Niobium-aluminum alloy target as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of aluminum powder alloy target materials, and particularly relates to a niobium-aluminum alloy target material and a preparation method and application thereof. The niobium-aluminum alloy target material comprises the following raw materials in atomic percent: 5%-10% of niobium and 90%-95% of aluminum. The preparation method comprises the following steps that Nb-MOF powder and aluminum powder are mixed and sintered after being subjected to cold isostatic pressing, and the niobium-aluminum alloy target material is obtained. According to the preparation method of the niobium-aluminum alloy target material, the Nb-MOF powder is adopted as the niobium source, the Nb-MOF powder is of a porous structure with the high specific surface area and the high porosity, the aluminum powder is easily embedded into the structure of the Nb-MOF powder during mixing, the niobium source and the aluminum powder are evenly mixed, and the niobium-aluminum alloy target material obtained after sintering is high in density and low in oxygen content.

Description

Technical Field

[0001] The invention belongs to the technical field of aluminum powder alloy target materials, and specifically relates to a niobium aluminum alloy target material and a preparation method and application thereof. Background Art

[0002] Niobium aluminum alloy targets have the advantages of high melting point, low density, good mechanical properties, excellent conductivity, good corrosion resistance, and easy processing and forming. These advantages make niobium aluminum alloy targets have broad application prospects and market demand in many fields. The density of the target has a great influence on its performance, and the density is closely related to its preparation method. The existing preparation methods of niobium aluminum alloy targets mainly include hot pressing sintering, powder metallurgy, chemical vapor deposition (CVD) and physical vapor deposition (PVD). Among them, hot pressing sintering and powder metallurgy optimize the density of the target by controlling parameters such as sintering temperature, pressure and time. In addition, the density of niobium aluminum alloy targets is also affected by the alloy composition. Different proportions of niobium and aluminum powder elements will cause changes in the microstructure and phase composition of the alloy, thereby affecting the density.

[0003] However, the density of existing niobium aluminum alloy target products still cannot meet the demand. Summary of the invention

[0004] In order to solve the above problems, the present invention provides a niobium-aluminum alloy target material and a preparation method and application thereof. The density of the niobium-aluminum alloy target material is above 99.5%.

[0005] The present invention is achieved through the following technical solutions:

[0006] In a first aspect, the present invention provides a niobium aluminum alloy target material, comprising the following raw materials in atomic percentage:

[0007] 5%~10% niobium, 90%~95% aluminum.

[0008] The niobium aluminum alloy target material provided by the invention has a density of 99.5% to 99.9% and an oxygen content of 15ppm to 30ppm.

[0009] In a second aspect, the present invention provides a method for preparing the above-mentioned niobium aluminum alloy target, comprising the following steps:

[0010] The Nb-MOF powder and the aluminum powder are mixed, and then cold isostatic pressing and sintering are performed to obtain a niobium aluminum alloy target;

[0011] The Nb-MOF powder is prepared by reacting niobium chloride and pyridinetetracarboxylic acid ethanol solution.

[0012] The preparation method of the niobium aluminum alloy target provided by the present invention adopts Nb-MOF powder as the niobium source. The Nb-MOF powder is a porous structure with high specific surface area and high porosity. When mixing, aluminum powder is easily embedded in the structure of the Nb-MOF powder, so that the niobium source and the aluminum powder are mixed evenly. The niobium aluminum alloy target obtained after sintering has high density and low oxygen content.

[0013] In some possible implementations, preparing the Nb-MOF powder comprises the following steps:

[0014] The niobium chloride and pyridinetetracarboxylic acid ethanol solution are mixed to undergo a solvothermal reaction, and then filtered and dried to obtain Nb-MOF;

[0015] The Nb-MOF is ground to obtain Nb-MOF powder.

[0016] In some possible implementations, the molar ratio of Nb to aluminum powder in the Nb-MOF powder is 1:(32-65).

[0017] In some possible implementations, the mixing process includes the following steps: mixing the Nb-MOF powder and the aluminum powder and then ball milling them.

[0018] In some possible implementations, during the ball milling, the ball milling atmosphere is argon, the ball-to-material ratio is 1:0.5-4, the rotation speed is 50 rpm-100 rpm, and the ball milling time is 24 h-36 h.

[0019] In some possible implementations, during the cold isostatic pressing, a pressing pressure of 190 MPa to 220 MPa is applied.

