CN104952583B - A kind of preparation method of amorphous metal soft-magnetic powder core - Google Patents
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Abstract
The invention discloses a kind of preparation method of amorphous metal soft-magnetic powder core.It comprises the steps：(1) amorphous band is carried out into brittle process, the amorphous band after embrittlement carries out break process, obtains amorphous metal powder；(2) by amorphous metal powder sieving, carry out grain size proportion；(3) the amorphous metal powder after proportioning is passivated into process；(4) the amorphous metal powder of phosphorus acid passivation is carried out into insulating wrapped process；(5) binding agent is added, the amorphous metal powder after cladding is carried out into pelletize process；(6) by the amorphous metal powder after pelletize, carry out magnetic field orientating molding；(7) magnetic core after oriented moulding is carried out into vertical magnetic heat treatment；(8) spray painting process is carried out after the magnetic core cooling after heat treatment, obtain product.The invention has the beneficial effects as follows：Magnetic domain is internally formed in amorphous magnetic core, coercivity and loss is reduced, core loss can be further reduced, pcrmeability is improved, and is improved magnetic core soft magnet performance, and reduces cost.
Description
Technical field
The present invention relates to metal magnetic powder core prepares correlative technology field, a kind of amorphous metal soft-magnetic powder core is referred in particular to
Preparation method.
Background technology
Metal magnetic powder core is a kind of new soft magnetic materials after silicon steel, ferrite, amorphous band, is widely used
In the middle of power electronic devices.Traditional metal magnetic powder core mainly has ferrocart core, ferrum sial, ferrum silicon, ferrum nickel molybdenum, ferrum nickel etc., but
It is that they have respective shortcoming, such as ferrum sial superposition poor performance, poor ferrocart core drain performance, ferrum nickel and ferrum nickel molybdenum has preferable
Performance, but the nickel containing higher proportion in the middle of its composition, need higher manufacturing cost, thus develop a kind of cost it is relatively low,
The powder core of function admirable is necessary.Amorphous powder core is a kind of Novel magnetic powder developed on the basis of amorphous band
Core, has the advantages that high Bs, low-loss and higher temperature stability, by industry extensive concern.General amorphous powder core system
Standby technique, is all that the techniques such as Jing bands broken powder processed, grain size proportion, insulating wrapped, compressing and heat treatment obtain corresponding
Amorphous soft magnet powder core, some patents are improved to this, but magnetic property cannot all be increased substantially.
Chinese patent " a kind of preparation method of amorphous metal soft magnetic-powder core ", patent No. CN104190945A describes one
The technology of preparing of kind of amorphous magnetic powder core, which employs isostatic pressed technology of preparing, improve the consistency of magnetic core, so as to improving magnetic core
Pcrmeability, there are some defects in this method, before one side amorphous powder core heat treatment, due to binding agent it is also solid
Change, magnetic core intensity is relatively low, and comprehending at isostatic pressed makes magnetic core rupture, reduce yield rate；On the other hand, isostatic pressed is processed needs soft shield
Set, increased cost, is not suitable for batch production, limits use.
Chinese patent " a kind of heat treatment method of amorphous powder core ", patent No. CN103658642A are described a kind of non-
The heat treatment technics of brilliant powder core, which adopts horizontal magnetic treatment, magnetic field to pass perpendicularly through magnet ring face, although this method is with certain
Drop loss effect, but which adopts larger magnetic field, and intensity is 1000-3000Gs, needs very big magnetic field to drive magnetic domain to take
To, cause heat treatment cost increase, make magnetic core cost increase；And the arrangement of magnetic powder is unordered in a jumble, horizontal magnetic effect is not obvious.
The content of the invention
The present invention is above-mentioned in order to overcome the shortcomings of to exist in prior art, there is provided a kind of to reduce core loss and raising
The preparation method of the amorphous metal soft-magnetic powder core of magnetic core magnetic property.
