CN106270553B - A kind of preparation method of Ni-Co alloy particles cladding graphene oxide composite material - Google Patents
A kind of preparation method of Ni-Co alloy particles cladding graphene oxide composite material Download PDFInfo
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- CN106270553B CN106270553B CN201610780137.2A CN201610780137A CN106270553B CN 106270553 B CN106270553 B CN 106270553B CN 201610780137 A CN201610780137 A CN 201610780137A CN 106270553 B CN106270553 B CN 106270553B
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- 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
- B22F9/30—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
- 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
- B22F1/16—Metallic particles coated with a non-metal
Abstract
The present invention relates to the preparation methods that stealth material field more particularly to a kind of Ni-Co alloy particles coat graphene oxide composite material.Preparation method of the present invention includes the following steps：Step 1 prepares graphene oxide；Step 2, carbonyl nickel, the thermal decomposition of carbonyl cobalt mixed liquor, prepares NiCo alloy particles；Graphene oxide is added dropwise in the process in step 3, thermal decomposition mixed liquor；Step 4, the preparation of graphene coated NiCo alloy powders.The graphene oxide of preparation of the present invention/Ni-Co alloy particle composite materials have the features such as magnetic conductivity is high, temperature stability is good, anti-oxidant, acid-proof alkaline is excellent, effective absorption wide-band of the composite material is 9.5-14.6GHz, when thickness is 1.5mm, it is -16.5dB to have obtained the maximum absorption in 12GHz, impedance matching is significantly improved after compound, there is good assimilation effect.
Description
Technical field
The present invention relates to stealth material fields more particularly to a kind of Ni-Co alloy particles to coat graphene oxide composite wood
The preparation method of material.
Background technology
Super-fine metal powder in traditional wave absorbing agent has higher magnetic conductivity, but bad with the impedance matching property of air, and
Absorber Bandwidth is relatively narrow, and density is larger, limits it and is widely applied in suction wave field.Use new material and traditional absorbing material
Carry out absorbent properties of the compound, improvement to electromagnetic wave.Graphene is the two-dimentional carbon material made of single layer of carbon atom Hexagonal packing,
With ideal lattice structure and unique electricity, optics, mechanics and thermal property.The graphene that chemical reduction method is prepared
Still the presence with a large amount of defect and functional group, these defects and functional group can enhance impedance matching property, promote electricity
Sub- energy level is changed into fermi level from continuous state.
It is multiple that 105295832 A of application for a patent for invention publication No. CN disclose a kind of redox graphene/Ni-Co ternarys
Close the preparation method of absorbing material.Using graphite oxide, cobalt salt and nickel salt as presoma, uses hydrazine hydrate for reducing agent, pass through water
Redox graphene/Ni-Co tri compound absorbing materials are made in thermal response, a step.Cobalt nickel bianry alloy prepared by the invention
Nano-particle is directly loaded in by growth in situ on redox graphene, stable structure, good dispersion, and preparation method
Efficiently, of low cost, short, composite wave-suction material better performances obtained are taken, and can be by adjusting graphite oxide, cobalt salt
With the additional proportion of nickel salt, effective absorption of the dosage of reducing agent and the thickness realization different-waveband of composite material.The invention
Compound particle, and uncoated Ni-Co alloy particles are prepared using one step of hydro-thermal reaction, it is poor with the impedance matching property of air,
Cause absorption frequency range relatively narrow, limits its use scope.