[0020] In some possible implementations, during the cold isostatic pressing, the holding time is 10 min to 15 min.

[0021] In some possible implementations, during the cold isostatic pressing, after maintaining the pressure, the pressure is reduced to normal pressure at a rate of 15 MPa / min to 20 MPa / min to obtain a niobium aluminum alloy compact.

[0022] In some possible implementations, the sintering includes hydrogen atmosphere sintering and vacuum sintering.

[0023] In some possible implementations, the sintering temperature of the hydrogen atmosphere sintering is 1200°C to 1400°C.

[0024] In some possible implementations, the holding time of the hydrogen atmosphere sintering is 5 h to 7 h.

[0025] In some possible implementations, the hydrogen flow rate of the hydrogen atmosphere sintering is 4m 3 / h~6m 3 / h.

[0026] In some possible implementations, the vacuum degree of the vacuum sintering is 10 -5 Pa~10 -3 Pa.

[0027] In some possible implementations, the sintering temperature of the vacuum sintering is 1500°C to 1600°C.

[0028] In some possible implementations, the insulation time of the vacuum sintering is 5 hours to 8 hours.

[0029] In a third aspect, the present invention provides an application of the niobium aluminum alloy target provided by the present invention in the electrical field, the optical field, the flat panel display field or the photovoltaic field. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is described and illustrated in conjunction with the embodiments below. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. Based on the embodiments provided by the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work belong to the scope of protection of the present invention.

[0031] Obviously, the following descriptions are only some examples or embodiments of the present invention, and for those of ordinary skill in the art, the present invention can also be applied to other similar scenarios without creative work. In addition, it can also be understood that although the efforts made in such a development process may be complex and lengthy, for those of ordinary skill in the art related to the contents disclosed in the present invention, some changes in design, manufacturing or production based on the technical contents disclosed in the present invention are just conventional technical means, and should not be understood as the contents disclosed in the present invention being insufficient.

[0032] However, unnecessary detailed descriptions may be omitted. For example, detailed descriptions of well-known matters and repeated descriptions of substantially the same structures may be omitted. This is to avoid the following description from becoming unnecessarily lengthy and to facilitate understanding by those skilled in the art. In addition, the following description is provided for those skilled in the art to fully understand the present invention and is not intended to limit the subject matter described in the claims.

[0033] If not otherwise specified, all embodiments and optional embodiments of the present invention may be combined with each other to form a new technical solution, and all technical features and optional technical features of the present invention may be combined with each other to form a new technical solution.

[0034] The density of the target material affects the sputtering rate and efficiency, thus affecting the quality, film performance and cost of the sputtering coating (a high-density target material can reduce waste and loss during the sputtering process, thereby reducing production costs), and further affects the service life of the target material (a high-density target material is not prone to cracking and peeling during use, thereby extending the service life of the target material; a target material with poor density may be more susceptible to thermal and mechanical stress during use, causing the target material to fail prematurely). It can be seen that the density of the target material is extremely important in the sputtering coating process. In order to ensure the quality and efficiency of sputtering coating, as well as to reduce production costs and extend the service life of the target material, it is necessary to select a target material with high density.

[0035] Nb-MOF powder material (metal organic framework material, with niobium as the central metal ion) is a new type of porous material. It has the advantages of high specific surface area, porous structure and environmental friendliness. Although it has been widely used in many fields such as catalysts, it has not yet been used in the preparation of niobium aluminum alloy targets.

[0036] In order to achieve the effective use of Nb-MOF powder materials in niobium aluminum alloy targets and improve the density of niobium aluminum alloy targets, the embodiments of the present invention provide a niobium aluminum alloy target and its preparation method and application. The niobium aluminum alloy target provided by the embodiment of the present invention has a density of 99.5% to 99.9% and an oxygen content of 15ppm to 30ppm. In the preparation method of the niobium aluminum alloy target provided by the embodiment of the present invention, Nb-MOF powder is used as the niobium source. During mixing, aluminum powder is easily embedded in the structure of Nb-MOF powder, so that the niobium source and aluminum powder are mixed evenly. The internal structure of the niobium aluminum alloy target obtained after sintering has no defects such as pores, cracks, delamination, inclusions, etc., and has high density and low oxygen content.

