CN110283429A - A kind of sheet ferrite electromagnetic composite material and preparation method - Google Patents
A kind of sheet ferrite electromagnetic composite material and preparation method Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The present invention relates to a kind of sheet ferrite electromagnetic composite material and preparation methods.Each raw material component is mixed, molding using the sheet ferrite made of ball milling, coupling modifier, resin, curing agent and diluent as raw material, the composite material is made by the preparation method；Wherein, pass through ball milling prepare the ferritic process conditions of sheet are as follows: by ferrite powder, steel ball, ball-milling additive and volatile solvents under 400-500r/min speed conditions ball milling 7-8h；The rigid ball includes 8mm diameter steel ball and 6mm diameter steel ball.The present invention prepares sheet ferrite powder using ball-milling method, it is compound with epoxy resin by coupling modifier, electromagnetic load composite material is formed with autoclave process or ultrasonic curing, it shows higher electromagnetic parameter in 1-18GHz, can be widely applied in each field electronic equipment such as radar, navigation, satellite communication, electronic countermeasure, radio and television, mobile communication.
Description
Technical field
The present invention relates to Electromagnetic Function Composite technical field more particularly to a kind of sheet ferrite electromagnetic composite materials
And preparation method.
Background technique
With the fast development of high-end electronic devices, the technical requirements of electronic component performance are also higher and higher in equipment.
Wherein, the electromagnetic interference between component has the communication function of antenna system serious with regard to inevitable in a limited space
Interference, weaken the intensity transmission of signal, or even antenna is made thoroughly to fail, must add between device has high magnetic conductance thus
Rate, the electromagnetic shielding material of magnetic loss carry out effective solution this problem.
Ferrite has the characteristics that cheap, preparation process is simple, absorbing property is good, is to study more and compare at present
Mature microwave attenuation absorbent.Ferrite includes simultaneously dielectric loss and magnetic loss to the loss of electromagnetic wave, wherein main
Loss mechanisms be residual loss in ferromagnetic natural resonance absorb.
Currently, gained ferrite powder is largely spherical structure in traditional mode of production.But it is used frequently in unit
The continuous improvement of section, spherical ferrite material have been difficult to meet.
In view of this, the present invention is specifically proposed.
Summary of the invention
The invention aims to by laminated structure ferrite powder and epoxy resin bonding it is compound, provide one kind have it is excellent
The preparation method of the functional composite material of different electromagnetic property meets in terms of high-performance electronic component and novel Electromagnetic Material
Using.
To achieve the goals above, the present invention provides the following technical scheme that
A kind of preparation method of sheet ferrite electromagnetic composite material, the preparation method is with the sheet made of ball milling
Ferrite, coupling modifier, resin, curing agent and diluent are raw material, each raw material component are mixed, molding, are made described multiple
Condensation material；
Wherein, the ferritic process conditions of sheet are prepared by ball milling are as follows:
By ferrite powder, steel ball, ball-milling additive and volatile solvents under 400-500r/min speed conditions ball milling 7-
8h；
The rigid ball includes 8mm diameter steel ball and 6mm diameter steel ball.
Preferably, the mass ratio of the ferrite powder, the steel ball, the ball-milling additive and the volatile solvents is
(100-130): (350-500): (0.01-0.05): (200-300)；
Preferably, the mass ratio of the ferrite powder, the steel ball, the ball-milling additive and the volatile solvents is
(115-120): (400-450): (0.02-0.03): (250-300).
Preferably, the mass ratio of the 8mm diameter steel ball and the 6mm diameter steel ball is 5:7.
Preferably, the ferrite is FeSiAl ferrite；
The ball-milling additive is calcium stearate；And/or
The volatile solvents are acetone.
Preferably, the mass ratio of the sheet ferrite and the resin is (70-80): (15-25), preferably (75-
80): (15-20)；
The quality of the coupling modifier is the 0.2-0.5wt% of the sheet ferrite quality；
The quality of the curing agent is the 20-25wt% of the resin quality；And/or
The quality of the diluent is the 15-20wt% of the resin quality.
