CN114807882A - Magnetron sputtering target material, preparation method and application thereof - Google Patents
Magnetron sputtering target material, preparation method and application thereof Download PDFInfo
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- CN114807882A CN114807882A CN202210487584.4A CN202210487584A CN114807882A CN 114807882 A CN114807882 A CN 114807882A CN 202210487584 A CN202210487584 A CN 202210487584A CN 114807882 A CN114807882 A CN 114807882A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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Abstract
The invention discloses a magnetron sputtering target material, a preparation method and application thereof, and relates to the technical field of magnetron sputtering. The preparation method of the magnetron sputtering target material comprises the following steps: coating the precursor solution on a substrate, designing the thickness according to the strength of magnetic field distribution of a magnetron sputtering device, wherein the coating thickness of a region with strong magnetic field is large, the coating thickness of a region with weak magnetic field is small, volatilizing the solvent by heating in the coating process, partially or completely converting the precursor into a target material, sintering at the temperature of 200-1500 ℃, and carrying out magnetron sputtering on the sintered target material to prepare the film. Compared with the existing method, the preparation process of the target is greatly shortened, the material utilization rate of the planar target is improved, and the preparation cost of the sputtering film is reduced; compared with the method for preparing the film by directly depositing through solution processing, the film prepared by sputtering the film target through solution processing has ideal density and adhesive force.
Description
Technical Field
The invention relates to the technical field of magnetron sputtering, in particular to a magnetron sputtering target material, and a preparation method and application thereof.
Background
The magnetron sputtering technology developed in the last 70 th century has the advantages of easy control, large-area film coating, high compactness and strong adhesive force, and is widely applied to the preparation of films of metals, semiconductors, insulators and the like by the industry. The film prepared by magnetron sputtering depends on a target material and vacuum equipment, the traditional block target material needs to be prepared by adopting a high-temperature high-pressure sintering method, the preparation process is complicated and energy consumption is reduced, and the cost of preparing the film by magnetron sputtering is limited to be further reduced.
The preparation process of the traditional magnetron sputtering target is complicated, for example, the ITO ceramic target is taken as (shown in figure 1), the preparation process comprises the links of nano powder preparation, powder granulation, biscuit forming, low-temperature degreasing, normal-pressure sintering, grinding, processing, binding and the like, and the whole preparation process consumes time and energy. In addition, because the magnetic field distribution of the magnetron sputtering target gun is uneven, the etching speed of the planar target material in the strong magnetic field area is higher, and the etching speed of the weak magnetic field area is lower, the target material is caused to have the uneven etching phenomenon (such as fig. 2 and fig. 3), so that the utilization rate of the planar target material is low, the highest utilization rate of the planar target material is only about 40%, and the resource waste is caused, and the further reduction of the preparation cost of the magnetron sputtering film is limited.
In order to reduce the preparation cost of the film, the academic and industrial fields also widely research solution processing methods to prepare metal, semiconductor and insulator films, and compared with the magnetron sputtering technology, the precursor material used for preparing the film by solution processing does not need the complicated flow of traditional target preparation and corresponding processing equipment, so that the film preparation cost is expected to be greatly reduced. Although the cost of the film prepared by the solution processing method is greatly reduced compared with the cost of the film prepared by sputtering, the compactness and the adhesion of the solution processed film are far inferior to those of the film prepared by magnetron sputtering, and the application of the solution processed film in the industry is also hindered.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a magnetron sputtering target material and a preparation method thereof, which aim to greatly shorten the preparation process of the traditional target material and solve the problems of low film density and insufficient adhesive force caused by directly depositing a film by solution processing.
The invention also aims to provide the target material applied to preparing the film by magnetron sputtering.
The invention is realized by the following steps:
in a first aspect, the present invention provides a method for preparing a magnetron sputtering target, including: coating the precursor solution on a substrate, volatilizing the solvent by heating in the coating process, partially or completely converting the precursor into a target material, and then sintering at the temperature of 200-1500 ℃.
In an alternative embodiment, the thickness of the film formed by coating the precursor solution on the substrate after coating and before sintering is 0.001-100mm, and the coating thickness of different areas is set according to the magnetic field intensity of the target gun of the magnetron sputtering device, and the coating thickness of the area is larger as the corresponding magnetic field intensity is stronger.
