CN105382252A - Monodispersed nickel microsphere powder electromagnetic wave absorbing material and preparing method thereof - Google Patents
Monodispersed nickel microsphere powder electromagnetic wave absorbing material and preparing method thereof Download PDFInfo
- Publication number
- CN105382252A CN105382252A CN201510795828.5A CN201510795828A CN105382252A CN 105382252 A CN105382252 A CN 105382252A CN 201510795828 A CN201510795828 A CN 201510795828A CN 105382252 A CN105382252 A CN 105382252A
- Authority
- CN
- China
- Prior art keywords
- nickel
- electromagnetic wave
- microballoon
- absorbent material
- microballoon powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention relates to a monodispersed nickel microsphere powder electromagnetic wave absorbing material and a preparing method thereof. The diameter of nickel microspheres ranges from 2 mm to 8 mm, the surfaces of the nickel microspheres are relatively coarse, and concave-convex parts with the height being 400 nm are arranged. By means of the monodispersed nickel microsphere powder electromagnetic wave absorbing material and the preparing method, nickelous salt serves as a precursor for synthesizing the nickel microspheres, sodium hydroxide and ammonium hydroxide serve as precipitators, polyethylene glycol, polyving akohol and polyvinylpyrrolidone serve as surface active agents, and triethanolamine and diethanol amine serve as reducing agents; and the nickel microspheres are synthesized through one-step water-heat method. The prepared nickel microspheres are high in saturation magnetization rate, large in coercive force, good in electromagnetic wave absorbing performance, good in oxidation resistance, simple in preparing process and low in cost.
Description
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
Along with the fast development of radio communication technology and high-frequency circuit equipment, electromagnetic wave absorbent material, as the means effectively reducing Electromagnetic Interference, can convert other forms of energy to electromagnetic wave and attenuate.Magnetic loss, dielectric absorption and loss of conduction material all can be used as electromagnetic wave absorb, and magnetic loss material becomes the focus of current research, because can prepare thinner electromagnetic wave absorb from it.For magnetic electromagnetic wave absorbing material, the magnetic conductivity of material and dielectric constant determine its absorbent properties.As traditional magnetic electromagnetic wave absorbing material, ferrite has ferromagnetism and low conductivity, such as: Ni
xzn
1-xfe
2o
4, Mg
xzn
1-xfe
2o
4study widely and pay close attention to Deng obtaining people, see document: J.Appl.Phys.88,348 (2000), J.Magn.Magn.Mater.256,340 (2003).But due to the Snoek limitation of material itself, ferrite is applicable to the frequency range lower than GHz, see document: Physica14,207 (1948).Within the scope of high-frequency GHz, because magnetic conductivity sharply reduces, the absorbent properties of ferrite in high-frequency range reduce greatly, cause the thickness of its absorbed layer to increase.But metallic magnet has very high saturated magnetization rate, its Snoek limitation is in very high frequency range, even if its magnetic conductivity can also keep very high in the scope of high frequency, thus just can prepare thinner, more lightweight, be suitable for the electromagnetic wave absorbent material that frequency range more widens.But also there is a serious problem when metallic magnet is used for electromagnetic wave absorbent material, they have very high conductance usually, and the eddy current loss produced in electromagnetic wave environment can make the magnetic conductivity of material reduce, thus has a strong impact on the absorbent properties of material.Just needing to use the metallic magnet of micron or nano-scale as electromagnetic wave absorbent material to reduce eddy current loss, metallic magnet uniform particles being distributed in non-conductor medium simultaneously or wrapping up one deck non-conductive film on the surface of magnetic particles and be used for suppressing eddy current loss.
