CN105382252B - A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof - Google Patents

A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof Download PDF

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CN105382252B
CN105382252B CN201510795828.5A CN201510795828A CN105382252B CN 105382252 B CN105382252 B CN 105382252B CN 201510795828 A CN201510795828 A CN 201510795828A CN 105382252 B CN105382252 B CN 105382252B
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nickel
microballoon
electromagnetic wave
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powder
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CN105382252A (en
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刘久荣
刘伟
邱松
刘玉珍
吴楠楠
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Shandong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions

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  • General Chemical & Material Sciences (AREA)
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Abstract

The present invention relates to a kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof, a diameter of 28 microns of the nickel microballoon, nickel ball surface is rougher, there is up to 400nm bumps.Presoma of the present invention using divalent nickel salt as synthesis nickel microballoon, sodium hydroxide, ammoniacal liquor are as precipitating reagent, polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone synthesize nickel microballoon as reducing agent as surfactant, triethanolamine, diethanol amine using one step hydro thermal method.Nickel microballoon saturated magnetization rate produced by the present invention is high, and coercivity is big, and electro-magnetic wave absorption performance is good, and oxidation resistance is good, and preparation technology is simple, cost is low.

Description

A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof
Technical field
The present invention relates to a kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof, belong to magnetic and Electromagnetic wave absorbent material technical field.
Background technology
With the fast development of radio communication technology and high-frequency circuit equipment, electromagnetic wave absorbent material is as effectively reduction The means of Electromagnetic Interference, electromagnetic wave can be converted into the energy of other forms and attenuated.Magnetic loss, dielectric absorption and lead Electric loss material can be used as electromagnetic wave absorb, and magnetic loss material turns into the focus of current research because from it Thinner electromagnetic wave absorb can be prepared.For magnetic electromagnetic wave absorbing material, the magnetic conductivity and dielectric constant of material are determined Its absorbent properties are determined.As traditional magnetic electromagnetic wave absorbing material, ferrite has ferromagnetism and low conductivity, example Such as:NixZn1-xFe2O4,MgxZn1-xFe2O4Widely study and pay close attention to Deng people have been obtained, referring to document: J.Appl.Phys.88,348 (2000), J.Magn.Magn.Mater.256,340 (2003).But due to material in itself Snoek limitations, ferrite is applied to the frequency range less than GHz, referring to document:Physica 14,207(1948).In height In the GHz range of frequency, because magnetic conductivity strongly reduces, absorbent properties of the ferrite in high-frequency range substantially reduce, and lead Causing the thickness of its absorbed layer increases.But metallic magnet has very high saturated magnetization rate, its Snoek limitations are very high Frequency range, its magnetic conductivity can also keep very high in the scope of high frequency, thus with regard to can prepare thinner and lighter matter, It is applicable the electromagnetic wave absorbent material that frequency range is more widened.But when metallic magnet is used for electromagnetic wave absorbent material, there is also one The problem of individual serious, generally they have very high conductance, in electromagnetic wave environment caused eddy current loss can make material Magnetic conductivity reduces, so as to have a strong impact on the absorbent properties of material.Micron or nanometer chi are just needed to use in order to reduce eddy current loss Very little metallic magnet as electromagnetic wave absorbent material, while by metallic magnet particle be evenly distributed in non-conductor medium or Wrap up one layer of non-conductive film and be used for suppressing eddy current loss in the surface of magnetic particles.
The microcosmic knot of studies have shown that electro-magnetic wave absorption intensity, absorption frequency, absorber thickness and absorption band width and nickel Structure has close relationship.Such as:The nickel microballoon and the composite of paraffin that mass fraction is 70% are in 1-18GHz frequency ranges With electro-magnetic wave absorption, but absorption intensity is weaker, when absorber thickness is 2.5mm, its maximum absorption intensity be only- 4.7dB (decibel), referring to document:Appl.Surf.Sci.332,112(2015).The main reason for its absorption intensity is weak is nickel The diameter of ball is adhered to one another into larger sized aggregate between 0.8-1.1 microns, nickel ball so that the nickel ball material is in paraffin In it is dispersed poor, nickel pelletizing aggressiveness be cross-linked with each other to be formed conduction network, larger vortex is produced in electromagnetic wave environment Loss, reduces magnetic conductivity, causes the electro-magnetic wave absorption intensity of material weaker.