In an alternative embodiment, the method of applying the precursor solution onto the substrate is selected from at least one of inkjet printing, spray pyrolysis, electrofluidic printing, and 3D printing;
preferably, the precursor solution is subjected to spray pyrolysis to form a target material;
preferably, the heating temperature of the substrate in the coating process is controlled to be 50-500 ℃;
preferably, the precursor solution is sintered for 20-60min at the temperature of 500-1000 ℃ after being coated on the substrate.
In an alternative embodiment, the target material is selected from at least one of a metal oxide, a metal sulfide, a metal iodide, a metal selenide, an inorganic perovskite material, and a metal material;
preferably, the target material is a metal oxide selected from any one of a metal oxide conductor, a metal oxide semiconductor and a metal oxide insulator; wherein the metal oxide conductor is any one of indium tin oxide, fluorine-doped tin oxide, aluminum zinc oxide and indium zinc oxide; the metal oxide semiconductor is any one of indium oxide, indium zinc oxide, indium gallium zinc oxide, indium tin zinc oxide, rare earth element doped indium zinc oxide, nickel oxide and lithium doped nickel oxide; the metal oxide insulator is any one of silicon oxide, aluminum oxide, hafnium oxide, zirconium oxide, and yttrium oxide.
In an optional embodiment, when the target material is a metal oxide, the precursor solution is a solution formed by a metal inorganic salt or a metal organic compound corresponding to the target material;
preferably, the preparation process of the precursor solution comprises: mixing metal inorganic salt or metal organic compound with a solvent, and controlling the concentration of a precursor solution to be 0.05-10 mol/L;
preferably, the metal inorganic salt is selected from at least one of metal nitrate and metal chloride;
preferably, the solvent is water or an organic solvent;
more preferably, the organic solvent is selected from at least one of ethanol, ethylene glycol monomethyl ether, acetonitrile, and ethylene glycol.
In an alternative embodiment, the substrate is a polished base selected from at least one of a metal, silicon, and a metal oxide;
preferably, the substrate is made of metal; more preferably, the material of the substrate is selected from at least one of Ti, Al, and Cu.
In an alternative embodiment, the substrate is a metal base covered by a buffer layer, and the precursor solution is coated on the buffer layer;
preferably, the buffer layer is made of a metal oxide insulator material;
more preferably, the material of the buffer layer is selected from ZrO 2 、SiO 2 And Y 2 O 3 At least one of; the material of the metal substrate is at least one selected from Ti, Al and Cu.
In an alternative embodiment, the substrate is a support layer with a polished surface, and the material of the support layer is at least one of silicon and metal oxide;
preferably, the preparation method further comprises: cooling the sintered material, and then connecting one side of the supporting layer, on which the target is not deposited, with the metal heat conduction layer through the bonding layer;
preferably, the material of the bonding layer is at least one selected from indium and its alloy, and tin and its alloy; the material of the metal heat conduction layer is selected from at least one of Cu, Ti and Al.
In a second aspect, the present invention provides a magnetron sputtering target material prepared by the preparation method according to any one of the foregoing embodiments.
In a third aspect, the invention provides the magnetron sputtering target material of the foregoing embodiment for preparing a thin film by magnetron sputtering.
The invention has the following beneficial effects: the invention provides a novel preparation method of a magnetron sputtering target material, which comprises the steps of coating a solution on a substrate in a solution processing mode, setting the coating thickness of different areas according to the thickness of a target gun of magnetron sputtering equipment, partially or completely converting a precursor film into a target material after coating is finished, and then sintering. Compared with the existing method, the preparation method of the magnetron sputtering target provided by the embodiment of the invention greatly shortens the preparation flow of the target, reduces the preparation cost of the sputtering film and improves the utilization rate of the target; compared with the method for preparing the film by directly depositing through solution processing, the method for preparing the magnetron sputtering target material through the solution processing in the selected area and preparing the film through the magnetron sputtering method have ideal density and adhesive force.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow of preparing a conventional ITO target;
FIG. 2 shows an Al planar target after a long time use;
FIG. 3 is a schematic cross-sectional view of a planar target after prolonged use;
FIG. 4 is a flow chart of the preparation of a metal oxide target;
FIG. 5 is a schematic cross-sectional view of a target deposited on a metal substrate;
FIG. 6 is a schematic cross-sectional view of a target deposited on a buffer metal substrate;
FIG. 7 is a flow chart of metal oxide target material preparation;
fig. 8 is a schematic cross-sectional view of a target.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. 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.
