CN111574217A - Rare earth doped indium gallium zinc oxide powder and preparation method and application thereof - Google Patents
Rare earth doped indium gallium zinc oxide powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of rare earth doped indium gallium zinc oxide powder, which comprises the following steps: sequentially adding water, a dispersing agent, gallium oxide powder and rare earth oxide powder into a first mixing barrel for pre-dispersion, and grinding the pre-dispersed solution to obtain first mixed slurry; sequentially adding water, a dispersing agent and zinc oxide powder into a second mixing barrel for pre-dispersion, and adding the pre-dispersed solution into the first mixed slurry for grinding to obtain second mixed slurry; sequentially adding water, a dispersing agent and indium oxide powder into a third mixing barrel for pre-dispersion, and adding the pre-dispersed solution into the second mixed slurry for grinding to obtain third mixed slurry; adding an adhesive into the third mixed slurry, and grinding to obtain a fourth mixed slurry; and granulating, mixing and screening the fourth mixed slurry to finally obtain the rare earth doped indium gallium zinc oxide powder. The method can solve the problem of non-uniform components caused by doping the large-particle-size rare earth elements into the IGZO powder.
Description
Technical Field
The invention relates to the field of preparation of indium gallium zinc oxide powder, in particular to rare earth doped indium gallium zinc oxide powder and a preparation method and application thereof.
Background
In the current Flat Panel Display (FPD) market, Thin Film Transistor (TFT) displays dominate, with annual worldwide production values of several billion dollars. In the preparation of a Thin Film Transistor (TFT) display, the core technology is the manufacture of a Thin Film Transistor (TFT) of a driving mechanism, and one of the keys influencing the performance of the Thin Film Transistor (TFT) is a semiconductor channel layer material which generates a switching action under an electric field. Such semiconductor channel materials can be classified into the following three categories: amorphous silicon (a-Si), polycrystalline silicon (poly-Si), and an oxide semiconductor (represented by indium gallium zinc oxide, abbreviated as IGZO). Amorphous silicon Thin Film Transistor (TFT) displays are part of the conventional TFT display technology, while IGZO TFTs are part of the new generation display technology. Compared with amorphous silicon materials, the oxide semiconductor channel materials have high carrier mobility. The electron mobility of crystalline IGZO is 20 to 50 times that of amorphous silicon. The IGZO TFT has the following advantages over the conventional amorphous silicon TFT: (1) the resolution is about twice that of the latter; (2) the power consumption of the display panel is saved by about 80-90%; (3) high precision touch performance (higher signal-to-noise ratio); (4) the screen image can be kept after the power supply is turned off; in view of this, the IGZO-TFT channel layer material has great application potential in Liquid Crystal Displays (LCDs) and Organic Light Emitting Displays (OLEDs).
The oxide semiconductor thin film has excellent characteristics of high electron mobility, high light transmittance and low growth temperature, is expected to replace the traditional silicon-based thin film transistor, and becomes a next generation display technology driving device. Among the known oxide semiconductor thin films, the amorphous IGZO thin film (a-IGZO) is again one of the most excellent materials. Nowadays, a-IGZO is mainly prepared by magnetron sputtering, the method needs to use high-performance IGZO target materials, and the properties of IGZO target materials such as relative density, microstructure and the like have close influence on the performance of sputtered films. Therefore, to obtain a high-performance a-IGZO, it is first necessary to obtain a high-quality IGZO target.
The indium gallium zinc oxide powder is the key for preparing excellent IGZO target material, if the indium gallium zinc oxide powder is unevenly distributed or the powder particles are large, the target material obtained by sintering has low density and may be accompanied by impurity phase (ZnGa)2O4) And the generation of the metal oxide leads to a plurality of holes and projections on the surface of the target material, and the quality of the coating film is seriously influenced.