Preferably, the coupling modifier is 3-aminopropyltriethoxysilane；And/or
The resin is epoxy resin.
Preferably, the molding uses the solidification of hot-press tank method of forming, pressure condition 1-5MPa, and temperature condition is 110-
120℃；Or
The molding uses the ultrasonic curing method of forming, and temperature condition is 90-100 DEG C.
Preferably, the preparation method includes the following steps:
(1) ball milling step: by ferrite powder, steel ball, ball-milling additive and volatile solvents in 400-500r/min revolving speed
Under the conditions of ball milling 7-8h, the rigid ball includes 8mm diameter steel ball and 6mm diameter steel ball, obtains sheet ferrite；
(2) coupling modifier step: sheet ferrite made from coupling modifier and step (1) is mixed, is obtained at coupling
Sheet ferrite after reason；
(3) it prepares slurry stage: sheet ferrite made from step (2) and resin, curing agent and diluent being mixed, obtained
To mixed slurry；
(4) forming step: the mixed slurry curing molding that step (3) are prepared obtains the composite material.
Preferably, it in the step of preparing slurry, is mixed under vacuum aided；Or
The ultrasonic disperse at 80-90 DEG C, 40-50kHz.
A kind of sheet ferrite electromagnetic composite material is made, the composite material using preparation method provided by the invention
With following performance:
The real part of opposite complex dielectric permittivity: 36.88-66.22；
The imaginary part of opposite complex dielectric permittivity: 7.51-34.02；
The real part of complex permeability: 0.47-3.42；
The imaginary part of complex permeability: 0.43-6.64.
Beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
The present invention prepares sheet ferrite powder using ball-milling method, compound with epoxy resin by coupling modifier, with heat
It presses tank technique or ultrasonic curing to form electromagnetic load composite material, shows higher electromagnetic parameter in 1-18GHz, it can be extensive
Applied in each field electronic equipment such as radar, navigation, satellite communication, electronic countermeasure, radio and television, mobile communication.
Sheet ferrite and resin compounded that ball milling obtains are prepared into electromagnetism and answered by this preparation method provided by the invention
Condensation material assigns sheet ferrite the electromagnetic parameter excellent in 1-18GHz frequency range by specific ball-milling technology, so that it is guaranteed that with
Composite material after resin compounded shows excellent electromagnetic performance in 1-18GHz frequency range；In addition, passing through this specific ball milling
Sheet ferrite made from technique can also realize preferable impedance matching with resin, and the optimization for being difficult to realize impedance matching is avoided to set
Meter.
Using the ferritic average grain diameter of sheet made from the ball-milling technology (referring to length of a film) at 30-35 μm, the piece of the partial size
Shape ferrite can easily be formed in later period formative stage, without biggish pressure condition, so that preparation process is more convenient.
Preparation method provided by the invention is in the ball milling stage according to the ferrite powder, the steel ball, the ball-milling additive
Mass ratio with the volatile solvents is (100-130): (350-500): (0.01-0.05): (200-300) this ingredient
Relationship carries out ball milling, so that it is guaranteed that the homogeneity of the uniformity of the ferritic granularity of sheet after ball milling and electromagnetic performance.More
Preferred ingredient relationship are as follows: the ferrite powder, the steel ball, the ball-milling additive and the volatile solvents mass ratio
For (115-120): (400-450): (0.02-0.03): (250-300), in the identical situation of other conditions, under the ingredient relationship
The ferritic granularity of the sheet that ball milling obtains is most uniform and electromagnetic performance is most uniform.
Preparation method provided by the invention makes 8mm diameter steel ball and 6mm diameter steel ball according to 5:7 mass ratio in ball milling
Used time, it is ensured that the uniformity of the ferritic granularity of sheet after ball milling and the homogeneity of electromagnetic performance.
Material property and process operability in order to balance, preparation method sheet ferrite and resin provided by the invention are pressed
According to mass ratio (70-80): (15-25) carries out compound.