[0037] The following is a detailed description of a niobium aluminum alloy target material and a preparation method and application thereof according to an embodiment of the present invention.

[0038]

Niobium aluminum alloy target

[0039] A first aspect of an embodiment of the present invention provides a niobium aluminum alloy target material, comprising the following raw materials in atomic percentage:

[0040] 5%~10% niobium, 90%~95% aluminum.

[0041] The niobium aluminum alloy target provided by the embodiment of the present invention has a density of 99.5% to 99.9% and an oxygen content of 15ppm to 30ppm.

[0042] In the embodiment, the atomic percentage content of niobium is 5% to 10%, which can be 5%, 8%, 10% or other typical but non-limiting atomic percentage content or any range between two atomic percentage content. In this case, niobium can refine the grains, increase the density and hardness of the target material, and thus improve the wear resistance and corrosion resistance.

[0043] In some embodiments, the raw material of the niobium aluminum alloy target further includes at least one of vanadium, titanium, tantalum, lanthanum, and cerium.

[0044] In some specific embodiments, the atomic percentage content of vanadium is 0.1% to 5%.

[0045] In some specific embodiments, the atomic percentage content of titanium is 0.1% to 5%.

[0046] In some specific embodiments, the atomic percentage content of tantalum is 0.1% to 5%.

[0047] In some specific embodiments, the atomic percentage content of lanthanum is 0.1% to 5%.

[0048] In some specific embodiments, the atomic percentage content of cerium is 0.1% to 5%.

[0049]

Preparation method of niobium aluminum alloy target

[0050] A second aspect of an embodiment of the present invention provides a method for preparing the above-mentioned niobium aluminum alloy target, comprising the following steps:

[0051] S10. The Nb-MOF powder and the aluminum powder are mixed, and then cold isostatically pressed and sintered to obtain a niobium aluminum alloy target;

[0052] Nb-MOF powder is prepared by reacting niobium chloride and pyridinetetracarboxylic acid ethanol solution.

[0053] The preparation method of the niobium aluminum alloy target provided in the embodiment of the present invention adopts Nb-MOF powder as the niobium source. The Nb-MOF powder is a porous structure with high specific surface area and high porosity. When mixing, the aluminum powder is easily embedded in the structure of the Nb-MOF powder, so that the niobium source and the aluminum powder are mixed evenly. The niobium aluminum alloy target obtained after sintering has high density and low oxygen content.

[0054] In some embodiments, in the above step S10, preparing Nb-MOF powder includes the following steps:

[0055] S101. Mix niobium chloride and pyridinetetracarboxylic acid ethanol solution to carry out a solvothermal reaction, filter and dry to obtain Nb-MOF.

[0056] S102. Grind Nb-MOF to obtain Nb-MOF powder.

[0057] In some embodiments, in the above step S101, the molar ratio of niobium chloride to pyridinetetracarboxylic acid is 1:(6-8). In this case, niobium metal ions and pyridinetetracarboxylic acid form a Nb-MOF material with six or more coordination.

[0058] In some embodiments, in the above step S101, the temperature of the solvothermal reaction is 120° C. to 150° C., and the time is 72 h to 96 h. In this case, niobium chloride and pyridinetetracarboxylic acid react fully to form Nb-MOF material, thereby improving the yield.

[0059] In some embodiments, in the above step S101, the filtration treatment includes the steps of: filtering the solvent thermal reaction product and washing it with clean water for 2 to 5 times to obtain a filter residue.

[0060] In some embodiments, in the above step S101, the drying temperature is 150°C to 180°C and the drying time is 6h to 12h.

[0061] In some embodiments, in the above step S10, the molar ratio of Nb to aluminum powder in the Nb-MOF powder is 1:(32-65).

[0062] In some embodiments, in the above step S10, the average particle size of the aluminum powder is 10 nm to 30 nm.

[0063] In some embodiments, in the above step S10, the mixing process includes the following steps:

[0064] S103. Mix the Nb-MOF powder and aluminum powder and then ball mill them.

[0065] In some embodiments, in the above step S103, the ball milling atmosphere is argon, the ball-to-material ratio is 1:(0.5-4), the rotation speed is 50 rpm-100 rpm, and the ball milling time is 24h-36h. In this case, the aluminum powder is fully embedded in and fills the structure of the Nb-MOF powder, and the Nb-MOF powder can be fully dispersed in the aluminum powder, so that the Nb-MOF powder and the aluminum powder are fully mixed, thereby providing a basis for the subsequent improvement of the density of the niobium aluminum alloy target.