Currently, there are two main methods for preparing IGZO powder and its target material. Firstly, the In is directly prepared by adopting a solid state reaction method2O3ZnO and Ga2O3Three kinds of powder (with micron grade average grain diameter) are directly mechanically ground, and are added with the steps of granulation grinding, pressure forming, high-temperature sintering (1200-2O4Spinel (spinel) precipitates are easily generated, which may increase the number of protrusions in the target, and further affect the stability of the coating process and the quality of the RF/DC sputtered IGZO thin film. In addition, the mixed particles are also large (0.6-1.0 μm), which is likely to cause unevenness when pressing the target, and reduce the target density, thereby affecting the sputtering effect. Although the solid-state reaction method can prepare IGZO palladium material In large quantity, the In is physically prepared2O3ZnO and Ga2O3The powder is directly and mechanically ground to dope proper Ga or In into the ZnO crystal structure to replace Zn atoms to control or reduce the resistance value, which may cause uneven Ga doping, and the uniform distribution of each element In the IGZO conductive material becomes the main problem of reducing the resistance value, thereby affecting the quality of RF/DC sputtering IGZO thin film. Secondly, three metal salt solutions of In, Ga and Zn are uniformly mixed, a proper precipitator is added, a chemical coprecipitation mode is adopted, indium gallium zinc oxide powder is obtained through presintering, and finally the IGZO target material is obtained through high-temperature sintering. This is because Zn2+(74 pm) radius and Ga3+(62 pm) and In3+(80 pm) has large difference and different valence states, so that the solid solubility between the doped ions and ZnO is low, and therefore, the industry needs to find a preparation technology of IGZO powder for a highly uniform target.
In view of the above, in order to further improve the oxide semiconductor thin film, many researchers have introduced rare earth elements into the preparation of ZnO thin films, and significant results have been obtained. This is because the unique physicochemical properties of rare earth elements determine their extremely wide use. The rare earth element has the characteristics of unique 4f electronic structure, large atomic magnetic distance, strong spin-orbit coupling and the like, when the rare earth element forms a rare earth complex with other elements, the coordination number can be changed between 3 and 12, and the crystal structure of the rare earth compound is diversified. In the field of new materials, the optical, electrical and magnetic properties of rare earth elements are widely applied. In the high technology field, new rare earth materials play an important role. However, the radius (mostly 80-100 pm) and valence (mostly 3 or 4) of the rare earth ions and the doped ions (Zn)2+) The difference is large, and the melting point is high, so that how to perform effective doping in IGZO with complex components is a problem to be solved in the field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides rare earth doped indium gallium zinc oxide powder, a preparation method and application thereof, which are used for avoiding the problem of nonuniform components caused by doping large-particle-size rare earth elements into the indium gallium zinc oxide powder and can be used for preparing the rare earth doped indium gallium zinc oxide powder with uniform components.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a preparation method of rare earth doped indium gallium zinc oxide powder, which comprises the following steps.
S1: and sequentially adding water, the first dispersing agent, the gallium oxide powder and the rare earth oxide powder into the first mixing barrel, pre-dispersing for a first preset time period to obtain a first mixed solution, and grinding the first mixed solution for a second preset time period to obtain a first mixed slurry.
S2: and sequentially adding water, a second dispersing agent and zinc oxide powder into a second mixing barrel for pre-dispersing for a third preset time period to obtain a second mixed solution, and adding the second mixed solution into the first mixed slurry for grinding for a fourth preset time period to obtain a second mixed slurry.
S3: and sequentially adding water, a third dispersing agent and indium oxide powder into a third mixing barrel for pre-dispersing for a fifth preset time period to obtain a third mixed solution, and adding the third mixed solution into the second mixed slurry for grinding for a sixth preset time period to obtain a third mixed slurry.
S4: and adding an adhesive into the third mixed slurry, and grinding for a seventh preset time period to obtain a fourth mixed slurry.
S5: and granulating, mixing and screening the fourth mixed slurry to finally obtain the rare earth doped indium gallium zinc oxide powder.
As a further improvement of the present invention, the first dispersant, the second dispersant and the third dispersant are one of polyvinylpyrrolidone, sodium dodecylbenzenesulfonate or sodium hexadecylbenzenesulfonate.
In a further improvement of the present invention, the first dispersant accounts for 1 to 15% of the total solid mass of the first dispersant, the gallium oxide powder and the rare earth oxide powder, the second dispersant accounts for 1 to 15% of the total solid mass of the second dispersant and the zinc oxide powder, and the third dispersant accounts for 1 to 15% of the total solid mass of the third dispersant and the indium oxide powder.
