CN109880377A - A kind of silica gel/carbonyl iron dust compound broadband inhales wave plate and preparation method thereof - Google Patents
A kind of silica gel/carbonyl iron dust compound broadband inhales wave plate and preparation method thereof Download PDFInfo
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Abstract
The present invention provides the preparation methods that a kind of silica gel/carbonyl iron dust compound broadband inhales wave plate, the following steps are included: A) it is wet-process modified to carbonyl iron dust and the progress of non-magnetic inorganic powder respectively using silane coupling agent, obtain modified carbonyl iron powder and modified non-magnetic inorganic powder；The mass ratio of the silane coupling agent and carbonyl iron dust is (0.3~2): 100；The mass ratio of the silane coupling agent and non-magnetic inorganic powder is (0.3~2): 100；B) the modified carbonyl iron powder for obtaining vinyl silicone oil composition, containing hydrogen silicone oil composition, the step A) and modified non-magnetic inorganic powder mixing, obtain premix sizing material；C) inhibitor and platinum catalyst are added in the premix sizing material, obtain blend glue stuff；D) by the blend glue stuff calendering formation, hot setting is carried out, silica gel/carbonyl iron dust compound broadband is obtained and inhales wave plate.The present invention also provides a kind of silica gel/carbonyl iron dust compound broadbands to inhale wave plate.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material technical fields more particularly to a kind of silica gel/carbonyl iron dust compound broadband to inhale
Wave plate and preparation method thereof.
Background technique
Electromagnetic wave is the important carrier of communication system transmitting information, is related to the fields such as communication, electronics, physics, aerospace,
While offering convenience to the mankind, electromagnetic wave influences whether the normal operation of all kinds of electronic devices, can also jeopardize the mankind
Health.
Electromagnetic wave absorbent material, abbreviation absorbing material are a kind of to convert electromagnetic wave energy to thermal energy or other forms
A kind of functional material of energy.The application of absorbing material provides for the problems such as solution electromagnetic radiation, electromagnetic interference, electromagnetic compatibility
Effective ways are studied and have important meaning to electronic equipment running environment and environment for human survival is improved using absorbing material
Justice.
With the development of high speed communication technology, electronic equipment increasingly minimized, Highgrade integration, the electromagnetism wave frequency used
Rate is also higher and higher, and if 5G communication will use hyper band, millimeter wave frequency band, car radar uses 24GHz and 77GHz
Etc. frequencies.These technology developing characteristics, so that electronic equipment faces more complicated electromagnetic environment, it is desirable that absorbing material has
Electromagnetic compatibility and anti-electromagnetic interference capability under wider frequency rate.
Summary of the invention
The purpose of the present invention is to provide a kind of silica gel/carbonyl iron dust compound broadbands to inhale wave plate and preparation method thereof, this hair
Suction wave plate in bright has good absorbing property under wider frequency rate, is conducive to related electromagnetic compatibility and electromagnetic interference problem
It solves.
The present invention provides a kind of preparation method of silica gel/carbonyl iron dust compound broadband suction wave plate, comprising the following steps:
A) wet-process modified to carbonyl iron dust and the progress of non-magnetic inorganic powder respectively using silane coupling agent, obtain modified carbonyl
Base iron powder and modified non-magnetic inorganic powder；
The non-magnetic inorganic powder is kaolin, phlogopite powder, alumina powder, precipitated calcium carbonate, silicon powder and gas phase
One or more of method silica；
The mass ratio of the silane coupling agent and carbonyl iron dust is (0.3~2): 100；
The mass ratio of the silane coupling agent and non-magnetic inorganic powder is (0.3~2): 100；
B) by modified carbonyl iron powder that vinyl silicone oil composition, containing hydrogen silicone oil composition, the step A) is obtained and change
Property non-magnetic inorganic powder mixing, obtain premix sizing material；
C) inhibitor and platinum catalyst are added in the premix sizing material, obtain blend glue stuff；
D) by the blend glue stuff calendering formation, hot setting is carried out, silica gel/carbonyl iron dust compound broadband is obtained and inhales wave
Piece.
