CN106340726B - Magnetic conductive nano metal/carbon aerogels absorbing material and preparation method thereof - Google Patents
Magnetic conductive nano metal/carbon aerogels absorbing material and preparation method thereof Download PDFInfo
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- CN106340726B CN106340726B CN201610930087.1A CN201610930087A CN106340726B CN 106340726 B CN106340726 B CN 106340726B CN 201610930087 A CN201610930087 A CN 201610930087A CN 106340726 B CN106340726 B CN 106340726B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
Abstract
The present invention discloses a kind of magnetic conductive nano metal/carbon aerogels absorbing material and preparation method thereof；The material is prepared by carbon aerogels through allergy China, chemical plating, freeze-drying or supercritical drying, aeroge is made of magnetic metal nano particle and porous carbon skeleton, nanometer magnetic metal uniform particle is distributed in carbon aerogels surface, has magnetism, electric conductivity, low-density, high-specific surface area and nano-porous structure simultaneously.Due to the above characteristic, such aerogel material has preferable application prospect in electromagnetic wave absorption field, can be compared under few additive, and realization electromagnetic wave wideband absorbs by force.
Description
Technical field
The present invention relates to absorbing material preparation technical fields, and in particular to a kind of magnetic conductive nano metal/carbon aerogels
Absorbing material and preparation method thereof.
Background technique
As the investigative techniques such as light, electricity, magnetic are in the extensive use of military field, corresponding counterreconnaissance technology receives people
More and more concerns.Wherein electromagnetic-wave absorbent can be effectively reduced under the premise of not changing weapon system configuration design
The radar cross section of weaponry improves its defence capability of surviving, becomes the research hotspot of the military of various countries.It is ideal to inhale wave material
Material needs to meet the requirement of " thickness is thin, light weight, absorption frequency is wide, absorbability is strong ".Traditional absorbing material mainly passes through
Electrical loss (such as conducting polymer, TiO2、SiO2、ZnO、BaTiO3Deng) or magnetic loss (such as Fe, Co, Ni, Fe3O4、γ-Fe2O3
Deng) thermal energy is converted electromagnetic waves into, realize the absorption to incident electromagnetic wave.This kind of material density usually with higher and single
Loss ability, need higher additive amount (50-70wt%) and thicker coating layer thickness, just can reach preferable absorbing property
(RLmax < -30dB is lost in maximum reflection), causes the weight of camouflage coating to be significantly increased.In recent years, changed with magnetic nano-particle
Property conducing composite material there is preferable impedance matching property, and have because can wave be inhaled by dielectric loss and magnetic loss simultaneously
There is stronger wave-sucking performance, it is considered to be the effective replacer of traditional stealth material.Though this kind of composite material can be in lower painting
In the case where thickness degree, realize that electromagnetic wave absorbs by force, but there is still a need for relatively high absorbing material additive amount (20-50wt%),
Absorbing material itself density with higher (> 1g/cm simultaneously-3), to reducing, camouflage coating self weight is totally unfavorable.Therefore, it is protecting
On the basis of holding the strong wave-sucking performance of magnetic conductive composite material, as far as possible reduction absorbing material density and required additive amount,
It is very necessary.
Aeroge has low-density, high-specific surface area and relatively rich pore structure, is one kind " star " material in recent years
Material.Recently the study found that compared to the non-hole wave absorbing agent of tradition, conductive or magnetic aeroge absorbing material has lower density, and
Certain wave-absorbing effect (Compos.Sci.Technol.117,2015,117,32) can be obtained under relatively low additive amount.
On the one hand porous structure can reduce density of material, on the other hand can be inhaled by interface multistep reflection-absorption electromagnetic wave, reinforcing material
Wave energy power.But this kind of material usually has single magnetism or electric conductivity, can not reach the requirement that wideband absorbs by force.If gas
Gel has magnetic and electric conductivity simultaneously, will have low-density and high impedance matching properties, can by electrical loss, magnetic loss,
Interfacial polarization loss and multistep reflection-absorption electromagnetic wave may realize that incidence wave wideband is strong in the case where very few additive
It absorbs.However the common document report of unifunctional magnetic or conductive aeroge, what difunctional magnetic conductive aeroge involved
Design of material and synthesis are complex, current rare report.
Summary of the invention
It is excellent it is an object of the invention to solve at least the above problems and/or defect, and provide at least to will be described later
Point.
In order to realize these purposes and other advantages according to the present invention, a kind of magnetic conductive nano metal/carbon is provided
Aeroge absorbing material, the nano metal/carbon aerogels absorbing material are mainly made of charcoal and metal nanoparticle, wherein charcoal
75~99% are calculated as with carbon aerogels weight, metal nanoparticle is calculated as 1~25% with carbon aerogels weight.
Preferably, the specific surface area of the absorbing material is between 300~700g/m2, conductivity between 0.01~1S/m,
Saturation magnetic field intensity between 0.5~10emu/g, and when absorbing material use, inhale between -20~-60dB by minimal reflection loss
Wave effective bandwidth is between 2-5dB.
