CN106270553A - A kind of preparation method of graphene oxide cladding Ni Co alloy particle composite - Google Patents
A kind of preparation method of graphene oxide cladding Ni Co alloy particle composite Download PDFInfo
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- CN106270553A CN106270553A CN201610780137.2A CN201610780137A CN106270553A CN 106270553 A CN106270553 A CN 106270553A CN 201610780137 A CN201610780137 A CN 201610780137A CN 106270553 A CN106270553 A CN 106270553A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
- B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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Abstract
The present invention relates to stealth material field, particularly relate to the preparation method of a kind of graphene oxide cladding Ni Co alloy particle composite.Preparation method of the present invention comprises the following steps: step one, prepares graphene oxide；Step 2, Nickel tetracarbonyl., carbonyl cobalt mixed liquor thermally decompose, and prepare NiCo alloy particle；Step 3, is added dropwise over graphene oxide during thermal decomposition mixed liquor；Step 4, the preparation of graphene coated NiCo alloy powder.The graphene oxide of preparation of the present invention/Ni Co alloy particle composite possesses the features such as pcrmeability is high, temperature stability is good, antioxidation, acid-proof alkaline are excellent, effective absorption wide-band of described composite is 9.5 14.6GHz, when thickness is 1.5mm, obtained the maximum absorption is had to be 16.5dB at 12GHz, significantly improve impedance matching after Fu He, have good assimilation effect.
Description
Technical field
The present invention relates to stealth material field, particularly relate to a kind of graphene oxide cladding Ni-Co alloy particle composite wood
The preparation method of material.
Background technology
Super-fine metal powder in tradition wave absorbing agent has higher pcrmeability, but bad with the impedance matching property of air, and
Absorber Bandwidth is narrower, and density is relatively big, limits it and is inhaling ripple field wider application.Use new material and tradition absorbing material
Carry out being combined, improving the absorbent properties to electromagnetic wave.Graphene is by the Two-dimensional Carbon material of monolayer carbon atom Hexagonal packing,
There is preferable lattice structure and unique electricity, optics, mechanics and thermal property.The Graphene that chemical reduction method prepares
Still having the existence of substantial amounts of defect and functional group, these defects and functional group can strengthen impedance matching property, promote electricity
Sub-energy level is changed into fermi level from continuous state.
Patent application publication No. CN 105295832 A discloses a kind of redox graphene/Ni-Co tri compound and inhales
The preparation method of wave material.With graphite oxide, cobalt salt and nickel salt as presoma, employing hydrazine hydrate is reducing agent, anti-by hydro-thermal
Should, a step prepares redox graphene/Ni-Co tri compound absorbing material.Cobalt nickel binary alloy nano prepared by this invention
Particle is directly loaded on redox graphene by growth in situ, Stability Analysis of Structures, good dispersion, and preparation method is high
Effect, with low cost, the shortest, prepare composite wave-suction material better performances, and can by regulation graphite oxide, cobalt salt and
The additional proportion of nickel salt, the consumption of reducing agent and the thickness of composite realize effective absorption of different-waveband.This invention is adopted
Compound particle, and uncoated Ni-Co alloy particle is prepared by hydro-thermal reaction one step, poor with the impedance matching property of air, lead
Cause to absorb frequency range narrower, limit its range.