Research display, the microstructure of electro-magnetic wave absorption intensity, absorption frequency, absorber thickness and absorption band width and nickel has close relationship.Such as: mass fraction is that the nickel microballoon of 70% and the composite of paraffin have electro-magnetic wave absorption in 1-18GHz frequency range, but absorption intensity is more weak, when absorber thickness is 2.5mm, its maximum absorption intensity is only-4.7dB (decibel), see document: Appl.Surf.Sci.332,112 (2015).The weak main cause of its absorption intensity is that the diameter of nickel ball is at 0.8-1.1 micron, the larger sized aggregate of one-tenth adhered to one another between nickel ball, make the dispersiveness of this nickel ball material in paraffin poor, nickel pelletizing aggressiveness is cross-linked with each other and forms the network of conduction, larger eddy current loss is produced in electromagnetic wave environment, reduce magnetic conductivity, cause the electro-magnetic wave absorption intensity of material more weak.
The preparation prior art of nickel microballoon mainly contains solvent-thermal method.Such as, CN103464781A mono-kind prepares the method for metallic nickel microballoon, comprise step: 1) be dissolved in organic solvent by four hydration nickel acetates, then add formic acid and obtain clear solution, four hydration nickel acetates molar concentration is in organic solvent 0.01M ~ 1M, and the mol ratio of four hydration nickel acetates and formic acid is 1:1 ~ 10; 2) by step 1) obtained solution transfers in solvent heat device, and at 190 ~ 240 DEG C, carry out solvent thermal reaction 30min ~ 100h, centrifugal, dry, obtain metallic nickel microballoon, average grain diameter is about 500 ~ 800nm.For another example, CN101024250A discloses the preparation method of the even nickel microballoon of a kind of polycrystalline and linear nickel chain thereof, be not more than in the low-intensity magnetic field of 0.40T without magnetic field or intensity, 10.0-160.0g/L polyvinylpyrrolidone is dissolved in ethanol and water by volume 0.6-6/1 mix in the solution be made into, then by hydrazine hydrate and divalent nickel salt with N
2h
4/ NI
2+the ratio that mol ratio is not less than 2.6 adds in above-mentioned system, is warming up to 90-200 DEG C after sealing, and insulation is no less than 1 hour; Be obtained by reacting the even nickel microballoon of polycrystalline when not adding magnetic field, microspherulite diameter is between 230-350nm.
The nickel microsphere diameter that the method for the above prior art obtains all is less than 1 micron, easily reunites, comparatively difficult when disperseing in the media such as paraffin, causes thus and produce larger eddy current loss in electromagnetic wave environment, reduce magnetic conductivity.
Summary of the invention
For the deficiency that prior art nickel microballoon electromagnetic wave absorbent material exists, the invention provides a kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof.
Terminological interpretation:
Height of concave convex: refer to the distance between the end of certain pit and the top of adjacent protrusion.
Technical scheme of the present invention is as follows:
A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material, the diameter of described nickel microballoon is 2-8 micron, and nickel microsphere surface is uneven, height of concave convex≤400nm.Described monodispersed nickel microballoon powder adopts hydro-thermal method one-step synthesis to obtain.
According to the present invention, preferably, the diameter of nickel microballoon is 2-5 micron.
According to the present invention, the saturated magnetization rate of described monodispersed nickel microballoon powder is 61.0 ± 0.5emu/g; Coercivity H
cjfor 316.0-324.4Oe; The requirement condition preparing thin electromagnetic wave absorbing layer can be met.
Described monodispersed nickel microballoon powder is at the electro-magnetic wave absorption RL<-20dB of 1.5-4GHz frequency range, and namely the electromagnetic wave of 99% is absorbed.
According to the present invention, the preparation method of described nickel microballoon powder electromagnetic wave absorbent material, adopts hydro-thermal method, comprises the steps:
With divalent inorganic nickel salt for raw material, one of NaOH, ammoniacal liquor or combination are as precipitating reagent, one of polyethylene glycol (PEG), polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) or combination are as surfactant, and one of triethanolamine, diethanol amine or combination are as reducing agent.
