CN107418512A - A kind of preparation method of ultra-thin paper base wave-absorbing material - Google Patents
A kind of preparation method of ultra-thin paper base wave-absorbing material Download PDFInfo
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- CN107418512A CN107418512A CN201710422278.1A CN201710422278A CN107418512A CN 107418512 A CN107418512 A CN 107418512A CN 201710422278 A CN201710422278 A CN 201710422278A CN 107418512 A CN107418512 A CN 107418512A
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- 239000011358 absorbing material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 31
- ZGDWHDKHJKZZIQ-UHFFFAOYSA-N cobalt nickel Chemical compound [Co].[Ni].[Ni].[Ni] ZGDWHDKHJKZZIQ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 229910000863 Ferronickel Inorganic materials 0.000 claims abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 3
- 239000010941 cobalt Substances 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 15
- 229920001131 Pulp (paper) Polymers 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- IQUGDGIIAQZHGL-UHFFFAOYSA-L iron(2+);dichloride;hydrochloride Chemical compound Cl.[Cl-].[Cl-].[Fe+2] IQUGDGIIAQZHGL-UHFFFAOYSA-L 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002041 carbon nanotube Substances 0.000 abstract description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 2
- 230000020477 pH reduction Effects 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000005291 magnetic effect Effects 0.000 description 8
- 239000003643 water by type Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 230000007246 mechanism Effects 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005381 magnetic domain Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000007903 penetration ability Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The present invention relates to a kind of preparation method of ultra-thin paper base wave-absorbing material, belong to electromangnetic spectrum field.The present invention is using multi-walled carbon nanotube as carrier, after concentrated nitric acid acidification, oxy radical is produced in carbon nano tube surface, deposition site is provided for cobalt ferronickel ion, through hydro-thermal reaction, cobalt nickel ferrite nano-particle is set uniformly to inlay on the carbon nanotubes by the electrostatic attraction effect between metal ion and oxy radical, it is effectively improved electromagnetic performance, cobalt nickel ferrite/CNT of the generation with good wave-absorbing effect, cobalt nickel ferrite/CNT and recycled paper fiber are finally dispersed into suspension in high speed shear dispersion machine, and manufacture paper with pulp into wet paper, moisture removal is removed through compacting and flattens paper web, press polish improves the smoothness of paper after drying, ultra-thin paper base wave-absorbing material is made.Ultra-thin paper base wave-absorbing material electromagnetic matching of the present invention is good, can effectively absorb and suppress Secondary Emission clutter, and frequency electromagnetic waves shield effectiveness is high.
Description
Technical field
The present invention relates to a kind of preparation method of ultra-thin paper base wave-absorbing material, belong to electromangnetic spectrum field.
Background technology
The nearly more than ten years, with using GHz frequency electromagnetics electronics and communication apparatus fast development and extensive use, by
This electromagnetic interference brought and radiation pollution are also serious all the more, while modern weapons equipment is also increasingly high to the demand of electromagnetism stealth
Rise.In order to eliminate or reduce electromagnetic interference and pollution, and the radar scattering interface of reduction military target to improve its energy of surviving
Power and penetration ability, the development of novel high-performance electromagnetic wave absorbent material are highly valued.It is well known that electro-magnetic wave absorption material
The absorbing property of material is mainly determined by its complex permeability and complex dielectric permittivity.The wave-absorbing effect that one material will obtain
It must simultaneously meet 2 conditions：First, impedance matching will get well, incoming electromagnetic wave energy is efficiently entering inside wave-absorber without anti-
Penetrate；Second, damping capacity is eager to excel, the electromagnetism wave energy for entering material internal is absorbed by promptly decay.