Summary of the invention:
Not enough for prior art, the present invention provides a kind of graphene oxide cladding Ni-Co alloy particle composite
Preparation method, it comprises the following steps:
Step one, prepares graphene oxide:
Graphite powder is placed in beaker, adds concentrated nitric acid, concentrated sulphuric acid, adds potassium permanganate, ultrasonic disperse 10min, spend
Ion is washed three times, adds strong aqua ammonia ultrasonic disperse 10min, after centrifuge washing 2 times, adds hydrogenperoxide steam generator ultrasonic
Dispersion 10min, centrifuge washing 2 times, add concentrated hydrochloric acid ultrasonic disperse 10min, wash twice, add dehydrated alcohol ultrasonic
Dispersion 10min, filtering and washing three times, 90-110 DEG C is drying to obtain graphite oxide；By graphite oxide supersound process 1h stripping in water
Completion graphene oxide sheet, obtains stable dispersions, and dropping content is the hydrazine hydrate solution of 80%, stirring, while heated to 100
DEG C, filter after reaction 10h with this understanding and clean, at 60 DEG C, be finally vacuum dried 12h obtain graphene oxide, seal and preserve
Standby；
Step 2, thermally decomposes Nickel tetracarbonyl., carbonyl cobalt mixed liquor, preparation NiCo alloy particle:
Nickel tetracarbonyl. and carbonyl cobalt are mixed, joins the mixed liquor of carrier fluid and surfactant, add 1mL γ-ammonia third
Ethyl triethoxy silicane alkane is as the surface conditioning agent of stuff and other stuff, ultrasonic disperse 0.5h, and evacuation and nitrogen charging operate repeatedly repeatedly,
Oxygen in discharge system, the Nickel tetracarbonyl. being uniformly mixed and carbonyl cobalt mixed solution；
Step 3, is added dropwise over graphene oxide during thermal decomposition mixed liquor:
The Nickel tetracarbonyl. that step 2 is obtained and carbonyl cobalt mixed solution, be added dropwise over the graphene oxide that step one obtains molten
Liquid, control the flow of graphene oxide be each second 3-5 drip, drip while stir, evacuation and nitrogen charging operate repeatedly repeatedly, discharge
Oxygen in system, post-heating；
Step 4, prepares graphene coated NiCo alloy powder:
When temperature rises to 60 DEG C, i.e. it is observed that there is gas slowly to emerge, temperature continues to raise, when temperature rises to 103
DEG C time, temperature do not continue to rise, it may be observed that in tail gas discharger, bubble fierceness is emerged continuously, simultaneously air set pipe
Mouth has the mixed liquor of yellow, and liquid refluxes, it is observed that the backflow ring of gas-liquid interface in condensing tube, now finely tunes heating mantle
Voltage, control backflow ring is at 2/3 height of first condensing tube, and after reacting 3-4 hour at this temperature, system temperature is certainly
Dynamic rising, is no longer having bubble to emerge less than 140 DEG C, and regulation electric furnace voltage makes system temperature rise to 140-150 DEG C, it may be observed that
Again having a large amount of bubble to emerge continuously, when tail gas outlet no longer has bubble to emerge, decomposition reaction completes the most；
Step 5, after mixed liquor thermal decomposition terminates, question response device cools down, and the product in flask is transferred to concentrator bowl and carries out
Centrifugation, is then filtered off unnecessary mixed liquor solvent, is vacuum dried and i.e. obtains described composite.
Further, in step 2, the ratio of the component materials amount of Nickel tetracarbonyl. and carbonyl cobalt is 2:1, the carrier fluid added in advance with
Surfactant volume is than for 50:1.
Further, the addition of graphene oxide in step 3, before thermal decomposition mixed liquor, add graphene oxide molten
Liquid, dropping limit, limit is stirred, until reaction terminates.
Further, described surfactant is amion-terminated polyurethane, and described carrier fluid is isopropanol.
Further, the volume ratio of concentrated sulphuric acid and concentrated nitric acid be the mass ratio of 1:2, graphite powder and potassium permanganate be 2:5.
Further, the mass ratio of graphite oxide and hydrazine hydrate is 1:150.
Compared with prior art, the beneficial effects of the present invention is:
1, preparation method of the present invention is with Graphene as raw material, deposits nano nickel particle, described composite wood on its surface
Effective absorption wide-band of material is 9.5-14.6GHz, when thickness is 1.5mm, has obtained the maximum absorption to be-16.5dB at 12GHz,
Significantly improve impedance matching after Fu He, have good assimilation effect.
2, answer after preparation method of the present invention utilizes coupling agent to process Ni-Co alloy powder and with graphene oxide
Close, form stable Graphene/Ni-Co alloy particle composite by cross-linking reaction, improve the coupling impedance operator of material,
Thus improve its absorbent properties.
3, in preparation method course of reaction of the present invention, graphene oxide is played reduction by iron ion, beneficially shape
Become defect to improve its complex dielectric permittivity, thus improve its impedance matching property.
4, composite of the present invention possesses pcrmeability height, temperature stability is good, antioxidation, acid-proof alkaline are excellent
Feature.
