CN-122013118-A - Nickel ferrite target material and preparation method thereof

Abstract

The application relates to the technical field of target preparation, and provides a nickel ferrite target and a preparation method thereof, wherein NiO powder and Fe 2 O 3 powder are provided, and mixed ball milling, drying and calcining treatment are sequentially carried out on the NiO powder and the Fe 2 O 3 powder, a dispersing agent and a solvent, so as to obtain NiFe 2 O 4 calcined powder; mixing, ball milling and drying Fe 3 O 4 powder doped with A, calcined NiFe 2 O 4 powder, a dispersing agent and a solvent to obtain mixed powder, wherein A is at least one of MnO 2 、CuO、CoO、Cr 2 O 3 and MgO, pre-pressing and hot pressing the mixed powder, and then machining to obtain the nickel ferrite target. According to the application, fe 3 O 4 powder doped with A is introduced, and Fe 2+ and Fe 3+ exist on octahedral sites in the crystal structure at the same time, so that electron exchange can be realized through an oxygen ion bridge, a conductive path is built in the material, the conductivity of the target is improved, and the requirements of a direct current sputtering process are met.

Inventors

• GUAN ZEHAN
• ZHOU XIANJIE
• HUANG YONGBIAO
• ZHANG ZHUOXUAN

Assignees

• 深圳众诚达应用材料股份有限公司

Dates

Publication Date

20260512

Application Date

20260408

Claims (10)

1. 1. The preparation method of the nickel ferrite target is characterized by comprising the following steps of: providing NiO powder and Fe 2 O 3 powder; sequentially carrying out mixed ball milling, drying and calcination treatment on the NiO powder, the Fe 2 O 3 powder, the dispersing agent and the solvent to obtain NiFe 2 O 4 calcined powder; Mixing, ball milling and drying Fe 3 O 4 powder doped with A, the NiFe 2 O 4 calcined powder, the dispersing agent and the solvent to obtain mixed powder, wherein the A is at least one of MnO 2 、CuO、CoO、Cr 2 O 3 and MgO; And (3) carrying out pre-pressing treatment and hot pressing treatment on the mixed powder, and then machining to obtain the nickel ferrite target.
2. 2. The preparation method of claim 1, wherein the mass ratio of the NiFe 2 O 4 calcined powder to the A-doped Fe 3 O 4 powder is (85-95): 5-15; And/or the mass ratio of the NiO powder to the Fe 2 O 3 powder is (1-1.2): 1.
3. 3. The method according to claim 1, wherein the content of a in the a-doped Fe 3 O 4 powder is 1 to 5wt%.
4. 4. The method of claim 1, wherein the step of preparing the a-doped Fe 3 O 4 powder comprises: Dissolving soluble metal salt, ferrous salt and ferric salt corresponding to the A in deoxidized distilled water to obtain a mixed salt solution; Adding a precipitator and a complexing agent into the mixed salt solution under the protection of inert atmosphere to carry out coprecipitation reaction to generate hydroxide colloid; And concentrating, washing and drying the hydroxide colloid, and calcining for 6-12 hours at 600-950 ℃ in vacuum or reducing atmosphere to obtain the Fe 3 O 4 powder doped with A.
5. 5. The method of claim 4, wherein at least one of the following conditions is satisfied: The soluble metal salt corresponding to the A is selected from at least one of manganese chloride, copper nitrate, copper sulfate, cobalt chloride, cobalt nitrate, chromium chloride, chromium sulfate, magnesium chloride and magnesium nitrate; the ferrous salt is selected from FeSO 4· 7H 2 O; the ferric salt is selected from FeCl 3· 6H 2 O; the precipitant is selected from saturated urea solution; the complexing agent is selected from ammonium chloride or ammonium nitrate.
6. 6. The method according to claim 1, wherein the atmosphere for the calcination treatment is air, the temperature is 950-1200 ℃, and the time is 4-6 hours.
7. 7. The preparation method of the heat press according to claim 1, wherein the heat press treatment process comprises the steps of heating to 500-600 ℃ at first, preserving heat for 20-40 min, continuously heating to 700-800 ℃ at the temperature of 60-90 min, continuously heating to 950-1200 ℃ at the temperature of 10-30 MPa, preserving heat and pressure for 60-120 min, removing pressure after the heat preservation and pressure preservation are finished, and cooling to room temperature along with a furnace.
8. 8. The method according to claim 1, wherein the particle size of the mixed powder is 5 to 20 μm.
9. 9. The method of claim 1, wherein the dispersant is selected from at least one of polyethylene glycol, hexadecyl sulfonate, polycarboxylate, polyacrylate, or triethanolamine; and/or the solvent is selected from ethanol or deionized water.
10. 10. A nickel ferrite target material, characterized in that it is prepared by the preparation method of the nickel ferrite target material according to any one of claims 1 to 9.

