CN103456480A - One-step heat treatment preparation process method for soft nanocrystalline magnetic powder core - Google Patents
One-step heat treatment preparation process method for soft nanocrystalline magnetic powder core Download PDFInfo
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Abstract
The invention relates to an one-step heat treatment preparation process method for a soft nanocrystalline magnetic powder core and belongs to a nanocrystalline magnetic powder core preparation technology. Amorphous ribbon fragments of which the component is Fe73.5Cu1Nb3Si13.5B9 are directly placed into a high-energy omnibearing planetary ball mill to carry out ball milling crushing without being subjected to heat treatment; the crushed amorphous ribbon fragments are sieved into amorphous powder with different particle sizes and the amorphous powder is mixed; the mixed amorphous powder is passivated and dried in phosphoric acid solution; the passivated amorphous powder is uniformly mixed with an insulating binding agent in a wet mode; the mixture is subjected to heating volatilization and insulating coating; the amorphous powder subjected to insulating coating is placed into a die to be subjected to pressing forming; and after a formed magnetic powder core is subjected to heat treatment under the protection of inert gas, the magnetic powder core is impregnated in insulating glue. The one-step heat treatment preparation process method has high magnetic conductivity, low loss and high stability; meanwhile, preparation process steps are reduced; and production energy consumption of the nanocrystalline magnetic powder core is reduced.
Description
Technical field
The invention belongs to the preparation method of Sol-Gel powder core, relate generally to an a kind of step heat treatment process of preparing of Sol-Gel powder core.
Background technology
At present, the preparation technology of Sol-Gel powder core commonly used is: processing is solidified in spray band → band crystallization processing → fragmentation → magnetic annealing in process → powder sieving and process → insulation of grain size proportion → Passivation Treatment → insulating wrapped → compression molding → powder core destressing, there is following problems in above-mentioned technique: the three step Technologies for Heating Processing that the processing of (1) band crystallization, magnetic annealing in process, destressing are processed cause energy consumption higher, reduce production efficiency; (2) step of preparation process is more, the more difficult control of properties of product stability; (3) for preventing nanocrystalline grain growth, the temperature of the 400 ℃ of left and right of stress relief annealing after the powder core compacting is lower, and destressing is incomplete, and the magnetic property of nanocrystalline magnetic core is lower.
Summary of the invention
Purpose of the present invention is exactly the problem existed in order to overcome above-mentioned existing technique, and a kind of Sol-Gel preparation process for magnetic powder core with high magnetic permeability, low high-frequency loss, good stability is provided.
Purpose of the present invention is achieved through the following technical solutions: a step heat treatment process of preparing of Sol-Gel powder core, and the method comprises the following steps:
(1) will be without the Fe of crystallization and thermal treatment and magnetic annealing in process
73.5cu
1nb
3si
13.5b
9the amorphous band fragment directly put into the comprehensive planetary ball mill ball mill crushing of high energy, obtain the amorphous metal powder;
(2) above-mentioned amorphous metal powder is sieved, then blend together by 10%～20% and pass through the hybrid particles powder of-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder, 60%～80% by-200～+ 250 order the second powder and 10%～20%;
(3) Passivation Treatment: above-mentioned hybrid particles powder is proceeded to preheating in baking oven, in the hybrid particles powder after preheating, slowly add phosphate aqueous solution to carry out Passivation Treatment, passivation time is 2～5 hours, subsequently the hybrid particles powder after passivation is proceeded in baking oven and dries;
(4) insulating wrapped: add mica powder, silicone resin, zinc stearate, absolute ethyl alcohol in the hybrid particles powder after Passivation Treatment, the heating wet mixing volatilization that stirs, complete insulating wrapped;
(5) compression molding: the hybrid particles powder after insulating wrapped is evenly packed in mould, exerted pressure to authorized pressure in 1～3 minute, pressurize 3～5 minutes, obtain compressing powder core;
(6) one step annealings are processed: the powder core after compacting is carried out to crystallization, destressing heat treatment under vacuum or inert gas shielding, obtain the powder core after heat treatment;
(7) processing is solidified in insulation: the powder core after a step annealing is processed solidifies in glue and floods 0.5～1 hour in insulation, obtains the Sol-Gel powder core.