Detailed description of the invention
Fig. 1 is sheet FeSiAl powder SEM shape appearance figure.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of preparation method of sheet ferrite electromagnetic composite material, the preparation side in first aspect
Method is using the sheet ferrite made of ball milling, coupling modifier, resin, curing agent and diluent as raw material, by each raw material group
Divide mixing, molding, the composite material is made；Wherein, the ferritic process conditions of sheet are prepared by ball milling are as follows: by ferrite
Powder, steel ball, ball-milling additive and volatile solvents (can be any number within the scope of this, for example, can in 400-500r/min
Think 400r/min, 410r/min, 420r/min, 430r/min, 440r/min, 450r/min, 460r/min, 470r/min,
480r/min, 490r/min, 500r/min) ball milling 7-8h under speed conditions (it can be any number within the scope of this, for example,
It can be 7h, 7.5h, 8h)；The rigid ball includes 8mm diameter steel ball and 6mm diameter steel ball.
Sheet ferrite and resin compounded that ball milling obtains are prepared into electromagnetism and answered by this preparation method provided by the invention
Condensation material assigns sheet ferrite the electromagnetic parameter excellent in 1-18GHz frequency range by specific ball-milling technology, so that it is guaranteed that with
Composite material after resin compounded shows excellent electromagnetic performance in 1-18GHz frequency range；In addition, passing through this specific ball milling
Sheet ferrite made from technique can also realize preferable impedance matching with resin, and the optimization for being difficult to realize impedance matching is avoided to set
Meter.
Inventor also found, using the ferritic average grain diameter of sheet made from the ball-milling technology (referring to length of a film) in 30-35 μ
The sheet ferrite of m, the partial size can easily be formed in later period formative stage, without biggish pressure condition, so that preparation
Technique is more convenient.
Other than rotational speed of ball-mill, steel ball size used and Ball-milling Time, inventor suggests in the ball milling stage according to described
Ferrite powder, the steel ball, the ball-milling additive and the volatile solvents mass ratio be (100-130): (350-
500): (0.01-0.05): (200-300) this ingredient relationship carries out ball milling, so that it is guaranteed that the ferritic grain of sheet after ball milling
The uniformity of degree and the homogeneity of electromagnetic performance.Preferred ingredient relationship are as follows: the ferrite powder, the steel ball, described
Ball-milling additive and the mass ratio of the volatile solvents are (115-120): (400-450): (0.02-0.03): (250-
300), in the identical situation of other conditions, the ferritic granularity of sheet that ball milling obtains under the ingredient relationship most uniformly and electromagnetism
Performance is most uniform.The ball-milling additive is preferably calcium stearate.The volatile solvents are preferably acetone.Specifically, matching
In material relationship, the dosage of above-mentioned each component can be any number in above range.For example, the mass number of the ferrite powder
It can be 100,105,110,115,120,125,130；For example, the mass number of the steel ball can for 350,360,370,380,
390,400,410,420,430,440,450,460,470,480,490,500；For example, the mass number of the ball-milling additive can be with
It is 0.01,0.02,0.03,0.04,0.05；For example, the mass number of the volatile solvents can for 200,210,220,
230、240、250、260、270、280、290、300。
In some preferred implementation methods, the mass ratio of the 8mm diameter steel ball and the 6mm diameter steel ball is 5:7.
Inventor is it has also been found that ball milling effect is best when using 8mm diameter steel ball and 6mm diameter steel ball according to this mass ratio, it is ensured that
The uniformity of the ferritic granularity of sheet after ball milling and the homogeneity of electromagnetic performance.
In some preferred embodiments, the mass ratio of the sheet ferrite and the resin is (70-80): (15-
25), preferably (75-80): (15-20).In order to obtain biggish magnetic loss, the raising ferritic additive amount of sheet, which is one, to be had
The means of effect.With the increase of sheet ferrite additive amount, the magnetic loss of composite material can be improved.But work as its additive amount mistake
Gao Shi, the difficulty of dispersion and the difficulty of subsequent forming all increase considerably.Therefore, process operability angle considers, it is proposed that
By sheet ferrite and resin according to mass ratio (70-80): (15-25) carries out compound.The resin can select epoxy resin.