[0066] In some embodiments, in the above step S103, the grinding balls are stainless steel grinding balls. In this case, the stainless steel grinding balls do not produce harmful substances during use and are environmentally friendly. At the same time, due to their good corrosion resistance and wear resistance, the stainless steel grinding balls are not easily damaged during use, reducing the potential safety hazards caused by damage to the grinding media.

[0067] In some embodiments, in the above step S102, the grinding balls include medium grinding balls and small grinding balls, the diameter of the medium grinding balls is 20 mm to 30 mm, and the diameter of the small grinding balls is 10 mm to 15 mm. In this case, the grinding balls include medium balls and small balls to increase the total surface area of ​​grinding and improve the grinding accuracy.

[0068] In some specific embodiments, the number ratio of the medium grinding balls to the small grinding balls is 1:(10-20). In exemplary embodiments, the ratio may be 1:10, 1:20, or other typical but non-limiting ratios or a range between any two ratios.

[0069] In some embodiments, in the above step S103, the ball milling method is dry ball milling.

[0070] Dry ball milling is a method of preparing powder without the involvement of liquid.

[0071] In some embodiments, in the above step S10, during the cold isostatic pressing, the pressing pressure applied is 190 MPa to 220 MPa.

[0072] In some embodiments, in the above step S10, during the cold isostatic pressing, the holding time is 10 min to 15 min.

[0073] In some embodiments, in the above step S10, during the cold isostatic pressing, after the pressure is maintained, the pressure is reduced to normal pressure at a rate of 15 MPa / min to 20 MPa / min to obtain a niobium aluminum alloy billet.

[0074] Normal pressure refers to the value of atmospheric pressure under standard conditions on the surface of the earth. The specific value of the pressure varies slightly depending on the altitude, and is generally 101.325 kPa.

[0075] In some embodiments, in the above step S10, sintering includes hydrogen atmosphere sintering and vacuum sintering. In this case, during hydrogen atmosphere sintering, the organic ligand will decompose during the heating process, and the oxygen element will be separated from the system under the hydrogen atmosphere, but some oxygen elements and / or carbon elements will remain; and niobium reduction and in-situ metallurgical bonding of niobium and aluminum metal will be promoted to improve the density of the target material; and the carbon element generated during the decomposition of the organic ligand may also combine with the oxygen element in the niobium aluminum alloy compact to achieve further removal of the oxygen element, so that the oxygen content of the prepared niobium aluminum alloy target is significantly reduced. During vacuum sintering, the oxygen elements and / or carbon elements that may remain in the system during hydrogen atmosphere sintering and the hydrogen elements that are doped are removed, further improving the density of the target material.

[0076] In some embodiments, the sintering temperature of the hydrogen atmosphere sintering is 1200°C to 1400°C.

[0077] In some embodiments, the holding time of hydrogen atmosphere sintering is 5 hours to 7 hours.

[0078] In some embodiments, the hydrogen flow rate of hydrogen atmosphere sintering is 4m 3 / h~6m 3 / h.

[0079] In some embodiments, the vacuum degree of vacuum sintering is 10 -5 Pa~10 -3 Pa.

[0080] In some embodiments, the sintering temperature of the vacuum sintering is 1500°C to 1600°C.

[0081] In some embodiments, the holding time of vacuum sintering is 5 hours to 8 hours.

[0082] In some other embodiments, a method for preparing a niobium aluminum alloy target is provided, comprising the following steps:

[0083] S11. The raw material powders are mixed and then cold isostatically pressed and sintered to obtain a niobium aluminum alloy target;

[0084] The raw material powder includes Nb-MOF powder and aluminum powder, and also includes at least one metal or metal element compound of vanadium, titanium, tantalum, lanthanum and cerium.

[0085] In other embodiments, the metal element compound includes a metal oxide.

[0086]

application

[0087] A third aspect of the embodiments of the present invention provides an application of the niobium aluminum alloy target provided by the embodiments of the present invention in the electrical field, the optical field, the flat panel display field or the photovoltaic field.

[0088] The following is further described in conjunction with specific embodiments.