Preferably, the carbon aerogels are resorcinol-formaldehyde carbon aerogels, phenol-formaldehyde carbon aerogels, to benzene two
Any one in phenol-formaldehyde carbon aerogels and phloroglucinol-formaldehyde carbon aerogels.
Preferably, the metal nanoparticle is Ni or Co.
The present invention also provides a kind of above-mentioned magnetic conductive nano metal/carbon aerogels absorbing material preparation method, packets
Include following steps:
Step 1: PdCl is added in carbon aerogels2Or SnCl2At least 1h is impregnated in sensitizing solution；Then it is rinsed with deionized water
To remove the PdCl of hydrogel surface enrichment2Or SnCl2；
Step 2: by treated in step 1, carbon aerogels are soaked into metallochemistry plating solution, carry out chemical plating 1-12
It, obtains nano metal/carbon composite；
Step 3: obtained nano metal/carbon composite is dried to get magnetic conductive nano metal/carbon airsetting is arrived
Glue absorbing material.
Preferably, the metallochemistry plating solution is chemical nickel-plating solution or electroless cobalt plating solution；The chemical nickel plating is molten
The formula of liquid are as follows: 0.05~0.3 parts by weight NiCl2·6H2O, 20 parts by volume deionized waters, 5 parts by volume of ethanol, 2 parts by volume ammonium hydroxide
And 2 parts by volume hydrazine hydrate；The formula of the electroless cobalt plating solution are as follows: 0.1~0.4 parts by weight CoCl2·6H2O, 20 parts by volume
Deionized water, 5 parts by volume of ethanol, 2 parts by volume ammonium hydroxide and 2 parts by volume hydrazine hydrates.
Preferably, the drying in the step 3 is one of supercritical drying or freeze-drying；It is described overcritical
In drying, nano metal/carbon composite washing by soaking be must be subjected to deionized water before it is dried, ethyl alcohol or acetone then used
Carry out solvent displacement and supercritical drying；In the freeze-drying, nano metal/carbon composite must be spent before it is dried from
Sub- water is freeze-dried after carrying out washing by soaking to get magnetic conductive nano metal/carbon aerogels are arrived.
Preferably, it is described freeze-drying the following steps are included:
Step I, by nano metal/carbon composite precooling: cryogenic temperature -30~-50 DEG C, cooling time 1~3 are small
When；
Nano metal/carbon composite after precooling is warming up to 25 DEG C by step II, is kept for 2~4 hours；
Step III, freeze-drying: vacuum freeze drier is added in the nano metal that step II is obtained/carbon composite
In, setting condenser temperature is -50~-85 DEG C, and vacuum degree is 500mpa~50pa, and sublimation drying 5-10h obtains magnetism and leads
Susceptance rice metal/carbon aeroge absorbing material.
Preferably, the metallochemistry plating solution is chemical nickel-plating solution, the formula of the chemical nickel-plating solution are as follows: 0.05
~0.3 parts by weight NiCl2·6H2O, 20 parts by volume deionized waters, 0.01~0.06 parts by weight inositol, six phosphate ester, 1 weight
Part aminoacetic acid, 0.1 parts by volume accelerator, 0.1 parts by weight of urea, 0.1 parts by weight antiaging agent, 0.05 parts by weight benzo, three nitrogen
Azoles, 0.05 parts by volume glycine, 0.06 parts by weight 2-aminopyridine, 5 parts by volume of ethanol, 2 parts by volume ammonium hydroxide and 2 parts by volume water
Close hydrazine；The metallochemistry plating solution is electroless cobalt plating solution, the formula of the electroless cobalt plating solution are as follows: 0.1~0.4 parts by weight
CoCl2·6H2O, 20 parts by volume deionized waters, 0.01~0.06 parts by weight inositol, six phosphate ester, 1 parts by weight aminoacetic acid,
0.1 parts by volume accelerator, 0.1 parts by weight of urea, 0.1 parts by weight antiaging agent, 0.05 parts by weight benzotriazole, 0.05 volume
Part glycine, 0.06 parts by weight 2-aminopyridine, 5 parts by volume of ethanol, 2 parts by volume ammonium hydroxide and 2 parts by volume hydrazine hydrates.
Preferably, the process replacement of the step 2 are as follows: carbon aerogels are placed on the bracket of rotation, with 100~
The speed of 150r/min rotates, then metallochemistry plating solution is sprayed onto the carbon airsetting of rotation with the speed of 50~100mL/min
It is carried out chemical plating 1~12 day on glue, obtains nano metal/carbon composite.
In the present invention, the PdCl2The preparation method of sensitizing solution is to weigh 0.05 parts by weight PdCl2In beaker, it is added
45 parts by volume EtOH and 5 parts by volume 1molL-1HCl is placed in ultrasonic dissolution in ultrasonic washing instrument and both obtained；The SnCl2Sensitization
The preparation method of liquid is to weigh 0.05 parts by weight SnCl2In beaker, 45 parts by volume EtOH and 5 parts by volume 1molL are added- 1HCl is placed in ultrasonic dissolution in ultrasonic washing instrument.