By above-mentioned divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent in mass ratio (3 ~ 5): (8 ~ 11): (1 ~ 3): (10 ~ 12) are soluble in water, in 100-400 DEG C of reaction 20-80 hour, washing is dry, obtains nickel microballoon powder.When divalent inorganic nickel salt is hydrate, above mass ratio is in the quality containing crystallization water raw material.
According to the present invention, preferably, described divalent inorganic nickel salt is selected from nickelous sulfate (NiSO
4), nickel chloride (NiCl
2), nickel nitrate (Ni (NO
3)
2) one of or combination.Preferably, described divalent inorganic nickel salt is Nickel dichloride hexahydrate (NiCl
26H
2o).
According to the present invention, preferably, the gross mass of described divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent and the mass volume ratio of water are 22 ~ 31:100, unit: g/mL.
According to the present invention, preferably, the reaction temperature of above-mentioned reaction is 160-270 DEG C.Further preferable reaction temperature is 200-210 DEG C.
According to the present invention, preferably, the reaction time of above-mentioned reaction is 24-50 hour.
According to the present invention, preferably, the mass ratio of divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent is (3 ~ 4): (8 ~ 10): (1 ~ 2): (10 ~ 11), and the mass ratio of most preferred presoma, precipitating reagent, surfactant, reducing agent is 3:10:2:10.
According to the present invention, preferred preparation method is as follows further:
Be raw material with Nickel dichloride hexahydrate, NaOH is as precipitating reagent, polyethylene glycol is as surfactant, and triethanolamine is as reducing agent, and above-mentioned raw materials joins in 100mL water by 3g:10g:2g:10g, in 200 DEG C of reactions 24 hours, washing is dry, obtained monodispersed nickel microballoon, and the diameter of microballoon is 2-5 micron, nickel ball surface is more coarse, and height of concave convex can reach 400nm.
The precursor material of the present invention using divalent inorganic nickel salt as synthesis nickel microballoon, one of NaOH, ammoniacal liquor or combination are as precipitating reagent, polyethylene glycol (PEG), polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) are as surfactant, and triethanolamine, diethanol amine are as reducing agent; Adopt one step hydro thermal method synthesis nickel microballoon.
NaOH and precursor material in reaction system, as Nickel dichloride hexahydrate (NiCl
26H
2o) be hydrolyzed, the OH that hydrolysis produces
-ion and Ni
2+reaction generates nickel hydroxide precipitate, and nickel hydroxide nano particle reduction is nickel particle by triethanolamine simultaneously, and with reaction temperature rising, time lengthening, nano nickel particles crystal growth, in order to reduce surface energy, the growth of nickel particle packing forms nickel micro-sphere structure together.Coarse surface is because the quick growth of some crystal face in nickel crystal produces.
Nickel microballoon of the present invention has higher saturated magnetization rate (61.0 ± 0.8emu/g), large coercivity H
cj(can reach 324.4Oe), even if it can also keep very high magnetic permeability in the scope of high frequency, is the precondition preparing thin electromagnetic wave absorbing layer.Excellent electro-magnetic wave absorption (RL<-20dB, the electromagnetic wave of meaning 99% is absorbed) is shown in 1.5-4GHz frequency range through measuring.The high frequency GHz scope electromagnetic wave absorb prepared with nickel micro-sphere material of the present invention, has excellent electro-magnetic wave absorption performance and important actual application value.
Nickel microballoon powder of the present invention as the application of electromagnetic wave absorbent material material, by nickel microballoon powder of the present invention in mass ratio 50% ratio mix with paraffin, compressing, make electromagnetic wave absorb.The electromagnetic wave absorb made is at 1.5-4GHz frequency range electro-magnetic wave absorption RL<-20dB.
The application of nickel microballoon powder body material of the present invention, for one of following: 1, electromagnetic shielding material in radio communication system, 2, anti-high frequency, microwave heating equipment electromagnetic radiation and leak material, 3, structure microwave dark room material, 4, stealth technology material.