As a further improvement of the present invention, the first preset time period, the third preset time period, the fifth preset time period and the seventh preset time period are between 10-30 min.
As a further improvement of the present invention, the second preset time period, the fourth preset time period and the sixth preset time period are all between 4 and 16 hours.
As a further improvement of the invention, the adhesive is one of a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol or polyvinyl butyral.
As a further development of the invention, the solids content of the fourth mixed slurry is between 35 and 75% and the particle size distribution D50<1.0 μm.
The invention also provides rare earth doped indium gallium zinc oxide powder, and the chemical formula of the rare earth doped indium gallium zinc oxide is as follows: in (Ga)xRe1-x) ZnO4Wherein Re represents rare earth elements, and X is between 0.01 and 0.2.
As a further improvement of the invention, the Re represents at least one of La, Ce, Pr, Nd and Y.
The invention also provides an application of the rare earth doped indium gallium zinc oxide powder, which comprises the rare earth doped indium gallium zinc oxide powder and a target material obtained by pressure-equalizing forming and sintering treatment.
According to the rare earth doped indium gallium zinc oxide powder and the preparation method and application thereof, the auxiliary agent is added into the mixed slurry, and under the action of the auxiliary agent, the problem of non-uniform components caused by doping large-particle-size rare earth elements into the indium gallium zinc oxide powder is solved through a step-by-step grinding mode, the rare earth doped indium gallium zinc oxide powder with uniform components can be prepared, and the rare earth doped indium gallium zinc oxide target material with high density, uniform tissue and excellent photoelectric characteristics can be prepared by specifically applying the indium gallium zinc oxide powder.
Drawings
Fig. 1 is a morphology chart of the rare earth doped indium gallium zinc oxide powder prepared in example 1 of the present invention. Fig. 2 is a graph showing the XRD (X-ray diffraction) analysis result of the rare earth-doped indium gallium zinc oxide powder prepared in example 1 of the present invention.
Detailed Description
The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to a first aspect of the present invention, a method for preparing rare earth doped indium gallium zinc oxide powder is provided, which comprises the following steps.
S1: and sequentially adding water, the first dispersing agent, the gallium oxide powder and the rare earth oxide powder into the first mixing barrel, pre-dispersing for a first preset time period to obtain a first mixed solution, and grinding the first mixed solution for a second preset time period to obtain a first mixed slurry.
In this example, the rare earth oxide (Re)2O3) And gallium oxide (Ga)2O3) The two oxide powders have relatively large particles and the grinding requirements are relatively high, so that the first grinding is required.
The first dispersant is one of polyvinylpyrrolidone (PVP), Sodium Dodecyl Benzene Sulfonate (SDBS) or sodium hexadecyl benzene sulfonate, the first dispersing agent is preferably polyvinylpyrrolidone, the pre-dispersing duration is between 10 and 30min, the pre-dispersion duration is preferably 15min, in the embodiment, the first dispersing agent accounts for 1-15% of the total mass of the solids of the first dispersing agent, the gallium oxide powder and the rare earth oxide powder, the grinding equipment for the pre-dispersed first mixed solution is a sand mill, after the pre-dispersion is carried out for a predetermined time, pumping the pre-dispersed solution into a sand mill by a pump, wherein the diameter of a zirconium ball used in the sand mill is between 0.2 and 2 mm, the grinding rotating speed is between 500 and 2000 r/min, and the grinding time is between 4 and 16 hours.
S2: and sequentially adding water, a second dispersing agent and zinc oxide powder into a second mixing barrel for pre-dispersing for a third preset time period to obtain a second mixed solution, and adding the second mixed solution into the first mixed slurry for grinding for a fourth preset time period to obtain a second mixed slurry.
In this example, the rare earth oxide (Re)2O3) And gallium oxide (Ga)2O3) Need to be doped together with oxygenZinc oxide (ZnO) requires intermediate grinding in the zinc oxide (ZnO) cells.
