Tape-casting temperature isostatic pressing composite molding preparation method of metal soft magnetic composite material

A composite material and warm isostatic pressing technology, which is applied in the fields of magnetism of inorganic materials, manufacturing of inductors/transformers/magnets, electrical components, etc., can solve the problems of non-dense green body structure, low molding density, and affecting the performance of functional materials, etc., to achieve The effect of high density uniformity, low porosity and smooth surface

Inactive Publication Date: 2014-09-10
ZHEJIANG UNIV
3 Cites 27 Cited by

AI-Extracted Technical Summary

Problems solved by technology

However, during the drying process of the casting green body, due to the volatilization of the solvent, many pits and holes will be generated on the surface and inside...
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Method used

[0044] The prepared sample structure is compact, low porosity, smooth surface, and a density of 6.9g/cm3. The samples were tested for soft magnetic properties and electrical properties, and the results are as follows: saturation magnetic flux density Bs=1.4T, coercive force Hc=235A/m, resistivity ρ=6×104Ω·cm. Excellent magnetic and electrical properties.
[0050] The prepared sample structure is compact, low porosity, smooth surface, and a density of 7.5g/cm3. The samples were tested for soft magnetic properties and electrical properties, and the results are as follows: saturation magnetic flux density Bs=1.6T, coercive force Hc=225A/m, resistivity ρ=1.8×105Ω·cm. Excellent magnetic and electrical properties.
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Abstract

The invention discloses a tapecasting temperature isostatic pressing composite molding preparation method of a metal soft magnetic composite material. The method comprises the following steps: (1) mixing a passivator and a solvent to obtain a passivating solution, and mixing, stirring and drying the passivating solution and magnetic metal powder to obtain passivated powder; (2) mixing the passivated powder, an organic solvent, a dispersing agent, an adhesive and a plasticizer according to a certain proportion, uniformly stirring, and filtering and de-foaming the mixture through a sieve to prepare slurry which is uniformly dispersed; (3) performing tape casting; (4) performing temperature isostatic pressing on a biscuit. According to the invention, solidification and isostatic pressing processes are simplified into a process, so that a metal soft magnetic composite film prepared by using the blade casting temperature isostatic composite molding method is high in resistivity and good in mechanical strength, and the density and the saturation flux density are greatly improved. By virtue of a more mature tape casting process and a temperature isostatic pressing process, the production process of the metal soft magnetic composite material is simplified, the cost is reduced, the performance is excellent, and the method has a wide application prospect in preparation of electronic devices such as film inductors.

Application Domain

Technology Topic

Examples

  • Experimental program(4)

Example Embodiment

[0039] Example 1:
[0040] 1) Mix phosphoric acid and acetone into a passivation solution with a mass fraction of 0.6%, and take reduced iron powder with an average particle size of 150 μm and passivation solution for passivation at a mass ratio of 1:0.01, and stir in a mixer 0.5h, put into the oven for passivation, passivation temperature is 70℃, passivation time is 1h, and passivation powder is obtained. Add a mixed solvent to the passivation powder. The solvent is trichloroethylene and ethanol mixed in a ratio of 1:1, and the dispersant triolein is added, the above raw materials are mixed, stirred for 30h, and then the binder epoxy resin is added to increase The plasticizer is glycerin and dioctyl phthalate, the mass fraction of the binder is 20%, and the mass ratio of the binder to the plasticizer is 0.5. Stir the slurry for another 36 hours, disperse it with ultrasound for 5 minutes, filter it through a screen, and vacuum degas to prepare a uniformly dispersed slurry. The volume fraction of solvent in the slurry is 60% of the slurry, and the volume fraction of dispersant is that of the slurry. 5%, slurry viscosity is 100mPa·s, pH value is 5.7, temperature is 32°C.
[0041] 2) The ambient temperature of the casting delay is 28°C, the casting speed used is 1.0cm/s, the height of the doctor blade is controlled at 0.5mm, and the high temperature resistant ceramic is used as the substrate during the casting process.
[0042] 3) Preform warm isostatic pressing
[0043] The green body is dried at a drying temperature of 24° C., a relative humidity of 40%, and the thickness of the green body after the slurry is dried is 0.2 mm. Cut the dried blank into a certain shape, and then perform warm isostatic pressing with 20 laminated sheets, the pressure is 350MPa, the pressing temperature is 120°C, and the pressure holding time is 1.5h. After the sample is cooled, the pressure is released to obtain the final sample .
[0044] The prepared sample has dense structure, low porosity, smooth surface and density of 6.9g/cm 3. The samples were tested for soft magnetic properties and electrical properties. The results are as follows: saturation magnetic flux density Bs=1.4T, coercivity Hc=235A/m, resistivity ρ=6×10 4 Ω·cm. Excellent magnetic and electrical properties.

