CN116425538A - Doped lithium niobate target material and preparation method and application thereof - Google Patents
Doped lithium niobate target material and preparation method and application thereof Download PDFInfo
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- CN116425538A CN116425538A CN202310451818.4A CN202310451818A CN116425538A CN 116425538 A CN116425538 A CN 116425538A CN 202310451818 A CN202310451818 A CN 202310451818A CN 116425538 A CN116425538 A CN 116425538A
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- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000013077 target material Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 51
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 44
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 70
- 239000007784 solid electrolyte Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 238000003754 machining Methods 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 5
- 238000001513 hot isostatic pressing Methods 0.000 claims description 4
- 239000002019 doping agent Substances 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 26
- 239000010408 film Substances 0.000 description 28
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 9
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 238000004544 sputter deposition Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 3
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000013462 industrial intermediate Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
The invention discloses a doped lithium niobate target material, a preparation method and application thereof. The total mole fraction of doping source elements in the doped lithium niobate target is not higher than 30%, the doping source elements are selected from one or more elements in Al, ga, zr, mo, ta, W, and the mole mass fraction range of the corresponding elements is selected as follows: 0-10% of Al element, 0-5% of Ga element, 0-15% of Zr element, 0-15% of Mo element, 0-7% of Ta element and 0-10% of W element; the doping source elements are all in the form of oxides in the target; the structure of the doped lithium niobate target material has a polycrystalline structure, and the square resistance is less than 10 6 Omega. The lithium niobate target material is optimized through doping and preparation processes, has the characteristics of good conductivity, high ionic conductivity of the prepared lithium niobate film and the like, can be suitable for radio frequency or medium frequency magnetron sputtering processes, and can be used as an electrolyte layer in an inorganic all-solid-state electrochromic device.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a doped lithium niobate target material, a preparation method and application thereof.
Background
In the preparation of the inorganic all-solid-state electrochromic device, the transparent conductive substrate, the electrochromic layer, the ion storage layer and the like are prepared by direct-current magnetron sputtering, and the technology is mature. The ion conductor layer has two technical schemes: sputtering a tantalum oxide film without lithium ions, sputtering by using a metal lithium target material after sputtering the tantalum oxide film, and performing heat treatment to finish the injection of lithium ions; the second is to use a lithium ion-containing thin film such as lithium niobate or lithium tantalate. The second scheme does not need to carry out the injection of lithium ions additionally, can realize the continuous production of multi-layer vacuum magnetron sputtering during the production, and avoids the efficiency reduction caused by the processes such as vacuum breaking, heat treatment and the like in the production line of the first scheme. In addition, the production, transportation, use, replacement and preservation of the metallic lithium target are difficult, and the productivity of the first technical scheme is limited.
However, the second technical route is only verified in a laboratory at present, and is limited by the conductivity of the lithium niobate ceramic target material, and the second technical route can only be prepared by adopting a radio frequency magnetron sputtering method, so that the radio frequency sputtering efficiency is low, the power supply cost is extremely high, and the large-scale industrialized popularization and application can not be realized. The lithium niobate material is used as photoelectric, piezoelectric and electricity-saving material, and the monocrystal crystal and film are used widely in acousto-optic converting device. Lithium niobate ceramics as magnetron sputtering targets have relatively few studies, and thus current applications of lithium niobate in the process of inorganic electrochromic industrialization are limited by the materials themselves. At least the following technical problems exist in the current application of lithium niobate materials in electrochromic: the pure lithium niobate target material has poor conductivity and can only be used for preparing a film by adopting a radio frequency magnetron sputtering method; the research on the preparation of lithium niobate ceramic is insufficient, the target tissue adopted in the current laboratory is relatively coarse, the average grain size is more than 20 mu m, and the surface roughness of the thin film obtained by sputtering is large and the quality is poor; the ionic conductivity of the pure lithium niobate solid electrolyte film is lower than that of liquid and colloid electrolytes, and the color change and response speed of the pure lithium niobate solid electrolyte film cannot be achieved as the pure lithium niobate solid electrolyte film is the same as that of the pure lithium niobate solid electrolyte film.