According to attenuating mechanism, absorbing material can be divided into magnetic loss type and the major class of dielectric loss type two.Magnetic loss type absorbs machine
System is a kind of magnetic loss relevant with the dynamic magnetization process of ferromagnetic media, and such loss can be refined as：Magnetic hystersis loss, rotation
Magnetic vortex, damping loss and magnetic aftereffect effect etc., its main source are the magnetic domain steering similar with magnetic hysteresis mechanism, neticdomain wall position
Shifting and magnetic domain natural resonance etc..Dielectric loss type is a kind of dielectric loss mechanism of absorption relevant with electrode, that is, passes through medium
" friction " effect dissipates electromagnetic energy into thermal energy consumption caused by polarization repeatedly.But absorbing material because of its electromagnetic matching relatively
Difference, the composite request for meeting advanced absorbing material " thin, light, wide, strong " is typically difficult in performance.It would therefore be highly desirable to develop one kind
The preferable absorbing material of electromagnetic matching, has necessary meaning to association area.
The content of the invention
The technical problems to be solved by the invention：For current absorbing material because its electromagnetic matching is relatively poor, in performance
On the problem of being difficult to meet the composite request of advanced absorbing material " thin, light, wide, strong ", the invention provides a kind of ultra-thin paper substrate
The preparation method of absorbing material.
To solve technical problem, the technical solution adopted by the present invention is：
（1）Take multi-walled carbon nanotube to add in salpeter solution, 5~6h of stirring reaction at 110~120 DEG C, add after standing 1~2h
Water dilutes, and filters to obtain filter residue, multi-walled carbon nanotube must be pre-processed after residue washing is dried；
（2）Pretreatment multi-walled carbon nanotube is added into ultrasonic disperse in deionized water, then it is 3~4 to adjust dispersion liquid pH with hydrochloric acid
Iron chloride, cobalt chloride, nickel chloride are added afterwards, and precursor liquid is obtained after stirring 1~2h；
（3）Is fitted into after being 9~10 with ammoniacal liquor regulation precursor liquid pH in autoclave, be heated to 160~180 DEG C react 18~
20h, cooled and filtered, filter cake is obtained, filter cake is dried after washing, alcohol are washed, obtains cobalt nickel ferrite/CNT；
（4）Take recycled paper fiber addition deionized water high speed shearing scattered, lower floor's suspension is collected after standing 2~3h, by under
Layer suspension is well mixed with cobalt nickel ferrite/CNT, obtains paper pulp, and paper pulp is manufactured paper with pulp, is compacted, press polish after drying, is obtained super
Thin paper base wave-absorbing material.
Step（1）The mass fraction of described salpeter solution be 50~65%, dosage for multi-walled carbon nanotube quality 75~
300 times.
Step（2）Described pretreatment multi-walled carbon nanotube, iron chloride, cobalt chloride, the parts by weight of nickel chloride for 0.8~
1.2 parts of pretreatment multi-walled carbon nanotubes, 0.16~0.24 part of iron chloride, 0.13~0.20 part of cobalt chloride, 0.06~0.10 part of chlorine
Change nickel.
Step（4）The parts by weight of described recycled paper fiber and cobalt nickel ferrite/CNT are 80~100 parts of recycled writing papers
Fiber, 0.1~0.5 part of cobalt nickel ferrite/CNT.
Step（4）It is described manufacture paper with pulp, be compacted, drying, burnishing process is quick by a diameter of 20cm of formation zone triumphant match
Handshcet former, most of water in paper pulp is filtered off to form wet paper, wet paper is compacted under 0.8~1.5MPa, is placed in
In vacuum drying chamber, 20~30min is dried at 80~90 DEG C, then dried paper press polish is adjusted to paper sheet thickness and is
0.1~0.2mm.