The present invention compared with prior art has following excellent results:
The technique of 1, synthesizing nickel microballoon is simple, and do not need complicated equipment, environmentally safe, cost of manufacture is lower.
2, the particle size of nickel microballoon that prepared by the present invention is micron order and even particle size distribution, gained nickel polymeric microspheres stabilize and uniformity good, anti-oxidant and corrosion resistance is strong.
3, with electromagnetic wave absorb prepared by nickel microballoon powder body material of the present invention, there is absorbing property good, absorption frequency coverage is wide, absorber thickness is thin, the feature that quality is light, can apply to the field such as electromagnetic radiation and leakage, structure microwave dark room and stealth technology of the equipment such as electromagnetic shielding in radio communication system, anti-high frequency and heating using microwave.
Accompanying drawing explanation
Fig. 1 is the XRD diffracting spectrum of embodiment 1 gained nickel microballoon.
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 1 gained nickel microballoon.
Fig. 3 is the magnetism testing curve of embodiment 1 gained nickel microballoon.
Fig. 4 is the electro-magnetic wave absorption curve of embodiment 1 gained nickel microballoon application experiment example 1 electromagnetic wave absorb.
Fig. 5 be embodiment 1 gained nickel microballoon application experiment example 2 electromagnetic wave absorb electro-magnetic wave absorption curve.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but is not limited thereto.The instrument measuring electro-magnetic wave absorption in example is AgilentTechnologiesE8363A electromagnetic wave vector network analyzer.The surfactant specification used in embodiment is: the MW:10000 of polyethylene glycol (PEG), the MW:31000 of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) K30.
Embodiment 1:
A kind of nickel microballoon powder electromagnetic wave absorbent material, described nickel microballoon is made up of monodispersed, that diameter dimension is 2-5 micron ball, described nickel microsphere surface is more coarse, height of concave convex≤400nm (referring to the distance between the end of certain pit and the top of adjacent protrusion).
Preparation method:
By NiCl
26H
2o: NaOH: polyethylene glycol (PEG): triethanolamine (TEA)=3g:10g:2g:10g mass ratio takes raw material, adds in 100mL water, and in 200 DEG C of reactions 24 hours, washing was dry, obtained nickel microballoon powder.
X-ray powder diffraction pattern (XRD) (as Fig. 1) shows that synthesized nickel microballoon is the nickel of face-centred cubic structure, and shows that the nickel purity of synthesizing is very high with standard diffraction data comparison.SEM (SEM) (Fig. 2) shows, the particle size of nickel microballoon is about 2-5 micron (Fig. 2, a), more SEM (Fig. 2 of high power, b) show, the nickel microsphere surface of synthesis is more coarse, and what have up to 400nm is concavo-convex.
With the result display that VSM magnetometer characterizes synthesized nickel microsphere sample, sample has the saturated magnetization rate of 61.0emu/g, and coercivity H
cjup to 324.4Oe, see Fig. 3.
Application experiment example 1: make electromagnetic wave absorb with nickel microballoon powder, and carry out test experiments
By nickel microballoon powder obtained for embodiment 1 in mass ratio 50% ratio mix with paraffin after be pressed into Both ring sam (D
outward× d
in× h=7 × 3.04 × 1.5mm), relevant parameter μ
rand ε
rrecord with AgilentTechnologiesE8363A electromagnetic wave vector network analyzer, reflection loss is by μ
r, ε
r, absorption frequency and sample thickness determine.The ε recorded
r' reduce gradually with the rising of frequency in 0-18GHz scope, numerical value is at 40.0-18.9.ε
r" within the scope of 6.0-16.0GHz, there is a wide formant, its peak value, at 11.2GHz place, is 8.6.μ
r' reduce gradually with the rising of frequency in 0-18GHz scope, numerical value is at 1.8-0.8.μ
r" numerical value fluctuate between 0.1-0.2.Its absworption peak minimum of a value is-29dB (decibel), and the frequency range that absorptivity is less than-20dB (99% electromagnetic wave is absorbed) is 1.5-4.0GHz, and its electro-magnetic wave absorption curve is shown in Fig. 4.