The second dispersing agent is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate or sodium hexadecylbenzene sulfonate, the second dispersing agent is preferably polyvinylpyrrolidone, the pre-dispersing duration is 10-30min, the pre-dispersing duration is preferably 15min, in the embodiment, the second dispersing agent accounts for 1-15% of the total mass of the second dispersing agent and the zinc oxide powder, the pre-dispersed second mixed solution is ground by a sand mill, after the pre-dispersing is carried out for a preset time, the pre-dispersed solution is pumped into the sand mill by a pump, the diameter of a zirconium ball used in the sand mill is 0.2-2 mm, the grinding rotating speed is 500-2000 r/min, and the grinding time is 4-16 hours.
S3: and sequentially adding water, a third dispersing agent and indium oxide powder into a third mixing barrel for pre-dispersing for a fifth preset time period to obtain a third mixed solution, and adding the third mixed solution into the second mixed slurry for grinding for a sixth preset time period to obtain a third mixed slurry.
In this example, indium oxide (In)2O3) Small size of particles, In3+Radius and Zn2+Relatively close, easy to mix, and less demanding for grinding, so it is necessary to grind at the end.
The third dispersing agent is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate or sodium hexadecylbenzene sulfonate, the third dispersing agent is preferably polyvinylpyrrolidone, the pre-dispersing duration is between 10 and 30min, the pre-dispersing duration is preferably 15min, in the embodiment, the third dispersing agent accounts for 1 to 15 percent of the total mass of the third dispersing agent and the indium oxide powder, the pre-dispersed third mixed solution is ground by a sand mill, the pre-dispersed solution is pumped into the sand mill by a pump after the pre-dispersing is performed for a preset time, the diameter of a zirconium ball used in the sand mill is between 0.2 and 2 mm, the grinding speed is between 500 and 2000 r/min, and the grinding time is between 4 and 16 hours.
The main reason for setting the milling sequence is to consider the difficulty of doping various metal ions and the difference of the oxide particle size.
S4: and adding an adhesive into the third mixed slurry, and grinding for a seventh preset time period to obtain a fourth mixed slurry.
In this embodiment, the adhesive is selected from one of a mixture of polyvinyl alcohol (PVA) and polyethylene glycol (PEG), polyvinyl alcohol (PVA), or polyvinyl butyral (PVB), and is preferably selected from a mixture of polyvinyl alcohol and polyethylene glycol, the grinding is performed by a sand mill, the diameter of zirconium balls used in the sand mill is between 0.2 mm and 2 mm, the grinding speed is between 500 and 2000 r/min, and the grinding time is between 4 hours and 16 hours.
S5: and granulating, mixing and screening the fourth mixed slurry to finally obtain the rare earth doped indium gallium zinc oxide powder.
In this embodiment, the equipment that granulation adopted is the cocurrent flow formula spray drying tower, through the air-out temperature of adjustment drying tower, adjusts material moisture and size, carries out the compounding through the spiral blendor again, sieves by ultrasonic vibration sieve at last, finally obtains tombarthite doping indium gallium zinc oxide powder.
Further, the first dispersing agent, the second dispersing agent and the third dispersing agent are one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate or sodium hexadecylbenzene sulfonate.
Further, the first dispersant accounts for 1-15% of the total solid mass of the first dispersant, the gallium oxide powder and the rare earth oxide powder, the second dispersant accounts for 1-15% of the total solid mass of the second dispersant and the zinc oxide powder, and the third dispersant accounts for 1-15% of the total solid mass of the third dispersant and the indium oxide powder.
Further, the first preset time period, the third preset time period, the fifth preset time period and the seventh preset time period are between 10 and 30 minutes.
Further, the second preset time period, the fourth preset time period and the sixth preset time period are all between 4 and 16 hours.
Further, the adhesive is one of a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol or polyvinyl butyral.
Further, the fourth mixed slurry has a solids content between 35-75% and a particle size distribution D50<1.0 μm.
According to a second aspect of the present invention, there is also provided a rare earth-doped indium gallium zinc oxide powder prepared by the above method, wherein the rare earth-doped indium gallium zinc oxide powder has a chemical formula: in (Ga)xRe1-x) ZnO4Wherein Re represents rare earth elements, and X is between 0.01 and 0.2.
Further, Re at least represents one of La, Ce, Pr, Nd and Y.
In this embodiment, the prepared rare earth-doped indium gallium zinc oxide powder has a single-phase crystal structure, the purity is greater than 99.99%, the moisture content is between 0.2 and 3%, the particle size range is between 60 and 150 μm, and the specific surface area is between 5 and 25m2Between/g.