Description

Nickel ferrite target material and preparation method thereof Technical Field The application belongs to the technical field of target preparation, and particularly relates to a nickel ferrite target and a preparation method thereof. Background Nickel ferrite (NiFe 2O4) is a Negative Temperature Coefficient (NTC) ceramic material whose resistivity decreases exponentially with temperature, and thus is widely used for preparing thermistors in the fields of home appliances, automotive electronics, medical devices, and the like. However, NTC thermistors are often ceramic bodies, limited by the sintering process, difficult to shrink in size, and inconvenient to integrate with silicon-based circuits, which has prompted thin film formation to become an important development direction. With the evolution of electronic devices toward miniaturization, chip formation and high performance, the preparation of soft magnetic ferrite films by Physical Vapor Deposition (PVD) techniques such as magnetron sputtering has become a necessary trend. In film preparation, nickel-iron alloy targets are usually adopted for reactive sputtering or NiFe 2O4 targets are directly used for sputtering coating. The former is easy to influence the functional characteristics of the film due to uneven oxygen content of the film and residual metal phase caused by incomplete reaction, and the latter is difficult to maintain stable glow discharge in direct current magnetron sputtering due to extremely high resistivity of NiFe 2O4, thereby causing the problems of unstable process, low speed, target loss and the like. Although the radio frequency magnetron sputtering can sputter an insulating target, the method has the limitations of complex equipment, high cost, low deposition rate, difficult film uniformity control and the like. The existing method for improving the conductivity of the NiFe 2O4 target material by doping metal powder or conductive oxide can introduce impurity phases, so that the final purity and performance of the film are affected. Therefore, how to effectively improve the conductivity of the NiFe 2O4 target material to meet the requirements of the direct-current sputtering process and ensure that the purity and the functional characteristics of the NiFe 2O4 film are not damaged is a key problem to be solved in urgent need of promoting the thinning and the application of the material. Disclosure of Invention The application aims to provide a nickel ferrite target and a preparation method thereof, and aims to solve the problem that a NiFe 2O4 target cannot adopt direct-current sputtering coating due to poor conductivity. In order to achieve the purposes of the application, the technical scheme adopted by the application is as follows: in a first aspect, the application provides a method for preparing a nickel ferrite target, comprising the following steps: providing NiO powder and Fe 2O3 powder; sequentially carrying out mixed ball milling, drying and calcination treatment on the NiO powder, the Fe 2O3 powder, the dispersing agent and the solvent to obtain NiFe 2O4 calcined powder; Mixing, ball milling and drying Fe 3O4 powder doped with A, the NiFe 2O4 calcined powder, the dispersing agent and the solvent to obtain mixed powder, wherein the A is at least one of MnO 2、CuO、CoO、Cr2O3 and MgO; And (3) carrying out pre-pressing treatment and hot pressing treatment on the mixed powder, and then machining to obtain the nickel ferrite target. In a second aspect, the application provides a nickel ferrite target material, which is prepared by the preparation method of the nickel ferrite target material. Compared with the prior art, the application has the following beneficial effects: (1) By introducing the Fe 3O4 powder doped with A, the conductivity of the target is obviously improved. Fe 2+ and Fe 3+ existing in the crystal structure of Fe 3O4 at the same time can exchange electrons through an oxygen ion bridge And the cation (Mn 4+、Cu2+、Co2+、Cr3+、Mg2+) of A is dissolved into Fe 3O4 crystal lattice to generate pinning effect, which enhances the thermal stability and structural integrity of Fe 3O4 phase, thereby effectively inhibiting phase change or decomposition in the hot-pressed sintering process, avoiding the degradation of conductivity and ensuring the reliability of the conductive network. (2) The two-part synthesis process is adopted, namely NiO powder and Fe 2O3 powder are calcined to synthesize NiFe 2O4 calcined powder, and then the NiFe 2O4 calcined powder and Fe 3O4 powder doped with A are subjected to hot-press sintering, so that on one hand, fe 3O4 is prevented from being decomposed into FeO and O 2 at high temperature, and is oxidized into Fe 2O3 with high resistivity after being cooled and contacted with air, and on the other hand, uncontrollable solid phase side reactions of NiO, fe 2O3 and Fe 3O4 are prevented from being directly co-fired, so that the structural purity and performance stability of a target material takin