To achieve these goals, the present invention is employed the following technical solutions：
A kind of preparation method of amorphous metal soft-magnetic powder core, comprises the steps：
(1) amorphous band is carried out into brittle process, the amorphous band after embrittlement carries out break process, obtains amorphous metal powder
End；
(2) by amorphous metal powder sieving, carry out grain size proportion；
(3) the amorphous metal powder after proportioning is passivated into process；
(4) the amorphous metal powder of phosphorus acid passivation is carried out into insulating wrapped process；
(5) binding agent is added, the amorphous metal powder after cladding is carried out into pelletize process；
(6) by the amorphous metal powder after pelletize, carry out magnetic field orientating molding；
(7) magnetic core after oriented moulding is carried out into vertical magnetic heat treatment；
(8) spray painting process is carried out after the magnetic core cooling after heat treatment, obtain product.
The preparation method is vertical by preferred amorphous granularity of magnet powder proportioning, amorphous magnetic powder oriented moulding and amorphous powder core magnetic field
The methods such as magnetic heat treatment, are internally formed magnetic domain in amorphous magnetic core, and serving reduces the effect of coercivity and loss, can be further
Core loss is reduced, pcrmeability is improve, and is improve magnetic core soft magnet performance, and reduce cost.
Preferably, in step (1), the composition of the amorphous band is Fe, Si, B, and its atomic percent is：Fe is accounted for
76-80at%, Si account for 7-10at%, and B accounts for 11-14at%；The thickness of the amorphous band is 20-30um.
Preferably, in step (1), described brittle process, its brittle temperature is 200-400 degree, its brittle time
For 10-200 minutes；Described break process, is divided into two steps, and the first step is Mechanical Crushing, and second step is broken for airflow milling.
Preferably, in step (2), described grain size proportion, its result is：+ 150 mesh account for 5%-30%, -150-+
200 mesh account for 40%-70%, and -200-+300 mesh accounts for 10-30%.
Preferably, in step (3), described Passivation Treatment, the passivating solution for being adopted are triosephosphate solution, wherein
0.1-3% of the phosphorus acid content for amorphous metal amount of powder, 2-10% of the content of acetone for amorphous metal amount of powder.
Preferably, in step (4), described insulating wrapped is processed, and the insulating wrapped agent for being adopted is for Kaolin, cunning
Stone powder, glass dust, B2O3、Al2O3, one or more in MgO, its granularity is -600 mesh, and addition is amorphous metal powder weight
The 0.1-2wt% of amount.
Preferably, in step (5), described binding agent is epoxy resin, phenolic resin, in novolac epoxy resin
One or more, 1-5wt% of the addition for amorphous metal powder weight, using acetone as diluent.
Preferably, in step (5), described pelletize is processed, and its granularity can pass through 60 eye mesh screens.
Preferably, in step (6), described magnetic field orientating molding, magnetic direction is horizontal direction, parallel to magnet ring
Lower planes, the magnetic field intensity adopted by which for 0.1-1T, adopted for pulsed magnetic field, plus the magnetic time be 5-20s, molding
Pressure is 12-25T/cm2, the dwell time is 2-10s.
Preferably, in step (6), described vertical magnetic heat treatment, magnet ring in horizontal magnetic field, magnetic field levels
Through magnet ring lower planes, the magnetic field intensity for adopting is for 10-1000Gs；Heat treatment temperature is 400-550 degree, and temperature retention time is
10-200 minutes, using nitrogen or noble gases, using multistage temperature lift-down curve, less than 200 degree heating rates less than 5 degree/
min。
The invention has the beneficial effects as follows：Magnetic domain is internally formed in amorphous magnetic core, coercivity and loss is reduced, can be further
Core loss is reduced, pcrmeability is improved, and is improved magnetic core soft magnet performance, and reduces cost.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1：
By Fe78Si9B13Amorphous band carries out brittle process, and brittle temperature is 200 degree, and brittle time is 200 minutes；It is brittle
Amorphous band afterwards is crushed with disintegrating machine first, is then crushed using airflow milling, obtains amorphous metal powder；Will be non-
Brilliant metal dust screening, carries out grain size proportion, and+150 mesh account for 5%, and -150-+200 mesh accounts for 70%, and -200-+300 mesh accounts for 25%；
