CN-117966135-B - Low-temperature preparation method of (222) oriented growth nickel zinc ferrite film

Abstract

The invention provides a low-temperature preparation method of a (222) oriented growth nickel-zinc ferrite film, belonging to the technical field of film preparation. Based on the principle of oxidation-reduction reaction, the invention utilizes rotary spraying equipment to uniformly attach oxidizing liquid and reducing liquid on a glass substrate according to a certain proportion through an ultrasonic atomization system, forms a continuous and compact ferrite film after a series of chemical reactions are completed, and controls the deposition rates of different crystal faces by changing the concentration of ferrous chloride in the reducing liquid so as to regulate the growth orientation of the NiZn ferrite film. The NiZn ferrite film prepared by the low-temperature deposition process can be compatible with a semiconductor process, meanwhile, the orientation of the NiZn ferrite film is gradually selected from the (311) orientation of the NiZn ferrite to grow along the (222) preferential orientation, and the microstructure gradually forms obvious triangular grains, so that the film growth is more uniform, and the film quality is obviously improved.

Inventors

• YU ZHONG
• CHEN JINGSHA
• WANG HONG
• LI QIFAN
• DOU HAIZHI
• WU CHUANJIAN
• SUN KE
• JIANG XIAONA
• LAN ZHONGWEN

Assignees

• 电子科技大学
• 江西尚朋电子科技有限公司

Dates

Publication Date

20260508

Application Date

20240228

Claims (2)

1. 1. The low-temperature preparation method of the (222) oriented growth nickel zinc ferrite film is characterized by comprising the following steps of: step1, cleaning a reaction table: Polishing the reaction table by using sand paper until the surface is smooth, cleaning by using absolute ethyl alcohol and acetone, and naturally airing; Step 2, preparing a solution: 2.1 Adding buffer acetate and oxidant soluble nitrite into deionized water, and uniformly mixing to obtain oxidant solution, wherein the molar concentration of acetate is 20-30 mmol/L, and the molar concentration of nitrite is 2-4 mmol/L; 2.2 Adding ferrous chloride, zinc chloride and nickel chloride into deionized water, and uniformly mixing to obtain a reducer solution, wherein the molar concentration of the ferrous chloride is 9-12 mmol/L, the molar concentration of the zinc chloride is 0.5-2 mmol/L, and the molar concentration of the nickel chloride is 1-2 mmol/L; Step3, preparing a film: Placing a glass substrate in the center of a reaction table cleaned in the step 1, depositing a film by adopting a rotary spraying method under the conditions that the temperature of the substrate is 85-95 ℃, the supply rate of an oxidant solution is 15-20 mL/min, the supply rate of a reducing agent solution is 15-20 mL/min, the atomization power is 0.1-0.5W, the working air pressure is 0.02-0.05 MPa and the rotating speed of the reaction table is 120-140 r/min, wherein the deposition time is 20-40 min, and obtaining the NiZn ferrite film after the deposition is completed; The deposition rates of different crystal faces are controlled by changing the concentration of ferrous chloride in the reducing solution, so that the growth orientation of the NiZn ferrite film is regulated and controlled.
2. 2. The method for preparing an orientated-growth nickel-zinc ferrite film according to claim 1, wherein in step 3, after the cleaned reaction table is heated to 50-60 ℃, the glass substrate is placed in the center of the reaction table.

