CN113560570B - Preparation method of iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance - Google Patents
Preparation method of iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance Download PDFInfo
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Abstract
The invention discloses a preparation method of an iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance, and belongs to the technical field of magnetic materials. The preparation method of the invention mainly prepares the iron-silicon-aluminum-nickel powder by combining mechanical ball milling with high-temperature solution treatment, and then combines with a nano silicon oxide insulation process and a matched forming and annealing heat treatment process to prepare the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance. The relative magnetic permeability of the iron-silicon-aluminum-nickel powder core at 100kHz/1V is 60.3-104.7, and the loss at 50kHz/100mT is 197.6-301.2 mW/cm 3 The DC bias performance under the magnetic field intensity of 100Oe is 68.7-82.3%, and the saturation magnetic polarization intensity is 1.40-1.49T. The preparation method can well improve the defects of poor direct current bias performance and low saturation magnetic polarization strength of the iron-silicon-aluminum powder core.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and relates to a preparation method of an iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance.
Background
Sendust was developed in the 30 s of the 20 th century in japan, hence the name sendust alloy. Because the magnetocrystalline anisotropy constant and the magnetostriction coefficient are zero, the resistivity is high, and the components do not contain precious metal elements, the ferrosilicon-aluminum alloy has the advantages of low loss, low noise, extremely low cost and the like, and is widely applied to various power electronic devices.
At present, the sendust core prepared by crushing sendust powder by ball milling becomes one of the most downstream powder cores, but the sendust cores have poor direct current bias performance and low saturation magnetic polarization strength, so that the development requirements of high power and microminiaturization of downstream power electronic equipment cannot be met. Therefore, technicians select the spherical sendust powder prepared by the gas atomization process to partially improve the direct current bias performance of the sendust powder core, but still cannot meet the anti-saturation requirement of high-power application occasions, and because the alloy components are not changed, the saturation magnetic polarization strength is only slightly improved due to the increase of the powder core density, but the improvement is not obvious.
For the iron-silicon-aluminum alloy, the addition of a proper amount of nickel element is beneficial to improving the magnetic polarization strength of the alloy and improving the anti-saturation capacity of the alloy, so that the iron-silicon-aluminum-nickel powder core can be prepared to realize the comprehensive improvement of the magnetic performance of the iron-silicon-aluminum powder core. However, the problems that silicon and aluminum elements are easy to ablate in a smelting process, and segregation often occurs to alloy components due to uneven cooling rate in a casting process and the like exist in the preparation process of the iron-silicon-aluminum-nickel alloy powder at present. Meanwhile, the existing sendust powder on the market is basically manufactured by using a gas atomization process, a large amount of nitrogen is consumed in production, and a high proportion of coarse powder waste is generated, so that the manufacturing cost is high. These problems all limit the manufacturing and wide application of the high cost performance sendust powder. In order to solve the problems, the invention provides a low-cost iron-silicon-aluminum-nickel alloy powder preparation process combining mechanical ball milling with high-temperature solution treatment, which can be used for preparing iron-silicon-aluminum-nickel alloy magnetic powder with uniform components and higher solid solubility.
Disclosure of Invention
The invention aims to provide a low-cost iron-silicon-aluminum-nickel alloy powder preparation process combining mechanical ball milling with high-temperature solid solution treatment, which is used for preparing iron-silicon-aluminum-nickel alloy magnetic powder with uniform components and higher solid solubility. The problems of ablation of silicon and aluminum elements during smelting of the conventional iron-silicon-aluminum-nickel alloy and alloy component segregation caused by uneven cooling rate during casting are avoided, a large amount of nitrogen does not need to be consumed, no coarse powder waste is generated, and the production cost of the iron-silicon-aluminum-nickel powder core can be effectively reduced on the premise of improving the magnetic performance.