Preferably, in the carbonyl iron dust, iron content >=95%, carbon element content≤1%, D50 is 2.0~6.5 μ
m。
Preferably, the vinyl silicone oil composition is the composition of vinyl-terminated silicone fluid and multi-vinyl silicone oil；
The viscosity of the vinyl silicone oil composition is 16000~50000mPas；
The content of the vinyl silicone oil composition medium vinyl is 0.03~0.15mmol/g.
Preferably, containing hydrogen silicone oil composition is the combination of the containing hydrogen silicone oil of different silicon hydrogen contents；
The viscosity of the containing hydrogen silicone oil composition is 45~500mPas；
Silicon hydrogen content in the containing hydrogen silicone oil composition is 2.1~6.5mmol/g.
Preferably, the step B) in raw material matched according to following parts by weight:
Vinyl silicone oil composition: 100 parts；
Containing hydrogen silicone oil composition: 6~12 parts；
Modified carbonyl iron powder: 160~300 parts；
Modified non-magnetic inorganic powder: 10~25 parts.
Preferably, the inhibitor be methyl three (1,1- dimethyl -1- acetylene ylmethoxy) silane, vinyl three (1,
1- dimethyl-1- acetylene ylmethoxy) silane, phenyl three (1,1- dimethyl-1- acetylene ylmethoxy) silane, 3- methyl-1-
Butine -3- alcohol, 1,3,5,7- tetramethyl -1,3,5,7- tetravinyl cyclotetrasiloxane, N, N, N ', N '-tetraallyl is to benzene two
One or more of formamide and maleic acid monoallyl.
Preferably, the platinum catalyst is platinum-divinyl tetramethyl disiloxane complex；
The mass content of Pt is 0.05% in the platinum catalyst.
Preferably, on the basis of by vinyl silicone oil composition for 100 parts by weight, the platinum catalyst is 0.1~0.5 weight
Part is measured, the inhibitor is 0.15~0.45 parts by weight.
Preferably, the step D) solidification temperature be 120~150 DEG C；
The step D) curing time be 10~50min.
The present invention provides a kind of silica gel/carbonyl iron dust compound broadband suction wave plate, is made according to above-mentioned preparation method.
The present invention provides the preparation methods that a kind of silica gel/carbonyl iron dust compound broadband inhales wave plate, comprising the following steps: A)
It is wet-process modified to carbonyl iron dust and the progress of non-magnetic inorganic powder respectively using silane coupling agent, it obtains modified carbonyl iron powder and changes
Property non-magnetic inorganic powder；The non-magnetic inorganic powder is that kaolin, phlogopite powder, alumina powder, precipitated calcium carbonate, silicon are micro-
One or more of powder and fumed silica；The mass ratio of the silane coupling agent and carbonyl iron dust is (0.3~2):
100；The mass ratio of the silane coupling agent and non-magnetic inorganic powder is (0.3~2): 100；B it) combines vinyl silicone oil
Object, containing hydrogen silicone oil composition, the step A) obtained modified carbonyl iron powder and modified non-magnetic inorganic powder mixing, it obtains pre-
Mixed sizing material；C) inhibitor and platinum catalyst are added in the premix sizing material, obtain blend glue stuff；D) by the blend glue stuff
Calendering formation carries out hot setting, obtains silica gel/carbonyl iron dust compound broadband and inhales wave plate.The present invention utilizes silane coupling agent pair
Carbonyl iron dust and the progress of non-magnetic inorganic powder are wet-process modified, and the silica gel being prepared/carbonyl iron dust compound broadband inhales wave plate in K
Wave band and Ka wave band have good absorbing property, and the reachable -20dB of reflection loss peak is hereinafter, maximum can arrive -34dB, -10dB
Bandwidth below is in 10GHz or more, maximum reachable 14GHz.Preparation method is simple in the present invention, is conducive to extensive life
It produces.