The preparation prior art of nickel microballoon mainly has solvent-thermal method.For example, to prepare metallic nickel micro- for CN103464781A one kind The method of ball, including step:1) four hydration nickel acetates are dissolved in organic solvent, then add formic acid and obtain clear solution, The molar concentration of four hydration nickel acetates in organic solvent is 0.01M~1M, and four mol ratios for being hydrated nickel acetates and formic acid are 1:1 ~10;2) solution made from step 1) is transferred in solvent thermal, solvent thermal reaction 30min is carried out at 190~240 DEG C ~100h, centrifuge, dry, obtain metallic nickel microballoon, average grain diameter is about 500~800nm.For another example, CN101024250A is disclosed The preparation method of a kind of uniform nickel microballoon of polycrystalline and its linear nickel chain, it is to be not more than 0.40T weak magnetic without magnetic field or intensity In, 10.0-160.0g/L polyvinylpyrrolidones are dissolved in into ethanol, and 0.6-6/1 mixes the solution being made into by volume with water In, then by hydrazine hydrate and divalent nickel salt with N2H4/NI2Ratio of+the mol ratio not less than 2.6 is added in above-mentioned system, is risen after sealing To 90-200 DEG C, insulation is no less than 1 hour temperature;React to obtain the uniform nickel microballoon of polycrystalline when being not added with magnetic field, microspherulite diameter exists Between 230-350nm.
The nickel microsphere diameter that the method for prior art described above obtains is respectively less than 1 micron, easily reunites, in paraffin Deng when disperseing in medium it is more difficult, thereby result in and larger eddy current loss produced in electromagnetic wave environment, reduce magnetic conductivity.
The content of the invention
For insufficient existing for prior art nickel microballoon electromagnetic wave absorbent material, it is micro- that the present invention provides a kind of monodispersed nickel Ball powder electromagnetic wave absorbent material and preparation method thereof.
Term is explained:
Height of concave convex:Refer to the distance between the bottom of certain pit and the top of adjacent protrusion.
Technical scheme is as follows:
A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material, a diameter of 2-8 microns of the nickel microballoon, nickel microballoon Surface irregularity, height of concave convex≤400nm.Described monodispersed nickel microballoon powder is to use hydro-thermal method one-step synthesis system .
, according to the invention it is preferred to, a diameter of 2-5 microns of nickel microballoon.
According to the present invention, the saturated magnetization rate of described monodispersed nickel microballoon powder is 61.0 ± 0.5emu/g;Coercive Power HcjFor 316.0-324.4Oe;The requirement condition for preparing thin electromagnetic wave absorbing layer can be met.
Electro-magnetic wave absorption RL of the described monodispersed nickel microballoon powder in 1.5-4GHz frequency ranges<- 20dB, i.e., 99% Electromagnetic wave absorbed.
According to the present invention, the preparation method of the nickel microballoon powder electromagnetic wave absorbent material, using hydro-thermal method, including it is as follows Step:
Using divalent inorganic nickel salt as raw material, one of sodium hydroxide, ammoniacal liquor or combination are used as precipitating reagent, polyethylene glycol (PEG), One of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) or combination are used as surfactant, triethanolamine, diethanol amine it One or combination be used as reducing agent.
By above-mentioned divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent (3~5) in mass ratio:(8~11):(1 ~3):(10~12) are soluble in water, react 20-80 hours in 100-400 DEG C, wash drying, produce nickel microballoon powder.Work as divalence When inorganic nickel is hydrate, above mass ratio is in terms of the quality of the raw material containing the crystallization water.