According to a third aspect of the present invention, there is provided an application of the rare earth-doped indium gallium zinc oxide powder, including the target material obtained by pressure-equalizing and sintering the rare earth-doped indium gallium zinc oxide powder.
For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1.
With cerium oxide (CeO)2) Powder and praseodymium oxide (Pr)6O11) The preparation method of the rare earth doped indium gallium zinc oxide powder by using the powder as a raw material comprises the following steps.
(1) Sequentially adding water, dispersant polyvinylpyrrolidone and gallium oxide (Ga) into a first mixing barrel2O3) Powder, cerium oxide powder (CeO)2) And praseodymium oxide (Pr)6O11) Pre-dispersing the powder for 10min, wherein the dispersant accounts for the dispersant and gallium oxide (Ga)2O3) Powder, cerium oxide powder (CeO)2) And praseodymium oxide (Pr)6O11) 10% of the total mass of solids such as powder, the mass of solids accounting for 35% of the total mass of solids and water. Pumping the pre-dispersed solution into a sand mill (using zirconium balls with the diameter of 0.2 mm) by a pump, wherein the grinding speed is 1800 r/min, and the grinding time is 8 hours, so as to obtain first mixed slurry.
(2) And sequentially adding water, a dispersant polyvinylpyrrolidone and zinc oxide (ZnO) powder into a second mixing barrel for pre-dispersion for 10min, wherein the mass of the dispersant accounts for 10% of the total mass of solids such as the dispersant and the zinc oxide (ZnO) powder, and the mass of the solids accounts for 40% of the total mass of the solids and the water. Adding the pre-dispersed solution into the first mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 0.2 mm), wherein the grinding speed is 1800 r/min, and the grinding time is 6 hours, so as to obtain second mixed slurry.
(3) Adding water, dispersant polyvinylpyrrolidone and indium oxide (In) into the third mixing barrel In sequence2O3) Pre-dispersing the powder for 10min, wherein the mass of the dispersing agent accounts for the dispersing agent and indium oxide (In)2O3) The total mass of the solid such as powder is 10%, and the mass of the solid accounts for 40% of the total mass of the solid and water. Adding the pre-dispersed solution into the second mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 0.2 mm), wherein the grinding speed is 1800 r/min, and the grinding time is 6 hours, so as to obtain third mixed slurry.
(4) And sequentially adding adhesive polyvinyl alcohol and polyethylene glycol into the third mixed slurry, wherein in the solution after the adhesive is added, the content of the adhesive polyvinyl alcohol and the content of the polyethylene glycol account for 2.5% of the mass of the solid, the mass of the solid accounts for 40% of the total mass of the solid and the water, putting the mixture into a sand mill (a zirconium ball with the diameter of 0.2 mm is used), the grinding speed is 1200 r/min, and the grinding time is 6 hours, so that the fourth mixed slurry is obtained.
(5) Will be describedThe fourth mixed slurry is injected into a parallel flow type spray drying tower for granulation, and then the materials are mixed and screened to obtain the material with the theoretical chemical formula of In (Ga)0.8Ce0.1Pr0.1)ZnO4The powder of (4) had a water content of 0.2% and an average particle diameter of 83 μm, as shown in FIG. 1.
Referring to fig. 2, a graph of XRD (X-ray diffraction) analysis results of the rare earth-doped indium gallium zinc oxide powder of this embodiment is shown, where an upper curve is a peak shape of the rare earth-doped indium gallium zinc oxide powder sample of this embodiment, a lower curve is a peak shape of the standard rare earth-doped indium gallium zinc oxide powder sample, and if the peak shapes of the upper curve and the lower curve are consistent, it indicates that the two curves are the same substance. Meanwhile, the XRD characteristic peak of the rare earth-doped indium gallium zinc oxide powder sample of the embodiment is shifted to the left (low angle) as a whole, because the rare earth element has a large radius and is doped into the host structure to enlarge the unit cell volume, thereby causing the phenomenon that the characteristic peak is shifted to the left as a whole. Therefore, it can be considered that the grinding method provided by the method for preparing the rare earth-doped indium gallium zinc oxide powder provided by the embodiment can effectively process the doping of the rare earth ions with large radius, and the rare earth-doped indium gallium zinc oxide powder processed by the method for preparing the rare earth-doped indium gallium zinc oxide powder provided by the embodiment can approach the performance of the standard rare earth-doped indium gallium zinc oxide powder sample.
