CN109721281A - A kind of feeding network electromagnetic load composite material and preparation method - Google Patents
A kind of feeding network electromagnetic load composite material and preparation method Download PDFInfo
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- CN109721281A CN109721281A CN201910069992.6A CN201910069992A CN109721281A CN 109721281 A CN109721281 A CN 109721281A CN 201910069992 A CN201910069992 A CN 201910069992A CN 109721281 A CN109721281 A CN 109721281A
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Abstract
The present invention relates to a kind of feeding network electromagnetic load composite material and preparation methods, the preparation method includes the following steps: (1) high-energy ball milling carbonyl iron dust: carbonyl iron dust, steel ball, ball-milling additive and solvent are mixed, high-energy ball milling, drying, obtains flaky carbonyl iron powder body；(2) mixing: flaky carbonyl iron powder body, silane coupling agent are uniformly mixed, and are added resin, diluent and curing agent and are uniformly mixed, obtain mixed glue solution；(3) solidify: mixed glue solution compression molding or ultrasonic curing being formed, the composite material is obtained.Higher electromagnetic parameter is shown in 0.1-18GHz using composite material made from preparation method provided by the invention, especially magnetic loss performance 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 feeding network electromagnetic load are compound
Material 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.
Carbonyl iron material has a wide range of applications and occupies an important position in electromagnetic transmission technology, is the core of electronic component
Material.Currently, carbonyl iron material employed in all kinds of devices is generally spherical structure, there is preferable electricity in microwave frequency band
Magnetic screening action.But with the continuous improvement of working frequency in unit, to this support materials used in feeding network
Electromagnetic property also proposed requirements at the higher level, spherical carbonyl iron material has been difficult to meet.
Summary of the invention
It is compound the invention aims to bond micro-nano laminated structure carbonyl iron dust with epoxy resin, one kind is provided and is had
The preparation method of the functional composite material of excellent electromagnetic characteristic meets in terms of high-performance electronic component and novel Electromagnetic Material
Application.
To achieve the goals above, the present invention provides the following technical scheme that
1, a kind of feeding network preparation method of electromagnetic load composite material, includes the following steps:
(1) high-energy ball milling carbonyl iron dust: carbonyl iron dust, steel ball, ball-milling additive and solvent being mixed, high-energy ball milling, drying,
Obtain flaky carbonyl iron powder body；
(2) mixing: flaky carbonyl iron powder body, silane coupling agent are uniformly mixed, and add resin, diluent and curing agent
It is uniformly mixed, obtains mixed glue solution；With
(3) solidify: mixed glue solution compression molding or ultrasonic curing being formed, the composite material is obtained.
2, preparation method according to technical solution 1, when carrying out high-energy ball milling, ratio of grinding media to material is (4.5~7): 1, wherein
Ball refers to that steel ball, material refer to carbonyl iron dust, ratio representation quality ratio；
It is further preferred that steel ball used includes the steel ball of 2mm diameter and the steel ball of 4mm diameter, the mass ratio of the two is
1:2。
3, preparation method according to technical solution 1, the high-energy ball milling under the revolving speed of 550~1000r/min；
Preferably, flaky carbonyl iron powder body of the particle diameter distribution at 1~3 μm is obtained by high-energy ball milling.
4, according to the described in any item preparation methods of technical solution 1 to 3, the solvent selects acetone, ethyl alcohol, appointing in water
It is one or more；
The ball-milling additive is selected from calcium stearate and/or calcium gluconate；
The silane coupling agent selects γ-(methacryloxypropyl) propyl trimethoxy silicane；
The resin selects epoxy resin；
The diluent selects epoxy propane butyl ether；And/or
The curing agent selects triethylene tetramine and/or 2-ethyl-4-methylimidazole.
5, the preparation method according to technical solution 4, the additional amount of the solvent meet following condition: carbonyl iron dust point
The mass percentage dissipated in a solvent reaches 50~70wt%；
The quality of the silane coupling agent accounts for 0.5~1.0wt% of flaky carbonyl iron powder weight；
The quality of the resin accounts for 5~10wt% of flaky carbonyl iron powder weight；
The quality of the diluent accounts for 2~5wt% of flaky carbonyl iron powder weight；And/or
The quality of the curing agent accounts for 1~3wt% of flaky carbonyl iron powder weight.