Example Embodiment

[0045] Example 2:
[0046] 1) Mix phosphoric acid and ethanol into a passivation solution with a mass fraction of 0.8%, take the iron-nickel alloy powder with an average particle size of 0.1μm and the passivation solution for passivation in a mass ratio of 1:0.08, in a mixer Stir for 0.1h, put into an oven for passivation, passivation temperature is 100℃, passivation time is 0.1h, and passivation powder is obtained. Add a mixed solvent to the passivation powder, the solvent is methyl ethyl ketone and ethanol mixed in 1:10, and add the dispersant herring oil, mix the above raw materials, stir for 20h, and then add the binder epoxy resin, plasticizer polyethylene Diol, the mass fraction of the binder is 10%, and the mass ratio of binder to plasticizer is 0.8. Stir the slurry for another 30 hours, disperse it by ultrasonic for 3 minutes, filter it through a screen, and vacuum degas to prepare a uniformly dispersed slurry. The volume fraction of the solvent in the slurry is 60% of the slurry, and the volume fraction of the dispersant is that of the slurry. 5%, the annual slurry is 1mPa·s, the pH is 12, and the temperature is 30°C.
[0047] 2) The ambient temperature of the casting delay is 28°C, the casting speed adopted is 1.0cm/s, the height of the doctor blade is controlled at 0.8mm, and the high temperature resistant ceramic is used as the substrate during the casting process.
[0048] 3) Preform warm isostatic pressing
[0049] The green body is dried at a drying temperature of 24° C., a relative humidity of 40%, and the thickness of the green body after drying of the slurry is 0.3 mm. Cut the dried blank into a certain shape, and then perform warm isostatic pressing with 20 laminated sheets, the pressure is 400MPa, the pressing temperature is 120℃, and the pressure holding time is 0.5h. After the sample is cooled, the pressure is released to obtain the final sample .
[0050] The prepared sample has compact structure, low porosity, smooth surface, and density of 7.5g/cm 3. The samples were tested for soft magnetic properties and electrical properties, and the results were as follows: saturation magnetic flux density Bs=1.6T, coercivity Hc=225A/m, resistivity ρ=1.8×10 5 Ω·cm. Excellent magnetic and electrical properties.

Example Embodiment

[0051] Example 3:
[0052] 1) Mix phosphoric acid and acetone into a passivation solution with a mass fraction of 0.1%, and take the iron-silicon-aluminum alloy powder with an average particle size of 150μm and the passivation solution for passivation in a mass ratio of 1:0.1, in a mixer Stir for 0.5h, put into the oven for passivation, passivation temperature is 40℃, passivation time is 4h, and passivation powder is obtained. Add a mixed solvent to the passivation powder, the solvent is trichloroethylene and methyl ethyl ketone mixed at 10:1, and the dispersant triethanolamine is added, the above raw materials are mixed, stirred for 36h, and then added W-6C magnetic powder glue, plasticizer glycerin, The mass fraction of the binder is 20%, and the mass ratio of binder/plasticizer is 1.0. Stir the slurry for another 40h, disperse it with ultrasound for 15 minutes, filter it through a screen, and vacuum degas to prepare a uniformly dispersed slurry. The volume fraction of solvent in the slurry is 20% of the slurry, and the volume fraction of dispersant is that of the slurry. 0.2%, the annual slurry is 80mPa·s, the pH is 7, and the temperature is 30°C.
[0053] 2) The ambient temperature of the casting delay is 23°C, the casting speed adopted is 0.8cm/s, the height of the doctor blade is controlled at 0.8mm, and the high temperature resistant ceramic is used as the substrate during the casting process.
[0054] 3) Preform warm isostatic pressing
[0055] The green body is dried at a drying temperature of 24° C., a relative humidity of 30%, and the thickness of the green body after the slurry is dried is 0.3 mm. Cut the dried blank into a certain shape, and then perform warm isostatic pressing with 20 laminated sheets at a pressure of 450 MPa, a pressing temperature of 150 °C, and a pressure holding time of 2 h. After the sample is cooled, the pressure is released to obtain the final sample.
[0056] The prepared sample has dense structure, low porosity, smooth surface and density of 6.2g/cm 3. The samples were tested for soft magnetic properties and electrical properties, and the results are as follows: saturation magnetic flux density Bs=1.2T, coercivity Hc=108A/m, resistivity ρ=3.6×10 6 Ω·cm. Excellent magnetic and electrical properties.
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PUM

PropertyMeasurementUnit
Density6.9g/cm³
Saturation flux density1.4t
Coercivity235.0a/m
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

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