITO waste target becomes oxide compound steam, and oxide compound steam forms ito powder after cooling off.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104032133A (en) * | 2014-05-14 | 2014-09-10 | 中国船舶重工集团公司第七二五研究所 | Method for recovering metal indium and tin from ITO waste target |
| 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 |
| CN105366709B (en) * | 2015-10-15 | 2017-03-22 | 中国船舶重工集团公司第七二五研究所 | Method for effectively recycling indium and tin oxide (ITO) waste targets |
| CN107129277A (en) * | 2017-04-07 | 2017-09-05 | 中国船舶重工集团公司第七二五研究所 | A kind of useless targets of ITO reclaim the method that powder prepares ITO target |
| CN108002815A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | A kind of preparation method of tubulose ITO target |
| CN110498443A (en) * | 2019-08-23 | 2019-11-26 | 云南锡业集团（控股）有限责任公司研发中心 | A method of with ITO give up target recasting ITO powder |
| CN111620367A (en) * | 2020-06-08 | 2020-09-04 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO residual target/waste target |
| CN113387682A (en) * | 2021-05-24 | 2021-09-14 | 芜湖映日科技股份有限公司 | ITO target waste target recycling method |
| CN113999000A (en) * | 2021-10-21 | 2022-02-01 | 宁波江丰电子材料股份有限公司 | Method for recycling ITO waste target |
| 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 |
| CN114956162A (en) * | 2022-07-04 | 2022-08-30 | 广东先导稀材股份有限公司 | Method for recovering indium oxide waste |
Citations (1)
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| CN101269834B (en) * | 2008-05-19 | 2011-04-06 | 昆明理工大学 | Method for producing nano-ITO powder with plasma electrical arc one-step method |
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2011
- 2011-09-16 CN CN2011102739546A patent/CN102367519B/en not_active Expired - Fee Related
Patent Citations (1)
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| CN101269834B (en) * | 2008-05-19 | 2011-04-06 | 昆明理工大学 | Method for producing nano-ITO powder with plasma electrical arc one-step method |
Non-Patent Citations (2)
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104032133A (en) * | 2014-05-14 | 2014-09-10 | 中国船舶重工集团公司第七二五研究所 | Method for recovering metal indium and tin from ITO waste target |
| 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 |
| CN105366709B (en) * | 2015-10-15 | 2017-03-22 | 中国船舶重工集团公司第七二五研究所 | Method for effectively recycling indium and tin oxide (ITO) waste targets |
| CN107129277B (en) * | 2017-04-07 | 2020-08-28 | 中国船舶重工集团公司第七二五研究所 | Method for preparing ITO target material by recovering powder from waste ITO target |
| CN107129277A (en) * | 2017-04-07 | 2017-09-05 | 中国船舶重工集团公司第七二五研究所 | A kind of useless targets of ITO reclaim the method that powder prepares ITO target |
| CN108002815A (en) * | 2017-11-29 | 2018-05-08 | 株洲冶炼集团股份有限公司 | A kind of preparation method of tubulose ITO target |
| CN110498443A (en) * | 2019-08-23 | 2019-11-26 | 云南锡业集团（控股）有限责任公司研发中心 | A method of with ITO give up target recasting ITO powder |
| CN110498443B (en) * | 2019-08-23 | 2021-08-20 | 云南锡业集团（控股）有限责任公司研发中心 | Method for reproducing ITO powder by using ITO waste target |
| CN111620367A (en) * | 2020-06-08 | 2020-09-04 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO residual target/waste target |
| CN111620367B (en) * | 2020-06-08 | 2022-06-28 | 福建阿石创新材料股份有限公司 | Method for recovering ITO powder from ITO residual target/waste target |
| CN113387682A (en) * | 2021-05-24 | 2021-09-14 | 芜湖映日科技股份有限公司 | ITO target waste target recycling method |
| CN113999000A (en) * | 2021-10-21 | 2022-02-01 | 宁波江丰电子材料股份有限公司 | Method for recycling ITO waste target |
| 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 |
| CN114956162A (en) * | 2022-07-04 | 2022-08-30 | 广东先导稀材股份有限公司 | Method for recovering indium oxide waste |
| CN114956162B (en) * | 2022-07-04 | 2023-10-13 | 广东先导稀贵金属材料有限公司 | Recovery method of indium oxide waste |
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