Embodiment 2:
As described in Example 1, difference substitutes triethanolamine as reducing agent with diethanol amine, and prepare nickel microballoon, SEM (SEM) shows, the Microsphere Size of synthesis is 2-6 micron.
X-ray powder diffraction pattern (XRD) shows that synthesized nickel microballoon is the nickel of face-centred cubic structure, and shows that the nickel purity of synthesizing is very high with standard diffraction data comparison.To the result show sample that synthesized nickel microsphere sample characterizes, there is the saturated magnetization rate of 61.2emu/g and the coercivity (H of 317.6Oe with VSM magnetometer
cj).
Embodiment 3:
As described in Example 1, difference is NiCl
26H
2o: NaOH: polyethylene glycol (PEG): triethanolamine (TEA)=3g:9g:1g:10g, prepare nickel microballoon, SEM (SEM) shows, the Microsphere Size of synthesis is 3-8 micron, and microballoon is better dispersed.
X-ray powder diffraction pattern (XRD) shows that synthesized nickel microballoon is the nickel of face-centred cubic structure, and shows that the nickel purity of synthesizing is very high with standard diffraction data comparison.To the result show sample that synthesized nickel microsphere sample characterizes, there is the saturated magnetization rate of 60.8emu/g and the coercivity (H of 316.4Oe with VSM magnetometer
cj).
Comparative example 1:
As described in Example 1, difference is with nickel acetate (Ni (CH
3cOO)
24H
2o) nickel chloride (NiCl is substituted
26H
2o) as the precursor of nickel, do not add Surfactant PEG, prepare nickel microballoon, SEM (SEM) shows, the nickel Microsphere Size of synthesis is 0.3-1 micron, and microballoon bad dispersibility, part ball is bonded together.
X-ray powder diffraction pattern (XRD) shows that synthesized nickel microballoon is the nickel of face-centred cubic structure, and shows that the nickel purity of synthesizing is very high with standard diffraction data comparison.To the result show sample that synthesized nickel microsphere sample characterizes, there is the saturated magnetization rate of 59.8emu/g and the coercivity (H of 315.5Oe with VSM magnetometer
cj).
Comparative example 2:
As described in Example 1, difference does not add surfactant polyethylene (PEG), prepares nickel microballoon, SEM (SEM) shows, the Microsphere Size of synthesis is 1-1.5 micron, and microballoon bad dispersibility, many microsphere adhesive together.
X-ray powder diffraction pattern (XRD) shows that synthesized nickel microballoon is the nickel of face-centred cubic structure, and shows that the nickel purity of synthesizing is very high with standard diffraction data comparison.
Comparative example 3:
As described in Example 1, difference is the mass ratio 1g:7g:5g:13g that raw starting material adds, and prepares nickel microballoon, SEM (SEM) shows, the Microsphere Size of synthesis is 0.5-1 micron, and microballoon bad dispersibility, many microsphere adhesive together.
X-ray powder diffraction pattern (XRD) shows that synthesized nickel microballoon is the nickel of face-centred cubic structure, and shows that the nickel purity of synthesizing is very high with standard diffraction data comparison.To the result show sample that synthesized nickel microsphere sample characterizes, there is the saturated magnetization rate of 60.8emu/g and the coercivity (H of 301.2Oe with VSM magnetometer
cj).
