CN103708819B - A kind of residual target of zinc oxide aluminum utilizing recovery prepares the method for the residual target powder of zinc oxide aluminum and the application of this powder - Google Patents
A kind of residual target of zinc oxide aluminum utilizing recovery prepares the method for the residual target powder of zinc oxide aluminum and the application of this powder Download PDFInfo
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Abstract
The present invention provides a kind of method that the residual target powder of zinc oxide aluminum prepared by residual target of zinc oxide aluminum utilizing recovery, comprises the following steps: residual for zinc oxide aluminum target clear water is cleaned, dried by (1); (2) by the residual target of zinc oxide aluminum after drying, put into the grinding in ball grinder of corundum, adopt 180 ~ 220 mesh standard sieves to sieve after grinding, obtain the residual target powder of zinc oxide aluminum. The invention solves the residual target of zinc oxide aluminum in prior art and directly abandon the wasting of resources and problem of environmental pollution that cause, and, obtained zinc oxide aluminum residual target powder can prepare new AZO target material again as the raw material of AZO target material.
Description
Technical field
The invention belongs to target recovery process, especially a kind of residual target of zinc oxide aluminum utilizing recovery prepares the method for the residual target powder of zinc oxide aluminum and the application of this powder.
Background technology
Along with the development of optoelectronics industry technology, zinc oxide aluminum transparent electroconductive film (abbreviation AZO transparent conductive film) oneself become the focus of Recent study and exploitation. AZO transparent conductive film is commonly used for the transparency electrode of various opto-electronic device (such as the transparency electrode (LED) of light emitting diode, flat faced display (FPD), copper and indium gallium stannum solaode (CIGS), silicon film solar batteries etc.). Owing to AZO transparent conductive film has the photoelectric properties of excellence, good stability, particularly in area of solar cell, AZO transparent conductive film is expected to substitute ito thin film, thus being paid close attention to widely.
Magnetron sputtering is the common film plating process being adapted to industrialized production most, its advantage is: the even film layer of deposition is fine and close, pin hole is few, purity is high, adhesive force is strong, deposition velocity is fast, rate of film build is high, and heating up of substrate is low, little to the damage of rete, it may be achieved large-area coating film. At present, commonly use elongated or square zinc oxide aluminum ceramic target and (be called for short AZO ceramic target, it is specially AZO ceramic flat surface target) carry out magnetron sputtering plating, AZO ceramic flat surface target is being carried out in magnetron sputtering process, the utilization rate of AZO ceramic target is generally relatively low (being usually no more than 30%), and most of (accounting for 70 ~ 80%) AZO ceramic target becomes residual target, owing to the recovery and utilization technology of residual target extremely lacks, all it is used as solid waste at present and abandons. Along with increasing sharply of optoelectronic film consumption, discarded AZO ceramic target (i.e. the residual target of AZO) quantity is also on the increase, and these residual targets directly abandon, and not only cause the wasting of resources, also environment is caused severe contamination owing to it is difficult to degraded.
Summary of the invention
It is desirable to provide a kind of method that the residual target powder of zinc oxide aluminum prepared by residual target of zinc oxide aluminum utilizing recovery, solve the residual target of zinc oxide aluminum in prior art and directly abandon the wasting of resources and problem of environmental pollution that cause, further, obtained zinc oxide aluminum residual target powder can prepare new AZO target material again as the raw material of AZO target material.
A kind of method that residual target of zinc oxide aluminum (being called for short the residual target of AZO) utilizing recovery prepares zinc oxide aluminum residual target powder (being called for short the residual target powder of AZO), comprises the following steps: residual for zinc oxide aluminum target (being called for short the residual target of AZO) is cleaned with clear water, dried by (1);(2) by the residual target of AZO after drying, put into the grinding in ball grinder of corundum, after grinding, adopt 180 ~ 220 mesh standard sieves to sieve, obtain zinc oxide aluminum residual target powder (being called for short the residual target powder of AZO).
The residual target of zinc oxide aluminum reclaimed according to above-mentioned utilization is prepared the residual target powder of zinc oxide aluminum that the method for zinc oxide aluminum residual target powder prepares and is belonged to protection scope of the present invention.
This AZO residual target powder can be used for preparing new AZO target material (AZO target), adopt concretely comprising the following steps of AZO residual target powder preparation AZO target: residual for zinc oxide aluminum target powder, alumina powder and Zinc oxide powder according to mass percent respectively 10 ~ 50%, 1.5 ~ 2.7%, 48.5 ~ 87.3% mix homogeneously, are made zinc oxide aluminum slip casting compound by (1); (2) with zinc oxide aluminum slip casting mixture quality for 100%, in zinc oxide aluminum slip casting compound, 20 ~ 35% water, 0.8 ~ 2% Radix Acaciae senegalis and 0.4 ~ 0.6% ammonium polyacrylate are added respectively; (3) according to existing target production technology, AZO target material (being called for short AZO target) is prepared.
