CN114163216A - Indium titanium ytterbium oxide powder and preparation method and application thereof - Google Patents

Indium titanium ytterbium oxide powder and preparation method and application thereof Download PDF

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CN114163216A
CN114163216A CN202111536233.XA CN202111536233A CN114163216A CN 114163216 A CN114163216 A CN 114163216A CN 202111536233 A CN202111536233 A CN 202111536233A CN 114163216 A CN114163216 A CN 114163216A
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titanium
nano
indium
ytterbium
ytterbium oxide
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李晴晴
邵学亮
李开杰
张来稳
王奇峰
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Vital Thin Film Materials Guangdong Co Ltd
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Abstract

The invention discloses indium titanium ytterbium oxide powder and a preparation method and application thereof, belonging to the technical field of indium oxide doped powder preparation; the structural formula of the indium titanium ytterbium oxide powder is In1‑x‑ yTixYbyO; wherein x is more than or equal to 0.001 and less than or equal to 0.171, and y is more than or equal to 0.001 and less than or equal to 0.139; d of the powder50=0.402‑0.475μm,D10≥0.196μm,D90Not more than 0.586 micron, particle size distribution coefficient P ═ D90‑D10)/D50Less than or equal to 0.746; according to the indium titanium ytterbium oxide powder provided by the technical scheme, titanium and ytterbium are selected as doping elements to be doped into the indium titanium ytterbium oxide powder, so that the indium titanium ytterbium oxide powder with uniform components and concentrated particle size distribution can be prepared; the technical scheme provided by the invention provides a preparation process of indium titanium ytterbium oxide powderThe method is simple and high in preparation efficiency, so that the method can be directly applied to industrial production, and the prepared product can be used for preparing the indium titanium ytterbium oxide target material with high density, high uniformity and excellent photoelectric characteristics.

Description

Indium titanium ytterbium oxide powder and preparation method and application thereof
Technical Field
The invention belongs to the technical field of indium oxide doped powder preparation, and particularly relates to indium titanium ytterbium oxide powder as well as a preparation method and application thereof.
Background
Indium oxide (In)2O3) The indium oxide is a novel N-type transparent semiconductor functional material, has wider forbidden bandwidth, smaller resistivity and higher catalytic activity, and is widely applied to the photoelectric field, gas sensors and catalysts, and when the size of indium oxide particles reaches the nanometer level, the indium oxide particles also have the functions of surface effect, quantum size effect, small size effect, macroscopic quantum tunneling effect and the like of the nanometer material, so that the nanometer indium oxide has wide application, and particularly, the research on doping the nanometer indium oxide to improve the performance of the nanometer indium oxide to perform application shows up endlessly; however, in the prior art, most of the N-type doping of nano indium oxide is carried out by doping rare metal elements, and since the rare elements are large, the doping is often uneven, so that the density of the doped product is insufficient, and the practical application of the product is affected.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides indium titanium ytterbium oxide powder and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: indium titanium ytterbium oxide powder, wherein the structural formula of the indium titanium ytterbium oxide powder is In1-x-yTixYbyO; wherein x is more than or equal to 0.001 and less than or equal to 0.171, and y is more than or equal to 0.001 and less than or equal to 0.139; d of the powder50=0.402-0.475μm,D10≥0.196μm,D90Not more than 0.586 micron, particle size distribution coefficient P ═ D90-D10)/D50≤0.746。
According to the technical scheme, the indium titanium ytterbium oxide powder provided by the invention takes titanium and ytterbium as doping elements of an indium oxide compound, the particle size distribution coefficient P of the obtained indium titanium ytterbium oxide powder is less than or equal to 0.746, and the powder has excellent uniformity.
In a preferred embodiment of the indium titanium ytterbium oxide powder of the present invention, the raw material of the indium titanium ytterbium oxide powder includes a nano titanium compound, a nano indium oxide, and a nano ytterbium compound.
In a preferred embodiment of the indium titanium ytterbium oxide powder of the present invention, the particle size of the nano titanium compound, the nano indium oxide and the nano ytterbium compound is 100-200 nm.
Due to D of the powder obtained50The particle size of the raw material of the provided powder is required to be between 0.402 and 0.475 mu m, so that the particle size of the raw material of the provided powder cannot be too large, and even though the raw material is too large, the raw material can be ground in a grinding mode, the phenomenon of powder adhesion caused by uneven grinding or too strong static electricity in the grinding process is difficult to avoid in the grinding process, and therefore, the nano-scale raw material is directly adopted for preparation, so that the problems can be effectively avoided; the particle size of the raw material is preferably 100-200nm, so that the problem of over-strong static electricity in subsequent grinding caused by over-fine particle size is avoided, and the problem of insufficient grinding caused by over-large particle size is avoided.