Invention content：
In view of the shortcomings of the prior art, the present invention provides a kind of Ni-Co alloy particles cladding graphene oxide composite material
Preparation method comprising following steps：
Step 1, graphite powder are placed in beaker, and concentrated nitric acid, the concentrated sulfuric acid is added, adds potassium permanganate, ultrasonic disperse
10min is washed with deionized water three times, is added concentrated ammonia liquor and ultrasonic disperse 10min, after centrifuge washing 2 times, adds hydrogen peroxide
Solution and ultrasonic disperse 10min, centrifuge washing 2 times are added concentrated hydrochloric acid and ultrasonic disperse 10min, wash twice, add anhydrous
Ethyl alcohol and ultrasonic disperse 10min, three times, 90-110 DEG C is drying to obtain graphite oxide to filtering and washing；Graphite oxide is surpassed in water
Sonication 1h is peeled off into graphene oxide sheet, obtains stable dispersions, and the hydrazine hydrate solution that content is 80% is added dropwise, stirring, together
When be heated to 100 DEG C, with this condition react 10h after filter cleaning, finally at 60 DEG C be dried in vacuo 12h obtain graphite oxide
Alkene is sealed spare；
Carbonyl nickel and carbonyl cobalt are mixed, are added to the mixed liquor of carrier fluid and surfactant, add 1mL by step 2
Surface conditioning agent of the gamma-aminopropyl-triethoxy-silane as stuff and other stuff, ultrasonic disperse 0.5h are vacuumized and are grasped with nitrogen charging repeatedly
Make repeatedly, the oxygen in discharge system obtains uniformly mixed carbonyl nickel and carbonyl cobalt mixed solution；
The oxidation that step 1 obtains is added dropwise in step 3, the carbonyl nickel that step 2 is obtained and carbonyl cobalt mixed solution
Graphene solution, the flow for controlling graphene oxide are 3-5 drops each second, are stirred in drop, vacuumize and operated with nitrogen charging repeatedly
Repeatedly, the oxygen in discharge system, is heated later；When temperature rises to 60 DEG C, i.e., it is observed that there is gas slowly to emerge, temperature
Continue to increase, when temperature rises to 103 DEG C, temperature does not continue to rise, it may be observed that bubble fierceness connects in tail gas discharger
It emerges continuously, while air setting nozzle has a mixed liquor of yellow, liquid reflux, it is observed that gas-liquid interface in condenser pipe
Backflow ring finely tunes the voltage of heating mantle at this time, and control backflow ring is at 2/3 height of first condenser pipe, at this temperature instead
After answering 3-4 hours, system temperature rises automatically, and less than 140 DEG C, there is no bubbles to emerge, adjusting electric furnace voltage makes system temperature
Degree rises to 140-150 DEG C, it may be observed that has a large amount of bubbles continuously to emerge again, when there is no bubbles to emerge for tail gas outlet
When, decomposition reaction is completed；
Step 4, after mixed liquor thermally decomposes, waits for that reactor cools down, and the product in flask, which is transferred to concentrator bowl, to carry out
Then centrifugation filters out extra mixed liquor solvent, be dried in vacuo up to the composite material.
Further, the ratio of the component materials amount of carbonyl nickel and carbonyl cobalt is 2 in step 2:1, pre-added carrier fluid with
Surfactant volume ratio is 50:1.
Further, in step 3 graphene oxide addition, before thermally decomposing mixed liquor be added graphene oxide it is molten
Liquid is stirred when being added dropwise, until reaction terminates.
Further, the surfactant is amion-terminated polyurethane, and the carrier fluid is isopropanol.
Further, the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 1：2, the mass ratio of graphite powder and potassium permanganate is 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 are：
1, preparation method of the present invention deposits NiCo alloy particles using graphene oxide as raw material on its surface, described
Effective absorption wide-band of composite material be 9.5-14.6GHz, thickness be 1.5mm when, 12GHz have obtained the maximum absorption be-
16.5dB significantly improves impedance matching after compound, there is good assimilation effect.
2, composite material of the present invention has magnetic conductivity is high, temperature stability is good, anti-oxidant, acid-proof alkaline is excellent etc.
Feature.
Description of the drawings
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 that NiCo alloy particles prepared by preparation method of the present invention coat graphene oxide composite material
Electron-microscope scanning figure.