[0089] The average particle size of the aluminum powder involved in the embodiment and the comparative example is 20 nm;

[0090] The molar ratio of Nb to aluminum powder in the Nb-MOF powder in the examples and comparative examples is 1:50.

[0091] Example 1

[0092] Example 1 provides a method for preparing a niobium aluminum alloy target, the steps are as follows:

[0093] S1-1. After mixing Nb-MOF powder and aluminum powder, ball milling is performed using stainless steel medium grinding balls (diameter 25 mm) and small grinding balls (diameter 15 mm), with the ratio of the number of medium grinding balls to the number of small grinding balls being 1:10; the ball milling atmosphere is argon, the ball-to-material ratio is 1:1, the rotation speed is 80 rpm, and the ball milling time is 30 h.

[0094] S1-2. The ball-milled product is subjected to cold isostatic pressing to form a niobium-aluminum alloy billet; during the cold isostatic pressing, a pressing pressure of 190 MPa is applied and the holding time is 15 min; after holding, the pressure is reduced to normal pressure at a rate of 15 MPa / min.

[0095] S1-3. The niobium aluminum alloy billet was sintered in a hydrogen atmosphere. The sintering temperature of the hydrogen atmosphere was 1300°C, the holding time was 6h, and the hydrogen flow rate was 5m 3 / h.

[0096] S1-4. The niobium aluminum alloy billet is sintered in a hydrogen atmosphere and then vacuum sintered. The vacuum degree of vacuum sintering is 10 -5 Pa, sintering temperature is 1550℃, and holding time is 6h.

[0097] Example 2

[0098] Example 2 provides a method for preparing a niobium aluminum alloy target, the steps are as follows:

[0099] S2-1. After mixing Nb-MOF powder and aluminum powder, ball milling was performed using stainless steel medium grinding balls (diameter 20 mm) and small grinding balls (diameter 10 mm), with the ratio of medium grinding balls to small grinding balls being 1:20; the ball milling atmosphere was argon, the ball-to-material ratio was 1:4, the rotation speed was 100 rpm, and the ball milling time was 36 h.

[0100] S2-2. The ball-milled product was subjected to cold isostatic pressing to form a niobium-aluminum alloy billet; during the cold isostatic pressing, a pressing pressure of 220 MPa was applied and the holding time was 13 min; after holding, the pressure was reduced to normal pressure at a rate of 20 MPa / min.

[0101] S2-3. The niobium aluminum alloy billet was sintered in a hydrogen atmosphere. The sintering temperature of the hydrogen atmosphere was 1400°C, the holding time was 7h, and the hydrogen flow rate was 6m 3 / h.

[0102] S2-4. The niobium aluminum alloy billet is sintered in a hydrogen atmosphere and then vacuum sintered. The vacuum degree of vacuum sintering is 10 -3 Pa, sintering temperature is 1600℃, and holding time is 8h.

[0103] Example 3

[0104] Example 3 provides a method for preparing a niobium aluminum alloy target, the steps are as follows:

[0105] S3-1. After mixing Nb-MOF powder and aluminum powder, ball milling is performed using stainless steel medium grinding balls (diameter 30 mm) and small grinding balls (diameter 15 mm), with the ratio of medium grinding balls to small grinding balls being 1:15; the ball milling atmosphere is argon, the ball-to-material ratio is 1:0.5, the rotation speed is 50 rpm, and the ball milling time is 28 h.

[0106] S3-2. The ball-milled product is subjected to cold isostatic pressing to form a niobium-aluminum alloy billet; during the cold isostatic pressing, a pressing pressure of 200 MPa is applied and the holding time is 10 min; after holding, the pressure is reduced to normal pressure at a rate of 18 MPa / min.

[0107] S3-3. The niobium aluminum alloy billet was sintered in a hydrogen atmosphere. The sintering temperature of the hydrogen atmosphere was 1200°C, the holding time was 5h, and the hydrogen flow rate was 4m 3 / h.

[0108] S3-4. The niobium aluminum alloy billet is sintered in a hydrogen atmosphere and then vacuum sintered. The vacuum degree of vacuum sintering is 10 -5 Pa, sintering temperature is 1500℃, and holding time is 5h.

[0109] Example 4

[0110] Example 4 provides a method for preparing a niobium aluminum alloy target, the steps are as follows:

[0111] S4-1. Preparation of Nb-MOF powder:

[0112] S4-1-1. A pyridinetetracarboxylic acid ethanol solution of niobium chloride is subjected to a solvothermal reaction; wherein the molar ratio of niobium chloride to pyridinetetracarboxylic acid is 1:7; the temperature of the solvothermal reaction is 130°C and the time is 84h.

