CN107338024A - A kind of Co Fe alloys/carbon ball composite microwave absorbent and preparation method thereof - Google Patents
A kind of Co Fe alloys/carbon ball composite microwave absorbent and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Co Fe alloys/carbon ball composite microwave absorbent and preparation method thereof,It is using carbon ball as core,The outside of the carbon ball is coated by Co Fe alloying pellets,The outside of the Co Fe alloying pellets is coated with one layer of graphite again,Multistage core shell structure is integrally formed,The preparation method of above-mentioned composite microwave absorbent is to be prepared into the polysaccharide microsphere being not exclusively carbonized with glucose and dispersant first,Afterwards with the mixed solution of cobalt ions and iron ion dipping polysaccharide microsphere,Finally gained mixture is placed under inert atmosphere high temperature and is heat-treated,So that the graphitization of carbon ball and the reduction of metal ion are carried out simultaneously,Gained composite microwave absorbent combines the advantages of carbon material and magnetic metal powder,The characteristics of while with good microwave absorbing property with lightweight,It can be widely applied for various environment and field.
Description
Technical field
The present invention relates to a kind of microwave absorption and preparation method thereof, more particularly to a kind of answering with multistage core shell structure
Close microwave absorption and preparation method thereof.
Background technology
With the rapid development of electronics industry, various electronic equipments become more popular.Promote industrial production change,
While improving our living conditions, electromagnetic wave can also pollute to environment as caused by electronic equipment.It is not only possible
The normal operation of other electronic equipments can be disturbed, goes back entail dangers to health.Electromagnetic wave has become after waste gas, waste residue, waste water
With the another pollution sources of environment for human survival after noise.Although electromagnetic wave is not seen, can not touch, can't smell, but nowhere not
When its frequency is more than 105Hz with regard to harmful.On the other hand, militarily, stealth technology is Future Information war
In important technological means.Radar wave absorbing stealth material can consume radar by itself absorption to electromagnetic wave
The portion of energy of ripple so that the echo of reflection is imperfect, so that target is not easy to be detected.
Radar absorbing is mainly made up of absorbent and macromolecule matrix material at present, wherein determining the pass of absorbing property
Key is the species and content of absorbent.It is different according to the principle of absorption of absorbent, it is commonly divided into dielectric loss type and magnetic loss type
Two major classes.The conventional wave absorbing agent of dielectric loss type absorbing material has conductive black, graphite, carbon fiber, carborundum, barium titanate ferroelectricity pottery
Porcelain, conducting polymer etc., carry out electromagnetic wave absorption by the electronic polarization of medium, ionic polarization, interfacial polarization decay.Dielectric loss type
The advantages of absorbing material is that density is small, and shortcoming is that absorption band is narrower, and absorbability is relatively weak.Magnetic loss type absorbing material
Conventional wave absorbing agent has ferrite, super-fine metal powder, carbonyl iron dust etc..They mainly pass through magnetic hystersis loss, natural resonance, farmland
The mechanism such as wall resonance are come electromagnetic wave absorption of decaying.Magnetic loss type absorbing material absorbability is strong, absorption band is wide, but exists close
Spend the shortcomings that big.The shortcomings that existing due to each of which, single magnetic loss type or dielectric loss type absorbent can not be complete
Meet the requirement of application.Both Dominant Facies are combined, develop lightweight, efficient NEW TYPE OF COMPOSITE absorbent is weight in recent years
Want research direction.