In addition, a kind of silica gel provided by the invention/carbonyl iron dust compound broadband, which inhales wave plate, also has good physical mechanical
Performance, hardness are Shao A40~55, and tensile strength has UL-94V0's 300% or more in 3.5MPa or more, elongation at break
Flame retardant rating.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the preparation technology flow chart that silica gel/carbonyl iron dust compound broadband inhales wave plate in the present invention；
Fig. 2 is the reflection loss curve that silica gel/carbonyl iron dust compound broadband that the embodiment of the present invention 1 obtains inhales wave plate；
Fig. 3 is the reflection loss curve that silica gel/carbonyl iron dust compound broadband that the embodiment of the present invention 2 obtains inhales wave plate；
Fig. 4 is the reflection loss curve that silica gel/carbonyl iron dust compound broadband that the embodiment of the present invention 3 obtains inhales wave plate.
Specific embodiment
The present invention provides the preparation methods that a kind of silica gel/carbonyl iron dust compound broadband inhales wave plate, comprising the following steps:
A) wet-process modified to carbonyl iron dust and the progress of non-magnetic inorganic powder respectively using silane coupling agent, obtain modified carbonyl
Base iron powder and modified non-magnetic inorganic powder；
The non-magnetic inorganic powder is kaolin, phlogopite powder, alumina powder, precipitated calcium carbonate, silicon powder and gas phase
One or more of method silica；
The mass ratio of the silane coupling agent and carbonyl iron dust is (0.3~2): 100；
The mass ratio of the silane coupling agent and non-magnetic inorganic powder is (0.3~2): 100；
B) by modified carbonyl iron powder that vinyl silicone oil composition, containing hydrogen silicone oil composition, the step A) is obtained and change
Property non-magnetic inorganic powder mixing, obtain premix sizing material；
C) inhibitor and platinum catalyst are added in the premix sizing material, obtain blend glue stuff；
D) by the blend glue stuff calendering formation, hot setting is carried out, silica gel/carbonyl iron dust compound broadband is obtained and inhales wave
Piece.
Present invention preferably uses silane coupler solutions to be modified carbonyl iron dust and non-magnetic inorganic powder, the silicon
Alkane coupling agent solution is preferably the ethanol water of silane coupling agent, and it is even that the present invention preferably prepares the silane according to the following steps
Join agent solution and material powder carried out wet-process modified:
Silane coupling agent is added in ethanol water, the hydrolyzate solution of silane coupling agent is obtained, then by the silicon
The hydrolyzate solution of alkane coupling agent respectively carries out carbonyl iron dust and non-magnetic inorganic powder by atomization method wet-process modified.
In the present invention, the mass fraction of the ethanol water is 90~95%；The pH value of the ethanol water is excellent
It is selected as 4~5.5.
The silane coupling agent is preferably tetraethoxysilane, γ-methacryloxypropyl trimethyl silane, γ-
Glycidyl ether oxygen propyl trimethoxy silicane, vinyl silanes, methacryloxypropyl silane, butadienyl triethoxysilicane
One of alkane, octyltri-ethoxysilane, hexadecyl trimethoxy silane and bis- (triethoxysilyl) ethane or
It is several；The mass concentration of silane coupling agent is preferably 1~5% in the silane coupler solution, and more preferably 2~4%, it is optimal
It is selected as 3%.
In the present invention, in the carbonyl iron dust, iron content >=95%, carbon element content≤1%, D50 be 2.0~
6.5 μm, it is preferred that iron content >=97%, carbon element content≤0.9%, D50 are 2.5~4.0 μm.
In the present invention, the non-magnetic inorganic powder is preferably kaolin, phlogopite powder, alumina powder, lightweight carbonic acid
One or more of calcium, silicon powder and fumed silica.
The mass ratio of the silane coupling agent and carbonyl iron dust is preferably (0.3~2): 100, more preferably (0.5~
1.5): 100, most preferably (0.8~1.2): 100, specifically, in an embodiment of the present invention, it can be 0.5:100,0.8:
100 or 1.2:100；The mass ratio of the silane coupling agent and the non-magnetic inorganic powder is preferably (0.3~2): 100, more
Preferably (0.5~1.6): 100, most preferably (0.8~1.2): 100, specifically, in an embodiment of the present invention, can be
0.35:100,0.5:100 or 1.6:100.