The present invention is include at least the following beneficial effects:
(1) present invention proposes a kind of with magnetic and electric conductivity nano metal/carbon aerogels absorbing material, such airsetting
Glue is to be made of magnetic metal nano particle and porous carbon skeleton, while having magnetism, electric conductivity, low-density, high-specific surface area
And nano-porous structure.Due to the above characteristic, such aerogel material can be compared under few additive, and realization electromagnetic wave wideband is inhaled by force
It receives.
(2) aeroge provided by the invention has suitable conductivity, magnetism, impedance matching property, porosity, low simultaneously
Density and higher specific surface area, inhaling wave field in microwave has preferable application prospect.
(3) aerogel material provided by the invention simultaneously have electrical loss inhale wave, magnetic loss inhale wave, interface loss inhale wave and
More Walk reflection losses inhale the characteristics such as wave, can realize that incident electromagnetic wave wideband is inhaled by force compared with (5wt%-15wt%) under few additive
Receive (minimal reflection loss inhales wave effective bandwidth between 2-5dB between -20~-60dB).
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention:
Fig. 1 is the scanning electron microscope sem figure of metal/carbon aeroge prepared by the embodiment of the present invention 1, it can be seen that the gas
Gel is fine and close cellular structures, and Ni nano particle is evenly distributed in carbon aerogels skeleton surface；
Fig. 2 is the suction wave schematic diagram of Ni/ carbon aerogels prepared by the embodiment of the present invention 1, therefrom it can be seen that Ni/ carbon airsetting
Glue shows strong absorbing property, the minimum reflection loss when additive amount is only 10wt%, when Wave suction composite material is with a thickness of 2mm
Reachable-the 57dB of RLmin, effective bandwidth is up to 3.7dB.
Specific embodiment:
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
In addition, it is necessary to which what is illustrated, which is the conductivity of the resulting aerogel material of following embodiment, is measured by four probe method
, magnetic property is measured by magnetometer, and metal nano content is measured by EDX, and specific surface area is measured by automatic adsorption device, inhales wave
Performance is measured by vector network analyzer.
Embodiment 1:
Step 1: mechanical stirring is used to clarifying after 8.08g resorcinol is mixed with formaldehyde with molar ratio 1:2
0.2mol·L-1NaOH solution constant volume solution obtains wet gel to 100ml at room temperature after gel 3 days.Pickling is carried out to wet gel
Aging, exchange of solvent, CO2Resorcinol-formaldehyde aeroge is obtained after supercritical fluid drying, and further the aeroge is carried out
Carbonization, is heated to 1050 DEG C with the heating rate of 1.5 DEG C/min, resorcinol-formaldehyde carbon aerogels is obtained after constant temperature 2h.
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Resorcinol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2In activating solution after 1d
It takes out, is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, it is subsequently placed in chemical nickel-plating solution under room temperature
Chemical plating is carried out, until solution is become colorless by bluish violet, obtains Ni/ carbon composite；Electroless Plating Ni formula are as follows: 0.3g
NiCl26H2O, 20mL deionized water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: the Ni/ carbon composite of acquisition is cleaned several times with deionized water, exchange of solvent then is carried out with acetone
Supercritical drying is carried out after 7d, i.e. acquisition Ni/ carbon aerogels；
Aeroge Ni content is 18wt%；Specific surface area is 416g/m2；Conductivity is 0.1S/cm；Ms is 4.7emu/
g；Mr is 1.7emu/g；Hc is 192Oe；Minimum reflection when additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
RL is lostminReachable -57dB, effective bandwidth is up to 3.7dB.
Embodiment 2:
Step 1: mechanical stirring uses 0.2molL to clarifying after 8.08g phenol is mixed with formaldehyde with molar ratio 1:2- 1NaOH solution constant volume solution obtains wet gel at room temperature, carries out pickling aging, solvent to wet gel to 100mL after gel 3 days
Exchange, CO2Obtain phenol-formaldehyde aeroge after supercritical fluid drying, be further carbonized to the aeroge, with 1.5 DEG C/
The heating rate of min is heated to 1050 DEG C, and phenol-formaldehyde carbon aerogels are obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Phenol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2It is taken after 1d in activating solution
Out, it is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, be subsequently placed in chemical nickel-plating solution under room temperature into
Row chemical plating obtains Ni/ carbon composite until solution is become colorless by bluish violet；Electroless Plating Ni formula are as follows: 0.2g
NiCl2·6H2O, 20mL deionized water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: the Ni/ carbon composite of acquisition is cleaned several times with deionized water, exchange of solvent then is carried out with acetone
Supercritical drying is carried out after 7d, i.e. acquisition Ni/ carbon aerogels.