Application experiment example 2: make electromagnetic wave absorb with nickel microballoon powder, and carry out test experiments
Adopt the nickel microballoon powder that embodiment 1 is obtained, the ratio of 30% is pressed into Both ring sam (D after mixing with paraffin in mass ratio
outward× d
in× h=7 × 3.04 × 1.5mm), relevant parameter μ
rand ε
rrecord with AgilentTechnologiesE8363A electromagnetic wave vector network analyzer, reflection loss is by μ
r, ε
r, absorption frequency and sample thickness determine.The real part ε recorded
r' within the scope of 0-4GHz, be down to 7.5 from 9.6, have two low ebbs in 11.8 and 15.1GHz frequency place thereafter, valley is respectively 7.3 and 6.7.Imaginary part ε
r" there are two formants in 11.2 and 14.2GHz place, peak value is respectively 1.1 and 1.4.μ
r' reduce gradually with the rising of frequency in 0-18GHz scope, numerical value is at 1.4-0.8.μ
r" numerical value fluctuate between 0.03-0.2.Its absworption peak minimum of a value is-18dB (decibel), and the frequency range that absorptivity is less than-10dB (90% electromagnetic wave is absorbed) is 6.0-15.5GHz, and its electro-magnetic wave absorption curve is shown in Fig. 5.Illustrate that the mass ratio of nickel microballoon powder is reduced to 30% thus, its electro-magnetic wave absorption intensity reduces due to the minimizing of nickel microballoon absorbent.
Claims (10)
1. a monodispersed nickel microballoon powder electromagnetic wave absorbent material, the diameter of described nickel microballoon is 2-8 micron, and preferred diameter is 2-5 micron; Described nickel microsphere surface is uneven, height of concave convex≤400nm;
Described monodispersed nickel microballoon powder adopts hydro-thermal method one-step synthesis to obtain.
2. monodispersed nickel microballoon powder electromagnetic wave absorbent material as claimed in claim 1, is characterized in that the saturated magnetization rate of described monodispersed nickel microballoon powder is 61.0 ± 0.5emu/g; Preferably, described monodispersed nickel microballoon powder is at the electro-magnetic wave absorption RL<-20dB of 1.5-4GHz frequency range.
3. the preparation method of the nickel microballoon powder electromagnetic wave absorbent material described in claim 1 or 2, adopts hydro-thermal method, comprises the steps:
With divalent inorganic nickel salt for raw material, one of NaOH, ammoniacal liquor or combination are as precipitating reagent, one of polyethylene glycol (PEG), polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP) or combination are as surfactant, and one of triethanolamine, diethanol amine or combination are as reducing agent;
By above-mentioned divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent in mass ratio (3 ~ 5): (8 ~ 11): (1 ~ 3): (10 ~ 12) are soluble in water, in 100-400 DEG C of reaction 20-80 hour, washing is dry, obtains nickel microballoon powder.
4. the preparation method of nickel microballoon powder electromagnetic wave absorbent material as claimed in claim 3, is characterized in that described divalent inorganic nickel salt is selected from one of nickelous sulfate, nickel chloride, nickel nitrate or combination; Preferably, described divalent inorganic nickel salt is Nickel dichloride hexahydrate.
5. the preparation method of nickel microballoon powder electromagnetic wave absorbent material as claimed in claim 3, is characterized in that the gross mass of described divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent and the mass volume ratio of water are 22 ~ 31:100, unit: g/mL.
6. the preparation method of nickel microballoon powder electromagnetic wave absorbent material as claimed in claim 3, it is characterized in that, the reaction temperature of described reaction is 160-270 DEG C; Preferable reaction temperature is 200-210 DEG C, and the reaction time is 24-50 hour.
7. the preparation method of nickel microballoon powder electromagnetic wave absorbent material as claimed in claim 3, it is characterized in that, the mass ratio of described divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent is (3 ~ 4): (8 ~ 10): (1 ~ 2): (10 ~ 11).
8. the preparation method of nickel microballoon powder electromagnetic wave absorbent material as claimed in claim 3, it is characterized in that, the mass ratio of described divalent inorganic nickel salt, precipitating reagent, surfactant, reducing agent is 3:10:2:10.