Accompanying drawing explanation
Fig. 1 is the graphene oxide preparation technology figure of preparation method of the present invention；
Fig. 2 is the flow chart of preparation method of the present invention；
Fig. 3 is the transmission of graphene oxide cladding NiCo alloy particle composite prepared by preparation method of the present invention
Electron-microscope scanning figure.
Detailed description of the invention
Embodiment 1
Step one: weigh 3.41g Nickel tetracarbonyl. respectively and 3.42g carbonyl cobalt is dissolved in 50mL isopropanol and the poly-ammonia of 1mL end amido
In the aqueous solution of ester configuration；Add the 1mL gamma-aminopropyl-triethoxy-silane surface conditioning agent as stuff and other stuff, ultrasonic
Dispersion 0.5h, the Nickel tetracarbonyl. being uniformly mixed and carbonyl cobalt mixed solution.
Step 2: weigh 2g graphite powder and be placed in 250mL beaker, adds 10mL concentrated nitric acid, 5mL concentrated sulphuric acid, adds 5g
Potassium permanganate, ultrasonic disperse 10min, it is washed with deionized water three times, adds 5mL strong aqua ammonia ultrasonic disperse 10min, centrifuge washing
After 2 times, add 10mL hydrogenperoxide steam generator ultrasonic disperse 10min, centrifuge washing 2 times, addition 5mL concentrated hydrochloric acid ultrasonic point
Dissipating 10min, wash twice, add 10mL dehydrated alcohol ultrasonic disperse 10min, filtering and washing three times, 90-110 DEG C is dried
I.e. it is prepared into graphite oxide；Taking 0.684g graphite oxide ultrasonic disperse in 6.8mL deionized water, supersound process 1h peels off into oxygen
Functionalized graphene sheet, obtains stable dispersions.Then being moved in there-necked flask by dispersion liquid, dropping 10mL content is 80% hydration
Hydrazine solution by magnetic stirrer, while heated to 100 DEG C, filter after reaction 10h with this understanding and clean, finally 60
Being vacuum dried 12h at DEG C and obtain graphene oxide, sealing saves backup；
Step 3: the graphene oxide solution of preparation utilizes glass reaction container be added dropwise to the mixing of step one molten
In liquid, controlling system temperature and slowly rise, limit dropping limit stirring in course of reaction, the flow controlling graphene oxide is each second
3-5 drips, and slowly controls system temperature and slowly rises, when temperature rises to 60 DEG C, i.e. it is observed that there is gas slowly to emerge, and temperature
Continuing to raise, when temperature rises to 103 DEG C, temperature does not continues to rise, it may be observed that in tail gas discharger, bubble fierceness is even
Emerging, the air setting mouth of pipe has a mixed liquor of yellow simultaneously continuously, liquid refluxes, it is observed that gas-liquid interface in condensing tube
Backflow ring, now finely tunes the voltage of heating mantle, and control backflow ring is at 2/3 height of first condensing tube, the most instead
After answering 3-4 hour, system temperature rises automatically, is no longer having bubble to emerge less than 140 DEG C, and regulation electric furnace voltage makes system temperature
Degree rises to 140-150 DEG C, it may be observed that again have a large amount of bubble to emerge continuously, when tail gas outlet no longer has bubble to emerge
Time, decomposition reaction completes the most；
Step 4: after mixed liquor thermal decomposition terminates, question response device cools down, and the product in flask is transferred to concentrator bowl and carries out
Centrifugation, is then filtered off unnecessary mixed liquor solvent, and it is multiple that vacuum drying obtains graphene oxide cladding NiCo alloy particle
Condensation material.
Graphene oxide cladding NiCo alloy particle composite is carried out electromagnetism test and absorbing property is tested:
Complex dielectric permittivity, compared with traditional oxo iron powder: real part increases to 6.5 from 4；
Coating layer thickness: 1.5mm；
Effectively Absorber Bandwidth (≤-10dB): 5.6-11.90GHz；
Obtained the maximum absorption: 48.64dB；
Graphene with the mass ratio of described composite is: 1:10.