After completing to the modification of the carbonyl iron dust and non-magnetic inorganic powder, the present invention combines vinyl silicone oil
Object, containing hydrogen silicone oil composition, modified carbonyl iron powder and modified non-magnetic inorganic powder mixing, are stirred under vacuum uniformly, are premixed
Sizing material.
In the present invention, the viscosity of the vinyl silicone oil composition is preferably 16000~50000mPas, more preferably
For 20000~40000mPas；Specifically, in an embodiment of the present invention, can be 18000mPas, 27000mPas
Or 31000mPas；The content of the vinyl silicone oil composition medium vinyl is preferably 0.03~0.15mmol/g, more preferably
For 0.05~0.12mmol/g, most preferably 0.08~0.1mmol/g, specifically, in an embodiment of the present invention, can be
0.03mmol/g, 0.08mmol/g or 0.12mmol/g.
In the present invention, the vinyl silicone oil composition is made of vinyl-terminated silicone fluid and multi-vinyl silicone oil, described
Vinyl-terminated silicone fluid has structure shown in Formulas I:
Wherein, R1And R2Independently selected from alkyl, halogenated alkyl, naphthenic base, aryl, substituted aryl and a kind of, n >=50；
The multi-vinyl silicone oil has structure shown in Formula II:
Wherein, R3、R4And R5Independently selected from one of alkyl, halogenated alkyl, naphthenic base, aryl and substituted aryl, a+
b≥50。
In the present invention, containing hydrogen silicone oil composition is the combination of the containing hydrogen silicone oil of different silicon hydrogen contents；The containing hydrogen silicone oil
The viscosity of composition is preferably 45~500mPas, more preferably 100~400mPas, most preferably 200~300mPa
S, specifically, in an embodiment of the present invention, can be 95mPas, 360mPas or 450mPas；The containing hydrogen silicone oil
Silicon hydrogen content is preferably 2.1~6.5mmol/g in composition, more preferably 3.0~5.6mmol/g, most preferably 3.2~
4.5mmol/g, specifically, in an embodiment of the present invention, can be 3.2mmol/g, 4.5mmol/g or 5.6mmol/g.
The containing hydrogen silicone oil composition has structure shown in formula III:
Wherein, R6For H or CH3, R7And R8Independently selected from alkyl, halogenated alkyl, naphthenic base, aryl and substituted aryl
One kind, a+b >=8；
In the present invention, on the basis of the vinyl silicone oil composition by 100 parts by weight, the containing hydrogen silicone oil composition
Parts by weight be preferably 6~12 parts, more preferably 7~10 parts, specifically, in an embodiment of the present invention, can be 6.6
Part, 7.8 parts or 10 parts；The parts by weight of the modified carbonyl iron powder are preferably 160~300 parts, and more preferably 200~250 parts,
Specifically, in an embodiment of the present invention, can be 215 parts, 294 parts or 162 parts；The weight of the modified non-magnetic inorganic powder
Measuring number is preferably 10~25 parts, more preferably 15~20 parts, specifically, in an embodiment of the present invention, can be 13.5 parts,
17 parts or 21 parts.
In the present invention, the vacuum degree of the vacuum stirring is preferably >=0.09MPa, and the time of the vacuum stirring is preferred
For 100~150min.
After obtaining premix sizing material, inhibitor and platinum catalyst are added in the premix sizing material present invention, are mixed
Sizing material.
In the present invention, the inhibitor is preferably methyl three (1,1- dimethyl -1- acetylene ylmethoxy) silane, ethylene
Base three (1,1- dimethyl -1- acetylene ylmethoxy) silane, phenyl three (1,1- dimethyl -1- acetylene ylmethoxy) silane, 3-
Methyl-1-butine-3- alcohol, 1,3,5,7- tetramethyl-1,3,5,7- tetravinyl cyclotetrasiloxane, N, N, N ', N '-tetraallyl
One or more of terephthalamide and maleic acid monoallyl；It is with the 100 parts by weight of ethylene base silicone oil composite
Benchmark, the parts by weight of the inhibitor are preferably 0.15~0.45 part, and more preferably 0.18~0.3 part, specifically, in this hair
In bright embodiment, 0.18 part, 0.15 part or 0.29 part can be.
