Preparation method of photocuring formed ferrite magnetic ceramic

The preparation of ferrite magnetic ceramics through photocuring technology solves the problems of insufficient body strength and high cost in traditional methods, and achieves high-precision manufacturing and cost reduction of complex shapes.

CN119118645APending Publication Date: 2024-12-13JIANGXI JINSHI 3D AM TECH CO LTD
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Patent Information

Application Number
CN202310688515.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-06-12
Publication Date
2024-12-13

AI Technical Summary

Technical Problem

The traditional method of preparing ferrite magnetic ceramics has problems such as insufficient body strength, inaccurate size, and high manufacturing cost of complex parts, and requires high precision mold support.

Method used

Ferrite magnetic ceramics are prepared by photocuring technology, and the parts are printed by mixing prepolymers, diluents, surface modifiers, dispersants, defoamers and MnO-ZnO-Fe2O3 powders using DLP printers and heat Degreasing and sintering treatments yield the finished product.

Benefits of technology

It realizes complex shape preparation without molds, improves the strength and dimensional accuracy of the blank, reduces the manufacturing cost, and solves the shortcomings in the traditional methods.

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Abstract

The invention is suitable for the field of photocuring additive manufacturing, and provides a preparation method of photocuring molded ferrite magnetic ceramic, and the system comprises 1-20 parts of a prepolymer, 1-25 parts of a diluent, 1-10 parts of a surface modifier, 1-15 parts of a dispersant, 0.1-2 parts of an antifoaming agent, 0.1-3 parts of an initiator, and 2-100 parts of MnO-ZnO-Fe2O3 powder. According to the preparation method for forming the ferrite magnetic ceramic through the photocuring technology, the ferrite magnetic ceramic can be widely applied to the fields of forming high-precision magnetic materials and the like.
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Description

Technical Field

[0001] The invention belongs to the field of material science and engineering-polymer, and in particular relates to a method for preparing photocured ferrite magnetic ceramics. Background Art

[0002] The traditional preparation process of magnetic materials mainly includes the preparation process of powder, the pressing process of powder and the sintering process of pressed samples. The first is the preparation of powder. According to the type of original reactants, the preparation of magnetic powder can be divided into three types: gas phase method, solid phase method and liquid phase method; then, the prepared magnetic powder is pressed into the desired shape, and then the pressed parts are sintered at a temperature below the melting point of the component. As the temperature rises, the magnetic particles are thermally activated, and the internal ions are excited to escape the surrounding ion constraints and migrate, forming metallurgical bonds between the particles and bonding to each other to form a sintered body; finally, the sintered parts are machined again as required. However, there are certain limitations in the traditional preparation of ferrite parts. For example, the green body strength is often insufficient during the pressing process, resulting in cracks, and the size is quite different from the design size. Secondly, for the manufacture of complex precision parts, pressing and forming has high requirements for molds and high cost consumption. Additive manufacturing technology can achieve the preparation of any complex shape without molds, successfully solving the problems of the above traditional manufacturing methods.

[0003] As an emerging battery preparation method, photocuring technology shows a good development prospect in the molding of ferrite magnetic ceramics. The present invention molds ferrite magnetic ceramics through photocuring technology, so that it can be widely used in the fields of magnetic materials and the like. Summary of the invention

[0004] The embodiments of the present application provide a method for forming ferrite magnetic ceramics using a photocuring technology to construct a photocurable magnetic material.

[0005] The embodiment of the present application implements the photocuring technology to form ferrite magnetic ceramics, including the following raw materials in parts by weight:

[0006] 1-20 parts of prepolymer, 1-25 parts of diluent, 1-10 parts of surface modifier, 1-15 parts of dispersant, 0.1-2 parts of defoamer, 0.1-3 parts of initiator, 2-100 parts of MnO-ZnO-Fe2O3 powder.

