CN110265202A - The prilling process and soft magnetic composite powder of adhesive, soft magnetic composite powder - Google Patents
The prilling process and soft magnetic composite powder of adhesive, soft magnetic composite powder Download PDFInfo
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- CN110265202A CN110265202A CN201910400531.2A CN201910400531A CN110265202A CN 110265202 A CN110265202 A CN 110265202A CN 201910400531 A CN201910400531 A CN 201910400531A CN 110265202 A CN110265202 A CN 110265202A
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- soft magnetic
- composite powder
- magnetic composite
- adhesive
- powder
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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
- B22F1/102—Metallic powder coated with 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to adhesive, the prilling process and soft magnetic composite powder of soft magnetic composite powder, the adhesive is dissolved in acetone by glue material to be made, wherein, the glue material includes that mass ratio is (2.5-3.5): (3.5-4.5): cyanate ester modified epoxy, methylnadic anhydride and the 4- cyclic ethylene -1 of (2.5-3.5), 2- dicarboxylic acid dimethyl ester, and the mass ratio of the glue material and acetone is 1: 10.The advantage of the invention is that, the apparent density height of the soft magnetic metal composite powder that adhesive combination fluidized bed prilling is obtained, good flowing properties, can continuous production, and it can guarantee the consistency of pelletizing material, without wasting phenomenon in granulation process, realize 100% yield.
Description
Technical field
The invention belongs to the preparation technical fields of soft magnetic metal powder material, and in particular to adhesive, soft magnetic composite powder
Prilling process and soft magnetic composite powder.
Background technique
Molding inductance includes pedestal and winding ontology, is that winding ontology is embedded to inside metallic magnetic powder by the pedestal
It is formed through die casting.The magnetic powder includes carbonyl iron dust, iron silicochromium powder, iron sial powder etc., and seperated partial size is about 10um.
The seperated stacking that easily agglomerates during storage of tiny magnetism, and will appear dust from flying, adherency in pressing die voltage inductance
The problem of wall, while feeding production is carried out without standard measure due to powder drying is without mobility；In addition, molding inductance component makes
With in the process, loss (mainly eddy-current loss) increases with the raising of frequency of use, and loss not only reduces the performance of device,
Also generate a large amount of Joule heats.Currently, being in magnetic powder outer cladding one to reduce loss to cause the universal method of energy loss
The higher organic or inorganic insulating layer of layer resistivity increases its resistance to reduce electric conductivity, this just need using adhesive come into
Row granulation processing.Traditional prilling process is extruding pelletization, as patent CN201710792019.8 has just carried out two to soft magnetic powder
Secondary extruding pelletization, the technique can complete granulation operations, but lead to not realize continuous production because of sieve cracky, make
Also the surface coated insulating layer of powder can be caused to fall off because of friction during grain, to destroy covered effect, reduce inductance
Safety, the loss for improving inductance.
Summary of the invention
Technical problem to be solved by the present invention lies in: traditional prilling process can not continuous production, and in granulation process easily
Destroy the insulating layer on magnetic powder surface.
The present invention solves above-mentioned technical problem using following technical scheme:
Glue material is dissolved in acetone and being made by adhesive, wherein the glue material includes that mass ratio is (2.5-3.5): (3.5-
4.5): cyanate ester modified epoxy, methylnadic anhydride and 4- cyclic ethylene -1,2- dicarboxylic acid dimethyl ester of (2.5-3.5),
And the mass ratio of the glue material and acetone is 1: 10.
Preferably, the cyanate ester modified epoxy, methylnadic anhydride, 4- cyclic ethylene -1,2- dioctyl phthalate diformazan
The mass ratio of ester is 3: 4: 3.
The prilling process of soft magnetic composite powder, using above-mentioned adhesive, comprising the following steps:
(1) it pre-processes: soft magnetic metal powder being added in the aqueous solution of aluminium dihydrogen phosphate, drained after stirring, heating；Wherein
The mass ratio of the soft magnetic metal powder, aluminium dihydrogen phosphate and water is 1: (0.005-0.01): (0.1-0.12):
(2) it prepares adhesive: weighing the glue material and acetone according to the ratio, then the glue material is dissolved in acetone, stirring is mixed
It is even to obtain the final product；
(3) it prepares magma: the glue that step (2) obtain is added in the pretreated soft magnetic metal powder that step (1) obtains
Stick stirs and evenly mixs to obtain the final product；Wherein the soft magnetic metal powder and the mass ratio of the glue material are 1: (0.025-0.035)；
(4) it is granulated: fluidization granulation is carried out to the magma that step (3) obtains.