6, the preparation method according to technical solution 5, in step (1), by 85g carbonyl iron dust, 500g steel ball,
0.015g ball-milling additive and the mixing of 150mL solvent, high-energy ball milling, Ball-milling Time is preferably 6~8 hours, and drying obtains sheet carbonyl
Base iron powder body；And/or
In step (2), 80~90g flaky carbonyl iron powder body, 0.4g silane coupling agent are uniformly mixed, 7g tree is added
Rouge, 1.8g diluent and 1.0~1.2g curing agent stir evenly under vacuum aided, obtain mixed glue solution.
7, preparation method according to technical solution 1, the process conditions of the compression molding are as follows: 15~30MPa of pressure,
100~120 DEG C of temperature.
8, preparation method according to technical solution 1, the molding process conditions of ultrasonic curing are as follows: supersonic frequency 40
~100kHz, ultrasonic time 20~50 minutes.
9, preparation method according to technical solution 1, using churned mechanically method by flaky carbonyl iron powder body, silane
Coupling agent is uniformly mixed；And/or
Be mixed under vacuum aided includes flaky carbonyl iron powder body, silane coupling agent, resin, diluent and curing agent
Mixture, obtain uniformly mixed mixed glue solution.
10, a kind of feeding network electromagnetic load composite material, using the described in any item preparation sides of technical solution 1 to 9
Method is made.
Beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
The present invention prepares flaky carbonyl iron powder body using ball-milling method, compound with epoxy resin by coupling modifier, with mould
Pressure or ultrasonic wave solidified technology form electromagnetic load composite material, show higher electromagnetic parameter in 0.1-18GHz, especially
It is magnetic loss performance, can be widely applied to radar, navigation, satellite communication, electronic countermeasure, radio and television, mobile communication etc. and respectively lead
In the electronic equipment of domain.
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 feeding network preparation method of electromagnetic load composite material, which includes
Following steps:
(1) high-energy ball milling carbonyl iron dust: carbonyl iron dust, steel ball, ball-milling additive and solvent being mixed, high-energy ball milling, drying,
Obtain flaky carbonyl iron powder body；High-energy ball milling can be carried out by existing high-energy ball milling device (for example, high energy ball mill)；
(2) mixing: flaky carbonyl iron powder body, silane coupling agent are uniformly mixed, and add resin, diluent and curing agent
It is uniformly mixed, obtains mixed glue solution；With
(3) solidify: mixed glue solution compression molding or ultrasonic curing being formed, the composite material is obtained.
In some preferred embodiments, when carrying out high-energy ball milling, ratio of grinding media to material is (4.5~7): 1, for example, can be
4.5:1,5:1,5.5:1,6:1,6.5:1,7:1, wherein ball refers to that steel ball, material refer to carbonyl iron dust, ratio representation quality ratio；
It is further preferred that steel ball used includes the steel ball of 2mm diameter and the steel ball of 4mm diameter, the mass ratio of the two is
1:2。
In some preferred embodiments, in 550~1000r/min (for example, can be 5500r/min, 600r/
min、650r/min、700r/min、750r/min、800r/min、850r/min、900r/min、950r/min、1000r/min)
Revolving speed under high-energy ball milling；
Preferably, flaky carbonyl iron powder body of the particle diameter distribution at 1~3 μm is obtained by high-energy ball milling.
Above-mentioned one or more ball-milling technologies (ratio of grinding media to material, ball milling steel ball size and dosage, rotational speed of ball-mill) can promote
Absorbent structure pattern changes, and has obvious effect to absorption loss electromagnetic wave.
In some preferred embodiments, the solvent selects acetone, ethyl alcohol, water any one or more of；
The ball-milling additive is selected from calcium stearate and/or calcium gluconate；
The silane coupling agent selects γ-(methacryloxypropyl) propyl trimethoxy silicane；
The resin selects epoxy resin；
The diluent selects epoxy propane butyl ether；And/or
The curing agent selects triethylene tetramine and/or 2-ethyl-4-methylimidazole.
