CN111434425A - Soft magnetic metal composite material water-based tape casting slurry and preparation method of film thereof - Google Patents
Soft magnetic metal composite material water-based tape casting slurry and preparation method of film thereof Download PDFInfo
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- CN111434425A CN111434425A CN201910027431.XA CN201910027431A CN111434425A CN 111434425 A CN111434425 A CN 111434425A CN 201910027431 A CN201910027431 A CN 201910027431A CN 111434425 A CN111434425 A CN 111434425A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a preparation method of soft magnetic metal composite water-based tape casting slurry and a film thereof, which is characterized by comprising the following steps: the material comprises 100 parts of sheet soft magnetic metal composite material, 350 parts of deionized water 150-350 parts, 0.5-2 parts of dispersant, 5-10 parts of binder, 2.5-5 parts of plasticizer, 0.5-1 part of defoamer, 1-10 parts of alkaline solution and 0.1-5 parts of coupling agent. The method comprises the following specific steps: 1) sheet processing and surface modification of the metal magnetic powder; 2) preparing a magnetic oxide coated soft magnetic metal composite material; 3) preparing composite material water-based tape casting slurry; 4) defoaming and casting. The invention realizes the preparation of the magnetic metal magnetic powder water-based tape casting slurry by modifying, compounding and proportioning the magnetic metal surface, has the advantages of good wettability, quick volatilization, short drying time, easy removal of bubbles from the slurry, better flexibility of a tape casting film, difficult cracking and high strength, has the characteristics of convenient preparation, environmental protection and low cost, and is suitable for industrial production.
Description
The invention belongs to the technical field of electronic component materials, and particularly relates to a soft magnetic metal composite water-based tape casting slurry and a preparation method of a film thereof.
Background
In recent years, wireless power transmission technology is rapidly developed in the fields of advanced electronic and electrical products such as mobile phone communication, computers, intelligent wearable equipment, smart homes, medical equipment and electric vehicles. As a novel energy conversion mode, the novel energy conversion device overcomes the limitation of the traditional cable conversion, and is excellent in the aspects of function diversification, convenience, attractiveness, flexibility and the like. However, in the practical application process, some technical bottlenecks, such as low conversion efficiency and high energy loss, exist, and due to the fact that the energy source belongs to secondary energy conversion, the safety problems of space electromagnetic loss and leakage, electromagnetic pollution, heating and the like exist. The existing solution uses ferrite sintered magnetsThe sheet is mostly prepared by rolling an organic system in a forming way, and nickel-zinc or manganese-zinc ferrite is used as a main powder raw material; the auxiliary materials comprise various auxiliary agents such as a solvent, a dispersant, a binder, a plasticizer and the like. The used solvent is ethanol, toluene, xylene or a mixture thereof, has great potential safety hazard to the environment and operators, has high requirements on the safety of production equipment, waste treatment and raw material recovery, and has high solvent recovery and reutilization cost. In addition, the saturated magnetic induction strength B of the magnetic isolation sheet material formed by pressing ferrite powder and polymer in a mixing waySThe value is low and is only 0.4T; and the saturation magnetic induction intensity B of the iron-based alloy, the amorphous alloy and the nanocrystalline alloySThe minimum value can reach 1T, which is 2.5 times of ferrite. For the wireless charging device, considering the beauty and portability of the charged product and the accessory products, the magnetic shielding sheet is required to be tightly attached to the antenna, and a magnetic metal soft magnetic flexible thin film material with high magnetic flux density, light weight and small volume is required, while the ferrite magnetic shielding sheet has poor flexibility, is not easy to process, thick and fragile, and has the phenomena of brittle cracking, falling off, magnetic flux leakage, heating and the like of the shielding layer, so that the light weight and thin requirement of using the wireless charging product cannot be met, and the wireless charging device cannot be applied to the fields of high-power devices, flexible electronic devices, micro-nano electronic devices and the like.
