CN114031372A - Indium titanium yttrium oxide powder and preparation method thereof - Google Patents

Indium titanium yttrium oxide powder and preparation method thereof Download PDF

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CN114031372A
CN114031372A CN202111536234.4A CN202111536234A CN114031372A CN 114031372 A CN114031372 A CN 114031372A CN 202111536234 A CN202111536234 A CN 202111536234A CN 114031372 A CN114031372 A CN 114031372A
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yttrium oxide
dispersion liquid
indium
slurry
oxide
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王奇峰
邵学亮
李开杰
张来稳
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Vital Thin Film Materials Guangdong Co Ltd
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    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract

The invention discloses indium titanium yttrium oxide powder and a preparation method thereof, belonging to the field of preparation of indium titanium yttrium oxide. The chemical formula of the indium titanium yttrium oxide powder is In1‑x‑yTixYyO1.5+0.5xWherein x is 0.001-0.2 and y is 0.001-0.2. The preparation method of the indium titanium yttrium oxide powder overcomes the problem of non-uniform components caused by adding large-particle rare earth metals, and finally obtains the indium titanium yttrium oxide powder with uniform particle size distribution and no uniform components.

Description

Indium titanium yttrium oxide powder and preparation method thereof
Technical Field
The invention relates to indium titanium yttrium oxide powder and a preparation method thereof, belonging to the field of preparation of indium titanium yttrium oxide.
Background
Due to the unique photoelectric characteristics of high transmittance in a visible light region and low resistivity of the transparent conductive film, the transparent conductive film is widely applied to the photoelectric fields of flat panel displays, solar cells and the like. With the development of science and technology, the demand of the photoelectric film is gradually increased, and higher requirements are put forward on the performance of the photoelectric film. In order to more efficiently produce materials with desirable properties, the relationship between the material properties and the corresponding process technology must be well understood, which is crucial for improving the material properties, increasing the productivity and reducing the cost.
The preparation of the powder is the first key process in the preparation process of the ITO target material. The existing powder used for the ITO target material generally has the problems of uneven particle size distribution, poor stability, high impurity content, irregular shape and the like, which brings great difficulty to the performance guarantee and subsequent application of the powder. Therefore, the invention optimizes the preparation method of the indium oxide powder on the basis of the prior art, overcomes the problem of non-uniform components caused by adding large-particle rare earth metal, and finally obtains the indium titanium yttrium oxide powder with uniform particle size distribution and uniform components.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides indium titanium yttrium oxide powder and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
in a first aspect, an indium titanium yttrium oxide powder is provided, wherein the chemical formula of the indium titanium yttrium oxide powder is In1-x- yTixYyO1.5+0.5xWherein x is 0.001-0.2 and y is 0.001-0.2.
Since titanium and yttrium are doped into indium oxide, the doping does not cause the problem of non-uniformity of the components due to the large particle size of indium oxide because the atomic radii of titanium and yttrium are small. The indium titanium yttrium oxide powder prepared by the invention has uniform grain diameter and uniform components, and can be used for preparing indium titanium yttrium oxide target materials with high density, uniform tissues and excellent photoelectric specificity.
In a second aspect, a method for preparing indium titanium yttrium oxide powder is provided, which comprises the following steps:
(1) sequentially adding titanium oxide and a first dispersing agent into a solvent for pre-dispersing to obtain a pre-dispersion liquid 1, and carrying out wet grinding on the pre-dispersion liquid 1 to obtain a first slurry;
(2) adding yttrium oxide and a second dispersing agent into the slurry I obtained in the step (1), performing pre-dispersion to obtain a pre-dispersion liquid 2, and performing wet grinding on the pre-dispersion liquid 2; obtaining a second slurry;
(3) adding indium oxide and a third dispersing agent into the slurry II obtained in the step (2), performing pre-dispersion to obtain a pre-dispersion liquid 3, and performing wet grinding on the pre-dispersion liquid 3; obtaining slurry III;
(4) adding a binder into the slurry III obtained in the step (3), performing pre-dispersion to obtain a pre-dispersion liquid 4, and performing wet grinding on the pre-dispersion liquid 4; obtaining slurry IV;
(5) and (4) carrying out spray granulation, mixing and screening on the slurry IV obtained in the step (4) to obtain indium titanium yttrium oxide powder.