The invention provides a preparation method of a magnetron sputtering target material, which is prepared by adopting a selective area solution processing method, greatly shortens the preparation flow of the traditional target material and reduces the preparation cost. As shown in fig. 4, the method specifically includes the following steps:
s1, preparation of precursor solution
The type of the raw materials adopted in the preparation process of the precursor solution is determined according to the target material, so that the target material is obtained by heating and removing the solvent after the precursor solution is coated on the substrate.
In some embodiments, the target material is selected from one of a metal oxide, a metal sulfide, a metal iodide, a metal selenide, an inorganic perovskite material, and a metallic material.
In a preferred embodiment, the target material is a metal oxide selected from any one of a metal oxide conductor, a metal oxide semiconductor, and a metal oxide insulator; wherein the metal oxide conductor is any one of indium tin oxide, fluorine-doped tin oxide, aluminum zinc oxide and indium zinc oxide; the metal oxide semiconductor is any one of indium oxide, indium zinc oxide, indium gallium zinc oxide, indium tin zinc oxide, rare earth element doped indium zinc oxide, nickel oxide and lithium doped nickel oxide; the metal oxide insulator is any one of silicon oxide, aluminum oxide, hafnium oxide, zirconium oxide, and yttrium oxide. The metal oxide target is more suitable for the method provided by the embodiment of the invention, and the type of the metal oxide is not limited and can be selected according to the requirement. When preparing the metal oxide target, preparing an oxide precursor solution.
Specifically, when the target material is a metal oxide, the precursor solution is a solution formed from a metal inorganic salt or a metal organic compound corresponding to the target material. In the practical operation process, the preparation process of the precursor solution comprises the following steps: mixing metal inorganic salt or metal organic compound with a solvent, and controlling the concentration of a precursor solution to be 0.05-10 mol/L; the metal inorganic salt is at least one selected from metal nitrate and metal chloride; the solvent is water or organic solvent. For example, the metal inorganic salt may be aluminum nitrate, zirconium chloride, yttrium chloride, etc., and the solvent may be used to rapidly dissolve the metal inorganic salt and keep the solution stable, and the specific kind is not limited.
In some embodiments, the organic solvent is at least one selected from ethanol, ethylene glycol monomethyl ether, acetonitrile, and ethylene glycol, and may be one or more of the above common organic solvents.
S2, coating
And coating the precursor solution on a substrate, and heating to volatilize the solvent and convert part or all of the precursor into a target material in the coating process.
The coating method is not limited, and may be a conventional coating method. In some embodiments, the method of applying the precursor solution onto the substrate is selected from at least one of inkjet printing, spray pyrolysis, electrofluidic printing, and 3D printing; preferably, the target material is formed by spray pyrolysis, and the spraying equipment for spray deposition of the thin film in the optional area is used for operation, and the coating step can also be referred to as oxide precursor spray pyrolysis.
In some embodiments, the heating temperature of the substrate during coating is controlled to be 50-500 ℃ so that the solvent is sufficiently volatilized and removed.
Further, referring to fig. 5, after the precursor solution is coated on the substrate, the thickness of the coating film before sintering is 0.001-100mm, and the coating thickness of different areas is set according to the magnetic field intensity distribution of the target gun of the magnetron sputtering apparatus, and the higher the corresponding magnetic field intensity is, the larger the coating thickness of the area is. Correspondingly, the target material in the area with strong magnetic field intensity is thick after sintering, the target material in the area with weak magnetic field intensity is thin, and the thickness distribution range is 0.001-100mm, so that the waste of the target material in the magnetron sputtering process is greatly reduced.