In order to realize to obtain lightweight, the target of efficient NEW TYPE OF COMPOSITE absorbent, based on graphite, CNT, bear
The carbon material modification of load magnetic metal or alloy becomes the important topic in terms of microwave absorbing material research.It is common
Method is first to prepare carbon material, then passes through the side such as mechanical mixture, sputtering method, pyrolysismethod, electroless plating method, co-precipitation and reduction
Method is in carbon material surface carried metal particle.But carbon material is the absence of defect as CNT, graphite powder etc surface
And dangling bonds, C -- C single bond is also very stable chemical bond, thus is difficult to be infiltrated by metal or compound, passes through physics
Absorption, sputtering or pyrolysis fill superincumbent metallic and are typically easy to skewness, oversized.Chinese patent
CN105820796A discloses the preparation method of the composite wave-suction material using porous carbon ball load magnetic alloy, and it utilizes porous
The precursor solution of magnetic metal is incorporated into the hole of carbon ball by the high-specific surface area of carbon ball and strong suction-operated by capillarity
Inside road, combined afterwards with hydrophily oxygen-containing functional group, but as it was previously stated, the surface of porous carbon ball is the absence of defect and dangling bonds
, due to porous carbon ball carbonization, the hydrophilic functional group on its surface is considerably less, it is difficult to and magnetic metal ion
Form chemical action or bonding, thus absorbing material its surface magnetism alloy particle skewness obtained by this method,
The binding capacity of magnetic alloy particle is very limited, and oversized, thus absorbing property is greatly affected, in addition, the gold on carbon ball surface
Category particle surface lacks protection, is easily oxidized, and absorbing material often uses in some conditions more harsh environment, and this is just
It greatly limit the application of material.
The content of the invention
The present invention is for deficiency existing for above-mentioned existing composite wave-suction material and preparation method thereof, there is provided a kind of Co-Fe is closed
Gold/carbon ball composite microwave absorbent and preparation method thereof.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of Co-Fe alloys/carbon ball composite microwave absorbent, using carbon ball as core, the outside of the carbon ball is closed by Co-Fe for it
Gold grain is coated, and the outside of the Co-Fe alloying pellets is coated with one layer of graphite again, and multistage core shell structure is integrally formed.
Further, a diameter of 1~10 μm of the carbon ball, the particle size of the Co-Fe alloying pellets is 20~80nm.
Further, the mass fraction of Co-Fe alloying pellets is 10~20%.
The beneficial effect of composite microwave absorbent provided by the invention is：
1) on the one hand the graphite linings on surface can protect ferro-cobalt particle not oxidized in use；On the other hand
Also ferro-cobalt particle agglomeration can be prevented to grow up, due to the refinement of metallic, activity greatly increases, and microwave absorbing property obtains
To raising；
2) ferro-cobalt particle is uniform in carbon ball surface distributed, and just the carbon ball activity of carbonization is completed very in heat-treatment process
Height, easily forms villous CNT under the catalysis of ferro-cobalt on carbon ball surface, and absorbing property obtains further
Raising；
3) composite wave-absorbing agent provided by the invention combines the advantages of carbon material and magnetic metal powder, has good microwave
There is the characteristics of lightweight while absorbent properties, can be widely applied for various environment and field.
The preparation method of above-mentioned Co-Fe alloys/carbon ball composite microwave absorbent, including following step is also claimed in the present invention
Suddenly：
1) polysaccharide microsphere is prepared：Weigh glucose and dispersant is dissolved in deionized water, be sufficiently stirred, treat that it is completely molten
Solution is poured into reactor after solution, reactor is placed under the conditions of 180~200 DEG C and reacted, wherein, glucose and dispersant
Dissolving is without sequencing, and the concentration for controlling glucose in solutions is 6~10wt%, and the concentration of dispersant is 2~2.5g/L, will be anti-
Should after reactor in mixture be cooled to room temperature, filtering and washing obtains sediment, dry polysaccharide microsphere；
2) alkali process：The polysaccharide microsphere of gained in step 1) is placed in 0.1~1.0mol/L inorganic alkali solution, in
Constant temperature stirs under the conditions of 40~80 DEG C, filtering and washing, dry alkali-treated polysaccharide microsphere；
3) Co, Fe are impregnated:Soluble cobalt and the mixed solution of soluble ferric iron salt obtained cobalt soluble in water and iron are weighed, its
In, the concentration for controlling cobalt ions is 0.2~0.3mol/L, and the amount of iron ion is every gram of carbon ball 1.4~3.0 × 10-3Mol, it will walk
It is rapid 2) obtained by alkali-treated polysaccharide microsphere ultrasonic disperse in the cobalt of gained and the mixed solution of iron, control final absorption
On cobalt ions and iron ion mol ratio be 1:2, stirring dipping is rear to filter, wash, drying；
4) it is heat-treated：Step 3) products therefrom is placed in inert atmosphere and is heat-treated in 900~1200 DEG C, it is rear natural
Cooling, produces Co-Fe alloys/carbon ball composite microwave absorbent.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Further, the dispersant is cetyl trimethylammonium bromide, lauryl sodium sulfate, DBSA
Any one in sodium.