Embodiment 2
Step one: weigh 6.82g Nickel tetracarbonyl. respectively and 6.84g carbonyl cobalt is dissolved in 100mL isopropanol and the poly-ammonia of 2mL end amido
In the aqueous solution of ester configuration, obtain mixed liquor；Add the 1mL gamma-aminopropyl-triethoxy-silane surface as stuff and other stuff
Inorganic agent, ultrasonic disperse 0.5h, the Nickel tetracarbonyl. being uniformly mixed and carbonyl cobalt mixed solution.
Step 2: weigh 4g graphite powder and be placed in 500mL beaker, adds 20mL concentrated nitric acid, 10mL concentrated sulphuric acid, adds
10g potassium permanganate, ultrasonic disperse 20min, it is washed with deionized water three times, adds 10mL strong aqua ammonia ultrasonic disperse 10min, centrifugal
After washing 2 times, add 20mL hydrogenperoxide steam generator ultrasonic disperse 10min, centrifuge washing 2 times, add 10mL concentrated hydrochloric acid also
Ultrasonic disperse 10min, washes twice, and adds 10mL dehydrated alcohol ultrasonic disperse 10min, filtering and washing three times, 90-110
DEG C be dried i.e. be prepared into graphite oxide；Taking 2.05g graphite oxide ultrasonic disperse in 6.8mL deionized water, supersound process 1h is shelled
Completion graphene oxide sheet, obtains stable dispersions.Then dispersion liquid is moved in there-necked flask, drips 30mL hydrazine hydrate
(80%) solution by magnetic stirrer, while heated to 100 DEG C, filter after reaction 10h with this understanding and clean, finally
Being vacuum dried 12h at 60 DEG C and obtain graphene oxide, sealing saves backup；
Step 3: the graphene oxide solution of preparation utilizes glass reaction container be added dropwise to the mixing of step one molten
In liquid, controlling system temperature and slowly rise, limit dropping limit stirring in course of reaction, the flow controlling graphene oxide is each second
3-5 drips, and slowly controls system temperature and slowly rises, when temperature rises to 60 DEG C, i.e. it is observed that there is gas slowly to emerge, and temperature
Continuing to raise, when temperature rises to 103 DEG C, temperature does not continues to rise, it may be observed that in tail gas discharger, bubble fierceness is even
Emerging, the air setting mouth of pipe has a mixed liquor of yellow simultaneously continuously, liquid refluxes, it is observed that gas-liquid interface in condensing tube
Backflow ring, now finely tunes the voltage of heating mantle, and control backflow ring is at 2/3 height of first condensing tube, the most instead
After answering 3-4 hour, system temperature rises automatically, is no longer having bubble to emerge less than 140 DEG C, and regulation electric furnace voltage makes system temperature
Degree rises to 140-150 DEG C, it may be observed that again have a large amount of bubble to emerge continuously, when tail gas outlet no longer has bubble to emerge
Time, decomposition reaction completes the most；
Step 4: after mixed liquor thermal decomposition terminates, question response device cools down, and the product in flask is transferred to concentrator bowl and carries out
Centrifugation, is then filtered off unnecessary mixed liquor solvent, and it is multiple that vacuum drying obtains graphene oxide cladding NiCo alloy particle
Condensation material.
Graphene oxide cladding NiCo alloy particle composite is carried out electromagnetism test and absorbing property is tested:
Complex dielectric permittivity, compared with traditional oxo iron powder: real part increases to 7 from 4；
Coating layer thickness: 1.5mm；
Effectively Absorber Bandwidth (≤-10dB): 4.4-11.98GHz；
Obtained the maximum absorption: 48.64dB.
Graphene with the mass ratio of described composite is: 3:20.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and is not right
The restriction of embodiments of the present invention, for those of ordinary skill in the field, the most also may be used
To make other changes in different forms, cannot all of embodiment be given exhaustive here, every belong to this
What bright technical scheme was extended out obviously changes or changes the row still in protection scope of the present invention.
