CN103435339A - Aluminum doped zinc oxide target and preparation method thereof - Google Patents
Aluminum doped zinc oxide target and preparation method thereof Download PDFInfo
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- CN103435339A CN103435339A CN2013103313889A CN201310331388A CN103435339A CN 103435339 A CN103435339 A CN 103435339A CN 2013103313889 A CN2013103313889 A CN 2013103313889A CN 201310331388 A CN201310331388 A CN 201310331388A CN 103435339 A CN103435339 A CN 103435339A
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Abstract
The invention provides an aluminum doped zinc oxide target and a preparation method thereof. The preparation method comprises the steps of dissolving aluminum salt and an adhesive agent in a solvent, adding zinc salt powder, stirring, drying, obtaining mixed powder, performing compression molding and sintering on the mixed powder sequentially, and obtaining the aluminum doped zinc oxide target. The preparation method is simple, low in production cost and suitable for industrial development, and the prepared aluminum doped zinc oxide target is higher in quality.
Description
Technical field
The present invention relates to photoelectric functional material, relate in particular to a kind of aluminium-doped zinc oxide target and preparation method thereof.
Background technology
Along with the fast development in the fields such as semi-conductor, computer, sun power, transparent conductive oxide (TCO) film, owing to having good electroconductibility and high-transmission rate concurrently, can be widely used in various indicating meters and various optoelectronic device.Now industrial most widely used transparent conductive film is tin-doped indium oxide (ITO, Tin doped Indium Oxide) film, but that it has is expensive, and under high temperature, transmitance reduces rapidly, and the shortcoming such as easily is reduced in hydrogen plasma; And ZnO is cheap, abundant raw material, more stable than ITO in hydrogen ion atmosphere, can not only make good semi-conductor and piezoelectric membrane, also can make good transparent conductive film by doping.Wherein, aluminium-doped zinc oxide (AZO, Al-doped in Zinc Oxide) target as sputter film is to be known as at present one of the most promising thin-film material.Therefore the quality good or not of AZO target is directly determining the quality of film.
At first the preparation method of AZO target is mainly zinc salt and aluminium salt is mixed at present, then at high temperature sintering obtains the AZO target, wherein the blending means of zinc salt and aluminium salt mainly contains two kinds, a kind of method is: zinc salt is directly mixed with solid form with aluminium salt, grind even (being the direct blending means of raw material solid), for example by the mode of ball milling, zinc salt and aluminium salt powder are mixed, but because the weight of aluminium salt is less, be difficult to guarantee to reach between aluminium salt and zinc salt the even mixing of atom magnitude by ball milling method, cause the inhomogeneous of target composition, and then have influence on the homogeneity of sputtered film photoelectric properties, secondly, in mechanical milling process between abrading-ball and between abrading-ball and tank body contact and wear and tear can be in system a large amount of impurity of introducing, cause the reduction of target purity.
Another kind method is: after zinc salt and aluminium salt are dissolved, then the method such as precipitated and zinc salt is mixed to (being material dissolution-precipitation blending means) with aluminium salt.As disclosed a kind of preparation method of doped zinc oxide nano powder in the publication number patent application that is CN101844917A, at first zinc salt and aluminium salt are dissolved in deionized water and form salts solution, then in salts solution, add precipitation agent to obtain coprecipitated product, finally coprecipitated product is carried out to sintering, obtain the AZO target.This method complexity, length consuming time and cost are high.
Summary of the invention
For addressing the above problem, the invention provides a kind of preparation method of aluminium-doped zinc oxide.Preparation method of the present invention is simple, cost is low, and the AZO target quality prepared is higher, and while having solved AZO preparation of target materials in the prior art, raw material mixes the problem of inhomogeneous and preparation method's complexity.
A kind of preparation method of aluminium-doped zinc oxide target comprises the following steps:
Aluminium salt and binding agent are dissolved in solvent and make mixing solutions, add zinc salt in described mixing solutions, stir, obtain mixed powder after oven dry, described mixed powder compression moulding is obtained to base substrate, described base substrate is placed in to 1200 ℃～1500 ℃ sintering 1～6 hour subsequently under air atmosphere, obtains described aluminium-doped zinc oxide target; Described solvent is at least one in water and organic solvent, and the weight of described solvent is 10～50 times of zinc salt weight; The weight of the weight of described aluminium salt, the weight of zinc salt and binding agent accounts for respectively 1%～8%, 90%～98.8% and 0.2%～2% of aluminium salt, zinc salt and weight of binder summation.
The present invention is in preparation AZO target, at first aluminium salt and binding agent are dissolved, then add zinc salt, again through mixed with moderate agitation, realize mixing of aluminium salt and zinc salt, after calcining, aluminum ion more easily enters in the lattice of zinc salt and replaces the zine ion in the zinc salt lattice again, obtains the uniform AZO target of composition.