In recent decades, the tape casting technology is applied to the production of various advanced ceramic films, has the advantages of high production efficiency, good product consistency and stable performance, and is suitable for mass production of ultrathin flexible films with the thickness of 0.04-1.0 mm. At present, there are many technologies for preparing magnetic shielding sheets based on casting technology, such as non-aqueous casting for metal systems (CN 101497132B, CN 108053008 a) and aqueous casting for ferrite materials (CN 104446518B, CN 104177077B), but from the literature and patent technology at home and abroad at present, the research data and data for aqueous casting for metal magnetic powder are very few, and especially the preparation of metal powder aqueous base slurry is still blank at home. Because the metal powder generally has larger granularity and is easy to oxidize, a water-based system is difficult to disperse, and particularly the slurry of the composite metal mixture with different surface properties increases the difficulty of improving the solid phase content of the casting slurry, the selection of organic additives such as proper solvents, dispersing agents, binding agents, plasticizers and the like and the adjustment of proper composite coating proportion are very important.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of nano magnetic oxide coated flaky composite metal magnetic powder, which can effectively prevent magnetic powder from contacting with each other, has good dispersibility and strong oxidation resistance. The invention also aims to provide a preparation method of the water-based tape casting slurry of the soft magnetic metal composite material and a film thereof, the slurry has the advantages of good powder wettability, quick volatilization, short drying time, easy removal of bubbles from the slurry, good flexibility of a tape casting film, difficult cracking and high strength, and the method has the characteristics of convenience in preparation, safety, environmental protection, high efficiency and low cost.
The purpose of the invention is realized by the following technical scheme: a preparation method of soft magnetic metal composite water-based tape casting slurry and a film thereof is characterized in that the soft magnetic metal composite water-based tape casting slurry comprises the following raw materials in parts by weight: 100 parts of soft magnetic metal composite material, 150 parts of deionized water and 350 parts of dispersant, 5-10 parts of binder, 2.5-5 parts of plasticizer, 0.5-1 part of defoamer, 1-10 parts of alkaline solution and 0.1-5 parts of coupling agent.
The magnetic metal powder comprises one or more of Fe-Si-Al, Fe-Si-Cr, Fe-Si-Ni, amorphous iron-based alloy and nanocrystalline iron-based alloy.
The soft magnetic material is one or more of nickel zinc ferrite and manganese zinc ferrite.
The dispersant is one or more of triethanolamine and polyethylene glycol.
The binder is one or more of polyvinyl alcohol, polyacrylic acid and waterborne polyurethane.
The plasticizer is one or more of glycerol and polyethylene glycol.
The defoaming agent is a high-carbon alcohol defoaming agent.
The alkaline solution is low-concentration sodium hydroxide or ammonia water.
The coupling agent is a silane coupling agent.
The preparation method of the soft magnetic metal composite water-based tape casting slurry and the film thereof comprises the following steps:
(1) adding 100 parts by mass of metal magnetic powder into a stirrer, adding 1-10 parts of alkaline solution and 90-100 parts of deionized water, stirring for 1 hour to fully wet and uniformly disperse the magnetic powder in water, filtering and drying;
(2) adding 100 parts of the magnetic powder prepared in the step (1), 0.1-5 parts of a coupling agent and 190-200 parts of deionized water into a stirrer, and stirring for 1 hour to fully wet and uniformly disperse the magnetic powder in a solvent;
(3) adding the magnetic metal powder prepared in the step (2), deionized water and a dispersing agent into a ball milling tank according to a ratio (ball-to-material ratio is 10: 1), ball milling for 15-20 h at a rotating speed of 250 revolutions per minute, and vacuum drying for later use;
(4) weighing the corresponding chloride salt required by the ferrite according to a proportion, adding 100ml of water, dissolving at 60 ℃, stirring by using a magnetic stirrer, adding 100 parts by mass of the flaky Fe-Si-Al magnetic powder prepared in the step (3), dropwise adding 2 mol/L of sodium hydroxide to adjust the pH to be 8-10, keeping the rotation speed at 200r/min for 60min, standing for 24h, washing, filtering and drying for later use;
(5) adding the soft magnetic composite material prepared in the step (4) into a ball milling tank, adding 60-100 parts by mass of deionized water, 5-10 parts by mass of a binder, 0.5-5 parts by mass of a plasticizer and 0.5-1 part by mass of a defoaming agent, carrying out ball milling for 18 hours, filtering to remove undissolved binder and plasticizer and agglomerated magnetic powder, and carrying out vacuum defoaming to remove bubbles generated in the ball milling process to obtain slurry for tape casting;
(6) and casting to obtain the final product.