The method have the benefit that：The present invention is using multi-walled carbon nanotube as carrier, after concentrated nitric acid acidification,
Produce oxy radical in carbon nano tube surface, deposition site provided for cobalt ferronickel ion, through hydro-thermal reaction, by metal ion with
Electrostatic attraction effect between oxy radical makes cobalt nickel ferrite nano-particle uniformly inlay on the carbon nanotubes, is effectively improved electricity
Magnetic property, generation with good wave-absorbing effect cobalt nickel ferrite/CNT, finally by cobalt nickel ferrite/CNT with
Recycled paper fiber is dispersed into suspension in high speed shear dispersion machine, and manufactures paper with pulp into wet paper, and moisture removal is removed and by paper through compacting
Width flattens, and the smoothness of press polish raising paper, is made ultra-thin paper base wave-absorbing material after drying；The ultra-thin paper substrate of the present invention inhales ripple material
Material, which can effectively absorb, suppresses Secondary Emission clutter, frequency electromagnetic waves shield effectiveness height, and frequency electromagnetic waves shielding rate is 96~98%,
Secondary Emission clutter absorptivity is 92~95%, and minimal reflection loss is -51.4~-48.1dB in 2~18GHz frequency ranges,
Product of the present invention is nontoxic simultaneously, free from environmental pollution, can be widely applied to family, office, audio-visual education room, communication base station, electricity
Believe the environment such as computer room, waiting hall for airplanes, subway station, shield ranges of the present invention are wide, shielding properties is lasting, and preparation technology is simple, are made
Product it is nontoxic, suitable large-scale production and application easy to use.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in understanding the present invention, is not construed as the concrete restriction to the present invention.
Weigh 1~2g multi-walled carbon nanotubes, adding 150~300mL mass fractions is in 65% salpeter solution, 110~
Under 120 DEG C of constant temperature oil baths, with 100~120r/min, 5~6h of stirring reaction, 3~5L is diluted with water to after standing 1~2h, then
Filter residue is filtered to obtain, filter residue is washed with deionized and is placed in cleaning solution in neutrality, then by filter residue in drying box, at 60~70 DEG C
Dry to constant weight, obtain pretreatment multi-walled carbon nanotube；Weigh 0.8~1.2g pretreatment multi-walled carbon nanotube, add 800~
In 1200mL deionized waters, 1~2h is disperseed with 300W ultrasonic echographies, multi-walled carbon nanotube dispersion liquid must be pre-processed, then use matter
Amount fraction is that 10% hydrochloric acid regulation pretreatment multi-walled carbon nanotube dispersion liquid pH is 3~4, and adds 0.16~0.24g iron chloride,
0.13~0.20g cobalt chlorides, 0.06~0.10g nickel chlorides, 1~2h is stirred with 300~400r/min, obtains precursor liquid；Forward
It is 9~10 to drive and adjust precursor liquid pH by 10% ammoniacal liquor of 1~3mL/min dropwise addition mass fractions in body fluid, and is transferred to reaction under high pressure
In device, 160~180 DEG C of 18~20h of reaction are heated to, 1~2h is stood after being cooled to room temperature, then filters to obtain filter cake, use successively
Deionized water and absolute ethyl alcohol wash filter cake 3~5 times, then filter cake is placed in drying box, are dried at 60~70 DEG C to constant weight,
Obtain cobalt nickel ferrite/CNT；80~100g recycled paper fibers are weighed, are added in 3~5L deionized waters, using 4000r/
Min high speed shears disperse 3~4h, collect lower floor's suspension after standing 2~3h, add 0.1~0.5g cobalt nickel ferrites/carbon and receive
Mitron, 2~3h is disperseed with 4000r/min high speed shears, paper pulp is obtained, is then quickly copied by a diameter of 20cm of formation zone triumphant match
Piece device, most of water in paper pulp is filtered off to form wet paper, wet paper is compacted under 0.8~1.5MPa, be placed in true
In empty drying box, 20~30min is dried at 80~90 DEG C, then by dried paper press polish, adjustment paper sheet thickness is 0.1~
0.2mm, obtain ultra-thin paper base wave-absorbing material.