Therefore, in order to expand the application range of the lithium niobate target material and promote the technical upgrading of electrochromic industry, a lithium niobate target material with good conductivity and high purity is needed.
It should be noted that the information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is well known to a person skilled in the art.
Disclosure of Invention
In view of the above, the invention aims to provide a doped lithium niobate target material, a preparation method and application thereof, wherein the doped source element is added into the lithium niobate target material, so that the problems of low conductivity and limited application of the pure lithium niobate ceramic target material in the prior art are solved, the conductivity of the lithium niobate ceramic target material is improved, the doped lithium niobate target material can be suitable for an intermediate frequency magnetron sputtering process, the polycrystalline lithium niobate target material with compact structure and uniform components is obtained by optimizing the preparation process, and the invention provides a foundation for industrialized popularization and application of the lithium niobate ceramic target material.
In a first aspect, the present invention provides a doped lithium niobate target, wherein the total mole fraction of doping source elements in the doped lithium niobate target is not higher than 30%, the doping source elements are selected from one or more elements in Al, ga, zr, mo, ta, W, and the mole fraction range of the corresponding elements is selected as follows: 0-10% of Al element, 0-5% of Ga element, 0-15% of Zr element, 0-15% of Mo element, 0-7% of Ta element and 0-10% of W element; the doping source elements are all in the form of oxides in the target; the doped lithium niobate target material has a polycrystalline structure, and the square resistance is less than 10 6 Ω。
Preferably, the doping source element is selected from one or more of Al, zr, mo, W. More preferably, the doping source element is W.
Furthermore, doping elements in the tissue of the target material enter the lithium niobate crystal lattice, the doping is uniform, and the average grain size is 800nm-15 mu m.
In a second aspect, the present invention provides a method for preparing the doped lithium niobate target material of the first aspect, including the following steps:
a, preparing powder, namely preparing doped lithium niobate powder by one of the following methods:
(1) The lithium niobate powder containing the doping source element is prepared into synthetic powder by a hydrothermal synthesis method;
(2) Performing ball milling dispersion and spray drying on pure lithium niobate powder and oxide powder doped with source elements to obtain optimized powder;
in the above (1) or (2), the purity of the synthesized powder prepared by the hydrothermal synthesis method and the optimized powder is higher than 99.95%;
and B, preparing a target: after the doped lithium niobate powder is obtained, a target material rough blank is obtained by adopting a target material preparation process;
and C, determining to carry out machining or not according to the rough blank of the target material and the use scene to obtain the doped lithium niobate target material.
Further, the average particle size of the synthesized powder prepared by the hydrothermal synthesis method is 50nm-500nm; the average particle size of the optimized powder is 500nm-5 mu m, and the D50 particle size is 200nm-3 mu m.
Furthermore, the target preparation process in the step B is a hot isostatic pressing method, wherein the hot isostatic pressing method adopts the pressure of 10-70MPa, the vacuum degree of 0.12-10Pa, the sintering temperature of 600-1000 ℃, the heat preservation time of 2-6h and the heating rate of 0.3-4 ℃/min.
In a third aspect, the present invention provides a solid electrolyte film prepared from the doped lithium niobate target material of the second aspect by radio frequency magnetron sputtering or medium frequency magnetron sputtering, the film being conductive by P-type holes and having a conductivity of 10 -7 Ion conductivity of S/cm or more.
Further, the invention also provides an application of the solid electrolyte film in the third aspect as an electrolyte layer in an inorganic all-solid-state electrochromic device.