Compared with the prior art, the invention has the following advantages and effects:
1. the surface of the magnetic powder is soaked in an alkaline solution, so that-OH active groups on the surface of the magnetic powder are increased, and the magnetic powder is more easily combined with a coupling agent;
2. the use of the coupling agent forms an insulating layer on the surface of the flaky magnetic powder, thereby effectively preventing the magnetic powder from contacting with each other and improving the dispersibility of the flaky magnetic powder in slurry;
3. according to the invention, the electromagnetic performance of the composite material is enhanced by the controllable growth of the ferrite material on the surface of the soft magnetic metal and the interface coupling effect of the two materials, and the designed core-shell structure composite material integrates the excellent performances of the ferrite material and the metal soft magnetic material and has high magnetic conductivity, low loss, broadband wave absorbing property and wide temperature stability;
4. the aqueous film forming material adopted in the invention solves the problems of slurry magnetic powder dispersibility, stability and viscosity, realizes large-scale preparation of environment-friendly, low-toxicity, harmless and ultrathin flexible film coiled materials, and the composite film material has the acid and alkali resistance of 14, the physical tensile strength of 1000N, no transverse lines, longitudinal lines and pitting holes in the tensile appearance, is free from cracking after being curled at will and is easy to cut.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments.
Example 1
(1) Putting 100 parts by mass of the Fe-Si-Al magnetic powder into a stirrer, adding 5 parts by mass of sodium hydroxide and 95 parts by mass of deionized water, stirring for 1 hour to fully wet and uniformly disperse the magnetic powder in water, and drying in vacuum;
(2) adding 100 parts by mass of iron-silicon-aluminum magnetic powder, 3 parts by mass of gamma-glycidyl ether oxypropyltrimethoxysilane and 197 parts by mass of deionized water into a stirrer, stirring for 1 hour, taking out, and vacuum drying for later use;
(3) adding 100 parts by mass of iron-silicon-aluminum magnetic powder, 1 part by mass of triethanolamine and 100 parts by mass of deionized water into a ball milling tank (ball-to-material ratio is 10: 1), ball milling for 20 hours at the rotating speed of 250r/min, and drying in vacuum for later use;
(4) weighing a proper amount of chloride salts of Fe, Zn and Mn according to the coating amount of the manganese-zinc ferrite of 2wt% (Mn: Zn = 0.6: 0.4), adding 100ml of water, dissolving the chloride salts in a water bath at 60 ℃, stirring the mixture by using a magnetic stirrer, adding 100 parts by mass of flaky iron-silicon-aluminum-magnetic powder, dropwise adding 2 mol/L of sodium hydroxide to adjust the pH to be 8-10 at the rotating speed of 200r/min, continuing for 60min, standing for 24h, washing, filtering, and drying;
(5) taking 100 parts by mass of a soft magnetic metal composite material, 85 parts by mass of deionized water, 6 parts by mass of a composite binder (PVA: PAA = 1: 1), 3.5 parts by mass of glycerol and 0.5 part by mass of a defoaming agent, carrying out ball milling for 18h, filtering to remove undissolved binder and plasticizer and agglomerated magnetic powder, and carrying out vacuum defoaming to remove bubbles generated in the ball milling process to obtain slurry for tape casting;
(6) casting on a casting machine, wherein the base material is a PET film, and the temperature of a heating section is 80 ℃, so that the film material can be obtained.