Further, inorganic base described in step 2) is appointing in potassium hydroxide, sodium hydroxide, ammonium hydroxide, barium hydroxide
The compounding for one or more of anticipating.
Further, the soluble ferric iron salt described in step 3) refers to Iron(III) chloride hexahydrate, ferric sulfate, ferric nitrate, oxalic acid
Any one in iron, frerrous chloride, ferrous sulfate, ferrous oxalate, described soluble cobalt refer to cobalt chloride, cobaltous sulfate,
Any one in cobalt nitrate.
Further, the time of reaction is 4~8h in step 1).
Further, the time that constant temperature stirs in step 2) is 12~18h.
Further, the time of stirring dipping is 12~24h in step 3), and the time being heat-treated in step 4) is 1~4h.
The superiority of preparation method provided by the invention is embodied in：
1) the carbon containing polysaccharide microsphere that method of the invention could be used without carbonization is template, in this polysaccharide microsphere
Surface have abundant hydroxyl, by alkali leaching processing after, make the hydroxyl quantity on its surface further increase, it is thus possible to
By chemisorbed combination magnetic metal ion, the positive charge phase of the electron cloud and magnetic metal ion on oxygen atom surface in hydroxyl
Mutually attract to form chemical bonding, compared with physical absorption, adsorption process is simple, and the amount of metal ion of absorption is big, and thisization
It is well-proportioned to learn absorption and combine；
2) method of the invention is combined the carbonisation of carbon ball together with the reduction process of metal ion, in Re Chu
During reason, the graphitization of polysaccharide microsphere and the reduction of metal ion are carried out simultaneously, and ferro-cobalt is coated on after carbon ball graphitization
The surface of alloying pellet, ferro-cobalt particle can be protected using process by being on the one hand coated on the graphite linings on ferro-cobalt surface
In it is not oxidized；On the other hand also ferro-cobalt particle agglomeration can be prevented to grow up, due to the refinement of metallic, activity is significantly
Increase, under microwave radiation, atom, electron motion aggravation, it can promote to magnetize, ferromagnetic ultrafine metallic micropowder has larger
Magnetic conductivity, there is strong interaction with frequency electromagnetic waves, it is possible to increase microwave absorbing property.
3) during being heat-treated under an inert atmosphere, the carbon ball activity for just completing to be carbonized is very high, in urging for ferro-cobalt
Villous CNT is easily formed under change on carbon ball surface, improves absorbing property.
The TG-DSC curves (see Fig. 4) of products obtained therefrom and heat treatment after dipping cobalt, iron before our combination heat treatments below
TEM the and SEM pictures (Fig. 3) of front and rear product, describe the chemical change occurred in heat treatment process in detail, below 200 DEG C,
Free water, constitution water in sample gradually lose, and weight loss 8.9%, show as absorbing heat in this stage；At 200~700 DEG C
In the range of, the cobalt and iron that are coated on outside carbon ball are gradually reduced, and discharge CO2Weight is drastically reduced, and reduction process is constantly put
Heat, it is not that apparent exothermic peak, in this process cobalt and iron form alloy to also have one in the range of 500~600 DEG C；
After temperature is more than 700 DEG C, carbon ball graphitization, there is obvious exothermic peak.Characterized with reference to SEM and TEM pictures, in whole process
Because metal ion is got on by chemical action absorption, thus it is tightly combined with carbon material, and just completes the carbon materials of carbonization
Material activity is very high, is easily infiltrated with metal, so ferro-cobalt particle surface can be coated on after carbon ball graphitization, and in cobalt
CNT easily is formed on carbon ball surface under the catalysis of ferroalloy, absorbing property is improved, is coated on so as to form graphite linings
The C@CoFe capsule structures on alloying pellet surface, and these Caplets are coated on carbon ball surface, so as to form C/ (C@
CoFe multistage core shell structure).