Preferably, described aluminium salt is aluminum oxide, aluminum nitrate or aluminium hydroxide.
More preferably, described aluminium salt is aluminum nitrate.
Preferably, described zinc salt is zinc oxide, zinc nitrate or zinc acetate.
More preferably, described zinc salt is zinc oxide.
Preferably, described binding agent is polyvinyl alcohol, polyethylene glycol, polymethyl acid alcohol or carboxymethyl cellulose.
More preferably, described binding agent is carboxymethyl cellulose.
Preferably, described organic solvent is dehydrated alcohol.
Preferably, described compression moulding is cold isostatic compaction, and the pressure of described cold isostatic compaction is 5Mpa～20Mpa.
The present invention also provides a kind of AZO target, and described AZO target is that above-mentioned preparation method makes.
Compared with prior art, the present invention has following outstanding advantages:
Preparation method of the present invention first is dissolved in aluminium salt and binding agent in solvent, add again zinc salt, zinc salt and aluminium salt mix, overcome the raw material solid direct method and mixed inhomogeneous shortcoming, also overcome the shortcoming that material dissolution-precipitation blending means preparation method is complicated, cost is high, preparation method of the present invention is applicable to industrialization production; The AZO target composition that preparation method of the present invention makes is even, and impurity is few, and the target quality is good.
Embodiment
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Embodiment 1
A kind of preparation method of AZO target, concrete steps are as follows:
Aluminum oxide and carboxymethyl cellulose are dissolved in dehydrated alcohol, obtain mixing solutions after mixing, add zinc oxide again in mixing solutions, stir, obtain mixed powder after oven dry, mixed powder cold isostatic compaction under 5Mpa pressure is obtained to base substrate, then by base substrate 1200 ℃ of sintering 6 hours under air atmosphere, obtain the AZO target, wherein, the weight of dehydrated alcohol is 20 times of zinc salt weight, the weight of aluminum oxide, the weight of zinc oxide and the weight of carboxymethyl cellulose account for respectively aluminum oxide, 1% of zinc oxide and carboxymethyl cellulose weight summation, 98.8% and 0.2%.
Comparative Examples 1-1
After aluminum oxide, zinc oxide and carboxymethyl cellulose powder are directly mixed, with ball mill grinding 3 hours, cross 300 mesh sieves after grinding and obtain mixed powder, mixed powder is carried out carrying out sintering after cold isostatic compaction again, obtain the AZO target, wherein the aluminum oxide of the present embodiment, zinc oxide and carboxymethyl cellulose weight, cold isostatic compaction condition and sintering condition are with the condition of embodiment 1.
Comparative Examples 1-2
Aluminum oxide, zinc oxide and carboxymethyl cellulose are dissolved in respectively in dehydrated alcohol and obtain alumina solution, burnett's solution and cmc soln, then alumina solution, burnett's solution and cmc soln are mixed to get to mixing solutions, in mixing solutions, add ammoniacal liquor to be precipitated, filter to obtain filter residue; Carry out cold isostatic compaction after filter residue is dried and obtain base substrate, sintered body, obtain the AZO target, the aluminum oxide of the present embodiment, zinc oxide and carboxymethyl cellulose weight, cold isostatic compaction condition and sintering condition are with the condition of embodiment 1, and the molar weight of ammoniacal liquor is identical with mole total amount of aluminum oxide and zinc oxide.
Embodiment 2
A kind of preparation method of AZO target, concrete steps are as follows:
Aluminum nitrate and polyvinyl alcohol are dissolved in to dehydrated alcohol and water be take volume ratio in the mixed solvent that 1:1 forms, obtain mixing solutions after mixing, add zinc nitrate again in mixing solutions, stir, obtain mixed powder after oven dry, mixed powder cold isostatic compaction under 20Mpa pressure is obtained to base substrate, then by base substrate 1500 ℃ of sintering 1 hour under air atmosphere, obtain the AZO target, wherein, the weight of dehydrated alcohol and water is 10 times of zinc salt weight, the weight of aluminum nitrate, the weight of zinc nitrate and the weight of polyvinyl alcohol account for respectively aluminum nitrate, 8% of zinc nitrate and polyvinyl alcohol weight summation, 90% and 2%.
Comparative Examples 2-1
After aluminum nitrate, zinc nitrate and polyvinyl alcohol are directly mixed, with ball mill grinding 1 hour, cross 150 mesh sieves after grinding and obtain mixed powder, mixed powder is carried out carrying out sintering after cold isostatic compaction again, obtain the AZO target, wherein the aluminum nitrate of the present embodiment, zinc nitrate and polyvinyl alcohol weight, cold isostatic compaction condition and sintering condition are with the condition of embodiment 2.