Doping titanium and yttrium into indium oxide, grinding the titanium oxide and the yttrium oxide to obtain titanium oxide and yttrium oxide with small particle size, mixing the titanium oxide and the yttrium oxide with indium oxide, and grinding to obtain indium titanium yttrium oxide powder. The grinding sequence of the oxides depends on the doping difficulty of titanium, yttrium and indium oxide, and the titanium and the yttrium cannot be ground simultaneously due to the large difference of the atomic radii.
The dispersibility of the powder mainly depends on the effects of van der waals force, electrostatic repulsion force, steric hindrance and the like among particles, and the particle size of solid in the slurry obtained after grinding is small, so that a dispersing agent needs to be added in the grinding process to fully disperse titanium oxide and yttrium oxide in a solvent so as to be doped with indium oxide; after titanium oxide, yttrium oxide and indium oxide are fully mixed, a binder is required to be added, so that the stability of the precursor slurry is further improved, later spray granulation is facilitated, and indium titanium yttrium oxide powder with uniform particle size is prepared.
Preferably, the first dispersant, the second dispersant and the third dispersant are one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate and sodium hexadecylbenzene sulfonate.
Polyvinylpyrrolidone belongs to high molecular polymer, after adding the high molecular polymer who contains the long chain in the nanoparticle, can adsorb partial macromolecular compound at the granule surface, because the long chain can fully extend in the solvent, and then form the adsorbed layer of certain thickness, this adsorbed layer can hinder the contact closely of particle spare, prevents effectively that the ion cluster from gathering together, can mix titanium, tantalum, cerium into indium oxide.
The sodium dodecyl benzene sulfonate and the sodium hexadecyl benzene sulfonate belong to anionic dispersing agents, charged polymers are added into a sample, and the charged polymers are adsorbed on the surface of particles, so that the existence of the same kind of charged ions is rejected, the polymerization is prevented, and the ion agglomeration is prevented due to the steric hindrance effect generated by a long polymer chain.
Preferably, the binder is at least one of polyvinyl alcohol, polyethylene glycol and polyvinyl butyral.
Polyvinyl alcohol, polyethylene glycol and polyvinyl butyral are used as binders, and the stability of the precursor slurry can be further improved.
Preferably, the mass ratio of the titanium oxide to the yttrium oxide to the indium oxide is titanium oxide: yttrium oxide: indium oxide 2-9.5:0.5-1.5: 89.5-97.
The doping amount of the titanium oxide and the yttrium oxide is controlled by adjusting the mass ratio of the titanium oxide to the yttrium oxide to the indium oxide, and further the component uniformity of the indium titanium yttrium oxide powder is controlled.
In order to improve the dispersibility and stability of the slurry, it is necessary to control the addition amount of the dispersant, the solid content of the slurry, and the addition amount of the binder.
Preferably, in the step (1), the addition amount of the first dispersing agent is 1-10% of the total mass of the pre-dispersing liquid 1.
Preferably, in the step (2), the addition amount of the second dispersing agent is 1-10% of the total mass of the yttrium oxide and the second dispersing agent.
Preferably, in the step (3), the addition amount of the third dispersing agent is 1-10% of the total mass of the indium oxide and the third dispersing agent.
Preferably, in the step (4), the addition amount of the binder is 1-10% of the total mass of the titanium oxide, the yttrium oxide and the indium oxide.
Compared with the prior art, the invention has the beneficial effects that: the invention provides indium titanium yttrium oxide powder and a preparation method thereof, the preparation method of the indium titanium yttrium oxide powder solves the problem of non-uniform components caused by adding large-particle rare earth metals, and finally the indium titanium yttrium oxide powder with uniform particle size distribution and uniform components is obtained.
Drawings
FIG. 1 is a process flow diagram of the method for preparing indium titanium yttrium oxide powder according to the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following detailed description and accompanying drawings.
FIG. 1 is a process flow diagram of the method for preparing indium titanium yttrium oxide powder.