The preparation operation steps of the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance are as follows:
(1) Preparation of alloy powder
Mixing iron powder, silicon powder, aluminum powder and nickel powder according to a mass ratio to obtain mixed powder, wherein the mass of silicon in the mixed powder is 10-20%, the mass of aluminum is 6-15%, the mass of nickel is 20-35%, and the balance is iron;
performing primary ball milling on the mixed powder, wherein the ball milling medium is ethanol, and stearic acid is added during ball milling, and the addition amount of the stearic acid is 5-15% of the mass of the mixed powder; obtaining alloy powder;
(2) First cleaning
Cleaning the alloy powder for 3-5 times by using acetone, and removing auxiliary materials on the surface of the magnetic powder;
(3) Preparation of iron-silicon-aluminum-nickel alloy solid solution
(3.1) annealing the cleaned alloy powder at the temperature of 600-800 ℃;
(3.2) carrying out high-temperature solution treatment at the temperature of 1000-1300 ℃ under the protection of nitrogen, and cooling to room temperature along with the furnace to obtain an iron-silicon-aluminum-nickel alloy solid solution;
(4) Second ball milling
Performing secondary ball milling on the iron-silicon-aluminum-nickel alloy solid solution, wherein the ball milling medium is ethanol; adding stearic acid during ball milling, wherein the adding amount of the stearic acid is 4-12% of the mass of the mixed powder, so as to obtain ball-milled powder;
(5) Second cleaning
Cleaning the ball-milling powder with acetone for 3-5 times, and removing auxiliary materials on the surface of the magnetic powder;
(6) Second annealing
Annealing the cleaned ball-milled powder at the temperature of 600-800 ℃ to obtain annealed powder;
(7) Preparation of green compact powder
Uniformly mixing the annealing powder with nanoscale silicon oxide, wherein the mass of the silicon oxide is 0.5-1% of that of the annealing powder, and obtaining green blank powder;
(8) Preparation of the Green bodies
Uniformly mixing the green body powder and a release agent, wherein the use amount of the release agent is 4-8 per mill of the mass of the green body powder, and the release agent passes through a 80-mesh screen; pressing and forming in a mould to obtain a green body;
(9) Preparation of iron-silicon-aluminum-nickel powder core
Annealing the green body to obtain an iron-silicon-aluminum-nickel powder core;
the relative magnetic permeability of the iron-silicon-aluminum-nickel powder core at 100kHz/1V is 60.3-104.7, and the loss at 50kHz/100mT is 197.6-301.2 mW/cm 3 The DC bias performance under the magnetic field intensity of 100Oe is 68.7-82.3%, and the saturation magnetic polarization intensity is 1.40-1.49T.
The further concrete technical scheme is as follows:
in the step (1), ball milling conditions are as follows: the rotating speed is 300-600 r/min, and the ball milling time is 9-36 h.
In the step (3), annealing conditions are as follows: the heating rate is 5-8 ℃/min, and the annealing heat preservation time is 60-90 min; high-temperature solid solution conditions: the heating rate is 5-8 ℃/min, and the heat preservation time is 120-180 min;
the purpose of annealing is to eliminate the internal stress generated by the alloy powder during ball milling through annealing, and to ensure that the components in the alloy powder are uniformly distributed through diffusion. The high-temperature solution treatment has the effect of further uniformly distributing the components of each component by utilizing the high-temperature solution treatment to form the iron-silicon-aluminum-nickel alloy solid solution with uniform components.
In the step (4), ball milling conditions are as follows: the rotating speed is 500-700 r/min, and the ball milling time is 4-12 h.
In the step (6), annealing conditions are as follows: the heating rate is 5-8 ℃/min, and the annealing heat preservation time is 60-90 min.
In the step (8), the pressing pressure is 1300-1800 MPa.
In the step (9), the green annealing conditions are as follows: firstly, the temperature is 200-400 ℃, the temperature is kept for 40-80 min, then the annealing temperature is increased to 700-900 ℃, and the temperature is kept for 60-90 min.