Preferably, the soft magnetic metal powder includes carbonyl iron dust, iron silicochromium powder, in sendust powder
It is one or more of.
Preferably, it is stirred in the step (1) using double planetary mixer, parameter setting are as follows: temperature 100-115
DEG C, time 45-55min.
Preferably, it is stirred in the step (3) using double planetary mixer, parameter setting are as follows: revolving speed 40-50r/
Min, time 20-30min.
Preferably, the fluidization granulation conveys the magma using peristaltic pump, and the inlet of the peristaltic pump is provided with sieve
Net.
Preferably, the mesh number of the sieve is 70 mesh.
Preferably, the parameter setting of the fluidization granulation are as follows: drying bed intake volume is 110-130m3/ h, drying bed into
90~110 DEG C of air temperature, 75 DEG C of drying bed leaving air temp, dry 300~350kPa of bed pressure drop, dry bed board is 50~
100 mesh screens, feeding 300~350r/min of centrifuge speed, 40~50Hz of feed inlet wriggling revolution speed.
Soft magnetic composite powder made from prilling process using above-mentioned soft magnetic composite powder.
The technology of the present invention the utility model has the advantages that
Adhesive described in technical solution of the present invention has the characteristics that adhesive strength is high, briquetting pressure is small, especially suitable for
Fluidization granulation, the apparent density of the soft magnetic metal composite powder obtained in the way of the adhesive and in conjunction with fluidized bed prilling
Height, good flowing properties, can continuous production, and can guarantee the consistency of pelletizing material, it is real without wasting phenomenon in granulation process
Existing 100% yield；Prilling process described in technical solution of the present invention improves the shaping characteristic of soft magnetic composite powder simultaneously, makes
It can obtain higher green density at lower pressures, and then keep the high inductance value and high stability of product.
Specific embodiment
For convenient for those skilled in the art understand that technical solution of the present invention, now in conjunction with specification specific embodiment to the present invention
Technical solution is described further.
The embodiment of the invention provides the prilling process of a kind of adhesive and soft magnetic composite powder, and compound using the soft magnetism
The prilling process of powder is granulated to obtain soft magnetic composite powder.
The adhesive specifically includes glue material and acetone, and the glue material is mainly (2.5-3.5): (3.5- by mass ratio
4.5): cyanate ester modified epoxy, methylnadic anhydride and 4- cyclic ethylene -1,2- dicarboxylic acid dimethyl ester of (2.5-3.5)
It mixes, and the mass ratio of the glue material and acetone is 1: 10.The glue material is dissolved in the acetone, is sufficiently stirred, mixes
The adhesive is obtained after closing uniformly.
The prilling process of the soft magnetic composite powder the following steps are included:
(1) it pre-processes: soft magnetic metal powder being added in the aqueous solution of aluminium dihydrogen phosphate, drained after stirring, heating；Wherein
The mass ratio of the soft magnetic metal powder, aluminium dihydrogen phosphate and water is 1: (0.005-0.01): (0.1-0.12), the soft magnetism gold
Belonging to powder includes one or more of carbonyl iron dust, iron silicochromium powder, sendust powder.
(2) it prepares adhesive: weighing the glue material and acetone according to the ratio, then the glue material is dissolved in acetone, stirring is mixed
It is even to obtain the final product；
(3) it prepares magma: the glue that step (2) obtain is added in the pretreated soft magnetic metal powder that step (1) obtains
Stick stirs and evenly mixs to obtain the final product；Wherein the soft magnetic metal powder and the mass ratio of the glue material are 1: (0.025-0.035)；
(4) it is granulated: fluidization granulation is carried out to the magma that step (3) obtains.
Next it will be described in detail herein by prilling process of the specific embodiment to above-mentioned soft magnetic composite powder.