The raw material used in the invention is titanium oxide with a chemical formula of TiO2Yttrium oxide of formula Y2O3Indium oxide of the formula In2O3Polyvinylpyrrolidone, PVP, sodium dodecylbenzenesulfonate, SDBS, sodium hexadecylbenzenesulfonate, whose molecular formula is C18H29SO3Na, polyvinyl alcohol, abbreviated as PVA, polyethylene glycol, abbreviated as PEG, polyvinyl butyral, abbreviated as PVB.
Example 1
In a first aspect, the present embodiment provides an indium titanium yttrium oxide powder, where the chemical formula of the indium titanium yttrium oxide powder is In0.964Ti0.008Y0.028O。
In a second aspect, this embodiment provides a method for preparing indium titanium yttrium oxide powder, including the following steps:
(1) the mass ratio of titanium oxide to yttrium oxide to indium oxide is as follows: yttrium oxide: titanium oxide, yttrium oxide and indium oxide were weighed out at 2:1:97 for use.
(2) Adding pure water, polyvinylpyrrolidone and TiO into a mixing barrel in sequence2Pre-dispersing for 20min to obtain pre-dispersion liquid 1. Wherein the mass of PVP accounts for TiO23% of the total mass of PVP and pure water; the mass of the solid in the pre-dispersion liquid 1 accounts for 50 percent of the total mass of the pre-dispersion liquid 1. Pumping the pre-dispersion liquid 1 into a sand mill by a pump for grinding at the grinding speed of 900r/min for 12h to obtain a first slurry D50＝0.350μm。
(3) Adding pure water, PVP and Y into the slurry obtained in the step (2) in sequence2O3And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 1. Wherein the mass of PVP accounts for PVP and Y2O33% of the total mass of the powder and the pure water; the mass of the solid in the pre-dispersion liquid 2 accounts for 50 percent of the total mass of the obtained pre-dispersion liquid 2. Pumping the obtained pre-dispersion liquid 2 into a sand mill by a pump for grinding at the grinding speed of 900r/min for 9h to obtain a second slurry D50＝0.415μm。
(4) Adding pure water, PVP and In into the slurry obtained In the step (3) In sequence2O3And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 3. Wherein the mass of PVP accounts for 2.5% of the total mass of PVP, In2O3 powder and pure water, and the mass of solids In the pre-dispersion liquid 3 accounts for 40% of the total mass of the pre-dispersion liquid 3. Pumping the pre-dispersion liquid 3 into a sand mill by a pump for grinding at the grinding speed of 900r/min for 15h to obtain slurry III and slurry D50＜0.566μm。
(5) And (4) sequentially adding the adhesive PVA and PEG into the slurry obtained in the step (4), and pre-dispersing for 20min to obtain a pre-dispersion liquid 4. Wherein, the mass of PVA and PEG is 4% of the mass of the solid in the pre-dispersion liquid 4, and the mass of the solid in the pre-dispersion liquid 4 accounts for 40% of the total mass of the pre-dispersion liquid 4. Pumping the pre-dispersion liquid 4 into a sand mill by a pump for grinding at the grinding speed of 900r/min for 5h to obtain slurry IV and D of the slurry IV50＜0.605μm。
(6) And (5) pumping the slurry obtained In the step (5) into a parallel flow type spray drying tower for spray granulation, mixing and screening to obtain indium titanium yttrium oxide powder with a chemical formula of In0.964Ti0.008Y0.028O; the powder was tested to give the following results: the water content is 0.74 percent; d10＝0.335μm，D50＝0.532μm，D90＝0.765μm。
Example 2
In a first aspect, the present embodiment provides an indium titanium yttrium oxide powder, where the chemical formula of the indium titanium yttrium oxide powder is In0.93Ti0.04Y0.029O。
In a second aspect, this embodiment provides a method for preparing indium titanium yttrium oxide powder, including the following steps:
(1) the mass ratio of titanium oxide to yttrium oxide to indium oxide is as follows: yttrium oxide: titanium oxide, yttrium oxide and indium oxide were weighed out for use 9:1.5: 89.5.
(2) Sequentially adding water, PVP dispersant and TiO into a mixing barrel2And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 1. Wherein, dispersant PVP is added into TiO23% of the total mass of the powder, the dispersing agent PVP and the pure water; the mass of the solid in the pre-dispersion liquid 1 accounts for 48 percent of the total mass of the pre-dispersion liquid 1. Pumping the pre-dispersion liquid 1 into a sand mill by a pump for grinding at the grinding speed of 1100r/min for 10h to obtain a first slurry D50＝0.362μm。
(3) Adding water, a dispersant PVP and Y into the slurry obtained in the step (2) in sequence2O3And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 2. Wherein the mass of the dispersant PVP accounts for PVP and Y2O3And 2.5% of the total mass of pure water; the mass of the solid in the pre-dispersion liquid 2 accounts for 48 percent of the total mass of the pre-dispersion liquid 2. Pumping the pre-dispersion liquid 2 into a sand mill by a pump for grinding at the grinding speed of 1100r/min for 7h to obtain a second slurry D50＝0.422μm。
(4) Adding pure water, PVP and In into the slurry obtained In the step (3) In sequence2O3And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 3. Wherein the mass of PVP accounts for PVP and In2O3And 3% of the total mass of pure water, and the mass of solids in the pre-dispersion liquid 3 accounts for 38% of the total mass of the pre-dispersion liquid 3. Pumping the pre-dispersion liquid 3 into a sand mill by a pump for grinding at the rotating speed of 1100r/min for 12h to obtain slurry III and slurry D50＝0.582μm。
(5) And (4) sequentially adding PVA and PEG into the slurry obtained in the step (4), and pre-dispersing for 20min to obtain a pre-dispersion liquid 4. Wherein, the mass of PVA and PEG accounts for 4% of the mass of the solid in the pre-dispersion liquid 4, and the mass of the solid in the pre-dispersion liquid 4 accounts for 38% of the total mass of the pre-dispersion liquid 4. Pumping the pre-dispersion liquid 4 into a sand mill by a pump for grinding at the rotating speed of 1100r/min for 5h to obtain slurry IV and slurry IV50＝0.654μm。
(6) And (5) pumping the slurry obtained In the step (5) into a parallel flow type spray drying tower for spray granulation, mixing and screening to obtain indium titanium yttrium oxide powder with a chemical formula of In0.93Ti0.04Y0.029O; the powder was tested to give the following results: the water content is 0.70 percent; d10＝0.313μm，D50＝0.513μm，D90＝0.792μm。
Example 3
In a first aspect, the present embodiment provides an indium titanium yttrium oxide powder, where the chemical formula of the indium titanium yttrium oxide powder is In0.949Ti0.036Y0.015O。
In a second aspect, this embodiment provides a method for preparing indium titanium yttrium oxide powder, including the following steps:
(1) the mass ratio of titanium oxide to yttrium oxide to indium oxide is as follows: yttrium oxide: titanium oxide, yttrium oxide and indium oxide were weighed out at 8.5:0.5:91 for future use.