Example 2.
With lanthanum oxide (La)2O3) The preparation method of the rare earth doped indium gallium zinc oxide powder by using the powder as a raw material comprises the following steps.
(1) Adding water, dispersant polyvinylpyrrolidone and gallium oxide (Ga) into a mixing barrel in sequence2O3) Powder and lanthanum oxide (La)2O3) Pre-dispersing the powder for 15min, wherein the powder is dispersedThe agent comprises dispersant and gallium oxide (Ga)2O3) Powder and lanthanum oxide (La)2O3) 1% of the total mass of solids such as powder, and the mass of solids accounts for 50% of the total mass of solids and water. Pumping the pre-dispersed solution into a sand mill (using zirconium balls with the diameter of 1.5 mm) by a pump, wherein the grinding speed is 800 r/min, and the grinding time is 5 hours, so as to obtain first mixed slurry.
(2) And sequentially adding water, a dispersant polyvinylpyrrolidone and zinc oxide (ZnO) powder into a second mixing barrel for pre-dispersion for 15min, wherein the mass of the dispersant accounts for 1% of the total mass of solids such as the dispersant and the zinc oxide (ZnO) powder, and the mass of the solids accounts for 50% of the total mass of the solids and the water. Adding the pre-dispersed solution into the first mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 1.5 mm), wherein the grinding speed is 800 r/min, and the grinding time is 5 hours, so as to obtain second mixed slurry.
(3) Adding water, dispersant polyvinylpyrrolidone and indium oxide (In) into the third mixing barrel In sequence2O3) Pre-dispersing the powder for 15min, wherein the mass of the dispersing agent accounts for the dispersing agent and indium oxide (In)2O3) 1% of the total mass of solids such as powder, and the mass of solids accounts for 50% of the total mass of solids and water. Adding the pre-dispersed solution into the second mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 1.5 mm), wherein the grinding speed is 800 r/min, and the grinding time is 4 hours, so as to obtain third mixed slurry.
(4) And sequentially adding adhesive polyvinyl alcohol and polyethylene glycol into the third mixed slurry, wherein in the solution after the adhesive is added, the content of the adhesive polyvinyl alcohol and the content of the polyethylene glycol account for 1% of the mass of the solid, the mass of the solid accounts for 50% of the total mass of the solid and the water, putting the mixture into a sand mill (a zirconium ball with the diameter of 1.5 mm is used), the grinding speed is 800 r/min, and the grinding time is 4 hours, so that fourth mixed slurry is obtained.
(5) The fourth mixed slurry is injected into a parallel flow type spray drying tower for granulation, and then the materials are mixed and screened to obtain the material with the theoretical chemical formula of In (Ga)0.95La0.05) ZnO4Powder of (2), theThe powder had a water content of 0.5% and an average particle diameter of 94 μm.
Example 3.
By praseodymium (Pr) oxide6O11) The preparation method of the rare earth doped indium gallium zinc oxide powder by using the powder as a raw material comprises the following steps.
(1) Sequentially adding water, dispersant polyvinylpyrrolidone and gallium oxide (Ga) into a first mixing barrel2O3) Powder and praseodymium oxide (Pr)6O11) Pre-dispersing the powder for 20 min, wherein the dispersant accounts for the dispersant and gallium oxide (Ga)2O3) Powder and praseodymium oxide (Pr)6O11) 5% of the total mass of the solids such as powder and the like, and the mass of the solids accounts for 60% of the total mass of the solids and the water. Pumping the pre-dispersed solution into a sand mill (using zirconium balls with the diameter of 0.8 mm) by a pump, wherein the grinding speed is 1000 r/min, and the grinding time is 5 hours, so as to obtain first mixed slurry.