Embodiment 1
The prilling process of soft magnetic composite powder described in the present embodiment includes the following steps:
(1) it pre-processes: weighing iron silicochromium powder (FeCrSi-A) 5000g, aluminium dihydrogen phosphate 40g, distilled water 600g,
The aluminium dihydrogen phosphate is dissolved in distilled water, then the iron silicochromium powder is added thereto, then sets mixture
In double planetary mixer, 50min is stirred under the conditions of 105 DEG C, while exhausting is to drying；Then take out powder；
(2) it prepares adhesive: weighing cyanate ester modified epoxy 45g, methylnadic anhydride 60g, 4- ring second respectively
Alkene -1,2- dicarboxylic acid dimethyl ester 45g and acetone 1250g, by the cyanate ester modified epoxy, methylnadic anhydride,
4- cyclic ethylene -1,2- dicarboxylic acid dimethyl ester is dissolved in the acetone；
(3) it prepares magma: the powder that step (1) obtains being added in the adhesive obtained to step (2), and mixture is set
It is stirred and evenly mixed in double planetary mixer, obtains emulsion of the bottom without precipitating；Wherein the revolving speed of the double planetary mixer is
40r/min, mixing time 25min；
(4) it is granulated: fluidization granulation is carried out to the magma that step (3) obtains；Specifically, swirl atomizer is pumped to by wriggling
Middle carry out centrifugal spray, while it is 120m that drying bed intake volume, which is arranged,3/ h, drying bed inlet air temperature are 100 DEG C, and drying bed goes out
Air temperature is 75 DEG C, and drying bed lamination is reduced to 320kPa, and dry bed board is 60 mesh screens, and feeding centrifuge speed is 320r/
Min, feed inlet wriggling revolution speed 40Hz；In granulation process, to avoid blocking, one can be arranged at peristaltic pump feed inlet
70 mesh screens.
In the above method, adhesive is pumped into centrifuge after mixing with iron silicochromium powder by wriggling, in centrifugal force
And spherical particles are formed under the action of the surface tension of adhesive and acetone and are fallen.During this, if the partial size of spherical particles is small
In a certain preset value (such as 60 mesh), then it can be directly over sieve and fall into discharge port progress rewinding, if the partial size of sphere is greater than
The preset value, then it passes through sieve after being broken into pellet shapes under the piping and druming of hot wind.The magma in the present embodiment exists as a result,
While obtaining 100% yield, the high powder granule of sphericity is also obtained.Utilize soft magnetism composition metal made from this method
The apparent density height of powder, good flowing properties, at the same time, the adhesive strength height of adhesive used in this method, insulating properties
Can be good, so that the molding inductance component of subsequent preparation has reduced loss.
Comparative example 1
Soft magnetism is prepared using extruding and pelletizing process using with the identical iron silicochromium powder of embodiment 1 and adhesive
Composite powder tests apparent density and mobility, the results are shown in Table 1.
Iron silicochromium composite powder property obtained by table 1, embodiment and comparative example compares
| Test item | Apparent density (g/cm3) | Mobility (s) |
| Fluidization granulation | 2.44 | 43 |
| Extruding pelletization method | 1.88 | 62 |
By table 1 it is found that the apparent density and mobility of the resulting soft magnetic composite powder of embodiment 1 are superior to extruding pelletization
Obtained soft magnetic composite powder.When the soft magnetic composite powder manufacture molding inductance obtained using embodiment 1, ensure that product at
The uniformity, stability and reliability of pan feeding during type, and can reduce the pan feeding time, improve working efficiency.