Epoxy resin generates the product of space network under the action of curing agent, shows various excellent performances.Specifically,
In ingredient relationship, the dosage of above-mentioned each component can be any number in above range.For example, the sheet is ferritic
Mass number can be 70,71,72,73,74,75,76,77,78,79,80.For example, the mass number of the resin can for 15,
16,17,18,19,20,21,22,23,24,25.In actual operation, coupling modifier is preferred first mixes with sheet ferrite,
Coupling modifier processing is carried out to sheet ferrite, then is mixed with resin.The advantage operated in this way is: the sheet obtained after ball milling
Ferritic flaking structure makes it be not easy to disperse when mixing with resin this material with certain viscosity, and passes through idol
Joining modified can be largely avoided this problem.In addition to this it is possible to be mixed by sheet ferrite and resin
When by vacuum aided condition, carried out under vacuum aided mixing or by ultrasound, (can be 80 DEG C, 81 at 80-90 DEG C
DEG C, 82 DEG C, 83 DEG C, 84 DEG C, 85 DEG C, 86 DEG C, 87 DEG C, 88 DEG C, 89 DEG C, 90 DEG C), 40-50kHz (can for 40kHz, 41kHz,
42kHz, 43kHz, 44kHz, 45kHz, 46kHz, 47kHz, 48kHz, 49kHz, 50kHz) under ultrasonic disperse.
In some preferred embodiments, the quality of the coupling modifier is the 0.2- of the sheet ferrite quality
0.5wt% can be the arbitrary value within the scope of this, for example, can be 0.2wt%, 0.3wt%, 0.4wt%, 0.5wt%.Institute
Stating coupling modifier is preferably 3-aminopropyltriethoxysilane also known as KH550 or KH-550, using KH-550 to sheet iron
Oxysome, which carries out coupling modifier, facilitates ferrite and the promotion of resin-bonded power, to improve composite materials property.It is described solid
The quality of agent is the 20-25wt% of the resin quality, can be the arbitrary value within the scope of this, for example, can for 20wt%,
21wt%, 22wt%, 23wt%, 24wt%, 25wt%.The curing agent can select this field to be commonly used in cured epoxy
The curing agent of resin, for example, 2-ethyl-4-methylimidazole.The quality of the diluent is the 15- of the resin quality
20wt% can be the arbitrary value within the scope of this, for example, can for 15wt%, 16wt%, 17wt%, 18wt%, 19wt%,
20wt%.The diluent suitable for epoxy resin that the diluent can select this field common, such as commercially available 501 dilution
Agent.
Process progress can be prepared as follows in the preparation method in some preferred embodiments:
(1) ball milling step: by ferrite powder, steel ball, ball-milling additive and volatile solvents in 400-500r/min revolving speed
Under the conditions of ball milling 7-8h, the rigid ball includes 8mm diameter steel ball and 6mm diameter steel ball, obtains sheet ferrite；
(2) coupling modifier step: sheet ferrite made from coupling modifier and step (1) is mixed, is obtained at coupling
Sheet ferrite after reason；
(3) it prepares slurry stage: sheet ferrite made from step (2) and resin, curing agent and diluent being mixed, obtained
To mixed slurry；
(4) forming step: the mixed slurry curing molding that step (3) are prepared obtains the composite material.
More fully, this preparation method provided by the invention may include following preparation step:
(1) ball milling step: by ferrite powder, steel ball, ball-milling additive and volatile solvents in 400-500r/min revolving speed
Under the conditions of ball milling 7-8h, the rigid ball includes 8mm diameter steel ball and 6mm diameter steel ball, obtains sheet ferrite.The ferrite
Powder, the steel ball, the ball-milling additive and the volatile solvents mass ratio be preferably (100-130): (350-500):
(0.01-0.05): (200-300), more preferably (115-120): (400-450): (0.02-0.03): (250-300).It is described
The mass ratio of 8mm diameter steel ball and the 6mm diameter steel ball is preferably 5:7.The ball-milling additive can be calcium stearate.It is described
Volatile solvents can be acetone.