9. the preparation method of nickel microballoon powder electromagnetic wave absorbent material as claimed in claim 3, it is characterized in that, step is as follows:
Be raw material with Nickel dichloride hexahydrate, NaOH is as precipitating reagent, polyethylene glycol is as surfactant, and triethanolamine is as reducing agent, and above-mentioned raw materials joins in 100mL water by 3g:10g:2g:10g, in 200 DEG C of reactions 24 hours, washing is dry, obtained monodispersed nickel microballoon, and the diameter of microballoon is 2-5 micron, nickel ball surface is more coarse, and height of concave convex can reach 400nm.
10. the nickel microballoon powder described in claim 1 or 2 as the application of electromagnetic wave absorbent material, it is characterized in that by described nickel microballoon powder in mass ratio 50% ratio mix with paraffin, compressing, the electromagnetic wave absorb made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510795828.5A CN105382252B (en) | 2015-11-18 | 2015-11-18 | A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510795828.5A CN105382252B (en) | 2015-11-18 | 2015-11-18 | A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105382252A true CN105382252A (en) | 2016-03-09 |
| CN105382252B CN105382252B (en) | 2017-12-01 |
Family
ID=55415390
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510795828.5A Active CN105382252B (en) | 2015-11-18 | 2015-11-18 | A kind of monodispersed nickel microballoon powder electromagnetic wave absorbent material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105382252B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109663930A (en) * | 2019-02-12 | 2019-04-23 | 闽江师范高等专科学校 | A kind of pyrophorisity micro-nano metal material and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030201427A1 (en) * | 2001-01-24 | 2003-10-30 | Kaken Tech Co., Ltd. | Conductiv powder and conductive composition |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| JP2009277403A (en) * | 2008-05-13 | 2009-11-26 | Kaken Tec Kk | Conductive powder and conductive composite |
| CN102019427A (en) * | 2010-12-20 | 2011-04-20 | 吴浩 | High-efficiency wave-absorbing particles, wave-absorbing material, and application and preparation method thereof |
| CN102190332A (en) * | 2011-04-01 | 2011-09-21 | 山东大学 | Electromagnetic wave absorbing material of monodisperse nanometer ferriferrous oxide hollow ball-shaped, its preparation method and application |
| CN103586460A (en) * | 2013-11-11 | 2014-02-19 | 山东大学 | Magnetic porous cobalt hollow ball electromagnetic wave absorption material, preparation method and application thereof |
| JP2014231643A (en) * | 2014-07-14 | 2014-12-11 | 住友電気工業株式会社 | Method of producing metal powder, metal powder and conductive paste for laminated ceramic capacitor |
| CN105018029A (en) * | 2014-04-25 | 2015-11-04 | 南京理工大学 | Metallic nickel/graphene composite wave-absorbing material and preparation method thereof |
-
2015
- 2015-11-18 CN CN201510795828.5A patent/CN105382252B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030201427A1 (en) * | 2001-01-24 | 2003-10-30 | Kaken Tech Co., Ltd. | Conductiv powder and conductive composition |
| JP2009277403A (en) * | 2008-05-13 | 2009-11-26 | Kaken Tec Kk | Conductive powder and conductive composite |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN102019427A (en) * | 2010-12-20 | 2011-04-20 | 吴浩 | High-efficiency wave-absorbing particles, wave-absorbing material, and application and preparation method thereof |
| CN102190332A (en) * | 2011-04-01 | 2011-09-21 | 山东大学 | Electromagnetic wave absorbing material of monodisperse nanometer ferriferrous oxide hollow ball-shaped, its preparation method and application |
| CN103586460A (en) * | 2013-11-11 | 2014-02-19 | 山东大学 | Magnetic porous cobalt hollow ball electromagnetic wave absorption material, preparation method and application thereof |
| CN105018029A (en) * | 2014-04-25 | 2015-11-04 | 南京理工大学 | Metallic nickel/graphene composite wave-absorbing material and preparation method thereof |
