A method for preparing a molybdenum oxide target

Abstract

This invention pertains to target preparation methods, specifically disclosing a method for preparing molybdenum oxide target material, comprising the following steps: (1) mixing MoO2 and Mo4O in a molar ratio of 1.4-1.7:1:0.4-0.8. 11 and Mo9O 26 Mixing to obtain a mixed powder, ball milling the mixed powder, binder and ethanol to obtain a uniform mixture, spray drying to obtain spherical powder, heat treatment, sieving to obtain a mixed powder; (2) subjecting the mixed powder to secondary oxygen supplementation in a muffle furnace to obtain oxygen-supplemented mixed powder; (3) pressing the oxygen-supplemented mixed powder into a billet; (4) drying the billet, placing it in a sleeve, vacuum sealing it, and then performing hot isostatic pressing treatment, removing the sleeve to obtain a crude molybdenum oxide target; (5) machining and cleaning the crude molybdenum oxide target to obtain a molybdenum oxide target. This invention provides a high-purity, high-density molybdenum oxide target.

Description

Technical Field

[0001] This invention pertains to target preparation methods, specifically relating to a method for preparing a molybdenum oxide target. Background Technology

[0002] Ceramic sputtering targets are targets made of ceramic materials used as raw materials in physical vapor deposition (PVD) processes such as magnetron sputtering and chemical vapor deposition (CVD). These targets play a crucial role in high-tech manufacturing, particularly in electronics, optics, data storage, decorative coatings, and the preparation of various functional thin films. They possess the following characteristics: High purity and stability: Ceramic sputtering targets require high purity to ensure the performance of the deposited thin film and exhibit good chemical stability under high-temperature conditions. Diverse functional properties: Depending on the type of ceramic sputtering target, thin films with various properties such as conductivity, insulation, transparency, wear resistance, and corrosion resistance can be prepared. Precision manufacturing: The preparation of ceramic sputtering targets requires precise powder metallurgy, hot pressing, and sintering processes to ensure the density, uniformity, and dimensional accuracy of the target. Wide range of industrial applications: From scratch-resistant coatings for smartphone screens and transparent conductive layers for solar cells to heat-resistant protective layers for aerospace components, ceramic sputtering targets are used in numerous high-tech fields.

[0003] The main types of ceramic sputtering targets include: Oxide sputtering targets: such as alumina (Al2O3), silicon dioxide (SiO2), zinc oxide (ZnO), indium tin oxide (ITO), titanium oxide (TiO2), and the aforementioned molybdenum oxide (MoO2 / MoO3), which are widely used in transparent conductive films, insulating layers, and protective coatings. Nitride sputtering targets: such as silicon nitride (Si3N4), titanium nitride (TiN), and aluminum nitride (AlN), which have good hardness and wear resistance and are often used in wear-resistant coatings, decorative coatings, and the manufacture of semiconductor devices. Carbide sputtering targets: such as silicon carbide (SiC), titanium carbide (TiC), and tungsten carbide (WC), which are used for hard coatings, cutting tools, and surface treatment of high-temperature components. Boride sputtering targets: such as titanium boride (TiB2) and hexagonal boron nitride (h-BN), which have high hardness and high melting point characteristics and are used for coatings with special properties.

[0004] Molybdenum oxide (MoOx) is a typical ceramic target material that plays an important role in thin film preparation technologies such as magnetron sputtering and chemical vapor deposition (CVD), mainly used to deposit high-quality molybdenum oxide thin films. These films have a wide range of applications in many high-tech fields, including but not limited to the following: (1) Semiconductor industry: In the semiconductor manufacturing process, molybdenum oxide films can be used as gate dielectric materials, barrier layers, or part of conductive layers. Due to their good thermal stability and electrical properties, they are suitable for advanced integrated circuit (IC) manufacturing. (2) Display technology: Molybdenum oxide can be used to produce transparent conductive layers in thin-film transistor (TFT) liquid crystal displays (LCDs) and flat panel displays (FPDs), especially as a substitute for ITO (indium tin oxide), because molybdenum oxide films also have high transmittance and conductivity. (3) Optoelectronics: In optoelectronic devices such as photovoltaic cells and photodetectors, molybdenum oxide films can be used as buffer layers or contact layers to optimize carrier transport and improve device efficiency. (4) Sensors and catalysts: The unique electrochemical and catalytic properties of molybdenum oxide make it an ideal material for making gas sensors, humidity sensors, and catalysts for certain chemical reactions. (5) Energy storage: In lithium-ion batteries and supercapacitors, molybdenum oxide thin films can be used as electrode materials to improve energy storage performance by utilizing their good capacitance characteristics and stability. (6) Electrochromic materials: Molybdenum oxide has an electrochromic effect, which means that it can change color under the action of an electric field. This property makes it a potential application in smart windows, displays and camouflage technology. (7) Research and development: Due to its special physical and chemical properties, molybdenum oxide targets are also an important material in materials science research, used to explore new electronic, optoelectronic and energy conversion materials.