The process conditions of the comprehensive planetary ball mill of described high energy are: material ball ratio 1:30, and the deep bid rotating speed is 240 rev/mins, Ball-milling Time is 8 hours.
Described phosphate aqueous solution concentration is 2wt%～5wt%, adopts the diluent of deionized water as phosphoric acid.
Described silicone resin is the high temperature resistant silicon ketone resin.
3～5wt% that described mica powder addition is the magnetic quality, the 2.5wt% that the silicone resin addition is the magnetic quality, the 1wt% that the zinc stearate addition is the magnetic quality, absolute ethyl alcohol is magnetic quality 15wt%～25wt%.
In the compression molding process, slowly exert pressure, briquetting pressure is 1600MPa～2200MPa.
One step annealing treatment temperature is 500 ℃～600 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min, and described inert gas is argon gas.
It is epoxy resin that the curing glue of the insulation described in processing is solidified in insulation.
With existing Sol-Gel preparation process for magnetic powder core, compare, the present invention has following advantage: (1) is merged into a step process by the destressing heat treatment of crystallization and thermal treatment, magnetic annealing in process and powder core and is carried out, like this destressing heat treatment temperature has been improved to 150 °, made powder core obtain better internal stresses release effect.Through Experimental Comparison, nanocrystalline magnetic core magnetic property prepared by the present invention has obtained obvious raising; (2) owing to having reduced two-step thermal treatment process, greatly reduce production cost and energy loss, simplified production technology, the powder core stable performance is easier to control, and is conducive to carry out the industrialization production of nanocrystalline magnetic core; (3) mixed method of insulating compound binding agent of the present invention and magnetic is wet mixing, mixes, and the magnetic insulating wrapped is effective, and the powder core adhesive strength is higher; (4) applied range of the present invention, the prepared Sol-Gel powder core of the present invention can be widely used on the various Electronic Components Manufacturing such as communication, the energy, automobile, household electrical appliances and inductor, filter, instrument transformer, inverter.
Embodiment
Below for embodiment, the present invention is described in detail.
Example 1: be Fe by composition
73.5cu
1nb
3si
13.5b
9fragment amorphous band ball mill crushing in the comprehensive planetary ball mill of high energy, ratio of grinding media to material is 1:30, the deep bid rotating speed is 240 rev/mins, Ball-milling Time is 8 hours.The amorphous metal powder is sieved, then blend together by 10% and distribute by-200～+ 250 order the second powder and 10% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 80%.The amorphous powder that proportioning is good carries out Passivation Treatment, and passivation time is 2 hours, after powder is dried.3wt% mica powder, 2.5wt% silicone resin, 1wt% zinc stearate, 15wt% absolute ethyl alcohol will be added, the heating wet mixing volatilization that stirs in the amorphous powder after Passivation Treatment.Amorphous powder after insulating wrapped is evenly packed in mould, in 3 minutes, exert pressure to 1700MPa, pressurize 3 minutes, obtaining specification is that Φ 27.00mm * 14.60mm * 11.75mm (is that external diameter is 27.00mm, internal diameter is 14.60mm, and height is 11.75mm) powder core.Powder core after compacting is carried out to " crystallization, destressing " heat treatment under argon shield, and heat treatment temperature is 500 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min.Powder core after heat treatment is flooded 1 hour in epoxide-resin glue, obtain nanocrystalline magnetic core.The performance parameter of specimen.
Example 2: be Fe by composition
73.5cu
1nb
3si
13.5b
9fragment amorphous band ball mill crushing in the comprehensive planetary ball mill of high energy, ratio of grinding media to material is 1:30, the deep bid rotating speed is 240 rev/mins, Ball-milling Time is 8 hours.The amorphous metal powder is sieved, then blend together by 15% and distribute by-200～+ 250 order the second powder and 15% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 70%.The amorphous powder that proportioning is good carries out Passivation Treatment, and passivation time is 2 hours, after powder is dried.3wt% mica powder, 2.5wt% silicone resin, 1wt% zinc stearate, 15wt% absolute ethyl alcohol will be added, the heating wet mixing volatilization that stirs in the amorphous powder after Passivation Treatment.Amorphous powder after insulating wrapped is evenly packed in mould, in 3 minutes, exert pressure to 1700MPa, pressurize 3 minutes, obtaining specification is that Φ 27.00mm * 14.60mm * 11.75mm (is that external diameter is 27.00mm, internal diameter is 14.60mm, and height is 11.75mm) powder core.Powder core after compacting is carried out to " crystallization, destressing " heat treatment under argon shield, and heat treatment temperature is 500 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min.Powder core after heat treatment is flooded 1 hour in epoxide-resin glue, obtain nanocrystalline magnetic core.The performance parameter of specimen.