| JP2014231643A (en) * | 2014-07-14 | 2014-12-11 | 住友電気工業株式会社 | Method of producing metal powder, metal powder and conductive paste for laminated ceramic capacitor |
Non-Patent Citations (2)
| Title |
|---|
| JING KONG ET AL: "Fabrication of monodispersed nickel flower-like architectures via a solvent-thermal process and analysis of their magnetic and electromagnetic properties", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
| 孔静: "磁性材料的制备及电磁波吸收性能研究", 《CNKI中国优秀硕士论文全文数据库（工程科技Ⅰ辑）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109663930A (en) * | 2019-02-12 | 2019-04-23 | 闽江师范高等专科学校 | A kind of pyrophorisity micro-nano metal material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105382252B (en) | 2017-12-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Tyagi et al. | Development of hard/soft ferrite nanocomposite for enhanced microwave absorption | |
| Olad et al. | Electromagnetic interference attenuation and shielding effect of quaternary Epoxy-PPy/Fe3O4-ZnO nanocomposite as a broad band microwave-absorber | |
| CN108154984B (en) | Porous ferroferric oxide/carbon nano rod-shaped electromagnetic wave absorption material and preparation method and application thereof | |
| CN102190332B (en) | Electromagnetic wave absorbing material of monodisperse nanometer ferriferrous oxide hollow ball, its preparation method and application | |
| CN105436498A (en) | Porous nickel-carbon nano-composite microsphere electromagnetic wave absorbing material and preparation method and application thereof | |
| CN111014712B (en) | Co/MnO@C composite electromagnetic wave absorbing material and preparation method and application thereof | |
| CN103586460A (en) | Magnetic porous cobalt hollow ball electromagnetic wave absorption material, preparation method and application thereof | |
| CN108124413B (en) | Porous hollow iron nanometer spherical electromagnetic wave absorbent material and preparation method and application | |
| KR101467993B1 (en) | Graphene―magnetic metal composite for absorbing electromagnetic wave and the preparation method thereof | |
| CN109005660A (en) | Cobalt nano-particle and redox graphene electromagnetic wave absorbent material preparation method | |
| CN109054741B (en) | Preparation method of cobalt-nickel alloy particle/reduced graphene composite material with sandwich structure | |
| CN105268997A (en) | Preparation method for NiFe2O4@alpha-Fe micro nanometer composite material of core-shell structure | |
| Luo et al. | Preparation and excellent electromagnetic absorption properties of dendritic structured Fe3O4@ PANI composites | |
| Tyagi et al. | Synthesis and characterization of microwave absorbing SrFe 12 O 19/ZnFe 2 O 4 nanocomposite | |
| Amiri et al. | Radar absorption of Ni0. 7Zn0. 3Fe2O4 nanoparticles | |
| Tyagi et al. | Reaction kinetic, magnetic and microwave absorption studies of SrFe 11.2 Ni 0.8 O 19 hexaferrite nanoparticles | |
| CN104319050A (en) | Diphasic nanocrystalline high-frequency soft magnetic material and preparation method thereof | |
| Sahu et al. | Enhanced microwave absorbing performance of Sr2+ substituted Nickel-Cobalt nano ferrite for radar and stealth applications | |
| CN109699165B (en) | Three-dimensional porous manganese oxide-cobalt composite electromagnetic wave absorption material and preparation method and application thereof | |
| Kaur et al. | Study of magnetic, elastic and Ka-band absorption properties of Zn1− xCoxFe2O4 (0.00≤ x≤ 1.00) spinel ferrites | |
| CN107541185B (en) | Zinc-doped ferrite/carbon nanotube wave-absorbing material and preparation method thereof | |
| Kıvrak et al. | PANI-coated YIG/CFO hybrid composites as advanced electromagnetic wave absorber through X-band | |
| CN105382252A (en) | Monodispersed nickel microsphere powder electromagnetic wave absorbing material and preparing method thereof | |
| Tyagi et al. | Reaction kinetic, magnetic and microwave absorption studies of SrFe 12 O 19/CoFe 2 O 4 ferrite nanocrystals | |
| CN110340376B (en) | Flower-shaped nickel wire wave-absorbing material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |