CN101186494A - Technique for preparing Li doping ZnO ceramic target material - Google Patents
Technique for preparing Li doping ZnO ceramic target material Download PDFInfo
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- CN101186494A CN101186494A CNA2007101789575A CN200710178957A CN101186494A CN 101186494 A CN101186494 A CN 101186494A CN A2007101789575 A CNA2007101789575 A CN A2007101789575A CN 200710178957 A CN200710178957 A CN 200710178957A CN 101186494 A CN101186494 A CN 101186494A
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Abstract
The invention relates to a preparation technique of ceramic target with Li doped with ZnO, which pertains to the preparation technical field of ceramic target material. The process is that: zinc nitrate, lithium nitrate, urea and glycine are fully mixed then put into a beaker; the obtained material is added with deionized water, and is stirred, so as to lead the material to be fully melt; the melted solution is heated and sent into an evaporator, leading combustion reaction to be occurred and synthesizing Li doped with ZnO powder body; the powder body is grinded, then is sintered in a discharging plasma sintering furnace; the obtained product is the Li doped with ZnO ceramic target. The invention has the advantages of raw material being easy to be obtained, short process period, high purity and being evenly doped; in addition, acceptor doping is realized for the element Li used for substituting for Zn in lattice ZnO, and the using of the ceramic target is in favor of the preparation of Li doped with a P-typed ZnO film.
Description
Technical field
The invention belongs to the ceramic target preparing technical field, a kind of Li doping ZnO ceramic target material preparation technology particularly is provided, it is that the preparation of p type ZnO film lays the foundation that this method prepares target.
Background technology
ZnO is a kind of novel II-VII family wide bandgap semiconductor compound, has high exciton bind energy, and epitaxial growth temperature is low, and nontoxicity, and advantage such as near ultraviolet Laser emission are expected to develop multiple luminescent devices such as near ultraviolet photodiode, laser apparatus.ZnO film is originally as polar semiconductor, and unadulterated ZnO is n type electricity to be led, thereby ZnO key in application aspect photoelectricity is to realize the p type ZnO film of stability and high efficiency.At present, the method for preparing p type ZnO film mainly is that doping I family (Li, Na, K) substitutes the position of Zn among the ZnO and V group element (N, P, As) and replaces among the ZnO 0 position to realize acceptor doping, it is calculated that as can be known, V group element doping acceptor level in ZnO is darker, be difficult for realizing the p type, the acceptor level of Li element in ZnO is more shallow comparatively speaking, is that ZnO realizes one of adulterated element at infinity of p type.
Magnetically controlled sputter method is that the preparation ZnO film is the most frequently used, easy, economic method, the ion that this method utilizes ion source (argon gas) to produce, in a vacuum through quickening the bombardment solid surface, ion and solid surface atom generation exchange of kinetic energy, make the atom of solid surface leave solid and be deposited on substrate surface, the solid that is bombarded is with the starting material of sputtering method deposit film, is called sputtering target material.Adopt the sedimentary film density of ZnO ceramic target height, and the tack between the base material is good, and can prepares high quality ZnO film.Preparation Li doping ZnO ceramic target adopts mechanical mixing usually at present, is exactly directly zinc oxide and Quilonum Retard directly to be mixed, and adopts normal pressure or hot pressed method Li doping ZnO ceramic target material.This method prepares low, inhomogeneous, the easy reunion of mixing of target purity, is difficult for forming acceptor doping.Realize the even doping ZnO target of Li for addressing the above problem, and then realize that the p type of ZnO film mixes.The present invention adopts chemical synthesis process that ZnO is carried out the doping of Li element, and Li mixes fully and enters the ZnO powder, and uniform doping adopts the method for Fast Sintering to realize the Li doping ZnO ceramic target material then, adopts this kind target deposition ZnO film to realize that easily the p type mixes.
Summary of the invention
The object of the invention provides a kind of preparation technology of Li doping ZnO target, this target is of value to the formation of p type ZnO film, realized that raw material cheaply is easy to get, process cycle is short, the target purity height of gained, uniform doping is incorporated in the ZnO lattice and the position of alternative Zn at Li, realize the acceptor doping of ZnO, utilize this ceramic target to be of value to the preparation of Li doped p type ZnO thin film.