In some preferred embodiments, the additional amount of the solvent meets following condition: carbonyl iron dust is dispersed in molten
Mass percentage in agent reaches 50~70wt%, for example, can for 50wt%, 55wt%, 60wt%, 65wt%,
70wt%；
The quality of the silane coupling agent accounts for 0.5~1.0wt% of flaky carbonyl iron powder weight, for example, can be
0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1.0wt%；
The quality of the resin accounts for 5~10wt% of flaky carbonyl iron powder weight, for example, can for 5wt%, 6wt%,
7wt%, 8wt%, 9wt%, 10wt%；
The quality of the diluent accounts for 2~5wt% of flaky carbonyl iron powder weight, for example, can for 2wt%,
3wt%, 4wt%, 5wt%；And/or
The quality of the curing agent accounts for 1~3wt% of flaky carbonyl iron powder weight, for example, can for 1wt%,
2wt%, 3wt%.
In some preferred embodiments, in step (1), by 85g carbonyl iron dust, 500g steel ball, 0.015g ball milling
Auxiliary agent and the mixing of 150mL solvent, high-energy ball milling, Ball-milling Time is preferably 6~8 hours, and drying obtains flaky carbonyl iron powder body；
And/or
In step (2), 80~90g flaky carbonyl iron powder body, 0.4g silane coupling agent are uniformly mixed, 7g tree is added
Rouge, 1.8g diluent and 1.0~1.2g curing agent stir evenly under vacuum aided, obtain mixed glue solution.
In some preferred embodiments, the process conditions of the compression molding are as follows: 15~30MPa of pressure, for example, can
Think 15MPa, 20MPa, 25MPa, 30MPa, 100~120 DEG C of temperature, for example, can be 100 DEG C, 110 DEG C, 120 DEG C.
In some preferred embodiments, the molding process conditions of the ultrasonic curing are as follows: supersonic frequency 40~
100kHz, for example, can be 40kHz, 50kHz, 60kHz, 70kHz, 80kHz, 90kHz, 100kHz, 20~50 points of ultrasonic time
Clock, for example, can be 20 minutes, 30 minutes, 40 minutes, 50 minutes.
In some preferred embodiments, using churned mechanically method by flaky carbonyl iron powder body, silane coupling agent
It is uniformly mixed；And/or
Be mixed under vacuum aided includes flaky carbonyl iron powder body, silane coupling agent, resin, diluent and curing agent
Mixture, obtain uniformly mixed mixed glue solution.Being mixed under vacuum aided can be deviate from using vacuum aided
Bubble.
The present invention also provides a kind of feeding network electromagnetic load composite material, which is provided using the present invention
Preparation method be made.Have using this composite material made from preparation method provided by the invention in 0.1-18GHz frequency range
Higher electromagnetic parameter, especially magnetic loss performance, can be widely applied to radar, navigation, satellite communication, electronic countermeasure, broadcast
In each field electronic equipment such as TV, mobile communication.
It is the embodiment that the present invention enumerates below.
Embodiment 1
Weigh 7g epoxy resin, 1.8g epoxy propane butyl ether, 0.6g triethylene tetramine, 0.6g2- ethyl -4- methyl miaow
Azoles, mechanical stirring 0.5h is to be uniformly mixed under room temperature；The untreated carbonyl iron dust of 80g is then added, then adds 0.4g KH-570,
6h then is mixed under vacuum aided；Finally, mixed glue solution is poured into mold, it is molded at 15MPa pressure, 100 DEG C
Molding, it is final to obtain carbonyl iron/epoxy resin composite material.
Embodiment 2
500g steel ball (the steel ball 333g of steel ball 167g and the 4mm diameter including 2mm diameter) and 85g carbonyl iron dust is mixed
It closes, 0.015g calcium stearate then is added together and 150mL acetone is placed in again in spheroidal graphite tank, fixed rotating speed 550r/min high energy ball
8h is ground, drying obtains flaky carbonyl iron powder.
Weigh 7g epoxy resin, 1.8g epoxy propane butyl ether, 0.6g triethylene tetramine, 0.6g2- ethyl -4- methyl miaow
0.5h is mixed under room temperature in azoles；The flaky carbonyl iron powder that 80g ball-milling treatment obtains then is added, then adds 0.4g KH-
570,6h is mixed under vacuum aided, obtains mixed glue solution.