Specifically, the target formed on the substrate comprises a basic thickness layer and two arc-shaped protrusions which are arranged on the basic thickness layer at intervals, the thicknesses of the arc-shaped protrusions are set according to the magnetic field intensity distribution of the target gun, the thickness of the basic thickness layer is 0.001-1mm, and the maximum distance between the highest point of each arc-shaped protrusion and the basic thickness layer is 0.001-9 mm. The magnetic field intensity of the thick area of the target material is Ar + A main region of ion etching; the thin area is weak magnetic field area or non-magnetic field area, and is Ar + Ion weak etching area or non-Ar + ion weak etching area.
S3 sintering of target material
Sintering at the temperature of 200 ℃ and 1500 ℃, improving the density of the target material by sintering and converting the unconverted precursor into the target material.
In a preferred embodiment, the precursor solution is coated on a substrate and then sintered for 20-60min at the temperature of 500-1000 ℃ to ensure the density and purity of the target material.
According to different substrate materials, the method is specifically divided into the following implementation forms:
case (1): as shown in fig. 5, the substrate is a polished substrate, the precursor solution is coated on the polished surface, and the other surface of the substrate is in direct contact with the magnetron sputtering target gun when in use. The prepared target material product comprises: the device comprises a substrate and a target.
The base is selected from at least one of metal, silicon and metal oxide, and the materials are all suitable for being directly used as the substrate.
In a preferred embodiment, the substrate is made of metal; the material of the substrate is selected from at least one of Ti, Al and Cu, and the target material formed directly on the metal material is more widely applied.
Case (2): as shown in fig. 6, the substrate is a metal base covered by the buffer layer, and the precursor solution is coated on the buffer layer, that is, the prepared target product includes: the device comprises a substrate, a buffer layer and a target.
The buffer layer is arranged between the metal substrate and the target material, the buffer layer material can prevent the metal material from diffusing to the target material, and the metal substrate is directly contacted with the magnetron sputtering target gun when in use.
Specifically, the buffer layer is made of a metal oxide insulator material; the material of the buffer layer is selected from ZrO 2 、SiO 2 And Y 2 O 3 At least one of; the material of the metal substrate is at least one selected from Ti, Al and Cu.
Case (3): as shown in fig. 7-8, the substrate is a support layer with a polished surface, and the prepared target product comprises: the target comprises a substrate (also called a heat conduction layer), an adhesive layer, a supporting layer and a target.
Specifically, a polished surface of the supporting layer is coated with a precursor solution to form a target, the other surface of the supporting layer is connected with a heat conducting layer through a bonding layer, and the heat conducting layer is directly contacted with a magnetron sputtering target gun when in use. The material of the supporting layer is at least one of silicon and metal oxide.
In this case, the preparation method further comprises: and sintering the target on the supporting layer, and then binding to obtain a target finished product. In the actual operation process, the sintered material is cooled, and then the side of the supporting layer, on which the target is not deposited, is connected with the metal heat conduction layer through the bonding layer.
In some embodiments, the material of the bonding layer is selected from at least one of indium and its alloy, and tin and its alloy; the material of the metal heat conduction layer is selected from at least one of Cu, Ti and Al.
The embodiment of the invention provides a magnetron sputtering target material, which is prepared by the preparation method, has low preparation cost, and solves the problems of low density and insufficient adhesive force of a directly-deposited film processed by a solution.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The present embodiment provides a method for preparing a magnetron sputtering target, referring to fig. 4 and 5, including the following steps:
(1) preparation of oxide precursor solution
Indium nitrate, gallium nitrate and water were mixed, and the atomic ratio of indium to gallium was set at 3/1, to prepare a precursor solution with a total metal ion concentration of 5 mol/L.
(2) Spray pyrolysis of oxide precursors
And (3) adopting spraying equipment for spraying and depositing the film in the optional area, depositing the sprayed film on the polished titanium-based substrate material, heating the substrate material in the coating process, and controlling the heating temperature to be 200 ℃ so as to volatilize the solvent and solidify the solvent to form the film. The thickness of the target material in different areas is controlled during coating as shown in fig. 5, the thickness of the basic thickness layer is 0.01mm, and the maximum distance between the highest point of each arc-shaped convex part and the basic thickness layer is 0.1 mm.
(3) Sintering of target material
And sintering the target material after the spraying is finished for 60min at 350 ℃ to obtain a target material finished product.