The beneficial effect of preparation method of the present invention is：
1) polysaccharide microsphere surface is made full use of to be rich in the characteristic of hydroxyl so that polysaccharide microsphere and magnetic metal ion shape
Into chemisorbed and bonding so that the amount of metal ion that polysaccharide microsphere surface combines is big, is firmly combined with, and is evenly distributed, energy
Enough improve the absorbent properties of microwave；
2) method of the invention causes the graphitization of polysaccharide microsphere and the reduction of metal ion while carried out, carbon ball surface
Graphite on the one hand play a part of protecting against oxidation to metal ion, on the other hand can also prevent ferro-cobalt cluster of grains
Poly- to grow up, the refinement of metal ion substantially increases microwave absorbing property；
3) it is very high that the carbon ball activity of carbonization is just completed in heat treatment process, easily in carbon ball table under the catalysis of ferro-cobalt
Face forms villous CNT, further improves absorbing property.
4) with lightweight while the composite wave-absorbing agent that the inventive method is prepared is with good microwave absorbing property
The characteristics of, it can be widely applied for various environment and field.
Brief description of the drawings
Fig. 1 is the XRD spectra of the gained composite wave-absorbing agent of the embodiment of the present invention 1；
Fig. 2 is the TG-DSC curves of the step 3) products obtained therefrom of embodiment 1；
Fig. 3 is TEM the and SEM pictures that embodiment 1 is heat-treated front and rear product；
Fig. 4 is the gained composite wave-absorbing agent of the embodiment of the present invention 1 and the reflection loss figure of carbon ball obtained by step 1).
In Fig. 3, the overall SEM image of microwave absorption after (a) heat treatment；(b) clad before argon gas atmosphere heat treatment
TEM image；(c) TEM image of clad after being heat-treated；(d) the CoFe particle TEM images of final gained graphite linings cladding；(e)
The CoFe particle high-resolution TEM images of final gained graphite linings cladding；(f) the carbon pipe that final products obtained therefrom surface departs from.
Embodiment
The principle and feature of the present invention are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
Embodiment 1：
A kind of preparation method of Co-Fe alloys/carbon ball composite microwave absorbent, comprises the following steps：
1) 36g glucose is weighed, 0.9g cetyl trimethylammonium bromides (CTAB), is added in 380ml deionized waters,
It is sufficiently stirred, waits to be fitted into 500ml reactor after being completely dissolved, is put into 180 DEG C of insulation 5h in baking oven.After to be cooled,
Filtering and washing, first with twice of deionized water supersound washing, then with twice of alcohol supersound washing, it is finally putting into 60 DEG C of baking oven
12h is to drying to obtain polysaccharide microsphere；
2) polysaccharide microsphere obtained by 1g steps 1) is weighed, 22.44g KOH, which are added, is made aqueous slkali in 400ml water, will be more
Glycan microballoon is immersed in aqueous slkali, after 80 DEG C of constant temperature stirring 12h, filtering and washing, is placed in 80 DEG C of baking oven and is dried；
3) 11.90g CoCl are taken2·6H2O, 0.45g FeCl3·6H2O is dissolved in 200ml deionized waters, by step 2) institute
Alkali process after polysaccharide microsphere ultrasonic disperse to the iron chloride of gained, cobalt chloride mixed solution in, stirring dipping
24h, the mol ratio of the final cobalt ions adsorbed and iron ion is 1:2, most filter, wash, dry afterwards；
4) sample after dipping cladding obtained by step 3) is loaded into porcelain boat, be heat-treated under an argon atmosphere, is heat-treated
Heating schedule it is as follows：50 DEG C are warming up to 900 DEG C by 180min, are incubated 240min, cool to 500 by 100min afterwards
DEG C, afterwards with stove natural cooling, the mass fraction for producing Co-Fe alloying pellets is 12% Co-Fe alloys/carbon ball composite microwave
Absorbent.
We are in order to disclose crystal structure, microscopic appearance and the heat treatment process of composite microwave absorbent obtained by the present invention
Middle change occurred, we have carried out XRD, TG-DSC and TEM to the gained composite microwave absorbent of embodiment 1, SEM is surveyed
Examination, as a result respectively as shown in Figure 1, 2, 3.