Finally, mixed glue solution is poured into mold, it is pressed and molded at 15MPa pressure, 100 DEG C, it is final to obtain sheet carbonyl
Iron/epoxy resin composite material.
Embodiment 3
500g steel ball (the steel ball 333g of steel ball 167g and the 4mm diameter including 2mm diameter) and 85g carbonyl iron dust is mixed
It closes, 0.015g calcium stearate then is added together and 150mL acetone is placed in again in spheroidal graphite tank, fixed rotating speed 550r/min high energy ball
8h is ground, drying obtains flaky carbonyl iron powder.
Weigh 7g epoxy resin, 1.8g epoxy propane butyl ether, 0.6g triethylene tetramine, 0.6g2- ethyl -4- methyl miaow
Azoles, mechanical stirring 0.5h is to be uniformly mixed under room temperature；The flaky carbonyl iron powder of 80g ball-milling treatment is then added, then adds 0.4g
KH-570, then composite mortar is placed in 60 DEG C, is slowly stirred 2h in the ultrasonic dispersers under the conditions of 40kHz；Finally, at 100 DEG C
Lower ultrasonic curing 1.5h, it is final to obtain sheet carbonyl iron/epoxy resin composite material.
Embodiment 4
550g steel ball (the steel ball 333g of steel ball 167g and the 4mm diameter including 2mm diameter) and 120g carbonyl iron dust is mixed
It closes, 0.02g calcium stearate then is added together and 180mL acetone is placed in again in spheroidal graphite tank, fixed rotating speed 550r/min high energy ball
8h is ground, drying obtains flaky carbonyl iron powder.
Weigh 7g epoxy resin, 1.8g epoxy propane butyl ether, 0.6g triethylene tetramine, 0.6g2- ethyl -4- methyl miaow
Azoles, mechanical stirring 0.5h is to be uniformly mixed under room temperature；The flaky carbonyl iron powder of 89g ball-milling treatment is then added, then adds
0.445g KH-570 is mixed 6h under vacuum aided, obtains mixed glue solution.
Finally, mixed glue solution is poured into mold, it is pressed and molded at 15MPa pressure, 100 DEG C, it is final to obtain sheet carbonyl
Iron/epoxy resin composite material.
The electromagnetic parameter testing result of 1 embodiment 1 to 4 of table
It can be seen that from embodiment 1-4 Comparative result, the carbonyl iron of the sheet as obtained by after ball-milling treatment/epoxy resin composite wood
Material is in high frequency points magnetic conductivity with higher, and dielectric constant is lower；
It can be seen that from the Comparative result of embodiment 2 and 3, using the magnetic loss with higher of composite material prepared by mould pressing process
Consumption；
It can be seen that from the Comparative result of embodiment 2 and 4, with the raising of flaky carbonyl iron powder additive amount, composite wood can be improved
Expect magnetic loss.But the additive amount of carbonyl iron dust is also not easy excessively, and it is excessive to will lead to viscosity too much, and dispersing uniformity is deteriorated, bubble
It is difficult to exclude, craftsmanship is deteriorated.
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 feeding network preparation method of electromagnetic load composite material, which comprises the steps of:
(1) high-energy ball milling carbonyl iron dust: carbonyl iron dust, steel ball, ball-milling additive and solvent being mixed, high-energy ball milling, and drying obtains
Flaky carbonyl iron powder body；
(2) mixing: flaky carbonyl iron powder body, silane coupling agent are uniformly mixed, and add resin, diluent and curing agent mixing
Uniformly, mixed glue solution is obtained；With
(3) solidify: mixed glue solution compression molding or ultrasonic curing being formed, the composite material is obtained.
2. preparation method according to claim 1, which is characterized in that when carrying out high-energy ball milling, ratio of grinding media to material is (4.5~7):
1, wherein ball refers to that steel ball, material refer to carbonyl iron dust, ratio representation quality ratio；
It is further preferred that steel ball used includes the steel ball of 2mm diameter and the steel ball of 4mm diameter, the mass ratio of the two is 1:2.