The beneficial effects of the invention are as follows:
1. according to the doped lithium niobate target material, a plurality of doping source elements are selected, the doping with higher content of which the total mole fraction is not higher than 30% is performed, more defects are introduced into the crystal structure of lithium niobate through the doping of Al, ga, zr, mo, ta, W, so that electrons are more easily transferred in the target material, the problems that the current pure lithium niobate target material is poor in conductivity and only suitable for radio frequency magnetron sputtering are effectively solved, the aim that the lithium niobate target material is applied to an intermediate frequency magnetron sputtering process is fulfilled, and guidance is provided for the application of the rotary-stage doped lithium niobate target material in an industrial intermediate frequency magnetron sputtering production line;
2. after Ga, mo and W elements enter a lithium niobate crystal lattice structure, the N-type conductivity of the target material can be obviously improved, and the conductivity of the target material is improved; the Al, zr and Ta elements can improve the P-type conductivity of the obtained sputtering film and improve the ion conductivity of the film; wherein, the Al element can improve the sintering property of the lithium niobate target material and the density of the target material;
3. the preparation process and the raw material parameters of the target material can influence the structure of the target material, so that the electric performance of the target material is influenced, and the hydrothermal synthesis method or the particle size optimization of the powder is adopted to ensure that the obtained doped lithium niobate powder has the purity of more than 99.95 percent, so that the target material performance is ensured to be influenced by no impurity element; the particle size of the powder is in the nano-scale and submicron-scale grades, and the powder is suitable for obtaining a high-density and fine and uniform grain size doped lithium niobate target through various target forming processes, so that the uniformity and stability of the electric performance of the target are ensured;
4. in a comprehensive view, the doping source element selected by the invention can improve the N-type conductivity of the lithium niobate target material, improve the P-type conductivity of the lithium niobate film, finally improve the ion conductivity of the lithium niobate film and obtain the ion conductivity larger than 10 - 7 The S/cm lithium niobate solid electrolyte film can be applied to all-solid-state electrochromic devices to improve the performance of the electrochromic devices.
Drawings
FIG. 1 shows an SEM photograph of the powder prepared according to example 1 of the present invention;
FIG. 2 shows SEM pictures of prepared target fractures according to example 1 of the present invention;
FIG. 3 shows the XRD pattern of a target according to example 1 of the present invention;
FIG. 4 shows a surface SEM photograph of a prepared film according to example 1 of the present invention;
fig. 5 shows a cross-sectional SEM photograph of the prepared film according to example 1 of the present invention.
Detailed Description
The technical features and advantages of the present invention will be described in more detail below with reference to the examples and the accompanying drawings, so that the advantages and features of the present application can be more easily understood by those skilled in the art, and thus the scope of the present invention is more clearly and clearly defined.
The magnetron sputtering process can be divided into three types of radio frequency, medium frequency and direct current magnetron sputtering according to the type of power supply, and the requirements of the three processes on the conductivity of the target material are gradually improved from the radio frequency to the medium frequency and then to the direct current, wherein the radio frequency process can sputter all types of target materials, including non-conductive ceramic target materials, but the medium frequency and the direct current sputtering require the target material to have better conductivity. While the square resistance of the pure lithium niobate target is generally more than 10 9 Omega, close to the resistance of the insulator, can only be applied in rf magnetron sputtering processes. However, the radio frequency power supply is expensive, can only be used at a laboratory level, and cannot be popularized in an industrial level. The intermediate frequency and direct current magnetron sputtering process requires that the square resistance of the target material is less than 10 6 Omega, wherein the direct current process further requires that the target material is a conductor with good conductivity, and the square resistance is less than 100 omega.
In order to apply the lithium niobate target material in a low-cost medium-frequency magnetron sputtering process, the embodiment of the invention provides a doped lithium niobate target material, and the square resistance of lithium niobate is reduced to 10 by optimizing the doping and preparation processes 6 Under omega, the method is suitable for low-cost medium-frequency magnetron sputtering process, and is used for industrial lithium niobate targetsThe application of the intermediate frequency magnetron sputtering production line provides guidance.