[0113] S4-1-2. Filter the solvent thermal reaction product and wash it with clean water three times to obtain a filter residue.

[0114] S4-1-3. Dry the filter residue at 170°C for 10 h to obtain Nb-MOF.

[0115] S4-1-4. Grind Nb-MOF to obtain Nb-MOF powder.

[0116] S4-2. After mixing Nb-MOF powder and aluminum powder, ball milling is performed using stainless steel medium grinding balls (diameter 20 mm) and small grinding balls (diameter 15 mm), with the ratio of the number of medium grinding balls to the number of small grinding balls being 1:15; the ball milling atmosphere is argon, the ball-to-material ratio is 1:2, the rotation speed is 100 rpm, and the ball milling time is 30 h.

[0117] S3-2. The ball-milled product is subjected to cold isostatic pressing to form a niobium-aluminum alloy billet; during the cold isostatic pressing, a pressing pressure of 210 MPa is applied and the holding time is 10 min; after holding, the pressure is reduced to normal pressure at a rate of 15 MPa / min.

[0118] S3-3. The niobium aluminum alloy billet was sintered in a hydrogen atmosphere. The sintering temperature of the hydrogen atmosphere was 1300°C, the holding time was 7h, and the hydrogen flow rate was 6m 3 / h.

[0119] S3-4. The niobium aluminum alloy billet is sintered in a hydrogen atmosphere and then vacuum sintered. The vacuum degree of vacuum sintering is 10 -4 Pa, sintering temperature is 1600℃, and holding time is 8h.

[0120] Example 5

[0121] This embodiment also provides a method for preparing a niobium aluminum alloy target, the steps of which are basically the same as those of embodiment 1, except that:

[0122] In step S1-1, Nb-MOF powder, aluminum powder and lanthanum powder are mixed; the average particle size of the lanthanum powder is 30 nm.

[0123] Example 6

[0124] This embodiment also provides a method for preparing a niobium aluminum alloy target, the steps of which are basically the same as those of embodiment 1, except that:

[0125] In step S1-1, Nb-MOF powder, aluminum powder and tantalum powder are mixed; the average particle size of the tantalum powder is 40 nm.

[0126] Example 7

[0127] Example 7 provides a niobium aluminum alloy target material, which is composed of the following raw materials in atomic percentage:

[0128] 5% niobium, 2% tantalum, 1% cerium, 92% aluminum.

[0129] This embodiment also provides a method for preparing a niobium aluminum alloy target, the steps of which are basically the same as those of embodiment 1, except that:

[0130] In step S1-1, Nb-MOF powder, aluminum powder, tantalum powder and cerium powder are mixed; the average particle size of the tantalum powder and the cerium powder is 20 nm.

[0131] Comparative Example 1

[0132] This comparative example also provides a method for preparing a niobium aluminum alloy target, and the steps are basically the same as those in Example 1, except that:

[0133] Niobium powder and aluminum powder are used for ball milling, and the average particle size of the niobium powder is 20nm.

[0134] Comparative Example 2

[0135] Comparative Example 2 provides a niobium aluminum alloy target material, and the raw material composition is the same as that of Example 1.

[0136] This comparative example also provides a method for preparing a niobium aluminum alloy target, and the steps are basically the same as those in Example 1, except that:

[0137] The niobium chloride and aluminum powders were mixed and then ball milled.

[0138] In order to verify the advancement of a niobium aluminum alloy target material and a preparation method thereof provided in an embodiment of the present invention, the density and oxygen content of the niobium aluminum alloy targets prepared in the embodiment and the comparative example were tested, and the results are shown in Table 1 below.

[0139] Table 1

[0140] -- Density(%) Oxygen content (ppm) Example 1 99.60 30 Example 2 99.50 28 Example 3 99.70 15 Example 4 99.70 25 Example 5 99.80 17 Example 6 99.80 21 Example 7 99.90 23 Comparative Example 1 99.10 55 Comparative Example 2 99.30 45

[0141] From Table 1 above, at least the following conclusions can be drawn:

[0142] (1) Under the same preparation method, when at least one of vanadium, titanium, tantalum, lanthanum and cerium is added to the niobium aluminum alloy target provided by the embodiment of the present invention, the density of the obtained target is higher, but the oxygen content is relatively increased, but not higher than 30 ppm; it can be seen that the niobium aluminum alloy target provided by the embodiment of the present invention has a higher density (99.5% to 99.9%) and a lower oxygen content (15 ppm to 30 ppm).