In a preferred embodiment of the indium titanium ytterbium oxide powder of the present invention, the raw material of the indium titanium ytterbium oxide powder includes 1 to 10 mass% of a nano titanium compound, 1 to 20 mass% of a nano ytterbium compound, and 70 to 98 mass% of nano indium oxide.
Because the nano indium oxide needs to be doped, the mass percent of the nano indium oxide serving as a base raw material is undoubtedly the highest, and the mass percent of the nano titanium compound and the nano ytterbium compound is controlled within the range, so that on one hand, enough titanium and ytterbium are ensured to enter the nano indium oxide for doping, and the performance of the powder is improved, and on the other hand, the phenomenon that the spatial distribution is uneven due to excessive addition of the titanium and the ytterbium is reduced, and the performance of the powder is reduced on the contrary, is avoided.
In a preferred embodiment of the indium titanium ytterbium oxide powder of the present invention, the nano titanium compound is nano titanium oxide, and the nano ytterbium compound is nano ytterbium oxide.
Because the nano indium oxide is doped, the nano titanium compound is preferably the nano titanium oxide, and the nano ytterbium compound is preferably the nano ytterbium oxide, so that on one hand, the introduction of new impurity elements due to the adoption of compounds of other elements of titanium and ytterbium can be avoided, and on the other hand, the use of expensive simple substances of titanium and ytterbium can also be avoided, thereby saving the cost and having economic benefits.
In a preferred embodiment of the indium titanium ytterbium oxide powder of the present invention, the purity of the nano titanium oxide is 4N or more, the purity of the nano indium oxide is 4N or more, and the purity of the nano ytterbium oxide is 4N or more.
When the purity of the preferable nanometer titanium oxide, nanometer indium oxide and nanometer ytterbium oxide is more than 4N, the problems that the doping is not uniform due to the introduction of impurities caused by too low purity, so that the density of later-stage preparation is high and low and the structure uniformity is influenced can be avoided.
In addition, the invention also provides a preparation method of the indium titanium ytterbium oxide powder, which comprises the following steps: adding nano titanium oxide, nano ytterbium oxide and a dispersing agent into pure water, uniformly dispersing, and grinding to obtain a mixture I; adding nano indium oxide into the mixture I, supplementing a dispersing agent, dispersing uniformly, and grinding to obtain a mixture II; then adding a binder into the mixture II, uniformly dispersing, and grinding to obtain a mixture III; and finally, carrying out spray granulation, mixing and screening on the mixture III to obtain the indium titanium ytterbium oxide powder.
As a preferred embodiment of the preparation method of the present invention, the dispersant is polyvinylpyrrolidone, sodium dodecylbenzenesulfonate or sodium hexadecylbenzenesulfonate.
As a preferred embodiment of the preparation method of the invention, the time for uniform dispersion is 15-35min, the time for grinding is 3-18h, and the rotation speed for grinding is 500-1800 r/min.
As a preferred embodiment of the preparation method of the invention, the mixture I and the mixture IIAnd D of the mixture III50Are all less than 1 μm.
As a preferable embodiment of the preparation method, in the mixture I and the mixture II, the mass percent of the dispersing agent is 1-10%.
As a preferred embodiment of the preparation process according to the invention, the mixture I has a solids content of from 30 to 60%.
As a preferred embodiment of the preparation method of the present invention, the binder is a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol, or polyvinyl butyral.
As a preferred embodiment of the preparation method of the invention, the mass percentage of the binder in the mixture III is 1-10%.
In addition, the invention also provides application of the indium titanium ytterbium oxide powder in preparation of the indium titanium ytterbium oxide target material.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the method comprises the following steps: the indium titanium ytterbium oxide powder provided by the technical scheme of the invention has uniform components and concentrated particle size distribution;
secondly, the method comprises the following steps: the indium titanium ytterbium oxide powder provided by the technical scheme provided by the invention is simple in preparation process and high in preparation efficiency, so that the indium titanium ytterbium oxide powder can be directly applied to industrial production, and the prepared product can be used for preparing indium titanium ytterbium oxide targets with high density, high uniformity and excellent photoelectric characteristics.
Drawings
FIG. 1: the preparation steps of the indium titanium ytterbium oxide powder are shown schematically.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The preparation steps of the examples of the present invention and the comparative examples were all the preparation steps shown in fig. 1; the reagents used in the examples of the present invention and comparative examples were obtained from conventional commercial sources unless otherwise specified.