Embodiment 2
The prilling process of soft magnetic composite powder described in the present embodiment includes the following steps:
(1) it pre-processes: carbonyl iron powder 5000g, aluminium dihydrogen phosphate 50g, distilled water 1000g is weighed, by the di(2-ethylhexyl)phosphate
Hydrogen aluminium is dissolved in distilled water, then the iron silicochromium powder is added thereto, and mixture is then placed in double-planet stirring
In machine, 55min is stirred under the conditions of 110 DEG C, while exhausting is to drying；Then take out powder；
(2) it prepares adhesive: weighing cyanate ester modified epoxy 48g, methylnadic anhydride 64g, 4- ring second respectively
Alkene -1,2- dicarboxylic acid dimethyl ester 48g and acetone 1500g, by the cyanate ester modified epoxy, methylnadic anhydride,
4- cyclic ethylene -1,2- dicarboxylic acid dimethyl ester is dissolved in the acetone；
(3) it prepares magma: the powder that step (1) obtains being added in the adhesive obtained to step (2), and mixture is set
It is stirred and evenly mixed in double planetary mixer, obtains emulsion of the bottom without precipitating；Wherein the revolving speed of the double planetary mixer is
50r/min, mixing time 30min；
(4) it is granulated: fluidization granulation is carried out to the magma that step (3) obtains；Specifically, swirl atomizer is pumped to by wriggling
Middle carry out centrifugal spray, while it is 130m that drying bed intake volume, which is arranged,3/ h, drying bed inlet air temperature are 110 DEG C, and drying bed goes out
Air temperature is 75 DEG C, and drying bed lamination is reduced to 350kPa, and dry bed board is 80 mesh screens, and feeding centrifuge speed is 350r/
Min, feed inlet wriggling revolution speed 50Hz；In granulation process, to avoid blocking, one can be arranged at peristaltic pump feed inlet
70 mesh screens.
Comparative example 2
Soft magnetic composite powder is prepared using extruding and pelletizing process using with the identical powder of embodiment 2 and adhesive,
Apparent density and mobility are tested, the results are shown in Table 2.
Iron silicochromium composite powder property obtained by table 2, embodiment and comparative example compares
| Test item | Apparent density (g/cm3) | Mobility (s) |
| Fluidization granulation | 2.58 | 38 |
| Extruding pelletization method | 2.06 | 58 |
Embodiment 3
The prilling process of soft magnetic composite powder described in the present embodiment includes the following steps:
(1) it pre-processes: weighing carbonyl iron powder 2500g, sendust powder 2500g is uniformly mixed, aluminium dihydrogen phosphate
25g, distilled water 500g, the aluminium dihydrogen phosphate is dissolved in distilled water, then the iron silicochromium powder is added thereto,
Then mixture is placed in double planetary mixer, stirs 50min under the conditions of 100 DEG C, while exhausting is to drying；Then take out
Powder；
(2) it prepares adhesive: weighing cyanate ester modified epoxy 37.5g, methylnadic anhydride 50g, 4- ring respectively
Ethylene -1,2- dicarboxylic acid dimethyl ester 37.5g and acetone 1250g, by the cyanate ester modified epoxy, methyl nadic acid
Acid anhydride, 4- cyclic ethylene -1,2- dicarboxylic acid dimethyl ester are dissolved in the acetone；
(3) it prepares magma: the powder that step (1) obtains being added in the adhesive obtained to step (2), and mixture is set
It is stirred and evenly mixed in double planetary mixer, obtains emulsion of the bottom without precipitating；Wherein the revolving speed of the double planetary mixer is
40r/min, mixing time 20min；
(4) it is granulated: fluidization granulation is carried out to the magma that step (3) obtains；Specifically, swirl atomizer is pumped to by wriggling
Middle carry out centrifugal spray, while it is 110m that drying bed intake volume, which is arranged,3/ h, drying bed inlet air temperature are 100 DEG C, and drying bed goes out
Air temperature is 75 DEG C, and drying bed lamination is reduced to 300kPa, and dry bed board is 50 mesh screens, and feeding centrifuge speed is 300r/
Min, feed inlet wriggling revolution speed 50Hz；In granulation process, to avoid blocking, one can be arranged at peristaltic pump feed inlet
70 mesh screens.
Comparative example 3
Soft magnetism composite powder is prepared using extruding and pelletizing process using with the identical mixed-powder of embodiment 3 and adhesive
End tests apparent density and mobility, the results are shown in Table 3.
Iron silicochromium composite powder property obtained by table 3, embodiment and comparative example compares
| Test item | Apparent density (g/cm3) | Mobility (s) |
| Fluidization granulation | 2.50 | 40 |
| Extruding pelletization method | 2.00 | 60 |
Cyanate ester modified epoxy used by the embodiment of the present invention is purchased from BASF joint-stock company, methyl nadic acid
Acid anhydride is purchased from BASF joint-stock company, 4- cyclic ethylene -1,2- dicarboxylic acid dimethyl ester (production and sales of Nanjing Chemical Industrial Co., Ltd),
Other products with identical physicochemical property also can be used.In addition, being carried out in above-described embodiment using using double planetary mixer
Stirring is a kind of preferable selection, other various types of mixing plants can be equally applicable in.