(2) Sequentially adding water, PVP dispersant and TiO into a mixing barrel2And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 1. Wherein, dispersant PVP is added into TiO23% of the total mass of the powder, the dispersing agent PVP and the pure water; the solid mass in the pre-dispersion liquid 1 accounts for pre-distribution48 percent of the total mass of the dispersion 1. Pumping the pre-dispersion liquid 1 into a sand mill by a pump for grinding at the rotating speed of 1500r/min for 6h to obtain a first slurry D50＝0.352μm。
(3) Adding water, a dispersant PVP and Y into the slurry obtained in the step (2) in sequence2O3And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 2. Wherein the mass of the dispersant PVP accounts for PVP and Y2O3And 2% of the total mass of pure water; the mass of the solid in the pre-dispersion liquid 2 accounts for 48 percent of the total mass of the pre-dispersion liquid 2. Pumping the pre-dispersion liquid 2 into a sand mill by a pump for grinding at the rotating speed of 1500r/min for 5h to obtain a second slurry D50＝0.433μm。
(4) Adding pure water, PVP and In into the slurry obtained In the step (3) In sequence2O3And (3) pre-dispersing the powder for 20min to obtain a pre-dispersion liquid 3. Wherein the mass of PVP accounts for PVP and In2O3And 3% of the total mass of pure water, and the mass of solids in the pre-dispersion liquid 3 accounts for 38% of the total mass of the pre-dispersion liquid 3. Pumping the pre-dispersion liquid 3 into a sand mill by a pump for grinding at the rotating speed of 1500r/min for 8h to obtain slurry III and slurry D50＝0.604μm。
(5) And (4) sequentially adding PVA and PEG into the slurry obtained in the step (4), and pre-dispersing for 20min to obtain a pre-dispersion liquid 4. Wherein, the mass of PVA and PEG accounts for 4% of the mass of the solid in the pre-dispersion liquid 4, and the mass of the solid in the pre-dispersion liquid 4 accounts for 38% of the total mass of the pre-dispersion liquid 4. Pumping the pre-dispersion liquid 4 into a sand mill by a pump for grinding at the grinding speed of 1000r/min for 5h to obtain slurry IV. D of slurry IV50＝0.676μm
(6) And (5) pumping the slurry obtained In the step (5) into a parallel flow type spray drying tower for spray granulation, mixing and screening to obtain indium titanium yttrium oxide powder with a chemical formula of In0.949Ti0.036Y0.015O; the powder was tested to give the following results: the water content is 0.75 percent; d10＝0.320μm，D50＝0.588μm，D90＝0.803μm。
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (9)

1. The indium titanium yttrium oxide powder is characterized In that the chemical formula of the indium titanium yttrium oxide powder is In1-x- yTixYyO1.5+0.5xWherein x is 0.001-0.2 and y is 0.001-0.2.
2. A method of making indium titanium yttrium oxide powder according to claim 1, comprising the steps of:
(1) sequentially adding titanium oxide and a first dispersing agent into a solvent for pre-dispersing to obtain a pre-dispersion liquid 1, and carrying out wet grinding on the pre-dispersion liquid 1 to obtain a first slurry;
(2) adding yttrium oxide and a second dispersing agent into the slurry I obtained in the step (1), performing pre-dispersion to obtain a pre-dispersion liquid 2, and performing wet grinding on the pre-dispersion liquid 2; obtaining a second slurry;
(3) adding indium oxide and a third dispersing agent into the slurry II obtained in the step (2), performing pre-dispersion to obtain a pre-dispersion liquid 3, and performing wet grinding on the pre-dispersion liquid 3; obtaining slurry III;
(4) adding a binder into the slurry III obtained in the step (3), performing pre-dispersion to obtain a pre-dispersion liquid 4, and performing wet grinding on the pre-dispersion liquid 4; obtaining slurry IV;
(5) and (4) carrying out spray granulation, mixing and screening on the slurry IV obtained in the step (4) to obtain indium titanium yttrium oxide powder.
3. The method of claim 2, wherein the first, second, and third dispersants are one of polyvinylpyrrolidone, sodium dodecylbenzenesulfonate, and sodium hexadecylbenzenesulfonate.
4. The method according to claim 2, wherein the binder is at least one of polyvinyl alcohol, polyethylene glycol, and polyvinyl butyral.
5. The method according to claim 2, wherein the mass ratio of the titanium oxide to the yttrium oxide to the indium oxide is titanium oxide: yttrium oxide: indium oxide 2-9.5:0.5-1.5: 89.5-97.
6. The method according to claim 2, wherein in the step (1), the first dispersant is added in an amount of 1 to 10% by mass based on the total mass of the predispersion 1.
7. The method according to claim 2, wherein in the step (2), the second dispersant is added in an amount of 1 to 10% by mass based on the total mass of the yttrium oxide and the second dispersant.
8. The production method according to claim 2, wherein in the step (3), the amount of the third dispersant added is 1 to 10% by mass of the total mass of the indium oxide and the third dispersant.
9. The method according to claim 2, wherein in the step (4), the amount of the binder added is 1 to 10% by mass of the total mass of the titanium oxide, yttrium oxide and indium oxide.
CN202111536234.4A 2021-12-15 2021-12-15 Indium titanium yttrium oxide powder and preparation method thereof Pending CN114031372A (en)

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Application publication date: 20220211