Specific implementation mode
Embodiment 1
Step 1：It weighs 2g graphite powders to be placed in 250mL beakers, 10mL concentrated nitric acids is added, the 5mL concentrated sulfuric acids add 5g
Potassium permanganate, ultrasonic disperse 10min are washed with deionized water three times, 5mL concentrated ammonia liquors and ultrasonic disperse 10min, centrifuge washing are added
After 2 times, 10mL hydrogenperoxide steam generators and ultrasonic disperse 10min are added, 5mL concentrated hydrochloric acids and ultrasound point is added in centrifuge washing 2 times
Dissipate 10min, wash twice, add 10mL absolute ethyl alcohols and ultrasonic disperse 10min, filtering and washing three times, 90-110 DEG C of drying
It is prepared into graphite oxide；It takes 0.684g graphite oxides ultrasonic disperse in 6.8mL deionized waters, is ultrasonically treated 1h and peels off into oxygen
Graphite alkene piece, obtains stable dispersions.Then dispersion liquid is moved into three-necked flask, it is 80% hydration that 10mL contents, which are added dropwise,
Hydrazine solution and with magnetic stirrer, while heated to 100 DEG C, cleaning is filtered after reacting 10h with this condition, finally 60
It is dried in vacuo 12h at DEG C and obtains graphene oxide, is sealed spare；
Step 2：3.41g carbonyl nickels are weighed respectively and 3.42g carbonyl cobalts are dissolved in 50mL isopropanols and the poly- ammonia of the ends 1mL amido
In the aqueous solution of ester configuration；Surface conditioning agent of the 1mL gamma-aminopropyl-triethoxy-silanes as stuff and other stuff is added, ultrasound
Disperse 0.5h, obtains uniformly mixed carbonyl nickel and carbonyl cobalt mixed solution.
Step 3：The mixing that the graphene oxide solution of preparation is added dropwise to step 2 using glass reaction container is molten
In liquid, control system temperature slowly rises, and is stirred in reaction process when being added dropwise, and the flow for controlling graphene oxide is each second
3-5 drops, slow control system temperature slowly rise, when temperature rises to 60 DEG C, i.e., it is observed that there is gas slowly to emerge, and temperature
Continue to increase, when temperature rises to 103 DEG C, temperature does not continue to rise, it may be observed that bubble fierceness connects in tail gas discharger
It emerges continuously, while air setting nozzle has a mixed liquor of yellow, liquid reflux, it is observed that gas-liquid interface in condenser pipe
Backflow ring finely tunes the voltage of heating mantle at this time, and control backflow ring is at 2/3 height of first condenser pipe, at this temperature instead
After answering 3-4 hours, system temperature rises automatically, and less than 140 DEG C, there is no bubbles to emerge, adjusting electric furnace voltage makes system temperature
Degree rises to 140-150 DEG C, it may be observed that has a large amount of bubbles continuously to emerge again, when there is no bubbles to emerge for tail gas outlet
When, decomposition reaction is completed；
Step 4：After mixed liquor thermally decomposes, wait for that reactor cools down, the product in flask, which is transferred to concentrator bowl, to carry out
Then centrifugation filters out extra mixed liquor solvent, it is multiple that vacuum drying obtains NiCo alloy particles cladding graphene oxide
Condensation material.
Electromagnetism test and absorbing property test are carried out to NiCo alloy particles cladding graphene oxide composite material：
Complex dielectric permittivity, compared with traditional oxo iron powder：Real part increases to 6.5 from 4；
Coating layer thickness：1.5mm；
Effective Absorber Bandwidth (≤- 10dB)：5.6-11.90GHz；
Obtained the maximum absorption：48.64dB；
The mass ratio of graphene oxide and the composite material is：1:10.