, according to the invention it is preferred to, the divalent inorganic nickel salt is selected from nickel sulfate (NiSO4), nickel chloride (NiCl2), nitric acid Nickel (Ni (NO3)2) one of or combination.Preferably, the divalent inorganic nickel salt is Nickel dichloride hexahydrate (NiCl2·6H2O)。
, according to the invention it is preferred to, the divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent gross mass with The mass volume ratio of water is 22~31:100, unit:g/mL.
, according to the invention it is preferred to, the reaction temperature of above-mentioned reaction is 160-270 DEG C.Further preferred reaction temperature is 200-210℃。
, according to the invention it is preferred to, the reaction time of above-mentioned reaction is 24-50 hours.
, according to the invention it is preferred to, divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent mass ratio for (3~ 4):(8~10):(1~2):(10~11), most preferred presoma, precipitating reagent, surfactant, the mass ratio of reducing agent are 3:10:2:10。
According to the present invention, further preferred preparation method is as follows:
It is raw material with Nickel dichloride hexahydrate, sodium hydroxide is as precipitating reagent, and polyethylene glycol is as surfactant, three ethanol Amine presses 3g as reducing agent, above-mentioned raw materials:10g:2g:10g is added in 100mL water, is reacted 24 hours in 200 DEG C, and washing is dry It is dry, monodispersed nickel microballoon is made, a diameter of 2-5 microns of microballoon, nickel ball surface is rougher, and height of concave convex is up to 400nm.
Precursor material, sodium hydroxide, ammoniacal liquor one of or group of the present invention using divalent inorganic nickel salt as synthesis nickel microballoon To cooperate as precipitating reagent, polyethylene glycol (PEG), polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) are used as surfactant, and three Monoethanolamine, diethanol amine are as reducing agent;Nickel microballoon is synthesized using one step hydro thermal method.
Sodium hydroxide and precursor material in reaction system, such as Nickel dichloride hexahydrate (NiCl2·6H2O) hydrolyze, OH-ion caused by hydrolysis and Ni2+ reaction generation nickel hydroxide precipitate, while triethanolamine by nickel hydroxide nano particle also Originally it was nickel particle, was raised with reaction temperature, time lengthening, nano nickel particles crystal growth, in order to reduce surface energy, nickel particle heap Product growth forms nickel micro-sphere structure together.Coarse surface is due in nickel crystal caused by the fast-growth of some crystal faces.
The nickel microballoon of the present invention has higher saturated magnetization rate (61.0 ± 0.5emu/g), big coercivity HcjIt is (reachable 324.4Oe), it can also keep very high magnetic permeability in the scope of high frequency, be the premise for preparing thin electromagnetic wave absorbing layer Condition.Excellent electro-magnetic wave absorption (RL is shown in 1.5-4GHz frequency ranges through measuring<- 20dB, mean 99% electricity Magnetic wave is absorbed).The high frequency GHz range electromagnetic wave absorb prepared with the nickel micro-sphere material of the present invention, has excellent electricity Electro-magnetic wave absorption performance and important actual application value.
Application of the nickel microballoon powder of the present invention as electromagnetic wave absorbent material material, the nickel microballoon powder of the present invention is pressed into matter The ratio than 50% is measured to mix with paraffin, it is compressing, electromagnetic wave absorb is made.Manufactured electromagnetic wave absorb is in 1.5- 4GHz frequency range electro-magnetic wave absorptions RL<-20dB.
The application of nickel microballoon powder body material of the present invention, for one below:1st, it is electromagnetically shielded material in radio communication system Material, 2, anti-high frequency, the electromagnetic radiation of microwave heating equipment and leakage material, 3, construction microwave dark room material, 4, stealth technology material Material.
The present invention has following excellent results compared with prior art:
1st, the technique for synthesizing nickel microballoon is simple, it is not necessary to which complicated equipment, environmentally safe, cost of manufacture is relatively low.
2nd, the particle size of nickel microballoon prepared by the present invention is micron order and even particle size distribution, gained nickel microballoon stability Good with uniformity, anti-oxidant and corrosion resistance is strong.