Technical solution of the present invention is exemplarily described invention above in conjunction with specific embodiment, it is clear that present invention tool
Body realization is not subject to the restrictions described above, as long as using the various non-realities that the inventive concept and technical scheme of the present invention carry out
Matter improve, or it is not improved the conception and technical scheme of invention are directly applied into other occasions, in guarantor of the invention
Within the scope of shield.
Claims (10)
1. adhesive, which is characterized in that glue material is dissolved in acetone and is made, wherein the glue material includes that mass ratio is (2.5-
3.5): (3.5-4.5): cyanate ester modified epoxy, methylnadic anhydride and the 4- cyclic ethylene -1,2- bis- of (2.5-3.5)
Formic acid dimethyl ester, and the mass ratio of the glue material and acetone is 1: 10.
2. a kind of adhesive according to claim 1, which is characterized in that the cyanate ester modified epoxy, methyl are received
Dick acid anhydrides, 4- cyclic ethylene -1,2- dicarboxylic acid dimethyl ester mass ratio be 3: 4: 3.
3. the prilling process of soft magnetic composite powder, using adhesive as claimed in claim 1 or 2, which is characterized in that including with
Lower step:
(1) it pre-processes: soft magnetic metal powder being added in the aqueous solution of aluminium dihydrogen phosphate, drained after stirring, heating；It is wherein described
The mass ratio of soft magnetic metal powder, aluminium dihydrogen phosphate and water is 1: (0.005-0.01): (0.1-0.12)；
(2) it prepares adhesive: weighing the glue material and acetone according to the ratio, then the glue material is dissolved in acetone, stir and evenly mix i.e.
?；
(3) it prepares magma: the adhesive that step (2) obtain is added in the pretreated soft magnetic metal powder that step (1) obtains,
It stirs and evenly mixs to obtain the final product；Wherein the soft magnetic metal powder and the mass ratio of the glue material are 1: (0.025-0.035)；
(4) it is granulated: fluidization granulation is carried out to the magma that step (3) obtains.
4. the prilling process of soft magnetic composite powder according to claim 3, which is characterized in that the soft magnetic metal powder packet
Include one or more of carbonyl iron dust, iron silicochromium powder, sendust powder.
5. the prilling process of soft magnetic composite powder according to claim 3, which is characterized in that used in the step (1)
Double planetary mixer is stirred, parameter setting are as follows: and 100-115 DEG C of temperature, time 45-55min.
6. the prilling process of soft magnetic composite powder according to claim 3, which is characterized in that used in the step (3)
Double planetary mixer is stirred, parameter setting are as follows: revolving speed 40-50r/min, time 20-30min.
7. the prilling process of soft magnetic composite powder according to claim 3, which is characterized in that the fluidization granulation is using compacted
Dynamic pump conveys the magma.
8. the prilling process of soft magnetic composite powder according to claim 7, which is characterized in that the inlet of the peristaltic pump
It is provided with sieve.
9. the prilling process of soft magnetic composite powder according to claim 3, which is characterized in that the parameter of the fluidization granulation
Setting are as follows: drying bed intake volume is 110-130m3/ h, 90~110 DEG C of drying bed inlet air temperature, drying bed leaving air temp 75
DEG C, dry 300~350kPa of bed pressure drop, dry bed board is 50~100 mesh screens, 300~350r/ of feeding centrifuge speed
Min, 40~50Hz of feed inlet wriggling revolution speed.
10. using the soft magnetic composite powder as made from the prilling process of the described in any item soft magnetic composite powders of claim 3-9.
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| CN201910400531.2A CN110265202A (en) | 2019-05-14 | 2019-05-14 | The prilling process and soft magnetic composite powder of adhesive, soft magnetic composite powder |
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| CN201910400531.2A CN110265202A (en) | 2019-05-14 | 2019-05-14 | The prilling process and soft magnetic composite powder of adhesive, soft magnetic composite powder |
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