Example 3: be Fe by composition
73.5cu
1nb
3si
13.5b
9fragment amorphous band ball mill crushing in the comprehensive planetary ball mill of high energy, ratio of grinding media to material is 1:30, the deep bid rotating speed is 240 rev/mins, Ball-milling Time is 8 hours.The amorphous metal powder is sieved, then blend together by 20% and distribute by-200～+ 250 order the second powder and 20% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 60%.The amorphous powder that proportioning is good carries out Passivation Treatment, and passivation time is 2 hours, after powder is dried.3wt% mica powder, 2.5wt% silicone resin, 1wt% zinc stearate, 15wt% absolute ethyl alcohol will be added, the heating wet mixing volatilization that stirs in the amorphous powder after Passivation Treatment.Amorphous powder after insulating wrapped is evenly packed in mould, in 3 minutes, exert pressure to 1700MPa, pressurize 3 minutes, obtaining specification is that Φ 27.00mm * 14.60mm * 11.75mm (is that external diameter is 27.00mm, internal diameter is 14.60mm, and height is 11.75mm) powder core.Powder core after compacting is carried out to " crystallization, destressing " heat treatment under argon shield, and heat treatment temperature is 500 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min.Powder core after heat treatment is flooded 1 hour in epoxide-resin glue, obtain nanocrystalline magnetic core.The performance parameter of specimen.
Example 4: be Fe by composition
73.5cu
1nb
3si
13.5b
9fragment amorphous band ball mill crushing in the comprehensive planetary ball mill of high energy, ratio of grinding media to material is 1:30, the deep bid rotating speed is 240 rev/mins, Ball-milling Time is 8 hours.The amorphous metal powder is sieved, then blend together by 15% and distribute by-200～+ 250 order the second powder and 15% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 70%.The amorphous powder that proportioning is good carries out Passivation Treatment, and passivation time is 2 hours, after powder is dried.3.5wt% mica powder, 2.5wt% silicone resin, 1wt% zinc stearate, 15wt% absolute ethyl alcohol will be added, the heating wet mixing volatilization that stirs in the amorphous powder after Passivation Treatment.Amorphous powder after insulating wrapped is evenly packed in mould, in 3 minutes, exert pressure to 1700MPa, pressurize 3 minutes, obtaining specification is that Φ 27.00mm * 14.60mm * 11.75mm (is that external diameter is 27.00mm, internal diameter is 14.60mm, and height is 11.75mm) powder core.Powder core after compacting is carried out to " crystallization, destressing " heat treatment under argon shield, and heat treatment temperature is 500 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min.Powder core after heat treatment is flooded 1 hour in epoxide-resin glue, obtain nanocrystalline magnetic core.The performance parameter of specimen.
Example 5: be Fe by composition
73.5cu
1nb
3si
13.5b
9fragment amorphous band ball mill crushing in the comprehensive planetary ball mill of high energy, ratio of grinding media to material is 1:30, the deep bid rotating speed is 240 rev/mins, Ball-milling Time is 8 hours.The amorphous metal powder is sieved, then blend together by 15% and distribute by-200～+ 250 order the second powder and 15% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 70%.The amorphous powder that proportioning is good carries out Passivation Treatment, and passivation time is 2 hours, after powder is dried.4wt% mica powder, 2.5wt% silicone resin, 1wt% zinc stearate, 15wt% absolute ethyl alcohol will be added, the heating wet mixing volatilization that stirs in the amorphous powder after Passivation Treatment.Amorphous powder after insulating wrapped is evenly packed in mould, in 3 minutes, exert pressure to 1700MPa, pressurize 3 minutes, obtaining specification is that Φ 27.00mm * 14.60mm * 11.75mm (is that external diameter is 27.00mm, internal diameter is 14.60mm, and height is 11.75mm) powder core.Powder core after compacting is carried out to " crystallization, destressing " heat treatment under argon shield, and heat treatment temperature is 500 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min.Powder core after heat treatment is flooded 1 hour in epoxide-resin glue, obtain nanocrystalline magnetic core.The performance parameter of specimen.