(2) coupling modifier step: sheet ferrite made from coupling modifier and step (1) is mixed, is obtained at coupling
Sheet ferrite after reason.The coupling modifier is preferably 3-aminopropyltriethoxysilane, and quality is the sheet
The 0.2-0.5wt% of ferrite quality.
(3) it prepares slurry stage: sheet ferrite made from step (2) and resin, curing agent and diluent being mixed, obtained
To mixed slurry.In this step, the mass ratio of the sheet ferrite and the resin is preferably (70-80): (15-25),
More preferably (75-80): (15-20).The quality of the curing agent is preferably the 20-25wt% of the resin quality.It is described dilute
The quality for releasing agent is preferably the 15-20wt% of the resin quality.It can be mixed by vacuum aided condition, i.e., in vacuum
It carries out mixing under auxiliary and either be mixed by ultrasonic means, the ultrasonic disperse at 80-90 DEG C, 40-50kHz.
(4) forming step: the mixed slurry curing molding that step (3) are prepared obtains the composite material.The molding
The solidification of hot-press tank method of forming can be used, pressure condition be that 1-5MPa (can be any number within the scope of this, for example, can be with
For 1MPa, 2MPa, 3MPa, 4MPa, 5MPa), it (can be any number within the scope of this, example that temperature condition, which is 110-120 DEG C,
Such as, can be 110 DEG C, 111 DEG C, 112 DEG C, 113 DEG C, 114 DEG C, 115 DEG C, 116 DEG C, 117 DEG C, 118 DEG C, 119 DEG C, 120 DEG C),
The ultrasonic curing method of forming can also be used, it (can be any number within the scope of this, for example, can that temperature condition, which is 90-100 DEG C,
Think 90 DEG C, 91 DEG C, 92 DEG C, 93 DEG C, 94 DEG C, 95 DEG C, 96 DEG C, 97 DEG C, 98 DEG C, 99 DEG C, 100 DEG C).
The present invention provides a kind of sheet ferrite electromagnetic composite material in second aspect, using preparation provided by the invention
Method is made, and the composite material has following performance:
The real part of opposite complex dielectric permittivity: 36.88-66.22；
The imaginary part of opposite complex dielectric permittivity: 7.51-34.02；
The real part of complex permeability: 0.47-3.42；
The imaginary part of complex permeability: 0.43-6.64, can be widely applied to radar, navigation, satellite communication, electronic countermeasure,
In each field electronic equipment such as radio and television, mobile communication.
It is the embodiment that the present invention enumerates below.
Embodiment 1
18g epoxy resin, 501 diluent of 4g, 3g 2-ethyl-4-methylimidazole are weighed, 0.5h is mixed under room temperature.
The untreated FeSiAl powder of 75g is then added, then adds 0.24g KH-550,8h is mixed under vacuum aided,
Obtain mixed slurry.
Finally, mixed slurry is poured into mold, solidification of hot-press tank is formed at 1.2MPa pressure, 110 DEG C, final to obtain iron
Oxysome/epoxy resin composite material.
Embodiment 2
400g steel ball (8mm diameter steel ball 167g+6mm diameter steel ball 233g) is mixed with 120gFeSiAl powder, with latter
It plays addition 0.02g calcium stearate and 250mL acetone is placed in ball grinder again, fixed rotating speed 450r/min high-energy ball milling 7.5h is obtained
To a length of 30-35 μm of average piece of sheet ferrite, microscopic appearance figure refers to Fig. 1.
18g epoxy resin, 501 diluent of 4g, 3g 2-ethyl-4-methylimidazole are weighed, 0.5h is mixed under room temperature,
The sheet FeSiAl powder of 75g ball-milling treatment is then added, then adds 0.24gKH-550,8h is mixed under vacuum aided, obtains
To mixed slurry.