In order to achieve the above object, the basic idea of the embodiment of the present invention is as follows:
the multi-component doped lithium niobate target material is doped by a plurality of doping elements, the doping source elements are selected from one or more elements in Al, ga, zr, mo, ta, W, the total mole fraction of the doping source elements is not higher than 30%, and the mole fraction range of the corresponding elements is selected as follows: 0-10% of Al element, 0-5% of Ga element, 0-15% of Zr element, 0-15% of Mo element, 0-7% of Ta element and 0-10% of W element. The doping source elements exist in the form of oxide in the target material, the structure of the target material is in a polycrystalline structure and has no obvious doping phase, the average grain size is 800nm-15 mu m, the density is more than 95 percent, and the square resistance is less than 10 6 Omega, can be suitable for radio frequency, intermediate frequency magnetron sputtering technology. The target material can be used for preparing lithium niobate solid electrolyte film by magnetron sputtering, and the solid electrolyte film prepared by the polycrystalline target material has 10 -7 The ionic conductivity above S/cm is higher than that of a pure lithium niobate film, and can be used as an electrolyte layer in an inorganic all-solid-state electrochromic device to improve the performance of the electrochromic device.
For a better understanding of the technical solution of the present invention, the following detailed description will refer to the accompanying drawings and specific embodiments.
Example 1
Preparing powder: the doping source element is W, zinc oxide powder and pure lithium niobate powder are adopted for ball milling dispersion, and optimized powder is obtained after spray drying, wherein the molar mass fraction of the W element is 10mol%. Mixing lithium niobate powder and tungsten oxide powder, adding pure water, ball milling in a nanometer sand mill at a rotating speed of 1800r/min for 6h, and completing the dispersion and ball milling of the powder. Adding the ball-milled doped slurry into a spray dryer, preparing doped lithium niobate powder at a spray temperature of 80 ℃, and finishing powder preparation after the slurry is exhausted. The purity of the doped lithium niobate powder after ball milling optimization is higher than 99.95 percent, the average grain diameter is 800nm, and the D50 grain diameter is 500nm.
And B, preparing a target: after the doped lithium niobate powder is obtained, a target material rough blank is prepared by adopting a hot pressing method, the technological parameters are pressure intensity of 20MPa, vacuum degree of 0.12Pa, sintering temperature of 900 ℃, heat preservation time of 3h and heating rate of 2 ℃/min.
And C, machining the target rough blank to obtain the doped lithium niobate target for magnetron sputtering.
The tungsten oxide doped lithium niobate target material is uniform in structure through fracture tissue analysis, the average grain size is 15 mu m, the target material is subjected to phase analysis through XRD, no obvious tungsten oxide phase exists in the XRD spectrum, and standard peaks of lithium niobate (012) are obvious in offset, so that tungsten elements enter the lithium niobate crystal lattice and are uniformly doped. Four probes test target square resistance 4.5X10 5 Omega, the target material is applicable to the intermediate frequency magnetron sputtering process besides the radio frequency magnetron sputtering process. The ionic conductivity of the tungsten oxide doped lithium niobate solid electrolyte film prepared by intermediate frequency magnetron sputtering is 2 multiplied by 10 -7 S/cm, the film is an amorphous film, surface growth particles are uniformly distributed, the section thickness is 397nm, and the amorphous form provides good conditions for ion conduction.
Example 2
Preparing powder: the doping source elements are Al and Mo, and the optimized powder is obtained by ball milling, dispersing and spray drying of alumina powder, molybdenum oxide powder and pure lithium niobate powder, wherein the mole mass fraction of the Al element is 5mol%, and the mole mass fraction of the Mo element is 10mol%. Mixing lithium niobate powder, aluminum oxide and molybdenum oxide powder, adding pure water, ball milling in a nanometer sand mill at a rotating speed of 2000r/min for 12h, and completing the dispersion and ball milling of the powder. Adding the ball-milled doped slurry into a spray dryer, and preparing doped lithium niobate powder at a spray temperature of 75 ℃, wherein the powder process is completed after the slurry is exhausted. The purity of the doped lithium niobate powder after ball milling optimization is higher than 99.95 percent, the average grain diameter is 2 mu m, and the D50 grain diameter is 1.5 mu m.