Example 1
The indium titanium ytterbium oxide powder of the embodiment of the invention has the structural formula In0.976Ti0.017Yb0.007O, D thereof50=0.475μm,D10=0.257μm,D900.586 micron, particle size distribution coefficient P ═ D90-D10)/D500.693, wherein in the raw materials for preparing the powder, the mass percent of the nano titanium oxide is 1%, the mass percent of the nano ytterbium oxide is 1%, and the mass percent of the nano indium oxide is 98%;
the preparation method comprises the following specific steps:
(1) weighing the following raw materials in parts by weight for later use: 1 part of nano titanium oxide, 1 part of nano ytterbium oxide, 98 parts of nano indium oxide and 122 parts of pure water;
(2) adding nano titanium oxide, nano ytterbium oxide and sodium dodecyl benzene sulfonate (2.5 parts) into pure water, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 800r/min, and the grinding time is 16h to obtain D50Mixture I at 0.563 μm;
(3) adding nano indium oxide and sodium dodecyl benzene sulfonate (4.5 parts) into the mixture I, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 800r/min, and the grinding time is 13h to obtain D500.535 μm of mixture II;
(3) adding a mixture (4.8 parts) of polyvinyl alcohol and polyethylene glycol into the mixture II, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 800r/min, and the grinding time is 10h to obtain D50Mixture III at 0.466 μm;
(4) the mixture III is injected into a parallel flow type spray drying tower for spray granulation, and then the mixture is mixed and screened to obtain the In with the structural formula0.976Ti0.017Yb0.007O indium titanium ytterbium oxide powder.
Example 2
The indium titanium ytterbium oxide powder of the embodiment of the invention has the structural formula In0.690Ti0.171Yb0.139O, D thereof50=0.432μm,D10=0.226μm,D900.539 μm, particle size distribution coefficient P ═ D90-D10)/D500.724, wherein in the raw materials for preparing the powder, the mass percent of the nano titanium oxide is 10%, the mass percent of the nano ytterbium oxide is 20%, and the mass percent of the nano indium oxide is 70%;
the preparation method comprises the following specific steps:
(1) weighing the following raw materials in parts by weight for later use: 10 parts of nano titanium oxide, 20 parts of nano ytterbium oxide, 70 parts of nano indium oxide and 100 parts of pure water;
(1) adding nano titanium oxide, nano ytterbium oxide and sodium dodecyl benzene sulfonate (2.8 parts) into pure water, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 900r/min, and the grinding time is 15h to obtain D500.506 μm of mixture I;
(2) adding nano indium oxide and sodium dodecyl benzene sulfonate (4.4 parts) into the mixture I, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 900r/min, and the grinding time is 11h to obtain D50Mixture II at 0.455 μm;
(3) adding a mixture (4.8 parts) of polyvinyl alcohol and polyethylene glycol into the mixture II, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 900r/min, and the grinding time is 9h to obtain D50Mixture III at 0.428 μm;
(4) the mixture III is injected into a parallel flow type spray drying tower for spray granulation, and then the mixture is mixed and screened to obtain the In with the structural formula0.690Ti0.171Yb0.139O indium titanium ytterbium oxide powder.
Example 3
The indium titanium ytterbium oxide powder of the embodiment of the invention has the structural formula In0.844Ti0.086Yb0.070O, D thereof50=0.402μm,D10=0.196μm,D900.496 μm, particle sizeDistribution coefficient P ═ D90-D10)/D500.746 percent, wherein in the raw materials for preparing the powder, the mass percent of the nano titanium oxide is 5 percent, the mass percent of the nano ytterbium oxide is 10 percent, and the mass percent of the nano indium oxide is 85 percent;
the preparation method comprises the following specific steps:
(1) weighing the following raw materials in parts by weight for later use: 5 parts of nano titanium oxide, 10 parts of nano ytterbium oxide, 85 parts of nano indium oxide and 82 parts of pure water;
(1) adding nano titanium oxide, nano ytterbium oxide and sodium dodecyl benzene sulfonate (1.3 parts) into pure water, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 1200r/min, and the grinding time is 13h to obtain D500.478 μm of mixture I;
(2) adding nano indium oxide and sodium dodecyl benzene sulfonate (1.3 parts) into the mixture I, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 1200r/min, and the grinding time is 9h to obtain D50Mixture II at 0.435 μm;
(3) adding a mixture (5.5 parts) of polyvinyl alcohol and polyethylene glycol into the mixture II, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 1200r/min, and the grinding time is 7h to obtain D50Mixture III at 0.382. mu.m;
(4) the mixture III is injected into a parallel flow type spray drying tower for spray granulation, and then the mixture is mixed and screened to obtain the In with the structural formula0.844Ti0.086Yb0.070O indium titanium ytterbium oxide powder.