Finally, composite mortar is poured into mold, solidification of hot-press tank is formed at 1.2MPa pressure, 110 DEG C, final to obtain piece
Shape FeSiAl/ epoxy resin composite material.
Embodiment 3
400g steel ball (8mm diameter steel ball 167g+6mm diameter steel ball 233g) is mixed with 120gFeSiAl powder, with latter
It plays addition 0.02g calcium stearate and 250mL acetone is placed in ball grinder again, fixed rotating speed 450r/min high-energy ball milling 7.5h is obtained
To a length of 30-35 μm of average piece of sheet ferrite.
18g epoxy resin, 501 diluent of 4g, 3g 2-ethyl-4-methylimidazole are weighed, 0.5h is mixed under room temperature,
The sheet FeSiAl powder of 75g ball-milling treatment is then added, then adds 0.24gKH-550, be placed in 80 DEG C, it is super under the conditions of 40kHz
It is slowly stirred 2h in sound disperser, obtains mixed slurry.
Finally, the ultrasonic curing 1.5h at 90-100 DEG C, final to obtain sheet FeSiAl/ epoxy resin composite material.
Embodiment 4
400g steel ball (8mm diameter steel ball 167g+6mm diameter steel ball 233g) is mixed with 120gFeSiAl powder, with latter
It plays addition 0.02g calcium stearate and 250mL acetone is placed in ball grinder again, fixed rotating speed 450r/min high-energy ball milling 7.5h is obtained
To a length of 30-35 μm of average piece of sheet ferrite.
18g epoxy resin, 501 diluent of 4g, 3g 2-ethyl-4-methylimidazole are weighed, 0.5h is mixed under room temperature,
The sheet FeSiAl powder of 58g ball-milling treatment is then added, then adds 0.18gKH-550,6h is mixed under vacuum aided, obtains
To mixed slurry.
Finally, mixed slurry is poured into mold, solidification of hot-press tank is formed at 1.2MPa pressure, 110 DEG C, final to obtain piece
Shape FeSiAl/ epoxy resin composite material.
Table 1 describes the preparation process of embodiment 1 to 4.
Table 1
| Number | Whether ball milling | Sheet FeSiAl powder dosage | Content of epoxy resin |
| Embodiment 1 | It is no | 75g* | 18g |
| Embodiment 2 | It is | 75g | 18g |
| Embodiment 3 | It is | 75g | 18g |
| Embodiment 4 | It is | 58g | 18g |
Indicate: 75g refers to the dosage of non-ball milling FeSiAl powder herein.
It is tested according to electromagnetic parameter of the SJ20512-1995 to composite material made from embodiment 1 to 4, composite material
Electromagnetic parameter testing the results are shown in Table 2.
Table 2
Note: ε ' is the real part of opposite complex dielectric permittivity；ε " is the imaginary part of opposite complex dielectric permittivity；μ ' is complex permeability
Real part；μ " is the imaginary part of complex permeability；tanσdFor electrical loss tangent angle；tanσmFor magnetic loss tangent angle.
It can be seen that from embodiment 1 (not carrying out ball milling) and the comparison of the test result of embodiment 2 and embodiment 3, pass through ball milling
Gained sheet FeSiAl/ epoxy resin composite material is in high frequency points magnetic conductivity with higher and dielectric constant after processing.
It can be seen that have using composite material prepared by ultrasonic curing higher from embodiment 2 and 3 Comparative result of embodiment
Magnetic loss.