(2) And sequentially adding water, a dispersant polyvinylpyrrolidone and zinc oxide (ZnO) powder into the second mixing barrel for pre-dispersion for 20 min, wherein the mass of the dispersant accounts for 5% of the total mass of solids such as the dispersant and the zinc oxide (ZnO) powder, and the mass of the solids accounts for 60% of the total mass of the solids and the water. Adding the pre-dispersed solution into the first mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 0.8 mm), wherein the grinding speed is 1000 r/min, and the grinding time is 4 hours, so as to obtain second mixed slurry.
(3) Adding water, dispersant polyvinylpyrrolidone and indium oxide (In) into the third mixing barrel In sequence2O3) Pre-dispersing the powder for 20 min, wherein the mass of the dispersing agent accounts for the dispersing agent and indium oxide (In)2O3) 5% of the total mass of the solids such as powder and the like, and the mass of the solids accounts for 60% of the total mass of the solids and the water. Adding the pre-dispersed solution into the second mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 0.8 mm), wherein the grinding speed is 1000 r/min, and the grinding time is 6 hours, so as to obtain third mixed slurry.
(4) And sequentially adding adhesive polyvinyl alcohol and polyethylene glycol into the third mixed slurry, wherein in the solution after the adhesive is added, the content of the adhesive polyvinyl alcohol and the content of the polyethylene glycol are both 5% of the mass of the solid, the mass of the solid is 60% of the total mass of the solid and the water, putting the mixture into a sand mill (using zirconium balls with the diameter of 0.8 mm), the grinding speed is 1000 r/min, and the grinding time is 6 hours, so as to obtain fourth mixed slurry.
(5) The fourth mixed slurry is injected into a parallel flow type spray drying tower for granulation, and then the materials are mixed and screened to obtain the material with the theoretical chemical formula of In (Ga)0.925Pr0.075)ZnO4The powder of (4), wherein the powder has a water content of 1.0% and an average particle diameter of 123 μm.
Example 4.
The preparation method of the rare earth doped indium gallium zinc oxide powder by using yttrium oxide powder as a raw material comprises the following steps.
(1) Sequentially adding water, dispersant polyvinylpyrrolidone and gallium oxide (Ga) into a first mixing barrel2O3) Powder and yttrium oxide (Y)2O3) Pre-dispersing the powder for 30min, wherein the dispersant accounts for the dispersant and gallium oxide (Ga)2O3) Powder and yttrium oxide (Y)2O3) 2% of the total mass of solids such as powder, and the mass of solids accounts for 70% of the total mass of solids and water. Pumping the pre-dispersed solution into a sand mill (using zirconium balls with the diameter of 0.5 mm) by a pump, wherein the grinding speed is 1200 r/min, and the grinding time is 4 hours, so as to obtain first mixed slurry.
(2) And sequentially adding water, a dispersant polyvinylpyrrolidone and zinc oxide (ZnO) powder into a second mixing barrel for pre-dispersion for 30min, wherein the mass of the dispersant accounts for 2% of the total mass of solids such as the dispersant and the zinc oxide (ZnO) powder, and the mass of the solids accounts for 70% of the total mass of the solids and the water. Adding the pre-dispersed solution into the first mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 0.5 mm), wherein the grinding speed is 1200 r/min, and the grinding time is 3 hours, so as to obtain second mixed slurry.
(3) Adding water, dispersant polyvinylpyrrolidone and indium oxide (In) into the third mixing barrel In sequence2O3) PowderPre-dispersing for 30min, wherein the dispersant accounts for the dispersant and indium oxide (In)2O3) 2% of the total mass of solids such as powder, and the mass of solids accounts for 70% of the total mass of solids and water. Adding the pre-dispersed solution into the second mixed slurry, and then putting the mixture into a sand mill (using zirconium balls with the diameter of 0.5 mm), wherein the grinding speed is 1200 r/min, and the grinding time is 6 hours, so as to obtain third mixed slurry.
(4) And sequentially adding adhesive polyvinyl alcohol and polyethylene glycol into the third mixed slurry, wherein in the solution after the adhesive is added, the content of the adhesive polyvinyl alcohol and the content of the polyethylene glycol account for 2% of the mass of the solid, the mass of the solid accounts for 70% of the total mass of the solid and the water, putting the mixture into a sand mill (a zirconium ball with the diameter of 0.5 mm is used), the grinding speed is 1200 r/min, and the grinding time is 7 hours, so that fourth mixed slurry is obtained.