The platinum catalyst is preferably platinum-divinyl tetramethyl disiloxane complex；In the platinum catalyst
The mass content of Pt is 0.05%；On the basis of the 100 parts by weight of ethylene base silicone oil composite, the weight of the platinum catalyst
Measuring number is preferably 0.1~0.5 part, and more preferably 0.2~0.4 part, specifically, in an embodiment of the present invention, can be
0.16 part, 0.2 part or 0.31 part.
The present invention is added after inhibitor and platinum catalyst preferably in the premix sizing material, is stirred under vacuum, is obtained
To blend glue stuff, the vacuum degree of the vacuum stirring preferably >=0.09MPa, the time of the vacuum stirring is preferably 30~
50min。
After obtaining blend glue stuff, the blend glue stuff calendering formation is carried out hot setting by the present invention, obtain silica gel/
Carbonyl iron dust compound broadband inhales wave plate.
In the present invention, the temperature of the hot setting is preferably 120~150 DEG C, and more preferably 135 DEG C；The high temperature
The cured time is preferably 10~50min, more preferably 20~40min, most preferably 30min.
Obtained silica gel/carbonyl iron dust compound broadband suction wave plate is with a thickness of 1 ± 0.1mm.
The present invention also provides a kind of silica gel/carbonyl iron dust compound broadbands to inhale wave plate, is prepared into according to above-mentioned preparation method
It arrives.
The present invention provides the preparation methods that a kind of silica gel/carbonyl iron dust compound broadband inhales wave plate, comprising the following steps: A)
It is wet-process modified to carbonyl iron dust and the progress of non-magnetic inorganic powder respectively using silane coupling agent, it obtains modified carbonyl iron powder and changes
Property non-magnetic inorganic powder；The non-magnetic inorganic powder is that kaolin, phlogopite powder, alumina powder, precipitated calcium carbonate, silicon are micro-
One or more of powder and fumed silica；The mass ratio of the silane coupling agent and carbonyl iron dust is (0.3~2):
100；The mass ratio of the silane coupling agent and non-magnetic inorganic powder is (0.3~2): 100；B it) combines vinyl silicone oil
Object, containing hydrogen silicone oil composition, the step A) obtained modified carbonyl iron powder and modified non-magnetic inorganic powder mixing, it obtains pre-
Mixed sizing material；C) inhibitor and platinum catalyst are added in the premix sizing material, obtain blend glue stuff；D) by the blend glue stuff
Calendering formation carries out hot setting, obtains silica gel/carbonyl iron dust compound broadband and inhales wave plate.The present invention utilizes silane coupling agent pair
Carbonyl iron dust and the progress of non-magnetic inorganic powder are wet-process modified, and the silica gel being prepared/carbonyl iron dust compound broadband inhales wave plate in K
Wave band and Ka wave band have good absorbing property, and the reachable -20dB of reflection loss peak is hereinafter, maximum can arrive -34dB, -10dB
Bandwidth below is in 10GHz or more, maximum reachable 14GHz.Preparation method is simple in the present invention, is conducive to extensive life
It produces.
In addition, a kind of silica gel provided by the invention/carbonyl iron dust compound broadband, which inhales wave plate, also has good physical mechanical
Performance, hardness are Shao A40~55, and tensile strength has UL-94V0's 300% or more in 3.5MPa or more, elongation at break
Flame retardant rating.
In order to further illustrate the present invention, multiple to a kind of silica gel/carbonyl iron dust provided by the invention with reference to embodiments
It closes broadband absorbing piece and preparation method thereof to be described in detail, but limiting the scope of the present invention cannot be understood as.