Aeroge Ni content is 12.3wt%；Specific surface area is 522g/m2；Conductivity is 0.1S/cm；Ms is
1.2emu/g；Mr is 0.17emu/g；Hc is 64Oe；When additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
Minimum reflection loss RLminReachable -32dB, effective bandwidth is up to 3.7dB.
Embodiment 3:
Step 1: mechanical stirring uses 0.2molL to clarifying after 8.08g phenol is mixed with formaldehyde with molar ratio 1:2- 1NaOH solution constant volume solution obtains wet gel to 100ml at room temperature after gel 3 days；Pickling aging, solvent are carried out to wet gel
Exchange, CO2Obtain phenol-formaldehyde aeroge after supercritical fluid drying, be further carbonized to the aeroge, with 1.5 DEG C/
The heating rate of min is heated to 1050 DEG C, and phenol-formaldehyde carbon aerogels are obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Phenol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2It is taken after 1d in activating solution
Out, it is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, be subsequently placed in chemical nickel-plating solution under room temperature into
Row chemical plating obtains Co/ carbon composite until solution is become colorless by bluish violet；Electroless cobalt plating formula are as follows: 0.4g
CoCl2·6H2O, 20mL deionized water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: the Co/ carbon composite obtained in step 2 is cleaned several times with deionized water, then carried out with acetone
Supercritical drying is carried out after exchange of solvent 7d, i.e. acquisition Co/ carbon aerogels.
Aeroge Co content is 25wt%；Specific surface area is 300g/m2；Conductivity is 0.01S/cm；Ms is 10emu/
g；Mr is 3.7emu/g；Hc is 262Oe；Minimum reflection when additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
RL is lostminReachable -60dB, effective bandwidth is up to 5dB.
Embodiment 4:
Step 1: mechanical stirring is used to clarifying after 8.08g hydroquinone is mixed with formaldehyde with molar ratio 1:2
0.2mol·L-1NaOH solution constant volume solution obtains wet gel to 100mL at room temperature after gel 3 days.Pickling is carried out to wet gel
Aging, exchange of solvent, CO2Hydroquinone-formaldehyde aerogels are obtained after supercritical fluid drying, and further the aeroge is carried out
Carbonization, is heated to 1050 DEG C with the heating rate of 1.5 DEG C/min, hydroquinone-formaldehyde carbon aerogels is obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Hydroquinone in step 1-formaldehyde carbon aerogels are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2In activating solution after 1d
It takes out, is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, it is subsequently placed in chemical nickel-plating solution under room temperature
Chemical plating is carried out, until solution is become colorless by bluish violet, obtains Co/ carbon composite；Electroless cobalt plating formula are as follows: 0.05g
NiCl2·6H2O, 20mL deionized water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: the Co/ carbon composite obtained in step 2 is cleaned several times with deionized water, then carried out with acetone
Supercritical drying is carried out after exchange of solvent 7d, i.e. acquisition Co/ carbon aerogels.
Aeroge Co content is 1wt%；Specific surface area is 700g/m2；Conductivity is 1S/cm；Ms is 0.5emu/g；Mr
For 0.07emu/g；Hc is 60Oe；Minimum reflection loss when additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
RLminFor -20dB, effective bandwidth is up to 3dB.
Embodiment 5
Step 1: mechanical stirring is used to clarifying after 8.08g phloroglucin is mixed with formaldehyde with molar ratio 1:2
0.2mol·L-1NaOH solution constant volume solution obtains wet gel to 100mL at room temperature after gel 3 days.Pickling is carried out to wet gel
Aging, exchange of solvent, CO2Phloroglucinol-formaldehyde aeroge is obtained after supercritical fluid drying, and further the aeroge is carried out
Carbonization, is heated to 1050 DEG C with the heating rate of 1.5 DEG C/min, phloroglucinol-formaldehyde carbon aerogels is obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Phloroglucinol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2In activating solution after 1d
It takes out, is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, it is subsequently placed in chemical nickel-plating solution under room temperature
Chemical plating is carried out, until solution is become colorless by bluish violet.Electroless cobalt plating formula are as follows: 0.3g CoCl2·6H2O, 20mL deionization
Water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate.
Step 3: the Co/ carbon composite obtained in step 2 is cleaned several times with deionized water, then carried out with acetone
Supercritical drying is carried out after exchange of solvent 7d, i.e. acquisition Co/ carbon aerogels.
Aeroge Co content is 15wt%；Specific surface area is 450g/m2；Conductivity is 0.2S/cm；Ms is 3.7emu/
g；Mr is 1.2emu/g；Hc is 103Oe；Minimum reflection when additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
RL is lostminReachable -45dB, effective bandwidth is up to 4.0dB.
Embodiment 6
Step 1: mechanical stirring uses 0.2molL to clarifying after 8.08g phenol is mixed with formaldehyde with molar ratio 1:2- 1NaOH solution constant volume solution obtains wet gel to 100mL at room temperature after gel 3 days.Pickling aging, solvent are carried out to wet gel
Exchange, CO2Obtain phenol-formaldehyde aeroge after supercritical fluid drying, be further carbonized to the aeroge, with 1.5 DEG C/
The heating rate of min is heated to 1050 DEG C, and phenol-formaldehyde carbon aerogels are obtained after constant temperature 2h.