And B, preparing a target: after the doped lithium niobate powder is obtained, a target material rough blank is prepared by adopting a hot pressing method, the technological parameters are that the pressure intensity is 30MPa, the vacuum degree is 2Pa, the sintering temperature is 950 ℃, the heat preservation time is 2h, and the heating rate is 3 ℃/min.
And C, machining the target rough blank to obtain the doped lithium niobate target for magnetron sputtering.
The alumina and molybdenum oxide co-doped lithium niobate target material has uniform structure, and the square resistance of the target material is 4 multiplied by 10 through four-probe test 4 Omega, the target material is suitable for the intermediate frequency magnetron sputtering process besides the radio frequency magnetron sputtering process. The ionic conductivity of the zinc oxide doped lithium niobate solid electrolyte film prepared by magnetron sputtering is 3 multiplied by 10 -5 S/cm。
Example 3
Preparing powder: the doping source elements are Al and W, the doping powder is directly synthesized by adopting a hydrothermal method, the molar mass fraction of the Al element is 10mol%, and the molar mass fraction of the W element is 10mol%. The purity of the doped lithium niobate powder synthesized by the hydrothermal method is higher than 99.95 percent, and the average grain diameter is 100nm.
And B, preparing a target: after the doped lithium niobate powder is obtained, a target material rough blank is prepared by adopting a hot pressing method, the technological parameters are pressure intensity of 25MPa, vacuum degree of 5Pa, sintering temperature of 700 ℃, heat preservation time of 5h and heating rate of 0.8 ℃/min.
And C, machining the target rough blank to obtain the doped lithium niobate target for magnetron sputtering.
The alumina and tungsten oxide co-doped lithium niobate target material has uniform structure, and the square resistance of the target material is 1.5x10 by four-probe test 5 Omega, the target material is applicable to the intermediate frequency magnetron sputtering process besides the radio frequency magnetron sputtering process. The ionic conductivity of the zinc oxide doped lithium niobate solid electrolyte film prepared by magnetron sputtering is 6.8x10 -4 S/cm。
Example 4
Preparing powder: al, zr and W are selected as doping source elements, alumina, zirconia, tungsten oxide powder and pure lithium niobate powder are adopted for ball milling dispersion, and optimized powder is obtained after spray drying, wherein the molar mass fraction of the Al element is 10mol%, the molar mass fraction of the Zr element is 5mol%, and the molar mass fraction of the W element is 5mol%. Mixing lithium niobate powder and three doped element oxide powder, adding pure water, ball milling in a nanometer sand mill at a rotating speed of 1500r/min for 18h, and completing the dispersion and ball milling of the powder. Adding the ball-milled doped slurry into a spray dryer, preparing doped lithium niobate powder at a spraying temperature of 85 ℃, and finishing powder preparation after the slurry is exhausted. The purity of the doped lithium niobate powder after ball milling optimization is higher than 99.95 percent, the average particle diameter is 850nm, and the D50 particle diameter is 900nm.
And B, preparing a target: after the doped lithium niobate powder is obtained, a target material rough blank is prepared by adopting a hot pressing method, the technological parameters are pressure intensity of 25MPa, vacuum degree of 3Pa, sintering temperature of 650 ℃, heat preservation time of 6h and heating rate of 0.9 ℃/min.
And C, machining the target rough blank to obtain the doped lithium niobate target for magnetron sputtering.
The alumina, zirconia and tungsten oxide co-doped lithium niobate target material has uniform structure, and the square resistance of the target material is 2.1 multiplied by 10 through four-probe test 4 Omega, the target material is applicable to the intermediate frequency magnetron sputtering process besides the radio frequency magnetron sputtering process. The ionic conductivity of the zinc oxide doped lithium niobate solid electrolyte film prepared by magnetron sputtering is 1.2 multiplied by 10 -4 S/cm。
Example 5
Preparing powder: ga, zr and W are selected as doping source elements, doping powder is directly synthesized by adopting a hydrothermal method, the molar mass fraction of Ga element is 5mol%, the molar mass fraction of Zr element is 5mol%, and the molar mass fraction of W element is 10mol%. The purity of the doped lithium niobate powder obtained by hydrothermal synthesis is higher than 99.95 percent, and the average grain diameter is 80nm.