[0005] In practical applications, the purity and density of molybdenum oxide sputtering targets are crucial to their performance and the quality of the final product. However, the purity and density of existing molybdenum oxide sputtering targets are not ideal, which affects their application in actual production. Summary of the Invention

[0006] The purpose of this invention is to provide a molybdenum oxide target material, its preparation method, and its application, which provides a high-purity, high-density molybdenum oxide target material.

[0007] To achieve the above objectives, the present invention provides the following technical solution:

[0008] A method for preparing a molybdenum oxide target includes the following steps:

[0009] (1) MoO2 and Mo4O in a molar ratio of 1.4-1.7:1:0.4-0.8 11 and Mo9O 26Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 600℃-650℃ at a heating rate of 4-6℃ / min and hold at that temperature for 3-4 hours. Sieve to obtain the mixed powder.

[0010] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 450℃-500℃ and the oxygen supplementation time is 30min-50min to obtain the oxygen-supplemented mixed powder.

[0011] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the pressure of the molding treatment is 60MPa-100MPa, the time is 100s-200s, and a blank is obtained;

[0012] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0013] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0014] Furthermore, the amount of the binder is 1-1.4% of the mass of the mixed powder.

[0015] Furthermore, the adhesive is polyvinyl alcohol.

[0016] Furthermore, the amount of ethanol used accounts for 55-57% of the sum of the mass of the mixed powder and ethanol.

[0017] Furthermore, the particle size of the mixed powder is 40μm-60μm.

[0018] Furthermore, the polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2-3:1:0.2-0.5, consisting of Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627), and Mw 146000-186000 (Merck, catalog number 363065).

[0019] Furthermore, the hot isostatic pressing treatment is carried out at a temperature of 500℃-600℃, a pressure of 50MPa-100MPa, and a time of 100min-200min.

[0020] The present invention provides a molybdenum oxide target material prepared by the aforementioned method.

[0021] Furthermore, the molybdenum oxide target material has a purity of ≥99.95% and a density of ≥99.2%.

[0022] This invention provides applications of molybdenum oxide sputtering targets.

[0023] Compared with existing technologies, the advantages and beneficial effects of this invention are as follows: This invention provides a molybdenum oxide target material, its preparation method, and its application. The molybdenum oxide target material has high purity and high density. This invention employs a ball milling process and adds a specific ratio of polyvinyl alcohol (PVA) to alter the microstructure of the molybdenum oxide powder layers, improving the density of the molybdenum oxide target material. The specific ratio of PVA helps improve powder dispersibility, reduce particle agglomeration, and simultaneously increases powder formability during subsequent molding processes, contributing to improved density of the final sintered product. In the preparation of the molybdenum oxide target material, molding and hot isostatic pressing (HIP) are two important molding and densification technologies, playing key roles in the early molding and late densification stages of the target material, respectively. Molding is the process of pressing molybdenum oxide powder through a mold. Hot isostatic pressing is a process that further densifies the material under high temperature and high pressure conditions, primarily aiming to eliminate porosity in the pressed blank and improve the material's density and properties. This invention further improves the purity and high density of molybdenum oxide targets by combining secondary oxygen replenishment, molding treatment and hot isostatic pressing. Detailed Implementation

[0024] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0025] The MoO2 and Mo4O used in the comparative examples and embodiments of this invention 11 and Mo9O 26 Its purity is 99.99%.

[0026] Example 1

[0027] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0028] (1) MoO2 and Mo4O in a molar ratio of 1.5:1:0.6 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 630℃ at a heating rate of 5℃ / min and hold at that temperature for 3.5h, sieve to obtain the mixed powder.

[0029] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 460℃ and the oxygen supplementation time is 40min to obtain the oxygen-supplemented mixed powder.

[0030] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the molding treatment pressure is 80MPa and the time is 150s, to obtain the blank;

[0031] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0032] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0033] The amount of binder used is 1.3% of the mass of the mixed powder.