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Ultrasonic dissolution in wave cleaning device；Phenol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl2It is taken after 1d in activating solution
Out, it is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, be subsequently placed in chemical nickel-plating solution under room temperature into
Row chemical plating obtains Co/ carbon composite until solution is become colorless by bluish violet.Electroless cobalt plating formula are as follows: 0.1g
CoCl2·6H2O, 20mL deionized water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: the Co/ carbon composite obtained in step 2 is cleaned several times with deionized water, then carried out with acetone
Supercritical drying is carried out after exchange of solvent 7d, i.e. acquisition Co/ carbon aerogels.
Aeroge Co content is 10wt%；Specific surface area is 510g/m2；Conductivity is 0.5S/cm；Ms is 1.7emu/
g；Mr is 0.6emu/g；Hc is 97Oe；Minimum reflection when additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
RL is lostminReachable -40dB, effective bandwidth is up to 4.0dB.
Embodiment 7:
Step 1: mechanical stirring uses 0.2molL to clarifying after 8.08g phenol is mixed with formaldehyde with molar ratio 1:2- 1NaOH solution constant volume solution obtains wet gel to 100mL at room temperature after gel 3 days.Pickling aging, solvent are carried out to wet gel
Exchange, CO2Obtain phenol-formaldehyde aeroge after supercritical fluid drying, be further carbonized to the aeroge, with 1.5 DEG C/
The heating rate of min is heated to 1050 DEG C, and phenol-formaldehyde carbon aerogels are obtained after constant temperature 2h.
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Ultrasonic dissolution in wave cleaning device；Phenol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl2It is taken after 1d in activating solution
Out, it is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, be subsequently placed in chemical nickel-plating solution under room temperature into
Row chemical plating obtains Co/ carbon composite until solution is become colorless by bluish violet.Electroless cobalt plating formula are as follows: 0.1g
CoCl2·6H2O, 20mL deionized water, six phosphate ester of 0.01g inositol, 1g aminoacetic acid, 0.1mL accelerator, 0.1g urine
Element, 0.1g antiaging agent, 0.05g benzotriazole, 0.05mL glycine, 0.06g 2-aminopyridine, 5mL ethyl alcohol, 2mL ammonium hydroxide
And 2mL hydrazine hydrate；
Step 3: the Co/ carbon composite obtained in step 2 is cleaned several times with deionized water, then carried out with acetone
Supercritical drying is carried out after exchange of solvent 7d, i.e. acquisition Co/ carbon aerogels.
Aeroge Co content is 10wt%；Specific surface area is 680g/m2；Conductivity is 1S/cm；Ms is 3.5emu/g；
Mr is 1.2emu/g；Hc is 100Oe；Minimum reflection damage when additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
Consume RLminReachable -45dB, effective bandwidth is up to 3.0dB.
Embodiment 8:
Step 1: mechanical stirring is used to clarifying after 8.08g resorcinol is mixed with formaldehyde with molar ratio 1:2
0.2mol·L-1NaOH solution constant volume solution obtains wet gel to 100ml at room temperature after gel 3 days.Pickling is carried out to wet gel
Aging, exchange of solvent, CO2Resorcinol-formaldehyde aeroge is obtained after supercritical fluid drying, and further the aeroge is carried out
Carbonization, is heated to 1050 DEG C with the heating rate of 1.5 DEG C/min, resorcinol-formaldehyde carbon aerogels is obtained after constant temperature 2h.
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Resorcinol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2In activating solution after 1d
It takes out, is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, it is subsequently placed in chemical nickel-plating solution under room temperature
Chemical plating is carried out, until solution is become colorless by bluish violet, obtains Ni/ carbon composite；Electroless Plating Ni formula are as follows: 0.3g
NiCl2·6H2O, 20mL deionized water, six phosphate ester of 0.02g inositol, 1g aminoacetic acid, 0.1mL accelerator, 0.1g urine
Element, 0.1g antiaging agent, 0.05g benzotriazole, 0.05mL glycine, 0.06g 2-aminopyridine, 5mL ethyl alcohol, 2mL ammonium hydroxide
And 2mL hydrazine hydrate；
Step 3: the Ni/ carbon composite of acquisition is cleaned several times with deionized water, exchange of solvent then is carried out with acetone
Supercritical drying is carried out after 7d, i.e. acquisition Ni/ carbon aerogels；
Aeroge Ni content is 18wt%；Specific surface area is 660g/m2；Conductivity is 0.8S/cm；Ms is 6.8emu/
g；Mr is 3.5emu/g；Hc is 200Oe；Minimum reflection when additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
RL is lostminReachable -58dB, effective bandwidth is up to 4.5dB.