(5) The fourth mixed slurry is injected into a parallel flow type spray drying tower for granulation, and then the materials are mixed and screened to obtain the material with the theoretical chemical formula of In2(Ga0.99Y0.01)ZnO4The powder of (4), wherein the powder has a water content of 2.2% and an average particle diameter of 134 μm.
According to the rare earth doped indium gallium zinc oxide powder and the preparation method and application thereof, the auxiliary agent is added into the mixed slurry, and under the action of the auxiliary agent, the problem of non-uniform components caused by doping large-particle-size rare earth elements into the indium gallium zinc oxide powder is solved through a step-by-step grinding mode, the rare earth doped indium gallium zinc oxide powder with uniform components can be prepared, and the rare earth doped indium gallium zinc oxide target material with high density, uniform tissue and excellent photoelectric characteristics can be prepared by specifically applying the indium gallium zinc oxide powder.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (10)
1. A preparation method of rare earth doped indium gallium zinc oxide powder is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: sequentially adding water, a first dispersing agent, gallium oxide powder and rare earth oxide powder into a first mixing barrel, pre-dispersing for a first preset time period to obtain a first mixed solution, and grinding the first mixed solution for a second preset time period to obtain a first mixed slurry;
s2: sequentially adding water, a second dispersing agent and zinc oxide powder into a second mixing barrel for pre-dispersing for a third preset time period to obtain a second mixed solution, adding the second mixed solution into the first mixed slurry for grinding for a fourth preset time period to obtain a second mixed slurry;
s3: adding water, a third dispersing agent and indium oxide powder into a third mixing barrel in sequence for pre-dispersing for a fifth preset time period to obtain a third mixed solution, adding the third mixed solution into the second mixed slurry for grinding for a sixth preset time period to obtain a third mixed slurry;
s4: adding an adhesive into the third mixed slurry, and grinding for a seventh preset time period to obtain a fourth mixed slurry;
s5: and granulating, mixing and screening the fourth mixed slurry to finally obtain the rare earth doped indium gallium zinc oxide powder.
2. The method for preparing rare earth doped indium gallium zinc oxide powder according to claim 1, characterized in that: the first dispersing agent, the second dispersing agent and the third dispersing agent are one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate or sodium hexadecylbenzene sulfonate.
3. The method for preparing rare earth doped indium gallium zinc oxide powder according to claim 1, characterized in that: the first dispersant accounts for 1-15% of the total solid mass of the first dispersant, the gallium oxide powder and the rare earth oxide powder, the second dispersant accounts for 1-15% of the total solid mass of the second dispersant and the zinc oxide powder, and the third dispersant accounts for 1-15% of the total solid mass of the third dispersant and the indium oxide powder.
4. The method for preparing rare earth doped indium gallium zinc oxide powder according to claim 1, characterized in that: the first preset time period, the third preset time period, the fifth preset time period and the seventh preset time period are between 10 and 30 min.
5. The method for preparing rare earth doped indium gallium zinc oxide powder according to claim 1, characterized in that: the second preset time period, the fourth preset time period and the sixth preset time period are all between 3 and 8 hours.
6. The method for preparing rare earth doped indium gallium zinc oxide powder according to claim 1, characterized in that: the adhesive is one of a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol or polyvinyl butyral.
7. The method for preparing rare earth doped indium gallium zinc oxide powder according to claim 1, characterized in that: the fourth mixed slurry has a solids content between 35-75% and a particle size distribution D50<1.0 μm.
8. A rare earth doped indium gallium zinc oxide powder prepared according to the preparation method of claim 1, which is characterized in that: the rare earth doped indium gallium zinc oxide has the chemical formula as follows: in (Ga)xRe1-x) ZnO4Wherein Re represents rare earth elements, and X is between 0.01 and 0.2.
9. The rare earth-doped indium gallium zinc oxide powder according to claim 8, wherein: the Re at least represents one of La, Ce, Pr, Nd and Y.
10. An application of rare earth doped indium gallium zinc oxide powder, which is a target material obtained by carrying out pressure-equalizing forming and sintering treatment on the rare earth doped indium gallium zinc oxide powder according to any one of claims 8 to 9.
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