Example 4
The indium titanium ytterbium oxide powder of the embodiment of the invention has the structural formula In0.889Ti0.069Yb0.042O, D thereof50=0.425μm,D10=0.214μm,D900.526 μm, particle size distribution coefficient P ═ D90-D10)/D500.734, wherein, in the preparation of powder raw materialIn the material, the mass percent of the nano titanium oxide is 4%, the mass percent of the nano ytterbium oxide is 6%, and the mass percent of the nano indium oxide is 90%;
the preparation method comprises the following specific steps:
(1) weighing the following raw materials in parts by weight for later use: 4 parts of nano titanium oxide, 6 parts of nano ytterbium oxide, 90 parts of nano indium oxide and 90 parts of pure water;
(1) adding nano titanium oxide, nano ytterbium oxide and sodium dodecyl benzene sulfonate (1.8 parts) into pure water, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 1500r/min, and the grinding time is 11h to obtain D500.525 μm of mixture I;
(2) adding nano indium oxide and sodium dodecyl benzene sulfonate (2.3 parts) into the mixture I, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 1500r/min, and the grinding time is 8h to obtain D500.462 μm of mixture II;
(3) adding a mixture (5.5 parts) of polyvinyl alcohol and polyethylene glycol into the mixture II, pre-dispersing for 30min, pumping the mixed system into a sand mill for grinding after uniform dispersion, wherein the rotation speed of the sand mill is 1500r/min, and the grinding time is 7h to obtain D50Mixture III at 0.416 μm;
(4) the mixture III is injected into a parallel flow type spray drying tower for spray granulation, and then the mixture is mixed and screened to obtain the In with the structural formula0.889Ti0.069Yb0.042O indium titanium ytterbium oxide powder.
As can be seen from examples 1 to 4, the particle size distribution coefficient P of the indium titanium ytterbium oxide powder prepared by the preparation method of the present invention is within 0.746, which indicates that the indium titanium ytterbium oxide powder provided by the present invention has good particle size distribution concentration.
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 ytterbium oxide powder is characterized In that the structural formula of the indium titanium ytterbium oxide powder is In1-x-yTixYbyO;
Wherein x is more than or equal to 0.001 and less than or equal to 0.171, and y is more than or equal to 0.001 and less than or equal to 0.139;
d of the powder50=0.402-0.475μm,D10≥0.196μm,D90Not more than 0.586 micron, particle size distribution coefficient P ═ D90-D10)/D50≤0.746。
2. The indium titanium ytterbium oxide powder according to claim 1, wherein a raw material of the indium titanium ytterbium oxide powder includes a nano titanium compound, a nano indium oxide, and a nano ytterbium compound.
3. The indium titanium ytterbium oxide powder according to claim 2, wherein the raw material of the indium titanium ytterbium oxide powder includes 1 to 10 mass% of a nano titanium compound, 1 to 20 mass% of a nano ytterbium compound, and 70 to 98 mass% of nano indium oxide.
4. The indium titanium ytterbium oxide powder according to claim 2, wherein the nano titanium compound is a nano titanium oxide and the nano ytterbium compound is a nano ytterbium oxide.
5. The method of preparing the indium titanium ytterbium oxide powder of any one of claims 1 to 4, wherein the method includes the steps of: adding nano titanium oxide, nano ytterbium oxide and a dispersing agent into pure water, uniformly dispersing, and grinding to obtain a mixture I; adding nano indium oxide into the mixture I, supplementing a dispersing agent, dispersing uniformly, and grinding to obtain a mixture II; then adding a binder into the mixture II, uniformly dispersing, and grinding to obtain a mixture III; and finally, carrying out spray granulation, mixing and screening on the mixture III to obtain the indium titanium ytterbium oxide powder.
6. The method according to claim 5, wherein the dispersant is polyvinylpyrrolidone, sodium dodecylbenzenesulfonate or sodium hexadecylbenzenesulfonate.
7. The process according to claim 5, wherein D is selected from the group consisting of mixtures I, II and III50Are all less than 1 μm.
8. The production method according to claim 5, wherein the binder is a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol, or polyvinyl butyral.
9. The use of the indium titanium ytterbium oxide powder of any one of claims 1 to 4 in the preparation of an indium titanium ytterbium oxide target.
CN202111536233.XA 2021-12-15 2021-12-15 Indium titanium ytterbium oxide powder and preparation method and application thereof Pending CN114163216A (en)

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