From figure 1 it appears that the wave absorbing agent of the gained of embodiment 1 is provided with the feature diffraction of graphite and ferro-cobalt simultaneously
Peak, cobalt, the iron ion for illustrating to coat after calcining are reduced, and form ferro-cobalt；Carbon containing polysaccharide microsphere graphitization to a certain degree,
A certain degree of crystallization is changed into by unformed shape.Wherein, the major parameter in XRD test process is set as follows：Scanning angle
10~90 degree, the degree per second of sweep speed 0.1.
From figure 2 it can be seen that when temperature is 200 DEG C, sample weightlessness is up to 8.9%, Free water, knot predominantly in sample
Structure water is gradually lost, and now shows as absorbing heat, and in the range of 200~700 DEG C, the cobalt and iron that are coated on outside carbon ball are gradually gone back
Original, discharge CO2Weight is drastically reduced, the continuous heat release of reduction process, and it is not very bright to also have one in the range of 500~600 DEG C
Aobvious exothermic peak, in this process cobalt and iron form alloy, sample weightlessness is up to 36.7% in the stage；In temperature more than 700
After DEG C, carbon ball graphitization, there is obvious exothermic peak, more than 700 DEG C after sample weightlessness 3.9%.
From figure 3, it can be seen that after Overheating Treatment, the surface of carbon ball forms Co-Fe alloying pellets, alloying pellet
Size is 20~80nm, and it is uniform in the surface distributed of carbon ball, and the guarantor of graphite linings is separately formd on the surface of Co-Fe alloying pellets
Sheath, while CNT is yet forms both on the outside of Co-Fe alloying pellets, it is favorably improved the absorbing property of wave absorbing agent.
In order to verify the absorbing property of composite wave-absorbing agent obtained by the present invention, we will inhale made from 40wt% embodiment 1
Ripple agent mixes with paraffin, is pressed into external diameter 7mm afterwards, is carried out after internal diameter 3mm annular sample using vector network analyzer
Test, in order to better illustrate the wave-absorbing effect of composite wave-absorbing agent, we are by the polysaccharide microsphere of the step 1) of embodiment 1 without alkali
Products obtained therefrom has carried out vector network using same method as a comparison case after processing and metal impregnation are directly heat-treated
The test of analyzer.Wherein, 1~18GHz of test scope of vector network analyzer, figure 4, it is seen that embodiment 1
The minimum decibel reflectivity of composite wave-absorbing agent has reached -16dB, RL<- 10dB bandwidth has 2GHz (7.6~9.6GHz).
Embodiment 2：
A kind of preparation method of Co-Fe alloys/carbon ball composite microwave absorbent, comprises the following steps：
1) 30g glucose is weighed, 0.94g lauryl sodium sulfate, is added in 470ml deionized waters, is sufficiently stirred, treat
It is fitted into after being completely dissolved in 600ml reactor, is put into 200 DEG C of insulation 1h in baking oven.After to be cooled, filtering and washing, first
With twice of deionized water supersound washing, then with twice of alcohol supersound washing, 12h is finally putting into 60 DEG C of baking oven to drying
Polysaccharide microsphere；
2) polysaccharide microsphere obtained by 1g steps 1), 8.57g Ba (OH) are weighed2Add and aqueous slkali be made in 500ml water,
Polysaccharide microsphere is immersed in aqueous slkali, after 40 DEG C of constant temperature stirring 18h, filtering and washing, is placed in 80 DEG C of baking oven and dries；
3) 11.25g CoSO are taken4˙7H2O, 0.25g Fe (NO3)3It is dissolved in 200ml deionized waters, by step
2) polysaccharide microsphere ultrasonic disperse after the alkali process obtained by is to the cobaltous sulfate of gained, the mixed solution of ferric nitrate
In, stirring dipping 24h, the mol ratio of the final cobalt ions adsorbed and iron ion is 1:2, filter, wash, dry afterwards；
4) sample after dipping cladding obtained by step 3) is loaded into porcelain boat, be heat-treated under an argon atmosphere, is heat-treated
Heating schedule it is as follows：50 DEG C are warming up to 1100 DEG C by 250min, are incubated 120min, cool to 500 by 100min afterwards
DEG C, afterwards with stove natural cooling, the mass fraction for producing Co-Fe alloying pellets is 10% Co-Fe alloys/carbon ball composite microwave
Absorbent.