Comparative Examples 2-2
Aluminum nitrate, zinc nitrate and polyvinyl alcohol are dissolved in respectively to dehydrated alcohol and water take volume ratio obtain aluminum nitrate solution, zinc nitrate solution and polyvinyl alcohol solution in the mixed solvent that 1:1 forms, aluminum nitrate solution, zinc nitrate solution and polyvinyl alcohol solution are mixed to get to mixing solutions, in mixing solutions, add ammoniacal liquor to be precipitated, to filter and to obtain filter residue; Carry out cold isostatic compaction after filter residue is dried and obtain base substrate, sintered body, obtain the AZO target, the aluminum nitrate of the present embodiment, zinc nitrate and polyvinyl alcohol weight, cold isostatic compaction condition and sintering condition are with the condition of embodiment 2, and the molar weight of ammoniacal liquor is identical with mole total amount of aluminum nitrate and zinc nitrate.
Embodiment 3
A kind of preparation method of AZO target, concrete steps are as follows:
Aluminium hydroxide and polyethylene glycol is soluble in water, obtain mixing solutions after mixing, add zinc acetate again in mixing solutions, stir, obtain mixed powder after oven dry, mixed powder cold isostatic compaction under 10Mpa pressure is obtained to base substrate, then by base substrate 1200 ℃ of sintering 4 hours under air atmosphere, obtain the AZO target, wherein, the weight of water is 50 times of zinc salt weight, and the weight of the weight of aluminium hydroxide, the weight of zinc acetate and polyethylene glycol accounts for respectively 5%, 94% and 1% of the weight of aluminium hydroxide, zinc acetate and polyethylene glycol summation.
Comparative Examples 3-1
After aluminium hydroxide, zinc acetate and polyethylene glycol powder are directly mixed, with ball mill grinding 2 hours, cross 200 mesh sieves after grinding and obtain mixed powder, mixed powder is carried out carrying out sintering after cold isostatic compaction again, obtain the AZO target, wherein the aluminium hydroxide of the present embodiment, zinc acetate and polyethylene glycol weight, cold isostatic compaction condition and sintering condition are with the condition of embodiment 3.
Comparative Examples 3-2
By aluminium hydroxide, zinc acetate and polyethylene glycol powder aluminium hydroxide solution, zinc acetate solution and the polyethylene glycol powder solution of obtaining soluble in water respectively, aluminium hydroxide solution, zinc acetate solution and polyethylene glycol powder solution are mixed to get to mixing solutions, in mixing solutions, add ammoniacal liquor to be precipitated, to filter and to obtain filter residue; Carry out cold isostatic compaction after filter residue is dried and obtain base substrate, sintered body, obtain the AZO target, the aluminium hydroxide of the present embodiment, zinc acetate and polyethylene glycol weight, cold isostatic compaction condition and sintering condition are with the condition of embodiment 3, and the molar weight of ammoniacal liquor is identical with mole total amount of aluminium hydroxide and zinc acetate.
The experimental result that table 1 is embodiment, outward appearance, color and luster, relative density and the yield rate of having observed the AZO target, concrete effect is in Table 1.
The experimental result of table 1 embodiment
As can be seen from Table 1, AZO target outward appearance, color and luster prepared by the present invention are good, the finished product rate of relative density more than 99% is more than 90%, and the AZO target outward appearance, the color and luster that adopt the direct blending means of raw material solid to prepare are poor, the above finished product rate of relative density 99% 75% left and right.Although the quality of AZO target prepared by the present invention slightly is inferior to the quality by material dissolution-precipitation blending means, but preparation method of the present invention is simpler, and cost is lower, therefore, advantage of the present invention is more obvious, is a kind of novel AZO target production technology.
The result concrete analysis of table 1 is as follows: the degree of mixedness of aluminium salt and zinc salt has determined the quality of target, and the degree of mixedness of aluminium salt and zinc salt is better, and the effect that aluminum ion enters lattice replacement zine ion is better, and the target quality is better; If it is more inhomogeneous that zinc salt and aluminium salt mix, the target quality is poorer, shows that the target appearance luster is bad, target easily splits (crackle is arranged), decrease in yield etc.The present invention is in preparation AZO target, at first aluminium salt and binding agent are dissolved, then the zinc salt that adds the weight maximum, again through mixed with moderate agitation, can realize mixing of aluminium salt and zinc salt, after calcining, aluminum ion more easily enters in the lattice of zinc salt and replaces the zine ion in the zinc salt lattice again, obtains the uniform AZO target of composition.