Concrete technology of the present invention is as follows:
1. adopt the synthetic adulterated ZnO powder of Li of combustion method, with the weighing in molar ratio of zinc nitrate, lithium nitrate, urea and glycine, this medicine mol ratio should meet the following conditions, and the mol ratio of lithium nitrate and zinc nitrate is 0.01～0.05, (NO in zinc nitrate and the lithium nitrate
3) (NH in summation and urea and the glycine
2) mol ratio of summation is 0.6～0.8, the mol ratio of urea and glycine is 2～5.To put into beaker behind the load weighted medicine uniform mixing, the injection deionized water also stirs, be the transparence sediment-free until solution, solution is poured in the furnace pot, be placed on the muffle furnace and heat, solution is gel, acutely putting should, until burning, the synthetic adulterated ZnO powder of Li is collected in the powder and the vacuum bag of packing at last.
2. the Li doping ZnO powder that above-mentioned burning synthesis method is prepared is placed in the corundum alms bowl and grinds 30～50min, pack into then in the discharge plasma sintering stove, be pre-stressed to 20～40MPa earlier, when vacuum tightness reaches 6～9Pa, begin to heat up, temperature rise rate is 90～100 ℃/min, when temperature is 800～900 ℃, adds axle pressure 30～40MPa, when temperature is 950～1050 ℃, insulation 2～5min, insulation finishes back release rapidly, naturally cools to room temperature and takes out.In sintering process, the time of pressurization is unsuitable long, and holding stage finishes back release rapidly.
Adopt burning synthesis method to prepare the adulterated ZnO powder of Li in the experimentation, it is cheap that this method has a raw material, technology is simple, experimental period is short, reaction system is reduced to room temperature suddenly from high temperature simultaneously, and higher thermograde makes the powder product be in metastable state, has very high defect density, therefore characteristics such as the active height of powder adopt low temperature combustion synthesis method to prepare the nanocrystalline doping that benefits the Li element more of ZnO.In sintering process, adopt discharge plasma sintering, this method homogeneous heating, heat-up rate is fast, sintering temperature is low, and sintering time is short, the production efficiency height, product is organized tiny even, can keep raw-material state of nature, can obtain the material of high-compactness, at high temperature run off so adopt this method can reduce doped element, guarantee original state of material, obtain highdensity ceramic target.
Description of drawings
Fig. 1 is the photomacrograph of Li doping ZnO target.From photo as can be seen, the target of this invention preparation does not have macroscopical slight crack, intactly ceramic target.
Fig. 2 is the stereoscan photograph of Li doping ZnO target.As seen from the figure, this target density is very high, does not have the cavity.
Fig. 3 is the XRD figure spectrum of Li doping ZnO target.This powder shows as single-phase ZnO, does not have other and exists mutually, illustrates that Li has mixed to enter among the ZnO.
Fig. 4 is the contrast of the diffraction angle of adulterated ZnO of Li and pure ZnO.The 2 θ angles of the ZnO of Li doped element increase with respect to unadulterated ZnO, and the ZnO lattice shrinks.Because the ionic radius of Li element is less than the Zn element, with this Li element substitution Zn element in the ZnO lattice, lattice should shrink, yet when Li is in the interstitial void position, lattice is expansion, so Fig. 4 illustrates that the Li element is the displacement doping rather than is in interstitial site in the ZnO lattice.
Embodiment
With zinc nitrate, lithium nitrate, urea and glycine 25: 1: 30 in molar ratio: put into beaker behind 10 uniform mixing, the injection deionized water also stirs, be the transparence sediment-free until solution, solution is poured in the furnace pot, be placed on the muffle furnace and heat, solution is gel, and acutely putting should, until burning, generate Li doping ZnO powder.Li doping ZnO powder is placed in the corundum alms bowl grinds 30min, pack into then in the discharge plasma sintering stove, be pre-stressed to 30MPa earlier, when vacuum tightness reaches 7Pa, begin to heat up, temperature rise rate is 100 ℃/min, when temperature is 900 ℃, adds axle pressure 30MPa, when temperature is 1000 ℃, insulation 3min, insulation finishes back release rapidly, naturally cools to room temperature and takes out.