The present invention is with the discarded residual target of AZO for raw material, and, density high for discarded AZO residual target purity greatly, do not absorb water, sinter, very stable feature, mechanical means is adopted to be ground by residual target, prepare the residual target powder of AZO, the residual target powder of this AZO can be directly incorporated in alumina powder and Zinc oxide powder as the raw material of AZO target, prepares the satisfactory new AZO target of performance.
The ball mill of the present invention adopts corundum material very crucial, and corundum ball mill is not only wear-resisting, and, without influence on the purity of target. Additionally, the fineness of grind of residual target is also critically important, the applicant is through test many times, finally just determining that the grind size of residual target controls when by 180 ~ 220 mesh sieve, the new target made just meets the basic demand to density of the use in magnetron sputtering coating AZO target, and (density of AZO target to reach 5.50g/cm3Above).
Detailed description of the invention
A kind of method that the residual target powder of AZO prepared by residual target of AZO utilizing recovery, comprises the following steps: residual for AZO target clear water is cleaned, dried by (1); (2) by the residual target of AZO after drying, put into the grinding in ball grinder of corundum, adopt 180 ~ 220 mesh standard sieves to sieve after grinding, obtain the residual target powder of AZO.
The residual target of zinc oxide aluminum reclaimed according to above-mentioned utilization is prepared the residual target powder of zinc oxide aluminum that the method for zinc oxide aluminum residual target powder prepares and is belonged to protection scope of the present invention.
This AZO residual target powder can be used for preparing new AZO target material (AZO target), adopt concretely comprising the following steps of AZO residual target powder preparation AZO target: residual for AZO target powder, alumina powder and Zinc oxide powder according to mass percent respectively 10 ~ 50%, 1.5 ~ 2.7%, 48.5 ~ 87.3% mix homogeneously, are made zinc oxide aluminum slip casting compound by (1); (2) with zinc oxide aluminum slip casting mixture quality for 100%, in zinc oxide aluminum slip casting compound, 20 ~ 35% water, 0.8 ~ 2% Radix Acaciae senegalis and 0.4 ~ 0.6% ammonium polyacrylate are added respectively; (3) according to existing target production technology, AZO target is prepared.
Embodiment 1 ~ embodiment 5 is applicant provided according to technical scheme. Now the parameter of embodiment 1 ~ 5 is listed below table 1:
Table 1
In step (3) in prior art and embodiment 1 ~ embodiment 5, the concrete steps of ceramic target production technology are: the slurry agitation for preparing in step (2) is uniform, carefully pour in the plaster model enclosed in advance, the demoulding after slurry curing; Being dried by base substrate after the demoulding, put in electrical kiln and burn till, firing temperature is 1400 ~ 1430 DEG C, is incubated 3 ~ 5 hours, cooling, prepares zinc oxide aluminum flat target.Measure the water absorption rate of AOZ target, density and linear shrinkage ratio, and observe uniform situation and the cracking situation of AZO target. Now the AOZ target obtained by embodiment 1 ~ 5 is listed below table 2 with the water absorption rate of AOZ target obtained by prior art, density, linear shrinkage ratio, the uniform situation of AZO target and five parametric results of cracking situation of AZO target.
Table 2
The discarded residual target of AZO adopted due to the present invention itself have purity height, density greatly, do not absorb water, sinter, very stable, therefore, the purity of the AOZ target that the AZO residual target powder preparation obtained by the present invention obtains is also higher. For AOZ target, density also being there are certain requirements, the basic demand of density is reach 5.50g/cm by use in magnetron sputtering coating AZO target3More than.
As can be seen from Table 2, the different from those of the AZO target that the AZO target that embodiments of the invention 2 ~ 4 prepare is obtained with prior art is little, and namely the AZO target obtained by embodiment 2 ~ 4 all meets the use in magnetron sputtering coating AZO target basic demand (5.50g/cm to density3Above). Further, AOZ target obtained by embodiment 2 ~ 4 uniformly, flawless. The AZO target that embodiment 1 prepares also complies with the basic demand to density of the use in magnetron sputtering coating AZO target, but, the consumption of AZO residual target powder is less, and namely the utilization rate of the residual target of AZO is low. Certainly, the mass percent of AZO residual target powder neither be The more the better, when the mass percent of the residual target powder of AZO is more than 50% (such as embodiment 5), obtained AZO ceramic target density diminishes, do not meet the basic demand of use in magnetron sputtering coating AZO target, further, the AZO target uniformity is poor, crackle occur. In general, the bulk density of AZO target is more big, and shrinkage factor is more big, and water absorption rate is more low simultaneously, and now, the sintering degree of AZO target is more good, and the quality of AZO target is more good.
The standard screen aperture of the present invention selects 180 ~ 220 orders very crucial, applicant finds in process of the test, when standard screen aperture > 220 order, owing to obtained AZO residual target powder particle is too thick, injection slurry easily produces precipitation, has a strong impact on the uniformity of AZO target; When standard screen aperture < 180 order, owing to obtained AZO residual target powder particle is too thin, the mobility of injection slurry can be affected again, the residual target powder of zinc oxide aluminum, alumina powder, Zinc oxide powder, Radix Acaciae senegalis and ammonium polyacrylate is made to be difficult to mix homogeneously, further, injection slurry poor fluidity also makes the final AZO target finished product prepared crackle easily occur. Additionally, the ball mill of the present invention adopts corundum material very crucial, owing to conventional mechanical crushing equipment is all that iron and steel is made, it is easy to ferrum element to enter in the process of lapping of residual target with the milling apparatus of these routines and affects the purity of target, and corundum ball mill is not only wear-resisting, and, the main component of corundum is Al2O3(raw material of AZO target), even if being so mixed into a little Al in process of lapping2O3, without the purity affecting target.