It can be seen that from embodiment 3 and 4 Comparative result of embodiment, with the raising of sheet ferrite additive amount, can improve multiple
Condensation material magnetic loss.In conjunction with the embodiments 1 and embodiment 4 comparing result it is found that can not be reached when ferritic loading is lower
To the effect for significantly improving composite material magnetic loss.But ferritic additive amount is also not easy excessively, and it is excessive to will lead to viscosity too much,
Dispersing uniformity is deteriorated, and bubble is difficult to exclude, and craftsmanship is deteriorated.The present invention is during the preparation process by sheet ferrite and resin
(70-80): the mixing of (15-25) consumption proportion, most preferably according to (75-80): the mixing of (15-20) this consumption proportion, Ji Kexian
The magnetic conductivity and magnetic loss for improving composite material are write, and the difficulty of preparation process can be reduced.
Embodiment 5
It is substantially the same with the preparation method of embodiment 2, the difference is that: coupling modifier used is KH-570
(chemical name are as follows: γ-(methacryloxypropyl) propyl trimethoxy silicane).
Embodiment 6
It is substantially the same with the preparation method of embodiment 2, the difference is that: revolving speed is 600r/min when ball milling.
Embodiment 7
It is substantially the same with the preparation method of embodiment 2, the difference is that: Ball-milling Time 9h.
Embodiment 8
It is substantially the same with the preparation method of embodiment 2, the difference is that: steel ball used includes 5mm diameter when ball milling
Steel ball 200g+3mm diameter steel ball 200g.
Table 3
The present invention prepares sheet ferrite powder using ball-milling method, compound with epoxy resin by coupling modifier, with heat
Tank technique or ultrasonic curing molding is pressed (preferably to form) electromagnetic load composite material using ultrasonic curing, in 1-18GHz frequency range
Higher electromagnetic parameter is shown, radar is can be widely applied to, navigation, satellite communication, electronic countermeasure, radio and television, moves and lead to
In each field electronic equipments such as news.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of preparation method of sheet ferrite electromagnetic composite material, which is characterized in that the preparation method is to pass through ball milling
Manufactured sheet ferrite, coupling modifier, resin, curing agent and diluent are raw material, each raw material component are mixed, molding,
The composite material is made；
Wherein, the ferritic process conditions of sheet are prepared by ball milling are as follows:
By ferrite powder, steel ball, ball-milling additive and volatile solvents under 400-500r/min speed conditions ball milling 7-8h；
The rigid ball includes 8mm diameter steel ball and 6mm diameter steel ball.
2. preparation method according to claim 1, which is characterized in that the ferrite powder, the steel ball, the ball milling help
The mass ratio of agent and the volatile solvents is (100-130): (350-500): (0.01-0.05): (200-300)；
Preferably, the mass ratio of the ferrite powder, the steel ball, the ball-milling additive and the volatile solvents is
(115-120): (400-450): (0.02-0.03): (250-300).
3. preparation method according to claim 2, which is characterized in that the 8mm diameter steel ball and the 6mm diameter steel ball
Mass ratio be 5:7.
4. preparation method according to claim 2, which is characterized in that the ferrite is FeSiAl ferrite；
The ball-milling additive is calcium stearate；And/or
The volatile solvents are acetone.
5. preparation method according to claim 1, which is characterized in that the mass ratio of the sheet ferrite and the resin
For (70-80): (15-25), preferably (75-80): (15-20)；
The quality of the coupling modifier is the 0.2-0.5wt% of the sheet ferrite quality；
The quality of the curing agent is the 20-25wt% of the resin quality；And/or
The quality of the diluent is the 15-20wt% of the resin quality.
6. preparation method according to claim 5, which is characterized in that the coupling modifier is three ethoxy of 3- aminopropyl
Base silane；And/or
The resin is epoxy resin.
7. preparation method according to any one of claims 1 to 6, which is characterized in that the molding uses solidification of hot-press tank
The method of forming, pressure condition 1-5MPa, temperature condition are 110-120 DEG C；Or
The molding uses the ultrasonic curing method of forming, and temperature condition is 90-100 DEG C.