3rd, the electromagnetic wave absorb prepared with nickel microballoon powder body material of the present invention has that absorbing property is good, absorption frequency covering Scope is wide, and absorber thickness is thin, the characteristics of light weight, can operate with electromagnetic shielding in radio communication system, anti-high frequency and micro- The electromagnetic radiation and leakage of the equipment such as Wave heating, construction microwave dark room and stealth technology etc. field.
Brief description of the drawings
Fig. 1 is the XRD diffracting spectrums of the gained nickel microballoon of embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the gained nickel microballoon of embodiment 1.
Fig. 3 is the magnetism testing curve of the gained nickel microballoon of embodiment 1.
Fig. 4 is the electro-magnetic wave absorption curve of the electromagnetic wave absorb of 1 gained nickel microballoon application experiment example of embodiment 1.
Fig. 5 is the electro-magnetic wave absorption curve of the electromagnetic wave absorb of 1 gained nickel microballoon application experiment example of embodiment 2.
Embodiment
The present invention is described in further detail with reference to specific embodiment, but not limited to this.Electromagnetism is determined in example The instrument that ripple absorbs is Agilent Technologies E8363A electromagnetic wave vector network analyzers.Used in embodiment Surfactant specification is:The MW of polyethylene glycol (PEG):10000th, the MW of polyvinyl alcohol (PVA):31000th, polyvinylpyrrolidine Ketone (PVP) K30.
Embodiment 1:
A kind of nickel microballoon powder electromagnetic wave absorbent material, it by monodispersed, diameter dimension is 2-5 microns that the nickel microballoon, which is, Ball composition, the nickel microsphere surface is rougher, and height of concave convex≤400nm (refers to bottom and the adjacent protrusion of certain pit The distance between top).
Preparation method:
By NiCl2·6H2O:Sodium hydroxide:Polyethylene glycol (PEG):Triethanolamine (TEA)=3g:10g:2g:10g mass Than weighing raw material, add in 100mL water, reacted 24 hours in 200 DEG C, wash drying, nickel microballoon powder is made.
X-ray powder diffraction pattern (XRD) (such as Fig. 1) shows the nickel that synthesized nickel microballoon is face-centred cubic structure, and And compared with standard diffraction data and show that the nickel purity of synthesis is very high.SEM (SEM) (Fig. 2) shows, nickel The particle size of microballoon is about that (Fig. 2, a), the SEM (Fig. 2, b) of more high power show 2-5 microns, synthesis Nickel microsphere surface is rougher, there is up to 400nm bumps.
The result characterized with VSM magnetometers to synthesized nickel microsphere sample shows that sample has 61.0emu/g's Saturated magnetization rate, and coercivity HcjUp to 324.4Oe, referring to Fig. 3.
Application experiment example 1:Electromagnetic wave absorb is made with nickel microballoon powder, and carries out test experiments
Both ring sam is pressed into after the ratio of nickel microballoon powder in mass ratio 50% made from embodiment 1 is mixed with paraffin (DOutside×dIt is interior× h=7 × 3.04 × 1.5mm), relevant parameter μrAnd εrWith Agilent Technologies E8363A electromagnetic waves Vector network analyzer measures, and reflection loss is by μr、εr, absorption frequency and sample thickness determine.The ε measuredr' in 0-18GHz Scope gradually reduces with the rise of frequency, and numerical value is in 40.0-18.9.εr" there is one wide be total in the range of 6.0-16.0GHz Shake peak, and its peak value is 8.6 at 11.2GHz.μr' gradually reduced with the rise of frequency in 0-18GHz scopes, numerical value exists 1.8-0.8。μr" numerical value fluctuated between 0.1-0.2.Its absworption peak minimum value is -29dB (decibel), absorptivity is less than - 20dB (99% electromagnetic wave is absorbed) frequency range is 1.5-4.0GHz, and its electro-magnetic wave absorption curve is shown in Fig. 4.