Certainly, the AZO residual target powder of the present invention can also be used for preparing Thermal camouflage coating or infrared/laser composite stealthy material etc., but, in the application of Thermal camouflage coating or infrared/laser composite stealthy material, the residual target powder of AZO is mainly as the source of Al element, and the demand of AZO residual target powder is relatively low.
The water absorption rate of the AZO target of the present invention and the computational methods of bulk density are:
Take out after the sample cooling sintered, with hairbrush, the removing of the powder on surface is clean, measure the dry weight of each sample, be designated as G1;Then sample is put in pottery water absorption rate tester, cover plastic closure, be evacuated down to-0.1MPa, keep 30min, soak 15min, take out sample, wipe surface attachment water with waterishlogged cloth, weigh the weight of each sample, be weight in wet base, be designated as G2; Being sandwiched by sample with tweezers is suspended in the copper wire basket filled in distilled water beaker, weighs the weight of sample, being suspension weight, being designated as G3.
Calculate the water absorption rate of sample as follows:
Formula (2-2)
In formula: Ma-water absorption rate, %;
The aerial quality of G1-sample, g;
The full aerial quality that absorbs water of G2-sample, g;
Calculate the bulk density of sample as follows:
Formula (2-3)
In formula: Da-bulk density, g/cm3;
The aerial quality of G1-sample, g;
The full aerial quality that absorbs water of G2-sample, g;
G3-sample is satisfied water suction quality in water, g;
The density of γ water-water, g/cm3.
The computational methods of the linear shrinkage ratio of the AZO target of the present invention are:
The sintering of target can represent with linear shrinkage ratio, and for there being the sample of certain standard shape, the shrinkage factor of sample is more big, and namely the quality of sample is more good. After having pressed slice, measure the diameter d1 of sample with slide gauge, after sintering, the diameter d2 of test specimens, calculate the linear shrinkage ratio of sample as follows:
Formula (2-1)
In formula: Wa-linear shrinkage ratio, %;
D1-green body diameter, cm;
D2-burns till specimen finish, cm.
The residual target of AZO of the present invention is the garbage after the magnetron sputtering that the applicant reclaims processes.
Claims (1)
1. the method for the residual target powder preparation AZO target material of zinc oxide aluminum that the residual target of zinc oxide aluminum utilizing recovery prepares, it is characterized in that, it concretely comprises the following steps: residual for zinc oxide aluminum target powder, alumina powder and Zinc oxide powder according to mass percent respectively 10～50%, 1.5～2.7%, 48.5～87.3% mix homogeneously, are made zinc oxide aluminum slip casting compound by (1); (2) with zinc oxide aluminum slip casting mixture quality for 100%, in zinc oxide aluminum slip casting compound, 20～35% water, 0.8～2% Radix Acaciae senegalis and 0.4～0.6% ammonium polyacrylate are added respectively; (3) according to existing target production technology, AZO target material is prepared;
Wherein, described zinc oxide aluminum residual target powder is prepared by the residual target of the zinc oxide aluminum reclaimed, and its preparation method comprises the following steps: residual for zinc oxide aluminum target clear water is cleaned, dried by (1); (2) by the residual target of zinc oxide aluminum after drying, put into the grinding in ball grinder of corundum, adopt 180～220 mesh standard sieves to sieve after grinding, obtain the residual target powder of zinc oxide aluminum.
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| CN107140972A (en) * | 2017-06-12 | 2017-09-08 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of preparation method of high density, low-resistivity AZO targets |
| CN111632730B (en) * | 2020-06-08 | 2022-06-28 | 福建阿石创新材料股份有限公司 | Extrusion grinding equipment and method for recycling 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 |
| CN112430082B (en) * | 2020-12-15 | 2022-10-04 | 湖南仁海科技材料发展有限公司 | Zinc oxide sagger and preparation method thereof |
| CN113174487A (en) * | 2021-04-13 | 2021-07-27 | 新疆众和股份有限公司 | Recovery method of aluminum residual target for liquid crystal panel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102942363A (en) * | 2012-11-22 | 2013-02-27 | 国家钽铌特种金属材料工程技术研究中心 | Method for preparing AZO target by powdery slurry pouring |
| CN103447535A (en) * | 2012-05-30 | 2013-12-18 | 宁波江丰电子材料有限公司 | Target manufacturing method |
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| CN103447535A (en) * | 2012-05-30 | 2013-12-18 | 宁波江丰电子材料有限公司 | Target manufacturing method |
| CN102942363A (en) * | 2012-11-22 | 2013-02-27 | 国家钽铌特种金属材料工程技术研究中心 | Method for preparing AZO target by powdery slurry pouring |
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