Embodiment 3：
A kind of preparation method of Co-Fe alloys/carbon ball composite microwave absorbent, comprises the following steps：
1) 33g glucose is weighed, 0.6g cetyl trimethylammonium bromides (CTAB), is added in 300ml deionized waters,
It is sufficiently stirred, waits to be fitted into 500ml reactor after being completely dissolved, is put into 180 DEG C of insulation 3h in baking oven.After to be cooled,
Filtering and washing, first with twice of deionized water supersound washing, then with twice of alcohol supersound washing, it is finally putting into 60 DEG C of baking oven
12h is to drying to obtain polysaccharide microsphere；
2) polysaccharide microsphere obtained by 1g steps 1), 14gNH are weighed4OH, which is added, is made aqueous slkali in 400ml water, by carbon ball
It is immersed in aqueous slkali, after 60 DEG C of constant temperature stirring 14h, filtering and washing, is placed in 80 DEG C of baking oven and dries；
3) 17.46g Co (NO are taken3)2·6H2O, 0.69g FeSO4·7H2O is dissolved in 200ml deionized waters, by step 2)
Polysaccharide microsphere ultrasonic disperse after the alkali process of gained to the cobalt nitrate of gained, ferrous sulfate mixed solution in, stirring leaching
Stain 24h, the mol ratio of the final cobalt ions adsorbed and iron ion is 1:2, filter, wash, dry afterwards；
4) sample after dipping cladding obtained by step 3) is loaded into porcelain boat, be heat-treated under an argon atmosphere, is heat-treated
Heating schedule it is as follows：50 DEG C are warming up to 1200 DEG C by 250min, are incubated 60min, cool to 500 by 100min afterwards
DEG C, afterwards with stove natural cooling, Co-Fe alloys/carbon ball that the mass fraction for producing Co-Fe alloying pellets is 17.5% is compound micro-
Wave absorbent.
Embodiment 4：
A kind of preparation method of Co-Fe alloys/carbon ball composite microwave absorbent, comprises the following steps：
1) 36g glucose is weighed, 0.95g neopelexes, is added in 380ml deionized waters, is sufficiently stirred,
Wait to be fitted into 500ml reactor after being completely dissolved, be put into 180 DEG C of insulation 5h in baking oven.After to be cooled, filtering and washing,
First with twice of deionized water supersound washing, then with twice of alcohol supersound washing, 12h is finally putting into 60 DEG C of baking oven to drying
Obtain polysaccharide microsphere；
2) polysaccharide microsphere obtained by 1g steps 1) is weighed, 10g NaOH, which are added, is made aqueous slkali in 500ml water, by poly
Sugared microballoon is immersed in aqueous slkali, after 80 DEG C of constant temperature stirring 12h, filtering and washing, is placed in 80 DEG C of baking oven and is dried；
3) 11.90g CoCl are taken2·6H2O, 0.38g FeCl2·4H2O is dissolved in 200ml deionized waters, by step 2) institute
Alkali process after polysaccharide microsphere ultrasonic disperse to the frerrous chloride of gained, cobalt chloride mixed solution in, stirring dipping
24h, filter, wash, dry afterwards；
4) sample after dipping cladding obtained by step 3) is loaded into porcelain boat, be heat-treated under an argon atmosphere, is heat-treated
Heating schedule it is as follows：50 DEG C are warming up to 1100 DEG C by 220min, are incubated 120min, cool to 500 by 100min afterwards
DEG C, afterwards with stove natural cooling, the mass fraction for producing Co-Fe alloying pellets is 20% Co-Fe alloys/carbon ball composite microwave
Absorbent.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (10)
1. a kind of Co-Fe alloys/carbon ball composite microwave absorbent, it is characterised in that it is using carbon ball as core, the outside of the carbon ball
Coated by Co-Fe alloying pellets, the outside of the Co-Fe alloying pellets is coated with one layer of graphite again, and multistage core is integrally formed
Shell structure.
2. composite microwave absorbent according to claim 1, it is characterised in that a diameter of 1~10 μm of the carbon ball, institute
The particle size for stating Co-Fe alloying pellets is 20~80nm.