[0007] The present application also provides a method for preparing ferrite magnetic ceramics formed by light curing technology, comprising:

[0008] 80 parts of MnO-ZnO-Fe2O3 powder and dispersant were put into a ball mill, and ball milled with anhydrous ethanol as a medium, and then taken out and dried in an oven, and then ground and sieved to obtain modified ferrite magnetic ceramics;

[0009] 1-20 parts of prepolymer, 1-25 parts of diluent, 1-10 parts of surface modifier, 1-15 parts of dispersant and 0.1-3 parts of initiator are mixed and stirred evenly to obtain a photosensitive resin;

[0010] The modified MnO-ZnO-Fe2O3 powder and the photosensitive resin are mixed, and then 0.1-2 parts of a defoaming agent are added to carry out ball milling. After taking out, vacuum stirring is used to remove bubbles to obtain the product.

[0011] The ferrite magnetic ceramic photocuring slurry is printed using a DLP printer to obtain a part blank, the printed part blank is cleaned by ultrasonic wave using distilled water as a medium, the attached slurry and water are washed away by air flow, and then dried;

[0012] The dried parts are subjected to thermal degreasing treatment, with a heating rate of 0.1-0.5°C / min at 100-500°C, and the temperature is raised to 900°C and kept after degreasing;

[0013] After degreasing, ferrite magnetic ceramics are obtained by sintering at 1250-1300°C for 2-4 hours. DETAILED DESCRIPTION

[0014] In order to make the purpose, technical solution and advantages of the present application more clear, the present application is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0015] The embodiment of the present application provides a ferrite magnetic ceramic formed by light curing technology, comprising the following raw materials in parts by weight:

[0016] 1-20 parts of prepolymer, 1-25 parts of diluent, 1-10 parts of surface modifier, 1-15 parts of dispersant, 0.1-2 parts of defoamer, 0.1-3 parts of initiator, 2-100 parts of MnO-ZnO-Fe2O3 powder.

[0017] Wherein, the oligomer is one or more of bisphenol A epoxy acrylate, polyurethane acrylate, and epoxidized oil acrylate.

[0018] Wherein, the diluent is one or more of 1,6-hexanediol diacrylate, 1,4-butanediol diacrylate, and propylene glycol diacrylate.

[0019] Wherein, the photoinitiator is one or more of benzoin and its derivatives, dialkoxyacetophenone, α-hydroxyalkyl phenone, and acylphosphine oxide.

[0020] Wherein, the dispersant is a polymer super dispersant, preferably one or more of DH-5038, DH-6000, and DH-5350.

[0021] The surface modifier is a silane coupling agent, and the dispersant is a polymer superdispersant, preferably one or more of KH550, KH560, and KH570.

[0022] Wherein, the defoaming agent is one of B-0846, B-0847, B-0848 or several of them in any proportion, provided by Nanjing Jiazhong Chemical Technology Co., Ltd.

[0023] Wherein, the MnO-ZnO-Fe2O3 is provided by Sinopharm Chemical Reagent Co., Ltd.

[0024] Implementation Case 1

[0025] The present application also provides a method for preparing a photocured ferrite magnetic ceramic, comprising:

[0026] Take 15 parts of polyurethane acrylate, 10 parts of propylene glycol diacrylate, 5 parts of KH570, 0.1 parts of α-hydroxyalkyl phenone, and 2 parts of defoamer B-0848, and stir them magnetically for 24 hours to obtain a photosensitive resin.

[0027] Take 50 parts of MnO-ZnO-Fe2O3 powder, dry it, sieve it, and put it into a ball mill. Use anhydrous ethanol as the medium for ball milling. After drying, grinding and sieving, zirconium oxide powder is obtained for use. The ball milling beads are all zirconium oxide. Use a planetary ball mill at 400rpm for 24 hours, take out the suspension, filter it, dry it, grind it, and sieve it to obtain modified MnO-ZnO-Fe2O3 powder.