Embodiment 2:
As described in Example 1, except that substituting triethanolamine as reducing agent by the use of diethanol amine, it is micro- that nickel is prepared Ball, SEM (SEM) show that the Microsphere Size of synthesis is 2-6 microns.
X-ray powder diffraction pattern (XRD) shows the nickel that synthesized nickel microballoon is face-centred cubic structure, and and standard Diffraction data, which compares, shows that the nickel purity of synthesis is very high.The knot characterized with VSM magnetometers to synthesized nickel microsphere sample Fruit shows that sample has 61.2emu/g saturated magnetization rate and 317.6Oe coercivity (Hcj)。
Embodiment 3:
As described in Example 1, except that NiCl2·6H2O:Sodium hydroxide:Polyethylene glycol (PEG):Triethanolamine (TEA)=3g:9g:1g:10g, nickel microballoon is prepared, SEM (SEM) shows, the Microsphere Size of synthesis For 3-8 microns, microballoon dispersiveness is preferably.
X-ray powder diffraction pattern (XRD) shows the nickel that synthesized nickel microballoon is face-centred cubic structure, and and standard Diffraction data, which compares, shows that the nickel purity of synthesis is very high.The knot characterized with VSM magnetometers to synthesized nickel microsphere sample Fruit shows that sample has 60.8emu/g saturated magnetization rate and 316.4Oe coercivity (Hcj)。
Comparative example 1:
As described in Example 1, except that with nickel acetate (Ni (CH3COO)2·4H2O nickel chloride (NiCl) is substituted2· 6H2O) the precursor as nickel, is added without Surfactant PEG, and nickel microballoon, SEM (SEM) table is prepared Sign shows, the nickel Microsphere Size of synthesis is 0.3-1 microns, microballoon bad dispersibility, and part ball is bonded together.
X-ray powder diffraction pattern (XRD) shows the nickel that synthesized nickel microballoon is face-centred cubic structure, and and standard Diffraction data, which compares, shows that the nickel purity of synthesis is very high.The knot characterized with VSM magnetometers to synthesized nickel microsphere sample Fruit shows that sample has 59.8emu/g saturated magnetization rate and 315.5Oe coercivity (Hcj)。
Comparative example 2:
As described in Example 1, except that not adding surfactant polyethylene (PEG), it is micro- that nickel is prepared Ball, SEM (SEM) show that the Microsphere Size of synthesis is 1-1.5 microns, and microballoon bad dispersibility is many micro- Ball is bonded together.
X-ray powder diffraction pattern (XRD) shows the nickel that synthesized nickel microballoon is face-centred cubic structure, and and standard Diffraction data, which compares, shows that the nickel purity of synthesis is very high.
Comparative example 3:
As described in Example 1, except that the mass ratio 1g that raw starting material adds:7g:5g:13g, it is prepared Nickel microballoon, SEM (SEM) show that the Microsphere Size of synthesis is 0.5-1 microns, microballoon bad dispersibility, is permitted More microsphere adhesives are together.
X-ray powder diffraction pattern (XRD) shows the nickel that synthesized nickel microballoon is face-centred cubic structure, and and standard Diffraction data, which compares, shows that the nickel purity of synthesis is very high.The knot characterized with VSM magnetometers to synthesized nickel microsphere sample Fruit shows that sample has 60.8emu/g saturated magnetization rate and 301.2Oe coercivity (Hcj)。
Application experiment example 2:Electromagnetic wave absorb is made with nickel microballoon powder, and carries out test experiments
Using nickel microballoon powder made from embodiment 1, in mass ratio 30% ratio is pressed into ring-type sample after being mixed with paraffin Product (DOutside×dIt is interior× h=7 × 3.04 × 1.5mm), relevant parameter μrAnd εrWith Agilent Technologies E8363A electromagnetism Wave vector Network Analyzer measures, and reflection loss is by μr、εr, absorption frequency and sample thickness determine.The real part ε measuredr' 7.5 are down to from 9.6 in the range of 0-4GHz, there are two low ebbs at 11.8 and 15.1GHz frequencies thereafter, valley is respectively 7.3 Hes 6.7.Imaginary part εr" there are two formants at 11.2 and 14.2GHz, peak value is respectively 1.1 and 1.4.μr' 0-18GHz scopes with The rise of frequency and gradually reduce, numerical value is in 1.4-0.8.μr" numerical value fluctuated between 0.03-0.2.Its absworption peak minimum value For -18dB (decibel), frequency range of the absorptivity less than -10dB (90% electromagnetic wave is absorbed) is 6.0-15.5GHz, its electromagnetism Ripple absorption curve is shown in Fig. 5.Thus illustrate that the mass ratio of nickel microballoon powder is reduced to 30%, its electro-magnetic wave absorption intensity is micro- due to nickel The reduction of ball absorbent and reduce.