Embodiment 9:
Step 1: mechanical stirring is used to clarifying after 8.08g phloroglucin is mixed with formaldehyde with molar ratio 1:2
0.2mol·L-1NaOH solution constant volume solution obtains wet gel to 100mL at room temperature after gel 3 days.Pickling is carried out to wet gel
Aging, exchange of solvent, CO2Phloroglucinol-formaldehyde aeroge is obtained after supercritical fluid drying, and further the aeroge is carried out
Carbonization, is heated to 1050 DEG C with the heating rate of 1.5 DEG C/min, phloroglucinol-formaldehyde carbon aerogels is obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Phloroglucinol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2In activating solution after 1d
It takes out, is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, it is subsequently placed in chemical nickel-plating solution under room temperature
Chemical plating is carried out, until solution is become colorless by bluish violet.Electroless cobalt plating formula are as follows: 0.3g CoCl2·6H2O, 20mL deionization
Water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate.
Step 3: several times by the Co/ carbon composite deionized water soaking and washing obtained in step 2, then freezing is dry
It is dry, that is, obtain Co/ carbon aerogels；
It is described freeze-drying the following steps are included:
Step I, by nano metal/carbon composite precooling: -30 DEG C of cryogenic temperature, cooling time 1 hour；
Nano metal/carbon composite after precooling is warming up to 25 DEG C by step II, is kept for 2 hours；
Step III, freeze-drying: vacuum freeze drier is added in the nano metal that step II is obtained/carbon composite
In, setting condenser temperature is -50 DEG C, vacuum degree 500mpa, sublimation drying 10h, obtains magnetic conductive Co/ carbon aerogels
Absorbing material.
The Co/ carbon aerogels absorbing material Co content is 15wt%；Specific surface area is 680g/m2；Conductivity is 0.3S/
cm；Ms is 3.9emu/g；Mr is 1.5emu/g；Hc is 115Oe；Additive amount be 10wt% when, Wave suction composite material with a thickness of
Minimum reflection loss RL when 2mmminReachable -55dB, effective bandwidth is up to 4.6dB.
Embodiment 10:
Step 1: mechanical stirring uses 0.2molL to clarifying after 8.08g phenol is mixed with formaldehyde with molar ratio 1:2- 1NaOH solution constant volume solution obtains wet gel at room temperature, carries out pickling aging, solvent to wet gel to 100mL after gel 3 days
Exchange, CO2Obtain phenol-formaldehyde aeroge after supercritical fluid drying, be further carbonized to the aeroge, with 1.5 DEG C/
The heating rate of min is heated to 1050 DEG C, and phenol-formaldehyde carbon aerogels are obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Phenol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2It is taken after 1d in activating solution
Out, it is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, phenol-formaldehyde carbon aerogels are then placed in rotation
Bracket on, rotated with the speed of 100r/min, metallochemistry plating solution be then sprayed onto rotation with the speed of 100mL/min
It is carried out chemical plating 1~12 day on carbon aerogels, until solution is become colorless by bluish violet, obtains Ni/ carbon composite；Chemical plating
Ni formula are as follows: 0.2g NiCl2·6H2O, 20mL deionized water, 5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: the Ni/ carbon composite of acquisition is cleaned several times with deionized water, exchange of solvent then is carried out with acetone
Supercritical drying is carried out after 7d, i.e. acquisition Ni/ carbon aerogels.
Aeroge Ni content is 12.3wt%；Specific surface area is 650g/m2；Conductivity is 0.8S/cm；Ms is
1.5emu/g；Mr is 0.25emu/g；Hc is 105Oe；When additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
Minimum reflection loss RLminReachable -45dB, effective bandwidth is up to 4.2dB.
Embodiment 11:
Step 1: mechanical stirring uses 0.2molL to clarifying after 8.08g phenol is mixed with formaldehyde with molar ratio 1:2- 1NaOH solution constant volume solution obtains wet gel at room temperature, carries out pickling aging, solvent to wet gel to 100mL after gel 3 days
Exchange, CO2Obtain phenol-formaldehyde aeroge after supercritical fluid drying, be further carbonized to the aeroge, with 1.5 DEG C/
The heating rate of min is heated to 1050 DEG C, and phenol-formaldehyde carbon aerogels are obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Phenol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2It is taken after 1d in activating solution
Out, it is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, phenol-formaldehyde carbon aerogels are then placed in rotation
Bracket on, rotated with the speed of 100r/min, metallochemistry plating solution be then sprayed onto rotation with the speed of 100mL/min
It is carried out chemical plating 1~12 day on carbon aerogels, until solution is become colorless by bluish violet, obtains Ni/ carbon composite；Chemical plating
Ni formula are as follows: 0.3g NiCl2·6H2O, 20mL deionized water, six phosphate ester of 0.02g inositol, 1g aminoacetic acid, 0.1mL
Accelerator, 0.1g urea, 0.1g antiaging agent, 0.05g benzotriazole, 0.05mL glycine, 0.06g 2-aminopyridine,
5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: the Ni/ carbon composite of acquisition is cleaned several times with deionized water, exchange of solvent then is carried out with acetone
Supercritical drying is carried out after 7d, i.e. acquisition Ni/ carbon aerogels.