Description

Low-temperature preparation method of (222) oriented growth nickel zinc ferrite film Technical Field The invention belongs to the technical field of film preparation, and particularly relates to a low-temperature preparation method of a (222) oriented growth nickel-zinc ferrite film. Background Today, the high-speed development of the integrated circuit industry has become a major trend of electronic devices, and in particular, the basic product devices have increasingly higher demands on the integration level and functionality of System On Chip (SOC), micro System (MS) and System In Package (SIP), which requires continuous innovations and breakthroughs of design and manufacturing technologies to achieve higher integration level and richer functions. The inductor is one of three passive linear components of an electronic circuit, has important application background in the fields of consumer electronics, industrial equipment, radio frequency communication, energy transmission and the like, and is highly integrated by a microelectronic manufacturing process, and integrated with other electronic elements and functional modules in the same chip or package, so that higher integration level and simplified circuit layout are realized, and the size and complexity of the system are reduced. Although the metal magnetic film can be compatible with a semiconductor process, the low resistivity of the metal magnetic film restricts the high frequency of an integrated device, and the NiZn ferrite film belongs to spinel materials, has the advantages of low eddy current loss and skin effect influence at high frequency due to high resistivity, has important application prospects in SOC, MS and SIP, and is particularly important for preparing the high-quality NiZn ferrite film. However, the conventional preparation method of the NiZn ferrite film comprises a physical method and a chemical method, wherein a sputtering method and a pulse laser deposition method are common in the physical method, and a chemical vapor deposition method and a sol-gel method are common in the chemical method, but the methods all require high-temperature (> 600 ℃) annealing treatment, so that the method is difficult to be compatible with a semiconductor process. Abe et al (Abe,Masanori,and Yutaka Tamaura."Ferrite-plating in aqueous solution:A new method for preparing magnetic thin film."Japanese journal of applied physics 22.8A(1983):L511.) first proposed a low temperature deposition technique to prepare Fe 2O3 and CoFe 2O4 films on copper, PET and stainless steel substrates, which are suitable for substrates of various material types, but which do not have oriented growth. N. Matsushita et al (N.Matsushita,Chee Ping Chong,T.Mizutani and M.Abe,"High-rate low-temperature(90℃)deposition of Ni-Zn ferrite films highly permeable in gigahertz range,"in IEEE Transactions on Magnetics,vol.38,no.5,pp.3156-3158,Sept.2002) realized the preparation of NiZn ferrite film on glass substrate at low temperature by spin-coating, studied the effect of pH value in the range of 6.8-9.2 on preferred orientation, and when pH value is 8.4, film sample had maximum saturation magnetization M s 482emu/cm3 and minimum coercive force H c-// Oe, which was apparent in preferred orientation at pH values of 6.8 and 8.7 (111) and disappeared in preferred orientation at pH value of 9.2, but none of (222) oriented growth. O.Obi et al (Obi O,Liu M,Lou J,et al.Spin-spray deposited NiZn-Ferrite films exhibitingμr′>50at GHz range[J].Journal of Applied Physics,2011,109(7).) prepared a 0.7 μm thick Ni 0.27Zn0.1Fe2.63O4 film on a 0.1mm thick glass substrate by spin-coating under the action of an external magnetic field of 360Oe, wherein the saturation magnetization M s is 358emu/cm 3, the in-plane coercivity H c-// is 11Oe, and the magnetic permeability is improved by 3 times as much as that of the film grown without magnetic field induction, but without obvious oriented growth. wang X et al (Wang X,Zhou Z,Behugn S,et al.Growth behavior and RF/microwave properties of low temperature spin-sprayed NiZn ferrite[J].Journal of Materials Science:Materials in Electronics,2015,26:1890-1894.) prepared a 0.7 μm Ni 0.27Zn0.1Fe2.63O4 film on a 0.2mm thick glass substrate by spin coating, controlled the grain size of the NiZn film by adjusting the pH of the oxidizing and reducing solutions, and further adjusted the magnetic properties, and studied to find that the film had a minimum grain size of 70nm and a maximum permeability at pH 9.6 for the oxidizing solution and pH 4.6 for the reducing solution, and that the initial permeability was greater than 200 at 0.5GHz, but the XRD pattern showed no preferential orientation. At present, researches on preparing a NiZn ferrite film by a rotary spraying method mainly focus on static magnetic properties (coercive force H c and saturation magnetization M s) and dynamic magnetic properties (ferromagnetic resonance line width FMR and magnetic permeability mu'