Example 1
Weigh 1g multi-walled carbon nanotubes, adding 150mL mass fractions is in 65% salpeter solution, under 110 DEG C of constant temperature oil baths, with
100r/min stirring reaction 5h, 3L is diluted with water to after standing 1h, then filters to obtain filter residue, filter residue is washed with deionized to washing
Liquid is washed in neutrality, then filter residue is placed in drying box, is dried at 60 DEG C to constant weight, obtains pretreatment multi-walled carbon nanotube；Weigh
0.8g pre-processes multi-walled carbon nanotube, adds in 800mL deionized waters, disperses 1h with 300W ultrasonic echographies, must pre-process more
Wall carbon nano tube dispersion liquid, then with mass fraction be 10% hydrochloric acid regulation pretreatment multi-walled carbon nanotube dispersion liquid pH be 3, and add
Enter 0.16g iron chloride, 0.13g cobalt chlorides, 0.06g nickel chlorides, 1h is stirred with 300r/min, obtains precursor liquid；To precursor liquid
In mass fraction is added dropwise to adjust precursor liquid pH as 10% ammoniacal liquor using 1mL/min is 9, and be transferred in high-pressure reactor, be heated to
160 DEG C of reaction 18h, stand 1h after being cooled to room temperature, then filter to obtain filter cake, wash filter with deionized water and absolute ethyl alcohol successively
Cake 3 times, then filter cake is placed in drying box, dried at 60 DEG C to constant weight, obtain cobalt nickel ferrite/CNT；Weigh 80g again
Raw paper fiber, is added in 3L deionized waters, disperses 3h using 4000r/min high speed shears, and lower floor's suspension is collected after standing 2h,
0.1g cobalt nickel ferrites/CNT is added, 2h is disperseed with 4000r/min high speed shears, paper pulp is obtained, then passes through formation zone
The a diameter of 20cm quick handshcet former of triumphant match, most of water in paper pulp is filtered off to form wet paper, wet paper is existed
It is compacted, is placed in vacuum drying chamber under 0.8MPa, 20min is dried at 80 DEG C, then by dried paper press polish, adjusts paper
Zhang Houdu is 0.1mm, obtains ultra-thin paper base wave-absorbing material.
Ultra-thin paper base wave-absorbing material prepared by the present invention folds and is processed into honeycomb type paper, is attached to high-accuracy, Gao Ling
Quick property electronic equipment surface；Ultra-thin paper base wave-absorbing material electromagnetic matching of the present invention is good, can effectively absorb suppression Secondary Emission
Clutter, frequency electromagnetic waves shield effectiveness are high, and frequency electromagnetic waves shielding rate is 96%, and Secondary Emission clutter absorptivity is 92%,
Minimal reflection loss is -48.1dB in 2GHz frequency ranges.
Example 2
Weigh 2g multi-walled carbon nanotubes, adding 220mL mass fractions is in 65% salpeter solution, under 115 DEG C of constant temperature oil baths, with
110r/min stirring reaction 6h, 4L is diluted with water to after standing 2h, then filters to obtain filter residue, filter residue is washed with deionized to washing
Liquid is washed in neutrality, then filter residue is placed in drying box, is dried at 65 DEG C to constant weight, obtains pretreatment multi-walled carbon nanotube；Weigh
1.0g pre-processes multi-walled carbon nanotube, adds in 1000mL deionized waters, disperses 2h with 300W ultrasonic echographies, must pre-process more
Wall carbon nano tube dispersion liquid, then with mass fraction be 10% hydrochloric acid regulation pretreatment multi-walled carbon nanotube dispersion liquid pH be 4, and add
Enter 0.20g iron chloride, 0.17g cobalt chlorides, 0.08g nickel chlorides, 2h is stirred with 350r/min, obtains precursor liquid；To precursor liquid
In mass fraction is added dropwise to adjust precursor liquid pH as 10% ammoniacal liquor using 2mL/min is 10, and be transferred in high-pressure reactor, be heated to
170 DEG C of reaction 19h, stand 2h after being cooled to room temperature, then filter to obtain filter cake, wash filter with deionized water and absolute ethyl alcohol successively
Cake 4 times, then filter cake is placed in drying box, dried at 65 DEG C to constant weight, obtain cobalt nickel ferrite/CNT；Weigh 90g again
Raw paper fiber, is added in 4L deionized waters, disperses 4h using 4000r/min high speed shears, and lower floor's suspension is collected after standing 3h,
0.3g cobalt nickel ferrites/CNT is added, 3h is disperseed with 4000r/min high speed shears, paper pulp is obtained, then passes through formation zone
The a diameter of 20cm quick handshcet former of triumphant match, most of water in paper pulp is filtered off to form wet paper, wet paper is existed
It is compacted, is placed in vacuum drying chamber under 1.2MPa, 25min is dried at 85 DEG C, then by dried paper press polish, adjusts paper
Zhang Houdu is 0.2mm, obtains ultra-thin paper base wave-absorbing material.