Aeroge Ni content is 12.3wt%；Specific surface area is 680g/m2；Conductivity is 0.85S/cm；Ms is
1.8emu/g；Mr is 0.3emu/g；Hc is 115Oe；When additive amount is 10wt%, when Wave suction composite material is with a thickness of 2mm
Minimum reflection loss RLminReachable -50dB, effective bandwidth is up to 4.5dB.
Embodiment 12:
Step 1: mechanical stirring uses 0.2molL to clarifying after 8.08g phenol is mixed with formaldehyde with molar ratio 1:2- 1NaOH solution constant volume solution obtains wet gel at room temperature, carries out pickling aging, solvent to wet gel to 100mL after gel 3 days
Exchange, CO2Obtain phenol-formaldehyde aeroge after supercritical fluid drying, be further carbonized to the aeroge, with 1.5 DEG C/
The heating rate of min is heated to 1050 DEG C, and phenol-formaldehyde carbon aerogels are obtained after constant temperature 2h；
Step 2: weighing 0.05g PdCl2In beaker, 45mL EtOH and 5mL 1molL is added-1HCl is placed in ultrasound
Phenol-formaldehyde carbon aerogels in step 1 are placed in above-mentioned PdCl by ultrasonic dissolution in wave cleaning device2It is taken after 1d in activating solution
Out, it is rinsed with deionized water to remove the PdCl of hydrogel surface enrichment2, phenol-formaldehyde carbon aerogels are then placed in rotation
Bracket on, rotated with the speed of 100r/min, metallochemistry plating solution be then sprayed onto rotation with the speed of 100mL/min
It is carried out chemical plating 1~12 day on carbon aerogels, until solution is become colorless by bluish violet, obtains Ni/ carbon composite；Chemical plating
Ni formula are as follows: 0.3g NiCl2·6H2O, 20mL deionized water, six phosphate ester of 0.02g inositol, 1g aminoacetic acid, 0.1mL
Accelerator, 0.1g urea, 0.1g antiaging agent, 0.05g benzotriazole, 0.05mL glycine, 0.06g 2-aminopyridine,
5mL ethyl alcohol, 2mL ammonium hydroxide and 2mL hydrazine hydrate；
Step 3: several times with deionized water soaking and washing by the Ni/ carbon composite of acquisition, being then freeze-dried, that is, obtaining
Obtain Ni/ carbon aerogels；
It is described freeze-drying the following steps are included:
Step I, by nano metal/carbon composite precooling: -50 DEG C of cryogenic temperature, cooling time 3 hours；
Nano metal/carbon composite after precooling is warming up to 25 DEG C by step II, is kept for 4 hours；
Step III, freeze-drying: vacuum freeze drier is added in the nano metal that step II is obtained/carbon composite
In, setting condenser temperature is -85 DEG C, vacuum degree 50pa, sublimation drying 10h, obtains the suction of magnetic conductive Ni/ carbon aerogels
Wave material；
The Ni/ carbon aerogels Ni content is 12.3wt%；Specific surface area is 700g/m2；Conductivity is 1S/cm；Ms is
2emu/g；Mr is 0.5emu/g；Hc is 125Oe；Additive amount be 10wt% when, Wave suction composite material with a thickness of when 2mm most
Low reflection loss RLminReachable -55dB, effective bandwidth is up to 4.8dB.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (8)
1. a kind of preparation method of magnetic conductive nano metal/carbon aerogels absorbing material, which is characterized in that including following step
It is rapid:
Step 1: PdCl is added in carbon aerogels2Or SnCl2At least 1h is impregnated in sensitizing solution；Then it is rinsed with deionized water to remove
The PdCl for going hydrogel surface to be enriched with2Or SnCl2；
Step 2: by treated in step 1, carbon aerogels are soaked into metallochemistry plating solution, are carried out chemical plating 1-12 days, are obtained
Obtain nano metal/carbon composite；
Step 3: obtained nano metal/carbon composite drying is inhaled to get to magnetic conductive nano metal/carbon aerogels
Wave material；
Wherein, the magnetic conductive nano metal/carbon aerogels absorbing material is mainly made of charcoal and metal nanoparticle, wherein
Charcoal is calculated as 75~99% with carbon aerogels absorbing material weight, and metal nanoparticle is calculated as 1 with carbon aerogels absorbing material weight
~25%；
The specific surface area of the absorbing material is between 300~700g/m2, conductivity is between 0.01~1S/m, saturation magnetic field intensity Jie
In 0.5~10emu/g, and when the absorbing material uses minimal reflection loss between -20~-60dB, inhale wave effective bandwidth between
2-5dB。
2. the preparation method of magnetic conductive nano metal/carbon aerogels absorbing material as described in claim 1, feature exist
In the carbon aerogels are resorcinol-formaldehyde carbon aerogels, phenol-formaldehyde carbon aerogels, hydroquinone-formaldehyde carbon airsetting
Any one in glue and phloroglucinol-formaldehyde carbon aerogels.