The beneficial technical effects of the invention are embodied in the following aspects:
1. the invention combines the mechanical ball milling with the high-temperature solid solution treatment method, utilizes the high-temperature diffusion principle to prepare the iron-silicon-aluminum-nickel alloy magnetic powder with uniform components and higher solid solubility, avoids the ablation of silicon and aluminum elements during alloy smelting and the alloy component segregation caused by uneven cooling speed in the casting process, reduces the nitrogen consumption, does not generate coarse powder waste, effectively reduces the manufacturing cost, and provides guarantee for preparing the iron-silicon-aluminum-nickel powder core with excellent cost performance. Fig. 1 shows an X-ray diffraction (XRD) spectrum of the fe-si-al-ni magnetic powder prepared by the present invention. As can be seen from fig. 1, since fe-si-al-ni takes fe as a matrix, ni is dissolved into fe crystal lattice to form a substitutional solid solution, and al and si form an interstitial solid solution, only the diffraction peak of FeNi solid solution is observed in fig. 1. The fact that the silicon and the aluminum are both dissolved into the crystal lattice of the iron proves that the iron-silicon-aluminum-nickel alloy powder prepared by the invention has higher solid solubility.
2. The relative permeability of the iron-silicon-aluminum-nickel powder core prepared by the invention is 60.3-104.7, the magnetic performance of the iron-silicon-aluminum-nickel powder core is compared with that of an iron-silicon-aluminum powder core and an air-atomized iron-silicon-aluminum powder core with the same permeability grade (60 +/-8%), and the comparison data is shown in Table 1. It can be seen that the loss of the iron-silicon-aluminum-nickel powder core at 50kHz/100mT is 301.2 mW/cm under the condition of the same magnetic permeability level 3 The direct current bias performance of 100Oe is 82.3%, and the magnetic performance is greatly improved compared with two conventional powder cores of sendust and gas atomization sendust. Fig. 2 shows the magnetization curves of the samples of the three cores listed in table 1, which are sendust, and aerosolised sendust, showing that the sendust core has a high saturation magnetic polarization strength of about 1.40T. In addition, the performance of the iron-silicon-aluminum-nickel powder core prepared by the invention (sample 1) is compared with that of the iron-silicon-aluminum-nickel powder core disclosed in publication document CN111261357a (sample 2), and the comparative data are shown in table 2. It can be seen that, when the magnetic permeability levels are the same, the loss of the two samples at 50kHz/100mT is close, but the iron-silicon-aluminum-nickel powder core prepared by the invention has higher saturation magnetic polarization strength and better direct current bias performance.
Drawings
FIG. 1 is an XRD diffraction pattern of the Fe-Si-Al-Ni magnetic powder prepared by the invention.
FIG. 2 is a graph of the magnetization curves for the sendust, and aerosolised sendust cores listed in Table 1.
Detailed Description
The present invention will be described with reference to specific examples.
Example 1
The preparation operation steps of the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance are as follows:
(1) Preparation of alloy powder
640g of iron powder, 100g of silicon powder, 60g of aluminum powder and 200g of nickel powder are added into a ball mill according to 1000g of total mass, 1000g of ethanol and 50g of stearic acid are added, and first ball milling is carried out. Ball milling conditions: the rotating speed is 300r/min, and the time is 9h; obtaining the alloy powder.
(2) First cleaning
And cleaning the alloy powder for 3 times by using acetone to remove the auxiliary materials on the surface of the magnetic powder.
(3) Preparation of iron-silicon-aluminum-nickel alloy solid solution
(3.1) firstly annealing the cleaned alloy powder at 600 ℃ for the first time, wherein the heating rate is 5 ℃/min, and the annealing heat preservation time is 60min;
(3.2) raising the temperature to 1000 ℃ for high-temperature solution treatment, wherein the temperature raising rate is 5 ℃/min, the heat preservation time is 120min, and the protective gas is nitrogen; obtaining the Fe-Si-Al-Ni alloy solid solution.