[0034] The adhesive is polyvinyl alcohol.

[0035] The amount of ethanol used accounts for 56% of the total mass of the mixed powder and ethanol. The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2.4:1:0.3, namely Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627) and Mw 146000-186000 (Merck, catalog number 363065).

[0036] The particle size of the mixed powder is 40μm-60μm.

[0037] The hot isostatic pressing (HIP) treatment was performed at a temperature of 550℃, a pressure of 80MPa, and a time of 150min.

[0038] Example 2

[0039] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0040] (1) MoO2 and Mo4O in a molar ratio of 1.4:1:0.4 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 600℃ at a heating rate of 4℃ / min and hold at 600℃ for 4h, sieve to obtain mixed powder.

[0041] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 450℃ and the oxygen supplementation time is 30min to obtain the oxygen-supplemented mixed powder.

[0042] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the molding treatment pressure is 60MPa and the time is 100s, to obtain the blank;

[0043] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0044] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0045] The amount of binder used is 1% of the mass of the mixed powder.

[0046] The adhesive is polyvinyl alcohol.

[0047] The amount of ethanol used accounts for 55% of the total mass of the mixed powder and ethanol.

[0048] The particle size of the mixed powder is 40μm-60μm.

[0049] The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2:1:0.2, consisting of Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627), and Mw 146000-186000 (Merck, catalog number 363065).

[0050] The hot isostatic pressing (HIP) treatment was performed at a temperature of 500℃, a pressure of 50MPa, and a time of 100min.

[0051] Example 3

[0052] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0053] (1) MoO2 and Mo4O in a molar ratio of 7:1:0.8 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 650℃ at a heating rate of 6℃ / min and hold at 6℃ for 4 hours, sieve to obtain mixed powder.

[0054] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 500℃ and the oxygen supplementation time is 50min to obtain the oxygen-supplemented mixed powder.

[0055] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the pressure of the molding treatment is 100MPa and the time is 200s, to obtain the blank;

[0056] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0057] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0058] The amount of binder used is 1.4% of the mass of the mixed powder.

[0059] The adhesive is polyvinyl alcohol.

[0060] The amount of ethanol used accounts for 57% of the total mass of the mixed powder and ethanol.

[0061] The particle size of the mixed powder is 40μm-60μm.

[0062] The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 3:1:0.5, consisting of Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627), and Mw 146000-186000 (Merck, catalog number 363065).

[0063] The hot isostatic pressing (HIP) treatment was performed at a temperature of 600℃, a pressure of 100MPa, and a time of 200min.

[0064] Example 4

[0065] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0066] (1) MoO2 and Mo4O in a molar ratio of 1.4:1:0.8 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 600℃ at a heating rate of 6℃ / min and hold at 6℃ for 4h, sieve to obtain mixed powder.

[0067] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 500℃ and the oxygen supplementation time is 30min to obtain the oxygen-supplemented mixed powder.

[0068] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the molding treatment pressure is 100MPa and the time is 100s, to obtain the blank;

[0069] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0070] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0071] The amount of binder used is 1.4% of the mass of the mixed powder.

[0072] The adhesive is polyvinyl alcohol.

[0073] The amount of ethanol used accounts for 55% of the total mass of the mixed powder and ethanol.

[0074] The particle size of the mixed powder is 40μm-60μm.

[0075] The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 3:1:0.2, consisting of Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627), and Mw 146000-186000 (Merck, catalog number 363065).

[0076] The hot isostatic pressing (HIP) treatment was performed at a temperature of 600℃, a pressure of 50MPa, and a time of 200min.

[0077] Comparative Example 1

[0078] The difference between this comparative example and Example 1 is that the molar ratio of MoO2 and Mo4O is 1:1:1. 11 and Mo9O 26 mix.

[0079] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0080] (1) MoO2 and Mo4O in a molar ratio of 1:1:1 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 630℃ at a heating rate of 5℃ / min and hold at that temperature for 3.5h, sieve to obtain the mixed powder.

[0081] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 460℃ and the oxygen supplementation time is 40min to obtain the oxygen-supplemented mixed powder.

[0082] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the molding treatment pressure is 80MPa and the time is 150s, to obtain the blank;

[0083] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0084] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0085] The amount of binder used is 1.3% of the mass of the mixed powder.

[0086] The adhesive is polyvinyl alcohol.

[0087] The amount of ethanol used accounts for 56% of the total mass of the mixed powder and ethanol. The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2.4:1:0.3, namely Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627) and Mw 146000-186000 (Merck, catalog number 363065).