Embodiment 1
The pH value of 95% ethanol water is adjusted to 4~5.5, γ-glycidyl ether oxygen propyl trimethoxy is then added
Base silane is hydrolyzed, and obtains the hydrolyzate solution of coupling agent, and the concentration of coupling agent is 3% (by γ-glycidyl ether oxygen propyl
Trimethoxy silane meter).By the hydrolyzate solution of above-mentioned coupling agent by atomization method to carbonyl iron dust (D50 be 3.0 μm) into
Row is wet-process modified, obtains modified carbonyl iron dust after dry, based on γ-glycidyl ether oxygen propyl trimethoxy silicane relative to
The dosage of carbonyl iron dust is 1.2%.By the hydrolyzate solution of above-mentioned coupling agent, by atomization method, to alumina powder, (D50 is
11.0 μm) carry out wet-process modified, modified alumina powder is obtained after dry, by γ-glycidyl ether oxygen propyl trimethoxy silicon
Alkane meter is 0.35% relative to the dosage of alumina powder.
By 100 parts of vinyl silicone oil compositions (viscosity 27000mPas, contents of ethylene 0.12mmol/g), 7.8
Part containing hydrogen silicone oil composition (viscosity 360mPas, silicon hydrogen content are 4.5mmol/g), 215 parts of modified carbonyl iron powders, 17 parts
Modified oxidized aluminium powder is mixed at room temperature, maintenance vacuum degree >=0.09MPa in whipping process, and mixing time 100~
150min obtains premix sizing material.
0.18 part of inhibitor methyl three (1,1- dimethyl -1- acetylene ylmethoxy) silane is added into above-mentioned premixing glue material
With 0.2 part of catalyst, continue to stir at room temperature, maintenance vacuum degree >=0.09MPa in whipping process, mixing time 30~
50min obtains blend glue stuff.
Above-mentioned blend glue stuff is transferred to calender, calendering formation, drying tunnel temperature is 135 DEG C, and rolling velocity control makes
Curing time is 30min, calendering thickness control make solidify film with a thickness of 1 ± 0.1mm, be die cut to film is solidified
Wave plate is inhaled to silica gel/carbonyl iron dust compound broadband.
The absorbing property that silica obtained/carbonyl iron dust compound broadband inhales wave plate, reflection loss curve are tested using arch method
As shown in Fig. 2, silica obtained/carbonyl iron dust compound broadband, which inhales wave plate, has good absorbing property, reflection loss in K and Ka wave band
There is peak value in 23.3GHz and 27.9GHz, corresponding reflection loss peak is respectively -32dB and -34dB, reflection loss -
10dB bandwidth below is 14GHz, covers the frequency range from 19GHz to 33GHz, and reflection loss is in -5dB bandwidth below
22GHz covers the frequency range from 14GHz to 36GHz.Meanwhile testing the object that silica obtained/carbonyl iron dust compound broadband inhales wave plate
Manage mechanical performance, density 2.59g/cm3, hardness is Shao A47, tensile strength 3.6MPa, elongation at break 330%.
By above-mentioned test data it is found that compound broadband manufactured in the present embodiment, which inhales wave plate, has excellent absorbing property.
Embodiment 2
The pH value of 95% ethanol water is adjusted to 4~5.5, base octyltri-ethoxysilane is then added and carries out water
Solution, obtains the hydrolyzate solution of coupling agent, and the concentration of coupling agent is 3% (based on octyltri-ethoxysilane).By above-mentioned coupling
The hydrolyzate solution of agent is wet-process modified to carbonyl iron dust (D50 is 3.6 μm) progress by atomization method, and modification is obtained after dry
Carbonyl iron dust, based on octyltri-ethoxysilane relative to the dosage of carbonyl iron dust be 0.5%.By the hydrolysate of above-mentioned coupling agent
Solution is wet-process modified to phlogopite powder (D50 is 13.0 μm) progress by atomization method, obtains modified phlogopite powder after dry,
Based on octyltri-ethoxysilane relative to the dosage of phlogopite powder be 1.6%.
By 100 parts of vinyl silicone oil compositions (viscosity 18000mPas, contents of ethylene 0.08mmol/g), 10
(viscosity 95mPas, silicon hydrogen content change part containing hydrogen silicone oil composition for 5.6mmol/g), 294 parts of modified carbonyl iron powders, 21 parts
Property phlogopite powder be mixed at room temperature, in whipping process maintain vacuum degree >=0.09MPa, mixing time 100~
150min obtains premix sizing material.