[0028] Mix 30 parts of modified MnO-ZnO-Fe2O3 powder and 20 parts of photosensitive resin, put them into a ball mill, add 50 parts of 10mm ball milling beads and 100 parts of 5mm ball milling beads, and after ball milling for 24 hours, take them out and put them into a vacuum stirring tank. After vacuum stirring and defoaming, MnO-ZnO-Fe2O3 photocuring slurry is obtained.

[0029] The part blank was printed with MnO-ZnO-Fe2O3 photocuring slurry using a DLP printer. The blank was cleaned with ultrasonic waves using distilled water as the medium, and the attached slurry and water were washed off with air flow before drying. The dried blank was thermally degreased in a degreasing furnace, with a heating rate of 0.1 / min at 100-500°C; after degreasing, the temperature was raised to 900°C and kept for 2 hours. After degreasing, the ferrite magnetic ceramic was sintered at 1200°C for 2 hours in a muffle furnace to obtain the ferrite magnetic ceramic.

Claims

1. Preparation method of ferrite magnetic ceramics formed by light curing technology, Features: Prepolymer 1-20 parts, diluent 1-25 parts, surface modifier 1-10 parts, dispersant 1-15 parts, defoamer 0.1-2 parts, initiator 0.1-3 parts, MnO-ZnO-Fe 2 O 3 Powder 2-100 parts.

2. The oligomer as claimed in claim 1 is one or more of bisphenol A epoxy acrylate, polyurethane acrylate, and epoxidized oil acrylate.

3. The diluent as claimed in claim 1 is one or more of 1,6-hexanediol diacrylate, 1,4-butanediol diacrylate and glycerol diacrylate.

4. The photoinitiator as claimed in claim 1 is one or more of benzoin and its derivatives, dialkoxyacetophenone, α-hydroxyalkyl phenone, and acylphosphine oxide.

5. The surface modifier as claimed in claim 1 is a silane coupling agent and the dispersant is a polymer super dispersant, preferably one or more of KH550, KH560, and KH570.

6. The dispersant as claimed in claim 1 is a polymer super dispersant, preferably one or more of DH-5038, DH-6000, and DH-5350.

7. The defoaming agent as claimed in claim 1 is one of B-0846, B-0847, B-0848 or several of them in any proportion, provided by Nanjing Jiazhong Chemical Technology Co., Ltd. Take 15 parts of polyurethane acrylate, 10 parts of propylene glycol diacrylate, 5 parts of KH570, 0.1 parts of α-hydroxyalkyl phenone, and 2 parts of defoamer B-0848, and stir them magnetically for 24 hours to obtain a photosensitive resin. Take 50 parts of MnO-ZnO-Fe 2 O 3 After the powder is dried and sieved, it is placed in a ball mill and ball milled with anhydrous ethanol as the medium. After drying, grinding and sieving, zirconium oxide powder is obtained for use. The ball milling beads are all zirconium oxide. A planetary ball mill is used for ball milling at 400 rpm for 24 hours. The suspension is taken out and filtered, dried, ground and sieved to obtain the modified MnO-ZnO-Fe 2 O 3 pink. 30 parts of modified MnO-ZnO-Fe 2 O 3 The powder and 20 parts of photosensitive resin were mixed and placed in a ball mill, and 50 parts of 10 mm ball milling beads and 100 parts of 5 mm ball milling beads were added. After ball milling for 24 hours, the mixture was taken out and placed in a vacuum stirring tank. After vacuum stirring and defoaming, MnO-ZnO-Fe 2 O 3 Light-curing slurry. Using DLP Printer MnO-ZnO-Fe 2 O 3 The photocurable slurry is printed to obtain the part body, which is then cleaned with ultrasonic waves using distilled water as the medium, and the attached slurry and water are washed away with air flow before drying. The dried body is thermally degreased in a degreasing furnace, with a heating rate of 0.1 / min at 100-500°C; after degreasing, the temperature is raised to 900°C and kept for 2 hours. After degreasing, the ferrite magnetic ceramic is sintered in a muffle furnace at 1200°C for 2 hours.