Ultra-thin paper base wave-absorbing material prepared by the present invention folds and is processed into honeycomb type paper, is attached to high-accuracy, Gao Ling
Quick property electronic equipment surface；Ultra-thin paper base wave-absorbing material electromagnetic matching of the present invention is good, can effectively absorb suppression Secondary Emission
Clutter, frequency electromagnetic waves shield effectiveness are high, and frequency electromagnetic waves shielding rate is 97%, and Secondary Emission clutter absorptivity is 93%,
Minimal reflection loss is -49.2dB in 10GHz frequency ranges.
Example 3
Weigh 2g multi-walled carbon nanotubes, adding 300mL mass fractions is in 65% salpeter solution, under 120 DEG C of constant temperature oil baths, with
120r/min stirring reaction 6h, 5L is diluted with water to after standing 2h, then filters to obtain filter residue, filter residue is washed with deionized to washing
Liquid is washed in neutrality, then filter residue is placed in drying box, is dried at 70 DEG C to constant weight, obtains pretreatment multi-walled carbon nanotube；Weigh
1.2g pre-processes multi-walled carbon nanotube, adds in 1200mL deionized waters, disperses 2h with 300W ultrasonic echographies, must pre-process more
Wall carbon nano tube dispersion liquid, then with mass fraction be 10% hydrochloric acid regulation pretreatment multi-walled carbon nanotube dispersion liquid pH be 4, and add
Enter 0.24g iron chloride, 0.20g cobalt chlorides, 0.10g nickel chlorides, 2h is stirred with 400r/min, obtains precursor liquid；To precursor liquid
In mass fraction is added dropwise to adjust precursor liquid pH as 10% ammoniacal liquor using 3mL/min is 10, and be transferred in high-pressure reactor, be heated to
180 DEG C of reaction 20h, stand 2h after being cooled to room temperature, then filter to obtain filter cake, wash filter with deionized water and absolute ethyl alcohol successively
Cake 5 times, then filter cake is placed in drying box, dried at 70 DEG C to constant weight, obtain cobalt nickel ferrite/CNT；Weigh 100g
Recycled paper fiber, add in 5L deionized waters, 4h is disperseed using 4000r/min high speed shears, collection lower floor is suspended after standing 3h
Liquid, 0.5g cobalt nickel ferrites/CNT is added, 3h is disperseed with 4000r/min high speed shears, paper pulp is obtained, then passes through into
The a diameter of 20cm in the shape area quick handshcet former of triumphant match, most of water in paper pulp is filtered off to form wet paper, wet paper is existed
It is compacted, is placed in vacuum drying chamber under 1.5MPa, 30min is dried at 90 DEG C, then by dried paper press polish, adjusts paper
Zhang Houdu is 0.2mm, obtains ultra-thin paper base wave-absorbing material.
Ultra-thin paper base wave-absorbing material prepared by the present invention folds and is processed into honeycomb type paper, is attached to high-accuracy, Gao Ling
Quick property electronic equipment surface；Ultra-thin paper base wave-absorbing material electromagnetic matching of the present invention is good, can effectively absorb suppression Secondary Emission
Clutter, frequency electromagnetic waves shield effectiveness are high, and frequency electromagnetic waves shielding rate is 98%, and Secondary Emission clutter absorptivity is 95%,
Minimal reflection loss is -51.4dB in 18GHz frequency ranges.