(4) Second ball milling
Putting the iron-silicon-aluminum-nickel alloy solid solution into a ball mill, adding 1000g of ethanol and 40g of stearic acid, and carrying out secondary ball milling; ball milling conditions: the rotating speed is 500r/min, and the ball milling time is 4h; and obtaining the ball-milling powder.
(5) Second cleaning
And cleaning the ball-milling powder material for 3 times by using acetone to remove auxiliary materials on the surface of the magnetic powder.
(6) Second annealing
And annealing the cleaned ball-milled powder at 600 ℃, wherein the heating rate is 5 ℃/min, and the annealing heat preservation time is 60min, so as to obtain the annealed powder.
(7) Preparation of green powder
The annealed powder was mixed uniformly with 5g of nano-grade silica to obtain green powder.
(8) Preparation of the Green bodies
Uniformly mixing the green body powder with 4g of release agent, and screening the mixture through a 80-mesh screen; and pressing and forming in a die to obtain a green body, wherein the pressing pressure is 1300MPa.
(9) Preparation of iron-silicon-aluminum-nickel powder core
Annealing the green body, firstly preserving heat at 200 ℃ for 40min, then increasing the annealing temperature to 700 ℃ and preserving heat for 60min to obtain an iron-silicon-aluminum-nickel powder core;
the iron-silicon-aluminum-nickel powder core has the relative magnetic permeability of 104.7 at 100kHz/1V and the loss of 197.6 mW/cm at 50kHz/100mT 3 The dc bias performance at 100Oe field strength was 68.7% and the saturation magnetic polarization strength was 1.49T.
Example 2
The preparation operation steps of the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance are as follows:
(1) Preparation of alloy powder
440g of iron powder, 150g of silicon powder, 110g of aluminum powder and 300g of nickel powder are added into a ball mill according to the total mass of 1000g, 3000g of ethanol and 100g of stearic acid are added, and the first ball milling is carried out. Ball milling conditions: the rotating speed is 500r/min, and the time is 18h; obtaining the alloy powder.
(2) First cleaning
And cleaning the alloy powder for 4 times by using acetone to remove the auxiliary materials on the surface of the magnetic powder.
(3) Preparation of iron-silicon-aluminum-nickel alloy solid solution
(3.1) firstly annealing the cleaned alloy powder at 700 ℃ for the first time, wherein the heating rate is 7 ℃/min, and the annealing heat preservation time is 70min;
(3.2) heating to 1200 ℃ for high-temperature solution treatment, wherein the heating rate is 7 ℃/min, the heat preservation time is 150min, and the protective gas is nitrogen; obtaining the Fe-Si-Al-Ni alloy solid solution.
(4) Second ball milling
Putting the iron-silicon-aluminum-nickel alloy solid solution into a ball mill, adding 3000g of ethanol and 80g of stearic acid, and carrying out secondary ball milling; ball milling conditions: the rotating speed is 600r/min, and the ball milling time is 8h; and obtaining the ball-milling powder.
(5) Second cleaning
And cleaning the ball-milling powder material with acetone for 4 times to remove the auxiliary materials on the surface of the magnetic powder.
(6) Second annealing
And annealing the cleaned ball-milled powder at 700 ℃, wherein the heating rate is 7 ℃/min, and the annealing heat preservation time is 75min, so as to obtain the annealed powder.
(7) Preparation of green compact powder
And uniformly mixing the annealing powder with 8g of nano-grade silicon oxide to obtain green body powder.
(8) Preparation of the Green bodies
Uniformly mixing the green blank powder with 6g of a release agent, and screening the mixture through a 80-mesh screen; and pressing and forming in a die to obtain a green body, wherein the pressing pressure is 1500MPa.