And (3) performance testing: the target material prepared by the embodiment is used as a target material for magnetron sputtering to prepare the indium gallium oxide film, and the prepared indium gallium oxide film is annealed for 30min at 350 ℃ in air. The results show that: the density of the indium gallium oxide film prepared by sputtering is 6.75g/cm 3 。
Example 2
The present embodiment provides a method for preparing a magnetron sputtering target, please refer to fig. 4 and 6, which includes the following steps:
(1) preparation of oxide precursor solution
Zirconium oxychloride and water were mixed to prepare a precursor solution with a concentration of 2M.
(2) Spray pyrolysis of oxide precursors
Spraying equipment for spraying and depositing film by adopting selectable areas, wherein the sprayed film is deposited on ZrO material 2 The substrate (made of copper) material is heated in the coating process, and the heating temperature is controlled to be 350 ℃ so as to volatilize and solidify the solvent to form a film. The thickness of the target material in different areas is controlled during coating as shown in fig. 6, the thickness of the basic thickness layer is 0.5mm, and the maximum distance between the highest point of each arc-shaped convex part and the basic thickness layer is 2 mm.
(3) Sintering of target material
And sintering the target material after the spraying is finished for 35min at the temperature of 350 ℃ to obtain a target material finished product.
And (3) performance testing: ZrO prepared by using the target prepared by the embodiment as the target for magnetron sputtering x And annealing the film at 350 ℃ for 30 min. The results show that: the density of the film was 5.59g/cm 3 。
Example 3
The present embodiment provides a method for preparing a magnetron sputtering target, please refer to fig. 7 and 8, which includes the following steps:
(1) preparation of oxide precursor solution
Mixing nickel nitrate and ethylene glycol monomethyl ether solvent to prepare a precursor solution with the concentration of 1M.
(2) Spray pyrolysis of oxide precursors
The spraying equipment for spraying and depositing the film in the optional area is adopted, the sprayed film is deposited on the supporting layer made of silicon, the supporting layer is heated in the coating process, and the heating temperature is controlled to be 300 ℃ so as to volatilize the solvent and solidify the solvent to form the film. The thickness of the target material in different areas is controlled during coating as shown in fig. 8, the thickness of the basic thickness layer is 0.2mm, and the maximum distance between the highest point of each arc-shaped convex part and the basic thickness layer is 0.5 mm.
(3) Sintering of target material
And sintering the target material after the spraying is finished for 40min at 350 ℃ to obtain a target material finished product.
(4) Binding
And cooling the sintered target material, and bonding the supporting layer deposited with the target material with a metal heat conduction block (namely a substrate) through indium (a bonding layer) to form the block target material.
And (3) performance testing: NiO is prepared by adopting the target prepared by the embodiment as the target for magnetron sputtering x And annealing the film for 1h at 350 ℃ under the air condition. The results show that: the density of the film was 6.31g/cm 3 。
Comparative example 1
This comparative example provides a method of preparing a film by solution processing, comprising the steps of:
(1) preparation of oxide precursor solution
Indium nitrate, gallium nitrate and water were mixed, and the atomic ratio of indium to gallium was set at 3/1, to prepare a precursor solution with a concentration of 5 mol/L.
(2) Spin-on annealing of oxide precursors to form films
And (2) spin-coating the precursor solution obtained in the step (1) on a glass substrate at the speed of 3000 revolutions per minute, and annealing for 1h at the temperature of 350 ℃ in air to obtain the indium gallium oxide thin film.
The results show that: the density of the obtained indium gallium oxide film is 4.85g/cm 3 Much lower than 6.75g/cm of the indium gallium oxide film obtained in example 1 3 The density of (c).
Comparative example 2
The only difference from example 2 is: after the zirconium oxide solution is prepared, the ZrO is prepared and formed by adopting a blade coating method x Precursor film of ZrO x Annealing temperature of the film was 350 ℃ and annealing was continued for 1 hour to obtain ZrO x The density of the film was 4.61g/cm 3 Lower than the ZrO obtained in example 2 x Film 5.59g/cm 3 The density value of (a).