3. preparation method according to claim 1, which is characterized in that the high energy ball under the revolving speed of 550~1000r/min
Mill；
Preferably, flaky carbonyl iron powder body of the particle diameter distribution at 1~3 μm is obtained by high-energy ball milling.
4. preparation method according to any one of claims 1 to 3, which is characterized in that the solvent select acetone, ethyl alcohol,
Water is any one or more of；
The ball-milling additive is selected from calcium stearate and/or calcium gluconate；
The silane coupling agent selects γ-(methacryloxypropyl) propyl trimethoxy silicane；
The resin selects epoxy resin；
The diluent selects epoxy propane butyl ether；And/or
The curing agent selects triethylene tetramine and/or 2-ethyl-4-methylimidazole.
5. the preparation method according to claim 4, which is characterized in that the additional amount of the solvent meets following condition: carbonyl
The mass percentage of base iron powder dispersion in a solvent reaches 50~70wt%；
The quality of the silane coupling agent accounts for 0.5~1.0wt% of flaky carbonyl iron powder weight；
The quality of the resin accounts for 5~10wt% of flaky carbonyl iron powder weight；
The quality of the diluent accounts for 2~5wt% of flaky carbonyl iron powder weight；And/or
The quality of the curing agent accounts for 1~3wt% of flaky carbonyl iron powder weight.
6. preparation method according to claim 5, which is characterized in that in step (1), by 85g carbonyl iron dust, 500g steel
Ball, 0.015g ball-milling additive and the mixing of 150mL solvent, high-energy ball milling, Ball-milling Time is preferably 6~8 hours, and drying obtains piece
Shape carbonyl iron powder；And/or
In step (2), 80~90g flaky carbonyl iron powder body, 0.4g silane coupling agent are uniformly mixed, add 7g resin,
1.8g diluent and 1.0~1.2g curing agent stir evenly under vacuum aided, obtain mixed glue solution.
7. preparation method according to claim 1, which is characterized in that the process conditions of the compression molding are as follows: pressure 15
~30MPa, 100~120 DEG C of temperature.
8. preparation method according to claim 1, which is characterized in that the molding process conditions of ultrasonic curing are as follows: super
40~100kHz of acoustic frequency, ultrasonic time 20~50 minutes.
9. preparation method according to claim 1, which is characterized in that use churned mechanically method by flaky carbonyl iron powder
Body, silane coupling agent are uniformly mixed；And/or
It is mixed under vacuum aided comprising the mixed of flaky carbonyl iron powder body, silane coupling agent, resin, diluent and curing agent
Object is closed, uniformly mixed mixed glue solution is obtained.
10. a kind of feeding network electromagnetic load composite material, which is characterized in that described in any item using claim 1 to 9
Preparation method is made.
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| CN110256848A (en) * | 2019-07-19 | 2019-09-20 | 航天特种材料及工艺技术研究所 | A kind of magnetoelectric composites and preparation method thereof |
| CN110283429A (en) * | 2019-07-19 | 2019-09-27 | 航天特种材料及工艺技术研究所 | A kind of sheet ferrite electromagnetic composite material and preparation method |
| CN112266200A (en) * | 2020-10-28 | 2021-01-26 | 航天特种材料及工艺技术研究所 | Carbonyl iron powder wave-absorbing material with high magnetic loss and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110256848A (en) * | 2019-07-19 | 2019-09-20 | 航天特种材料及工艺技术研究所 | A kind of magnetoelectric composites and preparation method thereof |
| CN110283429A (en) * | 2019-07-19 | 2019-09-27 | 航天特种材料及工艺技术研究所 | A kind of sheet ferrite electromagnetic composite material and preparation method |
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| CN112266200A (en) * | 2020-10-28 | 2021-01-26 | 航天特种材料及工艺技术研究所 | Carbonyl iron powder wave-absorbing material with high magnetic loss and preparation method thereof |
| CN112266200B (en) * | 2020-10-28 | 2022-05-06 | 航天特种材料及工艺技术研究所 | Carbonyl iron powder wave-absorbing material with high magnetic loss and preparation method thereof |
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