[0088] The particle size of the mixed powder is 40μm-60μm.

[0089] The hot isostatic pressing (HIP) treatment was performed at a temperature of 550℃, a pressure of 80MPa, and a time of 150min.

[0090] Comparative Example 2

[0091] The difference between this comparative example and Example 1 is that the molar ratio of MoO2 and Mo4O is 0.4:1:1.2. 11 and Mo9O 26 mix.

[0092] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0093] (1) MoO2 and Mo4O in a molar ratio of 0.4:1:1.2 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 630℃ at a heating rate of 5℃ / min and hold at that temperature for 3.5h, sieve to obtain the mixed powder.

[0094] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 460℃ and the oxygen supplementation time is 40min to obtain the oxygen-supplemented mixed powder.

[0095] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the molding treatment pressure is 80MPa and the time is 150s, to obtain the blank;

[0096] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0097] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0098] The amount of binder used is 1.3% of the mass of the mixed powder.

[0099] The adhesive is polyvinyl alcohol.

[0100] The amount of ethanol used accounts for 56% of the total mass of the mixed powder and ethanol. The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2.4:1:0.3, namely Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627) and Mw 146000-186000 (Merck, catalog number 363065).

[0101] The particle size of the mixed powder is 40μm-60μm.

[0102] The hot isostatic pressing (HIP) treatment was performed at a temperature of 550℃, a pressure of 80MPa, and a time of 150min.

[0103] Comparative Example 3

[0104] The difference between this comparative example and Example 1 is that the molar ratio of MoO2 and Mo4O is 1:1.7:0.5. 11 and Mo9O 26 mix.

[0105] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0106] (1) MoO2 and Mo4O in a molar ratio of 1:1.7:0.5 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 630℃ at a heating rate of 5℃ / min and hold at that temperature for 3.5h, sieve to obtain the mixed powder.

[0107] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 460℃ and the oxygen supplementation time is 40min to obtain the oxygen-supplemented mixed powder.

[0108] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the molding treatment pressure is 80MPa and the time is 150s, to obtain the blank;

[0109] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0110] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0111] The amount of binder used is 1.3% of the mass of the mixed powder.

[0112] The adhesive is polyvinyl alcohol.

[0113] The amount of ethanol used accounts for 56% of the total mass of the mixed powder and ethanol. The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2.4:1:0.3, namely Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627) and Mw 146000-186000 (Merck, catalog number 363065).

[0114] The particle size of the mixed powder is 40μm-60μm.

[0115] The hot isostatic pressing (HIP) treatment was performed at a temperature of 550℃, a pressure of 80MPa, and a time of 150min.

[0116] Comparative Example 4

[0117] The difference between this comparative example and Example 1 is that the polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 1:1:1, containing Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627), and Mw 146000-186000 (Merck, catalog number 363065).

[0118] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0119] (1) MoO2 and Mo4O in a molar ratio of 1.5:1:0.6 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 630℃ at a heating rate of 5℃ / min and hold at that temperature for 3.5h, sieve to obtain the mixed powder.

[0120] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 460℃ and the oxygen supplementation time is 40min to obtain the oxygen-supplemented mixed powder.

[0121] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the molding treatment pressure is 80MPa and the time is 150s, to obtain the blank;

[0122] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0123] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0124] The amount of binder used is 1.3% of the mass of the mixed powder.

[0125] The adhesive is polyvinyl alcohol.

[0126] The amount of ethanol used accounts for 56% of the total mass of the mixed powder and ethanol. The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 1:1:1, consisting of Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627), and Mw 146000-186000 (Merck, catalog number 363065).

[0127] The particle size of the mixed powder is 40μm-60μm.

[0128] The hot isostatic pressing (HIP) treatment was performed at a temperature of 550℃, a pressure of 80MPa, and a time of 150min.

[0129] Comparative Example 5

[0130] The difference between this comparative example and Example 1 is that the pressing conditions are different.

[0131] A molybdenum oxide target material, the preparation method of which includes the following steps:

[0132] (1) MoO2 and Mo4O in a molar ratio of 1.5:1:0.6 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol evenly, spray dry to obtain spherical powder, heat to 700℃ at a heating rate of 8℃ / min and hold at 700℃ for 2h, sieve to obtain mixed powder;

[0133] (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 400℃ and the oxygen supplementation time is 20min to obtain the oxygen-supplemented mixed powder.