Embodiment 2
Step 1：It weighs 4g graphite powders to be placed in 500mL beakers, 20mL concentrated nitric acids is added, the 10mL concentrated sulfuric acids add
10g potassium permanganate, ultrasonic disperse 20min are washed with deionized water three times, and 10mL concentrated ammonia liquors and ultrasonic disperse 10min, centrifugation is added
After washing 2 times, 20mL hydrogenperoxide steam generators and ultrasonic disperse 10min are added, 10mL concentrated hydrochloric acids are added simultaneously in centrifuge washing 2 times
Ultrasonic disperse 10min, washes twice, and adds 10mL absolute ethyl alcohols and ultrasonic disperse 10min, filtering and washing three times, 90-110
It is DEG C dry to be prepared into graphite oxide；It takes 2.05g graphite oxides ultrasonic disperse in 6.8mL deionized waters, is ultrasonically treated 1h strippings
Complete graphene oxide sheet, obtains stable dispersions.Then dispersion liquid is moved into three-necked flask, 30mL hydrazine hydrates is added dropwise
(80%) solution and with magnetic stirrer, while heated to 100 DEG C, cleaning is filtered after reacting 10h with this condition, finally
It is dried in vacuo 12h at 60 DEG C and obtains graphene oxide, is sealed spare；
Step 2：6.82g carbonyl nickels are weighed respectively and 6.84g carbonyl cobalts are dissolved in 100mL isopropanols and the poly- ammonia of the ends 2mL amido
In the aqueous solution of ester configuration, mixed liquor is obtained；Add surface of the 1mL gamma-aminopropyl-triethoxy-silanes as stuff and other stuff
Inorganic agent, ultrasonic disperse 0.5h obtain uniformly mixed carbonyl nickel and carbonyl cobalt mixed solution.
Step 3：The mixing that the graphene oxide solution of preparation is added dropwise to step 2 using glass reaction container is molten
In liquid, control system temperature slowly rises, and is stirred in reaction process when being added dropwise, and the flow for controlling graphene oxide is each second
3-5 drops, slow control system temperature slowly rise, when temperature rises to 60 DEG C, i.e., it is observed that there is gas slowly to emerge, and temperature
Continue to increase, when temperature rises to 103 DEG C, temperature does not continue to rise, it may be observed that bubble fierceness connects in tail gas discharger
It emerges continuously, while air setting nozzle has a mixed liquor of yellow, liquid reflux, it is observed that gas-liquid interface in condenser pipe
Backflow ring finely tunes the voltage of heating mantle at this time, and control backflow ring is at 2/3 height of first condenser pipe, at this temperature instead
After answering 3-4 hours, system temperature rises automatically, and less than 140 DEG C, there is no bubbles to emerge, adjusting electric furnace voltage makes system temperature
Degree rises to 140-150 DEG C, it may be observed that has a large amount of bubbles continuously to emerge again, when there is no bubbles to emerge for tail gas outlet
When, decomposition reaction is completed；
Step 4：After mixed liquor thermally decomposes, wait for that reactor cools down, the product in flask, which is transferred to concentrator bowl, to carry out
Then centrifugation filters out extra mixed liquor solvent, it is multiple that vacuum drying obtains NiCo alloy particles cladding graphene oxide
Condensation material.
Electromagnetism test and absorbing property test are carried out to NiCo alloy particles cladding graphene oxide composite material：
Complex dielectric permittivity, compared with traditional oxo iron powder：Real part increases to 7 from 4；
Coating layer thickness：1.5mm；
Effective Absorber Bandwidth (≤- 10dB)：4.4-11.98GHz；
Obtained the maximum absorption：48.64dB.