[0143] (2) According to the comparison between Example 1 and Comparative Examples 1 to 2, it can be seen that the preparation method of the niobium aluminum alloy target provided by the embodiment of the present invention adopts Nb-MOF powder as the niobium source. During mixing, the aluminum powder is easily embedded in the structure of the Nb-MOF powder, so that the niobium source and the aluminum powder are evenly mixed. The internal structure of the niobium aluminum alloy target obtained after sintering is free of defects such as pores, cracks, delamination, inclusions, etc., and has high density and low oxygen content.

[0144] It should be noted that the present invention is not limited to the above-mentioned embodiments. The above-mentioned embodiments are only examples, and the embodiments having the same structure as the technical idea and exerting the same effect within the scope of the technical solution of the present invention are all included in the technical scope of the present invention. In addition, without departing from the scope of the main purpose of the present invention, various modifications that can be thought of by those skilled in the art to the embodiments and other methods of combining some of the constituent elements in the embodiments are also included in the scope of the present invention.

Claims

1. A niobium aluminum alloy target, characterized in that: The following raw materials are included in atomic percentage: 5%~10% niobium, 90%~95% aluminum.

2. A method for preparing a niobium aluminum alloy target, characterized in that: The steps include: The Nb-MOF powder and the aluminum powder are mixed, and then cold isostatic pressing and sintering are performed to obtain a niobium aluminum alloy target; The Nb-MOF powder is prepared by reacting niobium chloride and pyridinetetracarboxylic acid ethanol solution.

3. The method for preparing a niobium aluminum alloy target according to claim 2, characterized in that: The preparation of the Nb-MOF powder comprises the following steps: The niobium chloride and pyridinetetracarboxylic acid ethanol solution are mixed to undergo a solvothermal reaction, and then filtered and dried to obtain Nb-MOF; The Nb-MOF is ground to obtain Nb-MOF powder.

4. The method for preparing a niobium aluminum alloy target according to claim 2 or 3, characterized in that: The molar ratio of Nb to aluminum powder in the Nb-MOF powder is 1:32-65; And / or, the mixing process comprises the following steps: mixing the Nb-MOF powder and the aluminum powder and then ball milling.

5. The method for preparing a niobium aluminum alloy target according to claim 4, characterized in that: In the ball milling, the ball milling atmosphere is argon, the ball-to-material ratio is 1:0.5-4, the rotation speed is 50 rpm-100 rpm, and the ball milling time is 24 h-36 h.

6. The method for preparing a niobium aluminum alloy target according to any one of claims 2 to 5, characterized in that: In the cold isostatic pressing, the pressing pressure applied is 190MPa to 220MPa; And / or, during the cold isostatic pressing, the holding time is 10 min to 15 min; And / or, in the cold isostatic pressing, after maintaining the pressure, the pressure is reduced to normal pressure at a speed of 15 MPa / min to 20 MPa / min to obtain a niobium aluminum alloy compact.

7. The method for preparing a niobium aluminum alloy target according to any one of claims 2 to 6, characterized in that: The sintering includes hydrogen atmosphere sintering and vacuum sintering.

8. The method for preparing a niobium aluminum alloy target according to claim 7, characterized in that: The sintering temperature of the hydrogen atmosphere sintering is 1200°C to 1400°C; And / or, the holding time of the hydrogen atmosphere sintering is 5h to 7h; And / or, the hydrogen flow rate of the hydrogen atmosphere sintering is 4m 3 / h~6m 3 / h.

9. The method for preparing a niobium aluminum alloy target according to claim 7 or 8, characterized in that: The vacuum degree of the vacuum sintering is 10 -5 Pa~10 -3 Pa; And / or, the sintering temperature of the vacuum sintering is 1500° C. to 1600° C.; And / or, the insulation time of the vacuum sintering is 5h to 8h.

10. Use of the niobium aluminum alloy target material as claimed in claim 1 in the electrical field, optical field, flat panel display field or photovoltaic field.