(9) Preparation of iron-silicon-aluminum-nickel powder core
Annealing the green body, firstly preserving heat at 300 ℃ for 60min, then increasing the annealing temperature to 800 ℃ and preserving heat for 70min to obtain an iron-silicon-aluminum-nickel powder core;
the iron-silicon-aluminum-nickel powder core has the relative magnetic permeability of 82.3 at 100kHz/1V and the loss of 256.4 mW/cm at 50kHz/100mT 3 The DC bias performance at 100Oe magnetic field strength was 74.9% and the saturation magnetic polarization strength was 1.44T.
Example 3
The preparation operation steps of the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance are as follows:
(1) Preparation of alloy powder
Adding 300g of iron powder, 200g of silicon powder, 150g of aluminum powder and 350g of nickel powder into a ball mill according to 1000g of total mass, adding 5000g of ethanol and 150g of stearic acid, and carrying out first ball milling. Ball milling conditions are as follows: the rotating speed is 600r/min, and the time is 36h; obtaining the alloy powder.
(2) First cleaning
And cleaning the alloy powder for 5 times by using acetone to remove the auxiliary materials on the surface of the magnetic powder.
(3) Preparation of iron-silicon-aluminum-nickel alloy solid solution
(3.1) firstly annealing the cleaned alloy powder at 800 ℃ for the first time, wherein the heating rate is 8 ℃/min, and the annealing heat preservation time is 90min;
(3.2) heating to 1300 ℃ for high-temperature solution treatment, wherein the heating rate is 8 ℃/min, the heat preservation time is 180min, and the protective gas is nitrogen; obtaining the Fe-Si-Al-Ni alloy solid solution.
(4) Second ball milling
Putting the iron-silicon-aluminum-nickel alloy solid solution into a ball mill, adding 5000g of ethanol and 120g of stearic acid, and carrying out secondary ball milling; ball milling conditions: the rotating speed is 700r/min, and the ball milling time is 12h; to obtain the ball-milling powder.
(5) Second cleaning
And cleaning the ball-milling powder with acetone for 5 times to remove the auxiliary materials on the surface of the magnetic powder.
(6) Second annealing
And annealing the cleaned ball-milled powder at 800 ℃, wherein the heating rate is 8 ℃/min, and the annealing heat preservation time is 90min, so as to obtain the annealed powder.
(7) Preparation of green compact powder
The annealed powder was mixed uniformly with 10g of nano-grade silica to obtain green powder.
(8) Preparation of the Green bodies
Uniformly mixing the green body powder with 8g of release agent, and screening the mixture through a 80-mesh screen; and pressing and forming in a die to obtain a green body, wherein the pressing pressure is 1800MPa.
(9) Preparation of iron-silicon-aluminum-nickel powder core
Annealing the green body, and keeping the temperature at 400 ℃ for 80min, then increasing the annealing temperature to 900 ℃ and keeping the temperature for 90min to obtain an iron-silicon-aluminum-nickel powder core;
the iron-silicon-aluminum-nickel powder core has the relative magnetic permeability of 60.3 at 100kHz/1V and the loss of 301.2 mW/cm at 50kHz/100mT 3 The DC bias performance at 100Oe magnetic field strength was 82.3%, and the saturation magnetic polarization strength was 1.40T.
It will be understood by those skilled in the art that the foregoing is only an exemplary embodiment of the present invention, and is not intended to limit the invention to the particular forms disclosed, since various modifications, substitutions and improvements within the spirit and scope of the invention are possible and within the scope of the appended claims.