The mass ratio of graphene oxide and the composite material is：3:20.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (6)
1. a kind of preparation method of Ni-Co alloy particles cladding graphene oxide composite material comprising following steps：
Step 1 graphite powder is placed in beaker, and concentrated nitric acid, the concentrated sulfuric acid is added, and adds potassium permanganate, and ultrasonic disperse 10min is used
Deionization is washed three times, is added concentrated ammonia liquor and ultrasonic disperse 10min, after centrifuge washing 2 times, is added hydrogenperoxide steam generator and is surpassed
Sound disperses 10min, and centrifuge washing 2 times is added concentrated hydrochloric acid and ultrasonic disperse 10min, washes twice, add absolute ethyl alcohol and surpass
Sound disperses 10min, and three times, 90-110 DEG C is drying to obtain graphite oxide to filtering and washing；Graphite oxide is ultrasonically treated 1h in water
Graphene oxide sheet is peeled off into, stable dispersions are obtained, the hydrazine hydrate solution that content is 80% is added dropwise, stirring, while heated to
100 DEG C, cleaning is filtered after reacting 10h with this condition, 12h is finally dried in vacuo at 60 DEG C obtains graphene oxide, seals
It saves backup；
Carbonyl nickel and carbonyl cobalt are mixed, are added to the mixed liquor of carrier fluid and surfactant, add 1mL γ-ammonia by step 2
Surface conditioning agent of the propyl-triethoxysilicane as stuff and other stuff, ultrasonic disperse 0.5h are vacuumized more with nitrogen charging operation repeatedly
Secondary, the oxygen in discharge system obtains uniformly mixed carbonyl nickel and carbonyl cobalt mixed solution；
The graphite oxide that step 1 obtains is added dropwise in step 3, the carbonyl nickel that step 2 is obtained and carbonyl cobalt mixed solution
Alkene solution, the flow for controlling graphene oxide are 3-5 drops each second, are stirred in drop, are vacuumized repeatedly with nitrogen charging operation repeatedly,
Oxygen in discharge system, is heated later；When temperature rises to 60 DEG C, i.e., it is observed that there is gas slowly to emerge, temperature continues
It increases, when temperature rises to 103 DEG C, temperature does not continue to rise, it may be observed that bubble fierceness is continuously in tail gas discharger
It emerges, while air setting nozzle has the mixed liquor of yellow, liquid reflux, it is observed that the reflux of gas-liquid interface in condenser pipe
Ring, finely tunes the voltage of heating mantle at this time, and control backflow ring reacts 3-4 at this temperature at 2/3 height of first condenser pipe
After hour, system temperature rises automatically, and less than 140 DEG C, there is no bubbles to emerge, adjusting electric furnace voltage makes system temperature liter
To 140-150 DEG C, it may be observed that there are a large amount of bubbles continuously to emerge again, when tail gas outlet is emerged there is no bubble, point
Solution reaction is completed；
Step 4 after mixed liquor thermally decomposes, waits for that reactor cools down, the product in flask is transferred to concentrator bowl and is centrifuged
Precipitation, then filters out extra mixed liquor solvent, is dried in vacuo up to the composite material.
2. preparation method according to claim 1, which is characterized in that the amount of substance ratio of carbonyl nickel and carbonyl cobalt described in step 2
It is 2:1, pre-added carrier fluid is 50 with surfactant volume ratio:1.
3. preparation method according to claim 1, which is characterized in that the addition of graphene oxide described in step 3, in heat point
Graphene oxide solution is added before solution mixed liquor, is stirred when being added dropwise, until decomposition reaction terminates.
4. preparation method according to claim 1, which is characterized in that the surfactant is amion-terminated polyurethane, described
Carrier fluid is isopropanol.
5. preparation method according to claim 1, which is characterized in that the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 1：2, stone
The mass ratio of ink powder and potassium permanganate is 2：5.
6. preparation method according to claim 1, which is characterized in that the mass ratio of the graphene oxide and hydrazine hydrate is 1：
150。
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| 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 |
| CN114262517B (en) * | 2021-12-28 | 2023-05-23 | 会通新材料股份有限公司 | Nylon composite material and preparation method thereof |
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| CN105295832A (en) * | 2014-07-25 | 2016-02-03 | 南京理工大学 | Preparation method for reduced graphene oxide/Ni-Co ternary composite wave-absorbing material |
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| CN101992303A (en) * | 2010-10-29 | 2011-03-30 | 江苏大学 | Method for preparing graphene/Ni nano composite material |
| JP2013091824A (en) * | 2011-10-25 | 2013-05-16 | Kri Inc | Carbon composite metal particulate and method for producing the same |
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