Amorphous powder after proportioning is passivated into process, the passivator for adopting is triosephosphate solution, and wherein phosphorus acid content is magnetic powder
The 0.1% of amount, content of acetone for magnetic powder amount 2%；The amorphous powder of phosphorus acid passivation is carried out into insulating wrapped process, covering is
Kaolin, Pulvis Talci, glass dust, B2O3、Al2O3, one or more in MgO, granularity is -600 mesh, and addition is amorphous gold
The 0.1wt% of category powder weight；One or more in addition epoxy resin, phenolic resin or novolac epoxy resin is used as bonding
Agent, using acetone as diluent, addition is the 1wt% of amorphous metal powder weight, the amorphous magnetic powder after cladding is made
Grain is processed, and granule size is -60 mesh；By the amorphous magnetic powder after pelletize, magnetic field orientating molding is carried out, magnetic direction is level side
To parallel to the lower planes of magnet ring, magnetic field intensity is 1T, plus the magnetic time is 5s, and briquetting pressure is 25T/cm2, the dwell time
For 2s, blank is obtained；Magnetic core after oriented moulding is carried out into vertical magnetic heat treatment, magnetic direction horizontal through magnet ring lower planes,
Magnetic core is internally formed magnetic domain in amorphous magnetic core in the middle of magnetic field, and playing reduces the purpose of coercivity and loss, employing
Magnetic field intensity is 10Gs, and heat treatment temperature is 400 degree, and temperature retention time is 200 minutes, is protected with nitrogen or noble gases
Shield, it is to avoid oxidation, deteriorates magnetic property, and using multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 °/min, with slow
Exclude glue inside magnetic core, it is to avoid cracking.Spray painting process is carried out after magnetic core cooling after heat treatment, final products, magnetic is obtained
Can be as shown in table 1.
Comparative example 1：
Process and condition are identical with embodiment 1, and magnetic field, the properties of product of acquisition are not added with molding and heat treatment process
As shown in table 1.
Embodiment 2：
By Fe79Si7B14Amorphous band carries out brittle process, and brittle temperature is 400 degree, and brittle time is 10 minutes；It is brittle
Amorphous band afterwards is crushed with disintegrating machine first, is then crushed using airflow milling, obtains amorphous metal powder；Will be non-
Brilliant metal dust screening, carries out grain size proportion, and+150 mesh account for 30%, and -150-+200 mesh accounts for 40%, and -200-+300 mesh accounts for 30%；
Amorphous powder after proportioning is passivated into process, the passivator for adopting is triosephosphate solution, and wherein phosphorus acid content is magnetic powder
The 3% of amount, content of acetone for magnetic powder amount 10%；The amorphous powder of phosphorus acid passivation is carried out into insulating wrapped process, covering is
Kaolin, Pulvis Talci, glass dust, B2O3、Al2O3, one or more in MgO, granularity is -600 mesh, and addition is 2wt%；
Add epoxy resin, one or more in phenolic resin or novolac epoxy resin as binding agent, using acetone as diluent,
Amorphous magnetic powder after cladding is carried out pelletize process by 1wt% of the addition for magnetic powder weight, and granule size is -60 mesh；By pelletize
Amorphous magnetic powder afterwards, carries out magnetic field orientating molding, and magnetic direction is horizontal direction, and parallel to the lower planes of magnet ring, magnetic field is strong
Spend for 0.1T, plus the magnetic time is 20s, briquetting pressure is 12T/cm2, the dwell time is 10s, obtains blank；After oriented moulding
Magnetic core carry out vertical magnetic heat treatment, magnetic direction horizontal through magnet ring lower planes, magnetic core in the middle of magnetic field, in amorphous
Magnetic core is internally formed magnetic domain, play reduce coercivity and loss purpose, the magnetic field intensity for adopting for 1000Gs, heat treatment temperature
Between 550 degree, temperature retention time is 10 minutes, is protected with nitrogen or noble gases, it is to avoid oxidation, deteriorates magnetic property,
Using multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 °/min, slowly to exclude glue inside magnetic core, it is to avoid open
Split.Spray painting process is carried out after magnetic core cooling after heat treatment, final products are obtained, magnetic property is as shown in table 1.
Comparative example 2：
Process and condition are identical with embodiment 2, and magnetic field, the properties of product of acquisition are not added with molding and heat treatment process
As shown in table 1.