And B, preparing a target: after the doped lithium niobate powder is obtained, a target material rough blank is prepared by adopting a hot pressing method, the technological parameters are pressure intensity 40MPa, vacuum degree 8Pa, sintering temperature 800 ℃, heat preservation time 3.5h and heating speed 1.5 ℃/min.
And C, machining the target rough blank to obtain the doped lithium niobate target for magnetron sputtering.
The gallium oxide, zirconium oxide and tungsten oxide co-doped lithium niobate target material has uniform structure, and the square resistance of the target material is 8.9 multiplied by 10 through four-probe test 5 Omega, the target material is applicable to the intermediate frequency magnetron sputtering process besides the radio frequency magnetron sputtering process. The ionic conductivity of the zinc oxide doped lithium niobate solid electrolyte film prepared by magnetron sputtering is 6.8x10 -5 S/cm。
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. The doped lithium niobate target is characterized in that the total mole fraction of doping source elements in the doped lithium niobate target is not higher than 30%, the doping source elements are selected from one or more elements in Al, ga, zr, mo, ta, W, and the mole fraction range of the corresponding elements is selected as follows: 0-10% of Al element, 0-5% of Ga element, 0-15% of Zr element, 0-15% of Mo element, 0-7% of Ta element and 0-10% of W element; the doping source elements are all in the form of oxides in the target; the doped lithium niobate target material has a polycrystalline structure, and the square resistance is less than 10 6 Ω。
2. The doped lithium niobate target of claim 1, wherein the dopant source element is selected from one or more of Al, zr, mo, W.
3. The doped lithium niobate target of claim 1, wherein the dopant source element is W.
4. The doped lithium niobate target according to claim 1, wherein the doping element in the tissue of the target enters the interior of the lithium niobate crystal lattice, the doping is uniform, and the average grain size is 800nm-15 μm.
5. The method for preparing a doped lithium niobate target according to any of claims 1 to 4, comprising the steps of:
a, preparing powder, namely preparing doped lithium niobate powder by one of the following methods:
(1) The lithium niobate powder containing the doping source element is prepared into synthetic powder by a hydrothermal synthesis method;
(2) Performing ball milling dispersion and spray drying on pure lithium niobate powder and oxide powder doped with source elements to obtain optimized powder;
in the step (1) or (2), the purity of the synthesized powder prepared by the hydrothermal synthesis method and the optimized powder is higher than 99.95 percent;
and B, preparing a target: after the doped lithium niobate powder is obtained, a target material rough blank is obtained by adopting a target material preparation process;
and C, determining to carry out machining or not according to the rough blank of the target material and the use scene to obtain the doped lithium niobate target material.
6. The method according to claim 5, wherein the average particle diameter of the synthesized powder prepared by the hydrothermal synthesis method is 50nm to 500nm; the average particle diameter of the optimized powder is 500nm-5 mu m, and the D50 particle diameter is 200nm-3 mu m.
7. The method according to claim 5, wherein the target preparation process in the step B is a hot isostatic pressing method, and the hot isostatic pressing method adopts the pressure of 10-70MPa, the vacuum degree of 0.12-10Pa, the sintering temperature of 600-1000 ℃ and the heat preservation time of 2-6h, and the heating rate of 0.3-4 ℃/min.
8. Use of the doped lithium niobate target material according to any one of claims 1 to 4 in preparing a lithium niobate solid electrolyte film by magnetron sputtering.
9. A solid electrolyte film, its special featureCharacterized in that the solid electrolyte film is prepared by the doped lithium niobate target material of any one of claims 1 to 4 through radio frequency magnetron sputtering or medium frequency magnetron sputtering, and the film is conductive through P-type holes, and the ion conductivity is more than 10 -7 S/cm。
10. Use of the solid electrolyte film according to claim 9 as an electrolyte layer in an inorganic all-solid-state electrochromic device.
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