Example 2
(1) Putting 100 parts by mass of the Fe-Si-Al magnetic powder into a stirrer, adding 5 parts by mass of sodium hydroxide and 95 parts by mass of deionized water, stirring for 1 hour to fully wet and uniformly disperse the magnetic powder in water, and drying in vacuum;
(2) adding 100 parts by mass of iron-silicon-aluminum magnetic powder, 5 parts by mass of gamma-aminopropyltriethoxysilane and 195 parts by mass of deionized water into a stirrer, stirring for 1h, taking out, and vacuum drying for later use;
(3) adding 100 parts by mass of iron-silicon-aluminum magnetic powder, 1 part by mass of polyethylene glycol 400 and 100 parts by mass of deionized water into a ball milling tank (ball-to-material ratio is 10: 1), ball milling for 20 hours at the rotating speed of 250r/min, and drying in vacuum for later use;
(4) weighing a proper amount of chloride salts of Fe, Zn and Ni according to the coating amount of 5wt% of nickel-zinc ferrite (Ni: Zn = 0.5: 0.5), adding 100ml of water, dissolving the chloride salts in water bath at 60 ℃, stirring the mixture by using a magnetic stirrer, adding 100 parts by mass of flaky iron-silicon-aluminum-magnetic powder, dropwise adding 2 mol/L of sodium hydroxide to adjust the pH to be 8-10 at the rotating speed of 200r/min, continuing for 60min, standing for 24h, washing, filtering, and drying;
(5) taking 100 parts by mass of a soft magnetic metal composite material, 90 parts by mass of deionized water, 8 parts by mass of a composite binder (PVA: PAA = 1: 1), 4 parts by mass of glycerol and polyethylene glycol 400 (the addition ratio is 1: 1), 0.5 part by mass of a defoaming agent, carrying out ball milling for 18h, filtering to remove undissolved binder and plasticizer and agglomerated magnetic powder, and carrying out vacuum defoaming to remove bubbles generated in the ball milling process to obtain slurry for tape casting;
(6) casting on a casting machine, wherein the base material is a PET film, and the temperature of a heating section is 80 ℃, so that the film material can be obtained.
Example 3
(1) Putting 100 parts by mass of iron-silicon-nickel magnetic powder into a stirrer, adding 5 parts by mass of sodium hydroxide and 95 parts by mass of deionized water, stirring for 1 hour to fully wet and uniformly disperse the magnetic powder in water, and drying in vacuum;
(2) adding 100 parts by mass of iron-silicon-nickel magnetic powder, 4 parts by mass of gamma-glycidoxypropyltrimethoxysilane and 196 parts by mass of deionized water into a stirrer, stirring for 1h, taking out, and vacuum drying for later use;
(3) adding 100 parts by mass of iron-silicon-nickel magnetic powder, 1 part by mass of triethanolamine and 100 parts by mass of deionized water into a ball milling tank (ball-material ratio is 10: 1), ball milling for 15 hours at the rotating speed of 250r/min, and drying in vacuum for later use;
(4) weighing a proper amount of chloride salts of Fe, Zn and Mn according to 5wt% of manganese-zinc ferrite coating amount (Mn: Zn = 0.6: 0.4), adding 100ml of water, dissolving the chloride salts in a water bath at 60 ℃, stirring the mixture by using a magnetic stirrer, adding 100 parts by mass of flaky iron-silicon-nickel magnetic powder, dropwise adding 2 mol/L of sodium hydroxide to adjust the pH to be 8-10 at the rotating speed of 200r/min, keeping the speed for 60min, standing for 24h, washing, filtering, and drying;
(5) taking 100 parts by mass of a soft magnetic metal composite material, 90 parts by mass of deionized water, 5 parts by mass of a composite binder (PVA: PAA = 1: 1), 2.8 parts by mass of glycerol and 0.5 part by mass of a defoaming agent, carrying out ball milling for 18h, filtering to remove undissolved binder and plasticizer and agglomerated magnetic powder, and carrying out vacuum defoaming to remove bubbles generated in the ball milling process to obtain slurry for tape casting;
(6) casting on a casting machine, wherein the base material is a PET film, and the temperature of a heating section is 80 ℃, so that the film material can be obtained. The films of examples 1-3 were subjected to the relevant tests of the following table, with the results of the performance tests shown in table 1.