In summary, the present invention provides a magnetron sputtering target material, a preparation method and an application thereof, the inventors creatively use a solution method to prepare the target material, and use the target material to prepare a thin film material by magnetron sputtering, and the magnetron sputtering target material has the following advantages:
(1) the target material is prepared by adopting a selective solution method, the method is simple, and the preparation energy consumption is low;
(2) the target material forms different thicknesses in different areas according to the distribution condition of the magnetic field, and the effective utilization rate of the target material is improved, so that the preparation cost of the target material and the preparation cost of the magnetron sputtering film are reduced;
(3) the problems of low density and insufficient adhesive force of the solution processing direct deposition film are solved, so that the solution processing film can be applied to various electronic device products.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the magnetron sputtering target material is characterized by comprising the following steps: coating the precursor solution on a substrate, volatilizing the solvent by heating in the coating process, partially or completely converting the precursor into a target material, and then sintering at the temperature of 200-1500 ℃.
2. The preparation method according to claim 1, wherein the thickness of the film formed by coating the precursor solution on the substrate after coating and before sintering is 0.001-100mm, and the coating thickness of different areas is set according to the magnetic field intensity of the target gun of the magnetron sputtering device, and the coating thickness of the area is increased as the corresponding magnetic field intensity is increased.
3. The method of manufacturing according to claim 2, wherein the precursor solution is applied to the substrate by at least one method selected from the group consisting of inkjet printing, spray pyrolysis, electrofluidic printing, and 3D printing;
preferably, the precursor solution forms the target material by spray pyrolysis;
preferably, the heating temperature of the substrate in the coating process is controlled to be 50-500 ℃;
preferably, the precursor solution is sintered for 20-60min at the temperature of 500-1000 ℃ after being coated on the substrate.
4. The production method according to claim 1, wherein the target material is at least one selected from the group consisting of a metal oxide, a metal sulfide, a metal iodide, a metal selenide, an inorganic perovskite material, and a metal material;
preferably, the target material is a metal oxide selected from any one of a metal oxide conductor, a metal oxide semiconductor and a metal oxide insulator; wherein the metal oxide conductor is any one of indium tin oxide, fluorine-doped tin oxide, aluminum zinc oxide and indium zinc oxide; the metal oxide semiconductor is any one of indium oxide, indium zinc oxide, indium gallium zinc oxide, indium tin zinc oxide, rare earth element doped indium zinc oxide, nickel oxide and lithium doped nickel oxide; the metal oxide insulator is any one of silicon oxide, aluminum oxide, hafnium oxide, zirconium oxide and yttrium oxide.
5. The method according to claim 4, wherein when the target material is a metal oxide, the precursor solution is a solution formed from a metal inorganic salt or a metal organic compound corresponding to the target material;
preferably, the preparation process of the precursor solution comprises: mixing metal inorganic salt or metal organic compound with a solvent, and controlling the concentration of a precursor solution to be 0.05-10 mol/L;
preferably, the metal inorganic salt is selected from at least one of metal nitrate and metal chloride;
preferably, the solvent is water or an organic solvent;
more preferably, the organic solvent is selected from at least one of ethanol, ethylene glycol monomethyl ether, acetonitrile, and ethylene glycol.
6. The production method according to claim 1, wherein the substrate is a polished base selected from at least one of a metal, silicon, and a metal oxide;
preferably, the substrate is made of metal; more preferably, the substrate is made of at least one material selected from the group consisting of Ti, Al, and Cu.
7. The method according to claim 1, wherein the substrate is a metal base covered with a buffer layer, and the precursor solution is coated on the buffer layer;
preferably, the buffer layer is made of a metal oxide insulator material;
more preferably, the material of the buffer layer is selected from ZrO 2 、SiO 2 And Y 2 O 3 At least one of; the material of the metal substrate is selected from at least one of Ti, Al and Cu.
8. The method according to claim 1, wherein the substrate is a support layer with a polished surface, and the material of the support layer is at least one of silicon and metal oxide;
preferably, the preparation method further comprises: cooling the sintered material, and then connecting one side of the supporting layer, on which the target is not deposited, with the metal heat conduction layer through the bonding layer;
preferably, the material of the bonding layer is at least one selected from indium and its alloy, and tin and its alloy; the material of the metal heat conduction layer is at least one selected from Cu, Ti and Al.
9. A magnetron sputtering target material prepared by the preparation method according to any one of claims 1 to 8.
10. The magnetron sputtering target material according to claim 9, which is applied to magnetron sputtering for preparing a film.
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