0.29 part of inhibitor methyl three (1,1- dimethyl -1- acetylene ylmethoxy) silane is added into above-mentioned premixing glue material
With 0.31 part of catalyst, continue to stir at room temperature, vacuum degree >=0.09MPa, mixing time 30 are maintained in whipping process
~50min, obtains blend glue stuff.
Above-mentioned blend glue stuff is transferred to calender, calendering formation, drying tunnel temperature is 135 DEG C, and rolling velocity control makes
Curing time is 30min, calendering thickness control make solidify film with a thickness of 1 ± 0.1mm, be die cut to film is solidified
Wave plate is inhaled to silica gel/carbonyl iron dust compound broadband.
The absorbing property that silica obtained/carbonyl iron dust compound broadband inhales wave plate, reflection loss curve are tested using arch method
As shown in figure 3, silica obtained/carbonyl iron dust compound broadband, which inhales wave plate, has good absorbing property, reflection loss in K and Ka wave band
There is peak value in 23GHz and 26.5GHz, corresponding reflection loss peak is respectively -34dB and -23dB, and reflection loss is in -10dB
Bandwidth below is 14GHz, covers the frequency range from 18GHz to 32GHz, and reflection loss is 21GHz in -5dB bandwidth below, is covered
Cover the frequency range from 14GHz to 35GHz.Meanwhile testing the Physical Mechanical that silica obtained/carbonyl iron dust compound broadband inhales wave plate
Can, density 2.64g/cm3, hardness is Shao A52, tensile strength 3.5MPa, elongation at break 340%.
By above-mentioned test data it is found that compound broadband manufactured in the present embodiment, which inhales wave plate, has excellent absorbing property.
Embodiment 3
Adjust the pH value of 95% ethanol water to 4~5.5, be then added bis- (triethoxysilyl) ethane into
Row hydrolysis, obtains the hydrolyzate solution of coupling agent, and the concentration of coupling agent is 3% (by bis- (triethoxysilyl) ethane
Meter).The hydrolyzate solution of above-mentioned coupling agent is wet-process modified to carbonyl iron dust (D50 is 2.5 μm) progress by atomization method, it does
Modified carbonyl iron dust is obtained after dry, the dosage based on bis- (triethoxysilyl) ethane relative to carbonyl iron dust is
0.8%.The hydrolyzate solution of above-mentioned coupling agent is wet-process modified to silicon powder (D50 is 12.0 μm) progress by atomization method,
Modified silicon powder is obtained after drying, based on bis- (triethoxysilyl) ethane relative to the dosage of silicon powder be 0.5%.
By 100 parts of vinyl silicone oil compositions (viscosity 31000mPas, contents of ethylene 0.03mmol/g), 6.6
Part containing hydrogen silicone oil composition (viscosity 450mPas, silicon hydrogen content are 3.2mmol/g), 162 parts of modified carbonyl iron powders, 13.5
The modified phlogopite powder of part is mixed at room temperature, and vacuum degree >=0.09MPa, mixing time 100 are maintained in whipping process
~150min obtains premix sizing material.
0.15 part of inhibitor methyl three (1,1- dimethyl -1- acetylene ylmethoxy) silane is added into above-mentioned premixing glue material
With 0.16 part of catalyst, continue to stir at room temperature, vacuum degree >=0.09MPa, mixing time 30 are maintained in whipping process
~50min, obtains blend glue stuff.
Above-mentioned blend glue stuff is transferred to calender, calendering formation, drying tunnel temperature is 135 DEG C, and rolling velocity control makes
Curing time is 30min, calendering thickness control make solidify film with a thickness of 1 ± 0.1mm, be die cut to film is solidified
Wave plate is inhaled to silica gel/carbonyl iron dust compound broadband.
The absorbing property that silica obtained/carbonyl iron dust compound broadband inhales wave plate, reflection loss curve are tested using arch method
As shown in figure 4, silica obtained/carbonyl iron dust compound broadband, which inhales wave plate, has good absorbing property, reflection loss in K and Ka wave band
There is peak value in 25GHz, corresponding reflection loss peak is -20dB, and reflection loss is 11GHz in -10dB bandwidth below, is covered
The frequency range from 21GHz to 32GHz is covered, reflection loss is 18GHz in -5dB bandwidth below, covers the frequency from 18GHz to 36GHz
Section.Meanwhile testing the physical mechanical property that silica obtained/carbonyl iron dust compound broadband inhales wave plate, density 2.46g/cm3,
Hardness is Shao A43, tensile strength 3.7MPa, elongation at break 310%.