Example 6: be Fe by composition
73.5cu
1nb
3si
13.5b
9fragment amorphous band ball mill crushing in the comprehensive planetary ball mill of high energy, ratio of grinding media to material is 1:30, the deep bid rotating speed is 240 rev/mins, Ball-milling Time is 8 hours.The amorphous metal powder is sieved, then blend together by 15% and distribute by-200～+ 250 order the second powder and 15% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 70%.The amorphous powder that proportioning is good carries out Passivation Treatment, and passivation time is 2 hours, after powder is dried.5wt% mica powder, 2.5wt% silicone resin, 1wt% zinc stearate, 15wt% absolute ethyl alcohol will be added, the heating wet mixing volatilization that stirs in the amorphous powder after Passivation Treatment.Amorphous powder after insulating wrapped is evenly packed in mould, in 3 minutes, exert pressure to 1700MPa, pressurize 3 minutes, obtaining specification is that Φ 27.00mm * 14.60mm * 11.75mm (is that external diameter is 27.00mm, internal diameter is 14.60mm, and height is 11.75mm) powder core.Powder core after compacting is carried out to " crystallization, destressing " heat treatment under argon shield, and heat treatment temperature is 500 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min.Powder core after heat treatment is flooded 1 hour in epoxide-resin glue, obtain nanocrystalline magnetic core.The performance parameter of specimen.
Example 7: be Fe by composition
73.5cu
1nb
3si
13.5b
9amorphous band under argon shield, heat-treat, heat treatment temperature is 550 ℃, annealing time is 1h.Ball mill crushing in the comprehensive planetary ball mill of high energy, ratio of grinding media to material is 1:30, and the deep bid rotating speed is 240 rev/mins, and Ball-milling Time is 2 hours.The amorphous metal powder is sieved, then blend together by 15% and distribute by-200～+ 250 order the second powder and 15% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 70%.The amorphous powder that proportioning is good carries out Passivation Treatment, and passivation time is 2 hours, after powder is dried.4wt% mica powder, 2.5wt% silicone resin, 1wt% zinc stearate, 15wt% absolute ethyl alcohol will be added, the heating wet mixing volatilization that stirs in the amorphous powder after Passivation Treatment.Amorphous powder after insulating wrapped is evenly packed in mould, in 3 minutes, exert pressure to 1700MPa, pressurize 3 minutes, obtaining specification is that Φ 27.00mm * 14.60mm * 11.75mm (is that external diameter is 27.00mm, internal diameter is 14.60mm, and height is 11.75mm) powder core.Powder core after compacting is carried out to destressing heat treatment under argon shield, and heat treatment temperature is 400 ℃, and annealing time is 1h, takes to heat up with stove, and heating rate is 10 ℃/min.Powder core after heat treatment is flooded 1 hour in epoxide-resin glue, obtain nanocrystalline magnetic core.The performance parameter of specimen.
Above-mentioned example product is tested and is described as follows:
Performance test and example explanation about above-mentioned different granularity of magnet powder proportioning powder cores
Impact about the metal dust particle size distribution on the nanocrystalline magnetic core performance.From product 1, product 2 and product 3 Data Comparisons, along with particle size increases, with respect to product 1, the quality factor of product 2 are in a slight decrease, but magnetic permeability obviously increases.The quality factor of product 3 are lower, and magnetic permeability slightly is improved.Through the inventor, experimental results demonstrate, be the optimal selection for preparing nanocrystalline magnetic by " 15% distributes by-200～+ 250 order the second powder and 15% powder particle by-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder and 70% ", possess lower loss value thering is higher magnetic permeability simultaneously.
Performance test and example explanation about above-mentioned different insulative agent addition powder core.
About the insulating compound addition, distribute on the impact of nanocrystalline magnetic core performance.From upper table product 2, product 3, product 4 and product 5 Data Comparisons, the insulating compound addition has considerable influence to the performance of product.When the insulating compound addition is too high, although the loss of powder core is lower, magnetic permeability is lower, causes quality factor lower, and comprehensive magnetic can be poor.When the insulating compound addition is less, although the magnetic permeability of powder core is higher, loss value is also larger.Through experimental results demonstrate of inventor, " the insulating compound addition is in 3.5wt%～4.5wt% interval " is the optimal selection for preparing nanocrystalline magnetic core.
The performance comparison test and the example explanation that prepare powder core about a step Technology for Heating Processing preparation method and traditional handicraft.
From the magnetism testing of upper table product 5 and product 7, powder core magnetic property prepared due to traditional handicraft by powder core magnetic property prepared by a step Technology for Heating Processing preparation method of Sol-Gel powder core.Through the inventor to product 5 and product 7 in magnetic internal stress test known, the magnetic internal stresses release effect of product 5 will be much better than the magnetic internal stresses release effect of product 7.
Claims (8)
1. a step heat treatment process of preparing of a Sol-Gel powder core is characterized in that the method comprises the following steps:
(1) will be without the Fe of crystallization and thermal treatment and magnetic annealing in process
73.5cu
1nb
3si
13.5b
9the amorphous band fragment directly put into the comprehensive planetary ball mill ball mill crushing of high energy, obtain the amorphous metal powder;
(2) above-mentioned amorphous metal powder is sieved, then blend together by 10%～20% and pass through the hybrid particles powder of-250 purposes the 3rd powder constituent by-120～+ 200 purpose the first powder, 60%～80% by-200～+ 250 order the second powder and 10%～20%;
(3) Passivation Treatment: above-mentioned hybrid particles powder is proceeded to preheating in baking oven, in the hybrid particles powder after preheating, slowly add phosphate aqueous solution to carry out Passivation Treatment, passivation time is 2～5 hours, subsequently the hybrid particles powder after passivation is proceeded in baking oven and dries;
(4) insulating wrapped: add mica powder, silicone resin, zinc stearate, absolute ethyl alcohol in the hybrid particles powder after Passivation Treatment, the heating wet mixing volatilization that stirs, complete insulating wrapped;
(5) compression molding: the hybrid particles powder after insulating wrapped is evenly packed in mould, exerted pressure to authorized pressure in 1～3 minute, pressurize 3～5 minutes, obtain compressing powder core;
(6) one step annealings are processed: the powder core after compacting is carried out to crystallization, destressing heat treatment under vacuum or inert gas shielding, obtain the powder core after heat treatment;
(7) processing is solidified in insulation: the powder core after a step annealing is processed solidifies in glue and floods 0.5～1 hour in insulation, obtains the Sol-Gel powder core.
2. a step heat treatment process of preparing of Sol-Gel powder core according to claim 1, the process conditions that it is characterized in that the comprehensive planetary ball mill of described high energy are: material ball ratio 1:30, the deep bid rotating speed is 240 rev/mins, and Ball-milling Time is 8 hours.
3. a step heat treatment process of preparing of Sol-Gel powder core according to claim 1, is characterized in that described phosphate aqueous solution concentration is 2wt%～5wt%, adopts the diluent of deionized water as phosphoric acid.
4. a step heat treatment process of preparing of Sol-Gel powder core according to claim 1, is characterized in that described silicone resin is the high temperature resistant silicon ketone resin.
5. a step heat treatment process of preparing of Sol-Gel powder core according to claim 1, it is characterized in that 3～5wt% that described mica powder addition is the magnetic quality, the 2.5wt% that the silicone resin addition is the magnetic quality, the 1wt% that the zinc stearate addition is the magnetic quality, absolute ethyl alcohol is magnetic quality 15wt%～25wt%.
6. a step heat treatment process of preparing of Sol-Gel powder core according to claim 1, is characterized in that slowly exerting pressure in the compression molding process, and briquetting pressure is 1600MPa～2200MPa.
7. a step heat treatment process of preparing of Sol-Gel powder core according to claim 1, it is characterized in that a step annealing treatment temperature is 500 ℃～600 ℃, annealing time is 1h, takes to heat up with stove, heating rate is 10 ℃/min, and described inert gas is argon gas.
8. a step heat treatment process of preparing of Sol-Gel powder core according to claim 1, is characterized in that insulating and solidify the insulation described in processing to solidify glue be epoxy resin.
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