Claims (9)

  1. A kind of 1. monodispersed nickel microballoon raw powder's production technology for electromagnetic wave absorbent material, using hydro-thermal method, including such as Lower step:Using divalent inorganic nickel salt as raw material, one of sodium hydroxide, ammoniacal liquor or combination are used as precipitating reagent, polyethylene glycol (PEG), One of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) or combination are used as surfactant, triethanolamine, diethanol amine it One or combination be used as reducing agent;By above-mentioned divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent (3~5) in mass ratio: (8~11):(1~3):(10~12) are soluble in water, react 20-80 hours in 100-400 DEG C, wash drying, produce nickel microballoon Powder;A diameter of 2-8 microns of the nickel microballoon powder, the nickel microballoon powder surface is uneven, and height of concave convex≤ 400nm;The saturated magnetization rate of described monodispersed nickel microballoon powder is 61.0 ± 0.5emu/g;The nickel microballoon powder is pressed Mixed with ratio of the Quality of Paraffin Waxes than 50%, it is compressing, electromagnetic wave absorb is made;Manufactured electromagnetic wave absorb is in 1.5- 4GHz frequency range electro-magnetic wave absorptions RL<-20dB.
  2. 2. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is that the divalent inorganic nickel salt is selected from one of nickel sulfate, nickel chloride, nickel nitrate or combination.
  3. 3. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is that the divalent inorganic nickel salt is Nickel dichloride hexahydrate.
  4. 4. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is, the divalent inorganic nickel salt, precipitating reagent, surfactant, the ratio between the volume of the gross mass of reducing agent and water for 22~ 31:100, the unit of aforementioned proportion:g/mL.
  5. 5. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is that the reaction temperature of the reaction is 160-270 DEG C.
  6. 6. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is that the reaction temperature of the reaction is 200-210 DEG C, and the reaction time is 24-50 hours.
  7. 7. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is that the divalent inorganic nickel salt, precipitating reagent, surfactant, the mass ratio of reducing agent are (3~4):(8~10):(1~ 2):(10~11).
  8. 8. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is that the divalent inorganic nickel salt, precipitating reagent, surfactant, the mass ratio of reducing agent are 3:10:2:10.
  9. 9. being used for the monodispersed nickel microballoon raw powder's production technology of electromagnetic wave absorbent material as claimed in claim 1, it is special Sign is that step is as follows:
    It is raw material with Nickel dichloride hexahydrate, sodium hydroxide is made as precipitating reagent, polyethylene glycol as surfactant, triethanolamine For reducing agent, Nickel dichloride hexahydrate, sodium hydroxide, polyethylene glycol and triethanolamine are respectively according to 3g:10g:2g:10g is added to In 100mL water, reacted 24 hours in 200 DEG C, wash drying, monodispersed nickel microballoon powder, the diameter of nickel microballoon powder is made For 2-5 microns, nickel ball surface is rougher, and height of concave convex reaches 400nm.
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Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
磁性材料的制备及电磁波吸收性能研究;孔静;《CNKI中国优秀硕士论文全文数据库(工程科技Ⅰ辑)》;20130215(第2期);第15、25-40页 *

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