8. preparation method according to any one of claims 1 to 7, which is characterized in that the preparation method includes following step
It is rapid:
(1) ball milling step: by ferrite powder, steel ball, ball-milling additive and volatile solvents in 400-500r/min speed conditions
Lower ball milling 7-8h, the rigid ball include 8mm diameter steel ball and 6mm diameter steel ball, obtain sheet ferrite；
(2) coupling modifier step: sheet ferrite made from coupling modifier and step (1) is mixed, after obtaining coupling processing
Sheet ferrite；
(3) it prepares slurry stage: sheet ferrite made from step (2) and resin, curing agent and diluent being mixed, mixed
Close slurry；
(4) forming step: the mixed slurry curing molding that step (3) are prepared obtains the composite material.
9. preparation method according to claim 8, which is characterized in that in the step of preparing slurry, under vacuum aided
It is mixed；Or
The ultrasonic disperse at 80-90 DEG C, 40-50kHz.
10. a kind of sheet ferrite electromagnetic composite material, which is characterized in that use the described in any item preparations of claim 1 to 9
Method is made, and the composite material has following performance:
The real part of opposite complex dielectric permittivity: 36.88-66.22；
The imaginary part of opposite complex dielectric permittivity: 7.51-34.02；
The real part of complex permeability: 0.47-3.42；
The imaginary part of complex permeability: 0.43-6.64.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574564A (en) * | 2020-11-23 | 2021-03-30 | 航天特种材料及工艺技术研究所 | High-temperature-resistant modified bismaleimide electromagnetic composite material and preparation method thereof |
| CN113403011A (en) * | 2021-05-28 | 2021-09-17 | 长江航道工程局有限责任公司 | Dredge pump repairing agent for dredger and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050007101A (en) * | 2003-07-11 | 2005-01-17 | 에이비씨 타이완 일렉트로닉스 코포레이션 | Epoxy resin of electromagnetic interference suppression and manufacturing method thereof and an inductor applied in the electromagnetic interference suppression |
| CN104575894A (en) * | 2013-10-28 | 2015-04-29 | 深圳光启创新技术有限公司 | Light magnetic material, preparation method thereof and wave-absorbing plate |
| CN106793725A (en) * | 2016-12-12 | 2017-05-31 | 浙江工业大学 | A kind of ferrite polymer composite and preparation method and application |
| CN108298973A (en) * | 2018-03-01 | 2018-07-20 | 北京环境特性研究所 | One kind is based on graphene/ferritic passive frequency control material and preparation method thereof |
| CN109721281A (en) * | 2019-01-24 | 2019-05-07 | 航天特种材料及工艺技术研究所 | A kind of feeding network electromagnetic load composite material and preparation method |
-
2019
- 2019-07-19 CN CN201910653696.0A patent/CN110283429B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050007101A (en) * | 2003-07-11 | 2005-01-17 | 에이비씨 타이완 일렉트로닉스 코포레이션 | Epoxy resin of electromagnetic interference suppression and manufacturing method thereof and an inductor applied in the electromagnetic interference suppression |
| CN104575894A (en) * | 2013-10-28 | 2015-04-29 | 深圳光启创新技术有限公司 | Light magnetic material, preparation method thereof and wave-absorbing plate |
| CN106793725A (en) * | 2016-12-12 | 2017-05-31 | 浙江工业大学 | A kind of ferrite polymer composite and preparation method and application |
| CN108298973A (en) * | 2018-03-01 | 2018-07-20 | 北京环境特性研究所 | One kind is based on graphene/ferritic passive frequency control material and preparation method thereof |
| CN109721281A (en) * | 2019-01-24 | 2019-05-07 | 航天特种材料及工艺技术研究所 | A kind of feeding network electromagnetic load composite material and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 汪多仁等: "《精细化工中间体》", 31 January 2008, 海洋出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574564A (en) * | 2020-11-23 | 2021-03-30 | 航天特种材料及工艺技术研究所 | High-temperature-resistant modified bismaleimide electromagnetic composite material and preparation method thereof |
| CN113403011A (en) * | 2021-05-28 | 2021-09-17 | 长江航道工程局有限责任公司 | Dredge pump repairing agent for dredger and preparation method and application thereof |
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