Embodiment 3：
By Fe80Si9B11Amorphous band carries out brittle process, and brittle temperature is 350 degree, and brittle time is 30 minutes；It is brittle
Amorphous band afterwards is crushed with disintegrating machine first, is then crushed using airflow milling, obtains amorphous metal powder；Will be non-
Brilliant metal dust screening, carries out grain size proportion, and+150 mesh account for 10%, and -150-+200 mesh accounts for 70%, and -200-+300 mesh accounts for 20%；
Amorphous powder after proportioning is passivated into process, the passivator for adopting is triosephosphate solution, and wherein phosphorus acid content is magnetic powder
The 0.8% of amount, content of acetone for magnetic powder amount 8%；The amorphous powder of phosphorus acid passivation is carried out into insulating wrapped process, covering is
Kaolin, Pulvis Talci, glass dust, B2O3、Al2O3, one or more in MgO, granularity is -600 mesh, and addition is
1.5wt%；One or more in addition epoxy resin, phenolic resin or novolac epoxy resin is made with acetone as binding agent
For diluent, 5wt% of the addition for magnetic powder weight, the amorphous magnetic powder after cladding is carried out into pelletize process, granule size is -60
Mesh；By the amorphous magnetic powder after pelletize, magnetic field orientating molding is carried out, magnetic direction is horizontal direction, putting down up and down parallel to magnet ring
Face, magnetic field intensity is 1T, plus the magnetic time is 5s, and briquetting pressure is 20T/cm2, the dwell time is 5s, obtains blank；To be orientated to
Magnetic core after type carries out vertical magnetic heat treatment, magnetic direction horizontal through magnet ring lower planes, magnetic core in the middle of magnetic field,
Amorphous magnetic core is internally formed magnetic domain, play reduce coercivity and loss purpose, the magnetic field intensity for adopting for 20Gs, heat treatment temperature
Spend for 450 degree, temperature retention time is 30 minutes, is protected with nitrogen or noble gases, it is to avoid oxidation, deteriorate magnetic property, adopt
Multistage temperature lift-down curve is used, less than 200 degree heating rates are less than 5 °/min, slowly to exclude glue inside magnetic core, it is to avoid cracking.
Spray painting process is carried out after magnetic core cooling after heat treatment, final products are obtained, magnetic property is as shown in table 1.
Comparative example 3：
Process and condition are identical with embodiment 3, and magnetic field, the properties of product of acquisition are not added with molding and heat treatment process
As shown in table 1.
Embodiment 4：
By Fe76Si10B14Amorphous band carries out brittle process, and brittle temperature is 380 degree, and brittle time is 40 minutes；It is brittle
Amorphous band afterwards is crushed with disintegrating machine first, is then crushed using airflow milling, obtains amorphous metal powder；Will be non-
Brilliant metal dust screening, carries out grain size proportion, and+150 mesh account for 25%, and -150-+200 mesh accounts for 55%, and -200-+300 mesh accounts for 20%；
Amorphous powder after proportioning is passivated into process, the passivator for adopting is triosephosphate solution, and wherein phosphorus acid content is magnetic powder
The 0.5% of amount, content of acetone for magnetic powder amount 6%；The amorphous powder of phosphorus acid passivation is carried out into insulating wrapped process, covering is
Kaolin, Pulvis Talci, glass dust, B2O3、Al2O3, one or more in MgO, granularity is -600 mesh, and addition is
1.2wt%；One or more in addition epoxy resin, phenolic resin or novolac epoxy resin is made with acetone as binding agent
For diluent, 2wt% of the addition for magnetic powder weight, the amorphous magnetic powder after cladding is carried out into pelletize process, granule size is -60
Mesh；By the amorphous magnetic powder after pelletize, magnetic field orientating molding is carried out, magnetic direction is horizontal direction, putting down up and down parallel to magnet ring
Face, magnetic field intensity is 0.8T, plus the magnetic time is 10s, and briquetting pressure is 22T/cm2, the dwell time is 5s, obtains blank；To take
Vertical magnetic heat treatment is carried out to the magnetic core after molding, magnetic direction is worked as generally in magnetic field horizontal through magnet ring lower planes, magnetic core
In, magnetic domain is internally formed in amorphous magnetic core, playing reduces the purpose of coercivity and loss, and the magnetic field intensity for adopting is for 200Gs, hot
Treatment temperature is 500 degree, and temperature retention time is 20 minutes, is protected with nitrogen or noble gases, it is to avoid oxidation, deteriorates magnetic
Can, using multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 °/min, slowly to exclude glue inside magnetic core, it is to avoid
Cracking.Spray painting process is carried out after magnetic core cooling after heat treatment, final products are obtained, magnetic property is as shown in table 1.