Claims (3)
1. Li doping ZnO ceramic target material preparation technology is characterized in that:
A. adopt combustion method to synthesize the adulterated ZnO powder of Li, to put into beaker behind zinc nitrate, lithium nitrate, urea and the glycine uniform mixing, the injection deionized water also stirs, and is the transparence sediment-free until solution, and solution is poured in the furnace pot, be placed on the muffle furnace and heat, solution is gel, acutely puts to answer, until burning, the synthetic adulterated ZnO powder of Li is collected in the powder and the vacuum bag of packing at last;
B. with the Li doping ZnO powder of above-mentioned burning synthesis method preparation, in the corundum alms bowl, grind 30～50min, in the discharge plasma sintering stove of packing into then, be pre-stressed to 20～40MPa earlier, when vacuum tightness reaches 6～9Pa, begin to heat up, temperature rise rate is 90～100 ℃/min, when temperature is 800～900 ℃, add axle pressure 30～40MPa, when temperature is 950～1050 ℃, insulation 2～5min, insulation finishes back release rapidly, naturally cools to room temperature and takes out.
2. in accordance with the method for claim 1, it is characterized in that: the mol ratio of lithium nitrate and zinc nitrate is 0.01～0.05, and the mol ratio of urea and glycine is 2～5, NO in zinc nitrate and the lithium nitrate
3With NH in urea and the glycine
2Mol ratio be 0.6～0.8
3. in accordance with the method for claim 1, it is characterized in that: at electric plasma agglomeration stove sintering, sintering temperature is 950～1050, the axle pressure 30～40MPa during sintering, insulation 2～5min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381228B (en) * | 2008-10-08 | 2011-09-14 | 吉林大学 | Ga-doped zinc oxide transparent polycrystal ceramics preparation method |
| CN102324509A (en) * | 2011-09-20 | 2012-01-18 | 北京工业大学 | Preparation method of metastable phase LiC6 alloy |
| CN101885609B (en) * | 2009-05-14 | 2012-09-05 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-based ceramic sputtering target material at intermediate temperature |
| TWI405609B (en) * | 2009-08-12 | 2013-08-21 | Iner Aec Executive Yuan | A chemical reactor with powder collection for preparation of fine (nano-scale/submicron-scale) ceramic powders via glycine-nitrate combustion process |
| CN104078531A (en) * | 2014-06-30 | 2014-10-01 | 景德镇陶瓷学院 | Method for manufacturing ZnO:Li transparent conducting thin film with wide spectral domain light transmission characteristic and directly-growing meteor crater fabric surface |
| CN113230453A (en) * | 2021-05-06 | 2021-08-10 | 长兴盛隆科技有限公司 | Preparation method of medical magnesium alloy corrosion-resistant coating |
| CN116120052A (en) * | 2023-02-21 | 2023-05-16 | 哈尔滨理工大学 | Zinc oxide-based giant dielectric ceramic material and preparation method and application thereof |
-
2007
- 2007-12-07 CN CN2007101789575A patent/CN101186494B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381228B (en) * | 2008-10-08 | 2011-09-14 | 吉林大学 | Ga-doped zinc oxide transparent polycrystal ceramics preparation method |
| CN101885609B (en) * | 2009-05-14 | 2012-09-05 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-based ceramic sputtering target material at intermediate temperature |
| TWI405609B (en) * | 2009-08-12 | 2013-08-21 | Iner Aec Executive Yuan | A chemical reactor with powder collection for preparation of fine (nano-scale/submicron-scale) ceramic powders via glycine-nitrate combustion process |
| CN102324509A (en) * | 2011-09-20 | 2012-01-18 | 北京工业大学 | Preparation method of metastable phase LiC6 alloy |
| CN102324509B (en) * | 2011-09-20 | 2013-07-24 | 北京工业大学 | Preparation method of metastable phase LiC6 alloy |
| CN104078531A (en) * | 2014-06-30 | 2014-10-01 | 景德镇陶瓷学院 | Method for manufacturing ZnO:Li transparent conducting thin film with wide spectral domain light transmission characteristic and directly-growing meteor crater fabric surface |
| CN113230453A (en) * | 2021-05-06 | 2021-08-10 | 长兴盛隆科技有限公司 | Preparation method of medical magnesium alloy corrosion-resistant coating |
| CN116120052A (en) * | 2023-02-21 | 2023-05-16 | 哈尔滨理工大学 | Zinc oxide-based giant dielectric ceramic material and preparation method and application thereof |
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| CN101186494B (en) | 2010-08-11 |
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