Claims (7)
1. A preparation method of an iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance is characterized by comprising the following operation steps:
(1) Preparing alloy powder:
mixing iron powder, silicon powder, aluminum powder and nickel powder according to a mass ratio to obtain mixed powder, wherein the mass of silicon in the mixed powder is 10-20%, the mass of aluminum is 6-15%, the mass of nickel is 20-35%, and the balance is iron;
performing first ball milling on the mixed powder, wherein the ball milling medium is ethanol, and stearic acid is added during ball milling, and the addition amount of the stearic acid is 5-15% of the mass of the mixed powder, so as to obtain alloy powder;
(2) Cleaning for the first time:
cleaning the alloy powder with acetone for 3-5 times to remove auxiliary materials on the surface of the alloy powder;
(3) Preparing an iron-silicon-aluminum-nickel alloy solid solution:
(3.1) annealing the cleaned alloy powder at the temperature of 600-800 ℃;
(3.2) carrying out high-temperature solution treatment at the temperature of 1000-1300 ℃ under the protection of nitrogen, and cooling to room temperature along with the furnace to obtain an iron-silicon-aluminum-nickel alloy solid solution;
(4) Ball milling for the second time:
performing secondary ball milling on the iron-silicon-aluminum-nickel alloy solid solution, wherein the ball milling medium is ethanol, and stearic acid is added during ball milling, wherein the adding amount of the stearic acid is 4-12% of the mass of the mixed powder, so as to obtain ball-milled powder;
(5) And (3) cleaning for the second time:
cleaning the ball-milling powder with acetone for 3-5 times, and removing auxiliary materials on the surface of the ball-milling powder;
(6) And (3) second annealing:
annealing the cleaned ball-milled powder at the temperature of 600-800 ℃ to obtain annealed powder;
(7) Preparing green body powder:
uniformly mixing the annealing powder with nanoscale silicon oxide, wherein the mass of the silicon oxide is 0.5-1% of that of the annealing powder, and obtaining green blank powder;
(8) Preparing a green body:
uniformly mixing the green body powder and a release agent, wherein the use amount of the release agent is 4-8 per mill of the mass of the green body powder, and the mixture of the green body powder and the release agent passes through a 80-mesh screen to be pressed and formed in a mold to obtain a green body;
(9) Preparing an iron-silicon-aluminum-nickel powder core:
annealing the green body to obtain an iron-silicon-aluminum-nickel powder core;
the relative magnetic permeability of the iron-silicon-aluminum-nickel powder core at 100kHz/1V is 60.3-104.7, and the loss at 50kHz/100mT is 197.6-301.2 mW/cm 3 The DC bias performance under the magnetic field strength of 100Oe is 68.7-82.3%, and the saturation magnetic polarization strength is 1.40-1.49T.
2. The method for preparing the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance according to claim 1, wherein the method comprises the following steps: in the step (1), ball milling conditions are as follows: the rotating speed is 300-600 r/min, and the ball milling time is 9-36 h.
3. The method for preparing the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance according to claim 1, wherein the method comprises the following steps: in the step (3), annealing conditions are as follows: the heating rate is 5-8 ℃/min, and the annealing heat preservation time is 60-90 min; high-temperature solid solution conditions: the heating rate is 5-8 ℃/min, and the heat preservation time is 120-180 min;
the annealing aims to eliminate the internal stress generated by the alloy powder during ball milling through annealing, and the components in the alloy powder are uniformly distributed through diffusion, and the high-temperature solid solution treatment is used for further uniformly distributing the components of each component through the high-temperature solid solution treatment to form the iron-silicon-aluminum-nickel alloy solid solution with uniform components.
4. The method for preparing the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance according to claim 1, wherein the method comprises the following steps: in the step (4), ball milling conditions are as follows: the rotating speed is 500-700 r/min, and the ball milling time is 4-12 h.
5. The method for preparing the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance according to claim 1, wherein the method comprises the following steps: in the step (6), annealing conditions are as follows: the heating rate is 5-8 ℃/min, and the annealing heat preservation time is 60-90 min.
6. The method for preparing the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance according to claim 1, wherein the method comprises the following steps: in the step (8), the pressing pressure is 1300-1800 MPa.
7. The method for preparing the iron-silicon-aluminum-nickel powder core with high saturation magnetic polarization strength and high direct current bias performance according to claim 1, wherein the method comprises the following steps: in the step (9), the green annealing conditions are as follows: firstly, the temperature is 200-400 ℃, the temperature is kept for 40-80 min, then the annealing temperature is increased to 700-900 ℃, and the temperature is kept for 60-90 min.
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