By above-mentioned test data it is found that compound broadband manufactured in the present embodiment, which inhales wave plate, has excellent absorbing property.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. the preparation method that a kind of silica gel/carbonyl iron dust compound broadband inhales wave plate, comprising the following steps:
A) wet-process modified to carbonyl iron dust and the progress of non-magnetic inorganic powder respectively using silane coupling agent, obtain modified carbonyl iron
Powder and modified non-magnetic inorganic powder；
The non-magnetic inorganic powder is kaolin, phlogopite powder, alumina powder, precipitated calcium carbonate, silicon powder and vapor phase method two
One or more of silica；
The mass ratio of the silane coupling agent and carbonyl iron dust is (0.3~2): 100；
The mass ratio of the silane coupling agent and non-magnetic inorganic powder is (0.3~2): 100；
B) the modified carbonyl iron powder for obtaining vinyl silicone oil composition, containing hydrogen silicone oil composition, the step A) and modification are non-
The mixing of magnetic inorganic powder obtains premix sizing material；
C) inhibitor and platinum catalyst are added in the premix sizing material, obtain blend glue stuff；
D) by the blend glue stuff calendering formation, hot setting is carried out, silica gel/carbonyl iron dust compound broadband is obtained and inhales wave plate.
2. preparation method according to claim 1, which is characterized in that in the carbonyl iron dust, iron content >=95%,
Carbon element content≤1%, D50 is 2.0~6.5 μm.
3. preparation method according to claim 1, which is characterized in that the vinyl silicone oil composition is end-vinyl silicon
The composition of oil and multi-vinyl silicone oil；
The viscosity of the vinyl silicone oil composition is 16000~50000mPas；
The content of the vinyl silicone oil composition medium vinyl is 0.03~0.15mmol/g.
4. preparation method according to claim 1, which is characterized in that containing hydrogen silicone oil composition is containing for different silicon hydrogen contents
The combination of hydrogen silicone oil；
The viscosity of the containing hydrogen silicone oil composition is 45~500mPas；
Silicon hydrogen content in the containing hydrogen silicone oil composition is 2.1~6.5mmol/g.
5. preparation method according to claim 1, which is characterized in that the step B) in raw material according to following parts by weight
Proportion:
Vinyl silicone oil composition: 100 parts；
Containing hydrogen silicone oil composition: 6~12 parts；
Modified carbonyl iron powder: 160~300 parts；
Modified non-magnetic inorganic powder: 10~25 parts.
6. preparation method according to claim 1, which is characterized in that the inhibitor is (1, the 1- dimethyl -1- of methyl three
Acetylene ylmethoxy) silane, vinyl three (1,1- dimethyl -1- acetylene ylmethoxy) silane, (the 1,1- dimethyl-of phenyl three
1- acetylene ylmethoxy) silane, 3- methyl-1-butine-3- alcohol, four silicon of 1,3,5,7- tetramethyl-1,3,5,7- tetravinyl ring
Oxygen alkane, N, N, N ', one or more of N '-tetraallyl terephthalamide and maleic acid monoallyl.
7. preparation method according to claim 1, which is characterized in that the platinum catalyst is platinum-divinyl tetramethyl
Base disiloxane complex；
The mass content of Pt is 0.05% in the platinum catalyst.
8. preparation method according to claim 5, which is characterized in that with vinyl silicone oil composition be that 100 parts by weight are
Benchmark, the platinum catalyst are 0.1~0.5 parts by weight, and the inhibitor is 0.15~0.45 parts by weight.
9. preparation method according to claim 1, which is characterized in that the step D) solidification temperature be 120~150
℃；
The step D) curing time be 10~50min.
10. a kind of silica gel/carbonyl iron dust compound broadband inhales wave plate, according to preparation method described in any one of claim 1 to 9
It is made.
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