Claims (6)
1. graphene oxide is coated with a preparation method for Ni-Co alloy particle composite, and it comprises the following steps:
Step one, prepares graphene oxide:
Graphite powder is placed in beaker, adds concentrated nitric acid, concentrated sulphuric acid, adds potassium permanganate, ultrasonic disperse 10min, use deionization
Wash three times, add strong aqua ammonia ultrasonic disperse 10min, after centrifuge washing 2 times, add hydrogenperoxide steam generator ultrasonic disperse
10min, centrifuge washing 2 times, add concentrated hydrochloric acid ultrasonic disperse 10min, wash twice, add dehydrated alcohol ultrasonic disperse
10min, filtering and washing three times, 90-110 DEG C is drying to obtain graphite oxide；Graphite oxide supersound process 1h in water is peeled off into
Graphene oxide sheet, obtains stable dispersions, and dropping content is the hydrazine hydrate solution of 80%, stirring, while heated to 100 DEG C,
Filtering after reaction 10h with this understanding and clean, be finally vacuum dried 12h at 60 DEG C and obtain graphene oxide, sealing preserves standby
With；
Step 2, thermally decomposes Nickel tetracarbonyl., carbonyl cobalt mixed liquor, preparation NiCo alloy particle:
Nickel tetracarbonyl. and carbonyl cobalt are mixed, joins the mixed liquor of carrier fluid and surfactant, add 1mL γ-aminopropyl three
Ethoxysilane is as the surface conditioning agent of stuff and other stuff, ultrasonic disperse 0.5h, and evacuation and nitrogen charging operate repeatedly repeatedly, discharge
Oxygen in system, the Nickel tetracarbonyl. being uniformly mixed and carbonyl cobalt mixed solution；
Step 3, is added dropwise over graphene oxide during thermal decomposition mixed liquor:
The Nickel tetracarbonyl. that step 2 is obtained and carbonyl cobalt mixed solution, be added dropwise over the graphene oxide solution that step one obtains,
Control the flow of graphene oxide be each second 3-5 drip, drip while stir, evacuation and nitrogen charging operate repeatedly repeatedly, discharge body
Oxygen in system, post-heating；
Step 4, prepares graphene coated NiCo alloy powder:
When temperature rises to 60 DEG C, i.e. it is observed that there is gas slowly to emerge, temperature continues to raise, when temperature rises to 103 DEG C,
Temperature does not continues to rise, it may be observed that in tail gas discharger, bubble fierceness is emerged continuously, and the air setting mouth of pipe has simultaneously
The mixed liquor of yellow, liquid refluxes, it is observed that the backflow ring of gas-liquid interface in condensing tube, now finely tunes the electricity of heating mantle
Pressure, control backflow ring is at 2/3 height of first condensing tube, and after reacting 3-4 hour at this temperature, system temperature is automatic
Rising, no longer having bubble to emerge less than 140 DEG C, regulation electric furnace voltage makes system temperature rise to 140-150 DEG C, it may be observed that again
Secondary have a large amount of bubble to emerge continuously, and when tail gas outlet no longer has bubble to emerge, decomposition reaction completes the most；
Step 5, after mixed liquor thermal decomposition terminates, question response device cools down, and the product in flask is transferred to concentrator bowl and is centrifuged
Precipitation, is then filtered off unnecessary mixed liquor solvent, is vacuum dried and i.e. obtains described composite.
Preparation method the most according to claim 1, it is characterised in that the thing mass ratio of Nickel tetracarbonyl. described in step 2 and carbonyl cobalt
For 2:1, the carrier fluid added in advance and surfactant volume are than for 50:1.
The most according to claim 1, preparation method, it is characterised in that the addition of graphene oxide described in step 3, divide in heat
Adding graphene oxide solution before solving mixed liquor, dropping limit, limit is stirred, until reaction terminates.
Preparation method the most according to claim 1, it is characterised in that described surfactant is amion-terminated polyurethane, described
Carrier fluid is isopropanol.
Preparation method the most according to claim 1, it is characterised in that the volume ratio of described concentrated sulphuric acid and concentrated nitric acid is 1:2, stone
The mass ratio of powdered ink and potassium permanganate is 2:5.
Preparation method the most according to claim 1, it is characterised in that the mass ratio of described graphene oxide and hydrazine hydrate is 1:
150。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111615320A (en) * | 2020-06-30 | 2020-09-01 | 福建美庆热传科技有限公司 | Cobalt-nickel-graphene composite wave-absorbing material and preparation method thereof |
| CN114262517A (en) * | 2021-12-28 | 2022-04-01 | 会通新材料股份有限公司 | Nylon composite material and preparation method thereof |
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