Comparative example 4：
Process and condition are identical with embodiment 4, and magnetic field, the properties of product of acquisition are not added with molding and heat treatment process
As shown in table 1.
Table 1
| Pcrmeability | Pcv (100kHz, 100mT) | DC-Bias(1000e) | |
| Embodiment 1 | 60 | 680 | 68 |
| Embodiment 2 | 63 | 650 | 65 |
| Embodiment 3 | 62 | 670 | 66 |
| Embodiment 4 | 61 | 630 | 68 |
| Comparative example 1 | 55 | 870 | 65 |
| Comparative example 2 | 54 | 830 | 67 |
| Comparative example 3 | 56 | 860 | 68 |
| Comparative example 4 | 53 | 820 | 66 |
Claims (6)
1. a kind of preparation method of amorphous metal soft-magnetic powder core, is characterized in that, comprise the steps：
(1) amorphous band is carried out into brittle process, the amorphous band after embrittlement carries out break process, obtains amorphous metal powder；
The composition of the amorphous band is Fe, Si, B, and its atomic percent is：Fe accounts for 76-80at%, and Si accounts for 7-10at%, and B accounts for 11-
14at%；The thickness of the amorphous band is 20-30um；
(2) by amorphous metal powder sieving, carry out grain size proportion；Described grain size proportion, its result is：+ 150 mesh account for 5%-
30%, -150-+200 mesh accounts for 40%-70%, and -200-+300 mesh accounts for 10-30%；
(3) the amorphous metal powder after proportioning is passivated into process；
(4) the amorphous metal powder of phosphorus acid passivation is carried out into insulating wrapped process；
(5) binding agent is added, the amorphous metal powder after cladding is carried out into pelletize process；
(6) by the amorphous metal powder after pelletize, carry out magnetic field orientating molding；Described magnetic field orientating molding, magnetic direction is
Horizontal direction, parallel to the lower planes of magnet ring, the magnetic field intensity adopted by which for 0.1-1T, adopted for pulsed magnetic field,
Plus the magnetic time is 5-20s, briquetting pressure is 12-25T/cm2, the dwell time is 2-10s；
(7) magnetic core after oriented moulding is carried out into vertical magnetic heat treatment；Described vertical magnetic heat treatment, magnet ring is generally in horizontal magnetic field
Interior, magnetic field levels pass through magnet ring lower planes, and the magnetic field intensity for adopting is for 10-1000Gs；Heat treatment temperature is 400-550 degree,
Temperature retention time is 10-200 minutes, using nitrogen or noble gases, using multistage temperature lift-down curve, less than the 200 degree speed that heat up
Rate is less than 5 degree/min；
(8) spray painting process is carried out after the magnetic core cooling after heat treatment, obtain product.
2. a kind of preparation method of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (1)
In, described brittle process, its brittle temperature are 200-400 degree, and its brittle time is 10-200 minutes；Described broken place
Reason, is divided into two steps, and the first step is Mechanical Crushing, and second step is that airflow milling is crushed.
3. a kind of preparation method of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (3)
In, described Passivation Treatment, the passivating solution for being adopted are triosephosphate solution, and wherein phosphorus acid content is amorphous metal amount of powder
0.1-3%, 2-10% of the content of acetone for amorphous metal amount of powder.
4. a kind of preparation method of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (4)
In, described insulating wrapped is processed, and the insulating wrapped agent for being adopted is for Kaolin, Pulvis Talci, glass dust, B2O3、Al2O3、MgO
In one or more, its granularity be -600 mesh, addition for amorphous metal powder weight 0.1-2wt%.
5. a kind of preparation method of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (5)
In, described binding agent is epoxy resin, phenolic resin, one or more in novolac epoxy resin, and addition is amorphous gold
The 1-5wt% of category powder weight, using acetone as diluent.
6. a kind of preparation method of amorphous metal soft-magnetic powder core according to claim 1 or 5, is characterized in that, in step
(5), in, described pelletize is processed, and its granularity can pass through 60 eye mesh screens.
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| CN112908603B (en) * | 2021-01-21 | 2023-09-26 | 广东省科学院材料与加工研究所 | Iron-based amorphous magnetic powder core and preparation method thereof |
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