Claims (5)
1. a kind of preparation method of ultra-thin paper base wave-absorbing material, it is characterised in that specifically preparation process is：
（1）Take multi-walled carbon nanotube to add in salpeter solution, 5~6h of stirring reaction at 110~120 DEG C, add after standing 1~2h
Water dilutes, and filters to obtain filter residue, multi-walled carbon nanotube must be pre-processed after residue washing is dried；
（2）Pretreatment multi-walled carbon nanotube is added into ultrasonic disperse in deionized water, then it is 3~4 to adjust dispersion liquid pH with hydrochloric acid
Iron chloride, cobalt chloride, nickel chloride are added afterwards, and precursor liquid is obtained after stirring 1~2h；
（3）Is fitted into after being 9~10 with ammoniacal liquor regulation precursor liquid pH in autoclave, be heated to 160~180 DEG C react 18~
20h, cooled and filtered, filter cake is obtained, filter cake is dried after washing, alcohol are washed, obtains cobalt nickel ferrite/CNT；
（4）Take recycled paper fiber addition deionized water high speed shearing scattered, lower floor's suspension is collected after standing 2~3h, by under
Layer suspension is well mixed with cobalt nickel ferrite/CNT, obtains paper pulp, and paper pulp is manufactured paper with pulp, is compacted, press polish after drying, is obtained super
Thin paper base wave-absorbing material.
A kind of 2. preparation method of ultra-thin paper base wave-absorbing material as claimed in claim 1, it is characterised in that step（1）Described
The mass fraction of salpeter solution is 50~65%, and dosage is 75~300 times of multi-walled carbon nanotube quality.
A kind of 3. preparation method of ultra-thin paper base wave-absorbing material as claimed in claim 1, it is characterised in that step（2）Described
It is 0.8~1.2 part of pretreatment multi-wall carbon nano-tube to pre-process multi-walled carbon nanotube, iron chloride, cobalt chloride, the parts by weight of nickel chloride
Pipe, 0.16~0.24 part of iron chloride, 0.13~0.20 part of cobalt chloride, 0.06~0.10 part of nickel chloride.
A kind of 4. preparation method of ultra-thin paper base wave-absorbing material as claimed in claim 1, it is characterised in that step（4）Described
The parts by weight of recycled paper fiber and cobalt nickel ferrite/CNT are 80~100 parts of recycled paper fibers, 0.1~0.5 part of cobalt ferronickel
Oxysome/CNT.
A kind of 5. preparation method of ultra-thin paper base wave-absorbing material as claimed in claim 1, it is characterised in that step（4）Described
Manufacture paper with pulp, be compacted, drying, burnishing process is the quick handshcet former of triumphant match by a diameter of 20cm of formation zone, by the big portion in paper pulp
Divide water to filter off to form wet paper, wet paper is compacted under 0.8~1.5MPa, is placed in vacuum drying chamber, 80~90
20~30min is dried at DEG C, then it is 0.1~0.2mm that dried paper press polish, which is adjusted to paper sheet thickness,.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113708086A (en) * | 2021-08-31 | 2021-11-26 | 河北科技大学 | Transition metal nano powder/carbon nano tube composite material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109148903A (en) * | 2018-09-03 | 2019-01-04 | 中南大学 | The preparation method of the spherical carbon-based nickel cobalt bimetallic oxide composite material of 3D sea urchin |
| CN110735362A (en) * | 2018-10-18 | 2020-01-31 | 嘉兴学院 | Preparation method of conductive paper for electromagnetic shielding protection cards |
| CN110735362B (en) * | 2018-10-18 | 2022-01-25 | 嘉兴学院 | Preparation method of conductive paper for electromagnetic shielding protection card |
| CN113708086A (en) * | 2021-08-31 | 2021-11-26 | 河北科技大学 | Transition metal nano powder/carbon nano tube composite material and preparation method and application thereof |
| CN113708086B (en) * | 2021-08-31 | 2023-12-22 | 河北科技大学 | Transition metal nano powder/carbon nano tube composite material and preparation method and application thereof |
| CN114291853A (en) * | 2021-12-10 | 2022-04-08 | 西安理工大学 | Biomass carbon/nanograss-like CoNiO2Method for preparing composite material |
| CN114291853B (en) * | 2021-12-10 | 2024-03-19 | 西安理工大学 | Biomass carbon/nano grass-like CoNiO 2 Preparation method of composite material |
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