3. the preparation method of magnetic conductive nano metal/carbon aerogels absorbing material as described in claim 1, feature exist
In the metal nanoparticle is Ni or Co.
4. the preparation method of magnetic conductive nano metal/carbon aerogels absorbing material as described in claim 1, feature exist
In the metallochemistry plating solution is chemical nickel-plating solution or electroless cobalt plating solution；The formula of the chemical nickel-plating solution are as follows: 0.05
~0.3 parts by weight NiCl2·6H2O, 20 parts by volume deionized waters, 5 parts by volume of ethanol, 2 parts by volume ammonium hydroxide and the hydration of 2 parts by volume
Hydrazine；The formula of the electroless cobalt plating solution are as follows: 0.1~0.4 parts by weight CoCl2·6H2O, 20 parts by volume deionized waters, 5 parts by volume
Ethyl alcohol, 2 parts by volume ammonium hydroxide and 2 parts by volume hydrazine hydrates.
5. the preparation method of magnetic conductive nano metal/carbon aerogels absorbing material as described in claim 1, feature exist
In the drying in the step 3 is one of supercritical drying or freeze-drying；In the supercritical drying, before it is dried
Nano metal/carbon composite must be subjected to washing by soaking with deionized water, then carry out solvent displacement simultaneously with ethyl alcohol or acetone
Supercritical drying；In the freeze-drying, nano metal/carbon composite impregnate with deionized water before it is dried and washed
It is freeze-dried after washing to get magnetic conductive nano metal/carbon aerogels are arrived.
6. the preparation method of magnetic conductive nano metal/carbon aerogels absorbing material as claimed in claim 5, feature exist
In, it is described freeze-drying the following steps are included:
Step I, by nano metal/carbon composite precooling: cryogenic temperature -30~-50 DEG C, cooling time 1~3 hour；
Nano metal/carbon composite after precooling is warming up to 25 DEG C by step II, is kept for 2~4 hours；
Step III, freeze-drying: the nano metal that step II is obtained/carbon composite is added in vacuum freeze drier, if
Setting condenser temperature is -50~-85 DEG C, and vacuum degree is 500mpa~50pa, and sublimation drying 5-10h obtains magnetic conductive and receives
Rice metal/carbon aeroge absorbing material.
7. the preparation method of magnetic conductive nano metal/carbon aerogels absorbing material as described in claim 1, feature exist
In the metallochemistry plating solution is chemical nickel-plating solution, the formula of the chemical nickel-plating solution are as follows: 0.05~0.3 parts by weight
NiCl2·6H2O, 20 parts by volume deionized waters, 0.01~0.06 parts by weight inositol, six phosphate ester, 1 parts by weight aminoacetic acid,
0.1 parts by volume accelerator, 0.1 parts by weight of urea, 0.1 parts by weight antiaging agent, 0.05 parts by weight benzotriazole, 0.05 volume
Part glycine, 0.06 parts by weight 2-aminopyridine, 5 parts by volume of ethanol, 2 parts by volume ammonium hydroxide and 2 parts by volume hydrazine hydrates；The gold
Category chemical plating fluid is electroless cobalt plating solution, the formula of the electroless cobalt plating solution are as follows: 0.1~0.4 parts by weight CoCl2·6H2O、20
Parts by volume deionized water, 0.01~0.06 parts by weight inositol, six phosphate ester, 1 parts by weight aminoacetic acid, 0.1 parts by volume accelerate
Agent, 0.1 parts by weight of urea, 0.1 parts by weight antiaging agent, 0.05 parts by weight benzotriazole, 0.05 parts by volume glycine, 0.06
Parts by weight 2-aminopyridine, 5 parts by volume of ethanol, 2 parts by volume ammonium hydroxide and 2 parts by volume hydrazine hydrates.
8. the preparation method of magnetic conductive nano metal/carbon aerogels absorbing material as described in claim 1, feature exist
In the process replacement of the step 2 are as follows: carbon aerogels are placed on the bracket of rotation, with the speed of 100~150r/min
Then metallochemistry plating solution is sprayed onto progress chemical plating 1 on the carbon aerogels of rotation with the speed of 50~100mL/min by rotation
~12 days, obtain nano metal/carbon composite.
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| CN108300983B (en) * | 2017-12-30 | 2020-04-10 | 苏州赛尔科技有限公司 | High-energy-efficiency hub type nickel-based blade and preparation method thereof |
| CN109112341B (en) * | 2018-07-29 | 2020-02-21 | 浙江大学 | Preparation method of hierarchical porous nickel-cobalt alloy-carbon composite block material with electromagnetic wave absorption performance |
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| CN111422866A (en) * | 2019-01-09 | 2020-07-17 | 天津晨祥丰凯新材料科技有限公司 | Composite material and preparation method thereof |
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