Preparation method of the present invention compares with the direct blending means of raw material solid, and aluminium salt of the present invention and zinc salt do not need ground and mixed, and the mixed effect of zinc salt and aluminium salt is better, and the impurity that can not induce one in preparation process, the target better quality made.
Preparation method of the present invention compares with material dissolution-precipitation blending means, the zinc salt of consumption maximum of the present invention does not need first to be dissolved in solvent and mixes with aluminium salt, do not need to add precipitation agent yet, preparation method of the present invention is simpler, and cost is lower, and the target quality for preparing of the present invention approaches the target quality prepared of material dissolution-precipitation blending means.
To sum up, preparation method of the present invention has overcome the raw material solid direct method and has mixed inhomogeneous shortcoming, has also overcome the shortcoming that material dissolution-precipitation blending means preparation method is complicated, cost is high, and preparation method of the present invention is more suitable for industrialization production; The AZO target composition that preparation method of the present invention makes is even, and impurity is few, and the target quality is good, and the market competitiveness is larger.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Claims (7)
1. the preparation method of an aluminium-doped zinc oxide target, is characterized in that, comprises the following steps:
Aluminium salt and binding agent are dissolved in solvent and make mixing solutions, add zinc salt in described mixing solutions, stir, obtain mixed powder after oven dry, described mixed powder compression moulding is obtained to base substrate, described base substrate is placed in to 1200 ℃～1500 ℃ sintering 1～6 hour subsequently under air atmosphere, obtains described aluminium-doped zinc oxide target; Described solvent is at least one in water and organic solvent, and the weight of described solvent is 10～50 times of zinc salt weight; The weight of the weight of described aluminium salt, the weight of zinc salt and binding agent accounts for respectively 1%～8%, 90%～98.8% and 0.2%～2% of aluminium salt, zinc salt and weight of binder summation.
2. the preparation method of aluminium-doped zinc oxide target as described as right 1, is characterized in that, described aluminium salt is aluminum oxide, aluminum nitrate or aluminium hydroxide.
3. the preparation method of aluminium-doped zinc oxide target as described as right 1, is characterized in that, described zinc salt is zinc oxide, zinc nitrate or zinc acetate.
4. the preparation method of aluminium-doped zinc oxide target as described as right 1, is characterized in that, described binding agent is polyvinyl alcohol, polyethylene glycol, polymethyl acid alcohol or carboxymethyl cellulose.
5. the preparation method of aluminium-doped zinc oxide target as described as right 1, is characterized in that, described organic solvent is dehydrated alcohol.
6. the preparation method of aluminium-doped zinc oxide target as described as right 1, is characterized in that, described compression moulding is cold isostatic compaction, and the pressure of described cold isostatic compaction is 5Mpa～20Mpa.
7. an aluminium-doped zinc oxide target, is characterized in that, described aluminium-doped zinc oxide target is that the described preparation method of claim 1～6 any one makes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264118A (en) * | 2014-10-13 | 2015-01-07 | 福州大学 | CdS (cadmium sulfide) ceramic target material and preparation method thereof |
| CN107365967A (en) * | 2017-07-06 | 2017-11-21 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of preparation method of AZO sputtering targets |
| CN112218840A (en) * | 2018-06-06 | 2021-01-12 | 杰富意矿物股份有限公司 | Zinc oxide powder for use in zinc oxide sintered body, and processes for producing these |
| CN113604778A (en) * | 2021-07-05 | 2021-11-05 | 广州市尤特新材料有限公司 | AZO target material applied to solar cell and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575207A (en) * | 2009-06-10 | 2009-11-11 | 中国南玻集团股份有限公司 | Ge-doped AZO target and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575207A (en) * | 2009-06-10 | 2009-11-11 | 中国南玻集团股份有限公司 | Ge-doped AZO target and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264118A (en) * | 2014-10-13 | 2015-01-07 | 福州大学 | CdS (cadmium sulfide) ceramic target material and preparation method thereof |
| CN104264118B (en) * | 2014-10-13 | 2017-01-18 | 福州大学 | CdS (cadmium sulfide) ceramic target material and preparation method thereof |
| CN107365967A (en) * | 2017-07-06 | 2017-11-21 | 安徽拓吉泰新型陶瓷科技有限公司 | A kind of preparation method of AZO sputtering targets |
| CN112218840A (en) * | 2018-06-06 | 2021-01-12 | 杰富意矿物股份有限公司 | Zinc oxide powder for use in zinc oxide sintered body, and processes for producing these |
| CN113604778A (en) * | 2021-07-05 | 2021-11-05 | 广州市尤特新材料有限公司 | AZO target material applied to solar cell and preparation method thereof |
| CN113604778B (en) * | 2021-07-05 | 2023-12-01 | 广州市尤特新材料有限公司 | AZO target material applied to solar cell and preparation method thereof |
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