TABLE 1 Performance testing of soft magnetic Metal cast films
| Experiment number | L1-1 | L1-2 | L1-3 | L2-1 | L2-2 | L2-3 | L3-1 | L3-2 | L3-3 |
| Thickness (mm) | 0.05 | 0.15 | 0.2 | 0.05 | 0.15 | 0.2 | 0.05 | 0.15 | 0.2 |
| Magnetic permeability | 150 | 180 | 260 | 130 | 165 | 225 | 120 | 150 | 210 |
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (11)
1. A preparation method of soft magnetic metal composite water-based tape casting slurry and a film thereof is characterized in that the soft magnetic metal composite water-based tape casting slurry comprises the following raw materials in parts by weight: 100 parts of soft magnetic metal composite material, 150 parts of deionized water and 350 parts of dispersant, 5-10 parts of binder, 2.5-5 parts of plasticizer, 0.5-1 part of defoamer, 1-10 parts of alkaline solution and 0.1-5 parts of coupling agent.
2. A soft magnetic metal composite according to claim 1, characterized in that: the magnetic metal powder comprises one or more of Fe-Si-Al, Fe-Si-Cr, Fe-Si-Ni, amorphous iron-based alloy and nanocrystalline iron-based alloy.
3. A soft magnetic metal composite according to claim 1, characterized in that: the soft magnetic material is one or more of nickel zinc ferrite and manganese zinc ferrite.
4. A soft magnetic metal composite water based casting slurry according to claim 1, characterized in that: the dispersant is one or more of triethanolamine and polyethylene glycol.
5. A soft magnetic metal composite water based casting slurry according to claim 1, characterized in that: the binder is one or more of polyvinyl alcohol, polyacrylic acid and waterborne polyurethane.
6. A soft magnetic metal composite water based casting slurry according to claim 1, characterized in that: the plasticizer is one or more of glycerol and polyethylene glycol.
7. A soft magnetic metal composite water based casting slurry according to claim 1, characterized in that: the defoaming agent is a high-carbon alcohol defoaming agent.
8. A soft magnetic metal composite water based casting slurry according to claim 1, characterized in that: the alkaline solution is low-concentration sodium hydroxide or ammonia water.
9. A soft magnetic metal composite water based casting slurry according to claim 1, characterized in that: the coupling agent is a silane coupling agent.
10. The preparation method of the soft magnetic metal composite water-based tape casting slurry and the film thereof according to any one of claims 1 to 9, characterized by comprising the following steps:
(1) adding 100 parts by mass of metal magnetic powder into a stirrer, adding 1-10 parts of alkaline solution and 90-100 parts of deionized water, stirring for 1 hour to fully wet and uniformly disperse the magnetic powder in water, filtering and drying;
(2) adding 100 parts of the magnetic powder prepared in the step (1), 0.1-5 parts of a coupling agent and 190-200 parts of deionized water into a stirrer, and stirring for 1 hour to fully wet and uniformly disperse the magnetic powder in a solvent;
(3) adding the magnetic metal powder prepared in the step (2), deionized water and a dispersing agent into a ball milling tank according to a ratio (ball-to-material ratio is 10: 1), ball milling for 15-20 h at a rotating speed of 250 revolutions per minute, and vacuum drying for later use;
(4) weighing corresponding chloride salt required by ferrite according to a ratio, adding 100ml of water, dissolving the chloride salt in water bath at 60 ℃, stirring the mixture by using a magnetic stirrer, adding 100 parts by mass of the flaky metal magnetic powder prepared in the step (3), dropwise adding 2 mol/L of sodium hydroxide to adjust the pH to be 8-10, keeping the rotation speed at 200r/min for 60min, standing for 24h, washing, filtering and drying for later use;
(5) adding the soft magnetic composite material prepared in the step (4) into a ball milling tank, adding 60-100 parts by mass of deionized water, 5-20 parts by mass of a binder, 1-10 parts by mass of a plasticizer and 0.5-1 part of a defoaming agent, carrying out ball milling for 18 hours, filtering to remove undissolved binder and plasticizer and agglomerated magnetic powder, and carrying out vacuum defoaming to remove bubbles generated in the ball milling process to obtain slurry for tape casting;
(6) and casting to obtain the final product.
11. The method for preparing a soft magnetic metal composite material thin film according to claim 10, characterized in that: the thickness of the prepared film material is 0.02-2 mm.
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| CN104036906A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | Tape-casting temperature isostatic pressing composite molding preparation method of metal soft magnetic composite material |
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Application publication date: 20200721 |