[0134] (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the pressure of the molding treatment is 30MPa, the time is 300s, and a blank is obtained;

[0135] (4) After drying the billet, it is put into the sleeve and vacuum-sealed. Then, it is subjected to hot isostatic pressing. After removing the sleeve, the crude molybdenum oxide target material is obtained.

[0136] (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain the molybdenum oxide target material.

[0137] The amount of binder used is 1.3% of the mass of the mixed powder.

[0138] The adhesive is polyvinyl alcohol.

[0139] The amount of ethanol used accounts for 56% of the total mass of the mixed powder and ethanol. The polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2.4:1:0.3, namely Mw 13000-23000 (Merck, catalog number 363170), Mw 9000-10000 (Merck, catalog number 360627) and Mw 146000-186000 (Merck, catalog number 363065).

[0140] The particle size of the mixed powder is 40μm-60μm.

[0141] The hot isostatic pressing (HIP) treatment was performed at a temperature of 650℃, a pressure of 40MPa, and a time of 70min.

[0142] Performance testing

[0143] The purity and density of the molybdenum oxide targets prepared in Examples 1-4 and Comparative Examples 1-5 were tested. The results are shown in Table 1, which is a table of purity and density performance tests.

[0144] Table 1. Test results for purity and density:

[0145]

[0146] The results show that the molybdenum oxide targets prepared in Examples 1-4 of this invention have high purity and high density. Changing the preparation conditions leads to varying degrees of performance degradation. This invention employs a ball milling process and adds a specific ratio of polyvinyl alcohol (PVA), which alters the microstructure of the molybdenum oxide powder layers and improves the density of the molybdenum oxide target. The specific ratio of PVA helps improve powder dispersibility, reduces particle agglomeration, and increases powder formability during subsequent molding, contributing to improved density of the final sintered product. In Comparative Example 4, changing the PVA ratio resulted in a decrease in density. This invention further improves the purity and high density of the molybdenum oxide target by combining secondary oxygen supplementation, molding treatment, and hot isostatic pressing. In Comparative Example 5, changing the treatment conditions resulted in a significant decrease in both the purity and high density of the molybdenum oxide target.

[0147] The above description represents the preferred embodiments of the present invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing a molybdenum oxide target, characterized in that, Includes the following steps: (1) MoO2 and Mo4O in a molar ratio of 1.4-1.7:1:0.4-0.8 11 and Mo9O 26 Mix to obtain a mixed powder. Ball mill the mixed powder, binder and ethanol to obtain a uniform mixture. Spray dry to obtain spherical powder. Heat to 600℃-650℃ at a heating rate of 4-6℃ / min and hold at that temperature for 3-4 hours. Sieve to obtain the mixed powder. The particle size of the mixed powder is 40μm-60μm. (2) The mixed powder is subjected to secondary oxygen supplementation in a muffle furnace. The temperature inside the muffle furnace is 450℃-500℃ and the oxygen supplementation time is 30min-50min to obtain the oxygen-supplemented mixed powder. (3) Press the oxygenated mixed powder into a blank, specifically: put the oxygenated mixed powder into a mold for molding treatment, the pressure of the molding treatment is 60MPa-100MPa, the time is 100s-200s, and a blank is obtained; (4) After drying the billet, put it into the sleeve and vacuum weld it. Then perform hot isostatic pressing treatment. After removing the sleeve, the crude molybdenum oxide target material is obtained. The temperature of hot isostatic pressing treatment is 500℃-600℃, the pressure is 50MPa-100MPa, and the time is 100min-200min. (5) The crude molybdenum oxide target material is mechanically processed and cleaned to obtain a molybdenum oxide target material with a purity ≥99.95% and a density ≥99.2%; The binder is polyvinyl alcohol; the polyvinyl alcohol is a blend of polyvinyl alcohol with a mass ratio of 2-3:1:0.2-0.5, consisting of polyvinyl alcohol with a mass of 13000-23000, polyvinyl alcohol with a mass of 9000-10000, and polyvinyl alcohol with a mass of 146000-186000; the amount of binder used is 1-1.4% of the mass of the mixed powder.

2. The method for preparing molybdenum oxide target material according to claim 1, characterized in that, The amount of ethanol used accounts for 55-57% of the total mass of the mixed powder and ethanol.

3. The molybdenum oxide target material prepared by the preparation method according to any one of claims 1-2.

4. Application of the molybdenum oxide target as described in claim 3.

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