3. composite microwave absorbent according to claim 2, it is characterised in that the mass fraction of Co-Fe alloying pellets is
10~20%.
4. the preparation method of the composite microwave absorbent any one of a kind of claim 1-3, it is characterised in that including such as
Lower step：
1) polysaccharide microsphere is prepared：Weigh glucose and dispersant is dissolved in deionized water, be sufficiently stirred, after it is completely dissolved
Solution is poured into reactor, reactor is placed under the conditions of 180~200 DEG C and reacted, wherein, the dissolving of glucose and dispersant
Without sequencing, the concentration for controlling glucose in solutions is 6~10wt%, and the addition of dispersant is 2~2.5g/L, will be reacted
After reactor in mixture be cooled to room temperature, filtering and washing obtains sediment, dry polysaccharide microsphere；
2) alkali process：The polysaccharide microsphere of gained in step 1) is placed in 0.1~1.0mol/L inorganic alkali solution, in 40~
Constant temperature stirs under the conditions of 80 DEG C, filtering and washing, dry alkali-treated polysaccharide microsphere；
3) Co, Fe are impregnated:Soluble cobalt and the mixed solution of soluble ferric iron salt obtained cobalt soluble in water and iron are weighed, wherein,
The concentration for controlling cobalt ions is 0.2~0.3mol/L, and the amount of iron ion is every gram of carbon ball 1.4~3.0 × 10-3Mol, by step 2)
The alkali-treated polysaccharide microsphere ultrasonic disperse of gained is controlled in final absorption in the cobalt of gained and the mixed solution of iron
The mol ratio of cobalt ions and iron ion is 1：2, stirring dipping is rear to filter, wash, drying；
4) it is heat-treated：Step 3) products therefrom is placed in inert atmosphere and is heat-treated in 900~1200 DEG C, it is rear naturally cold
But, Co-Fe alloys/carbon ball composite microwave absorbent is produced.
5. preparation method according to claim 4, it is characterised in that the dispersant is cetyl trimethyl bromination
Any one of ammonium, lauryl sodium sulfate, neopelex.
6. the preparation method according to 4 or 5 are required in power, it is characterised in that inorganic base described in step 2) be potassium hydroxide,
The compounding of any one or more in sodium hydroxide, ammonium hydroxide, barium hydroxide.
7. preparation method according to claim 6, it is characterised in that the soluble ferric iron salt described in step 3) refers to six water
Any one in ferric trichloride, ferric sulfate, ferric nitrate, ferric oxalate, frerrous chloride, ferrous sulfate, ferrous oxalate is closed, it is described
Soluble cobalt refers to any one in cobalt chloride, cobaltous sulfate, cobalt nitrate.
8. preparation method according to claim 6, it is characterised in that the time of reaction is 4~8h in step 1).
9. preparation method according to claim 6, it is characterised in that the time that constant temperature stirs in step 2) is 12~18h.
10. preparation method according to claim 6, it is characterised in that in step 3) time of stirring dipping for 12~
24h, the time of the middle heat treatment of step 4) is 1~4h.
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| CN109943285A (en) * | 2019-04-16 | 2019-06-28 | 贵州大学 | A kind of high-performance wave-absorbing material core-shell structure CoxFe3-xO4@MoS2Nano-complex and its synthetic method |
| CN110177449A (en) * | 2019-05-17 | 2019-08-27 | 同济大学 | A kind of carbon nanotube base Electromagnetic heating absorbing material and its preparation method and application |
| CN111303833A (en) * | 2020-03-12 | 2020-06-19 | 西安工程大学 | Preparation method of cobalt-iron alloy/porous carbon electromagnetic wave absorption composite material |
| CN112892480A (en) * | 2021-01-20 | 2021-06-04 | 宜春惠众生物能源有限公司 | Porous biochar and preparation method thereof |
| CN113381199A (en) * | 2020-03-10 | 2021-09-10 | 武汉理工大学 | Iron-cobalt/silicon-barium composite alloy particle temperature-resistant magnetic wave absorbing agent and preparation method thereof |
| CN113423254A (en) * | 2021-05-26 | 2021-09-21 | 西安理工大学 | Composite wave absorbing agent with electromagnetic wave absorbing performance and preparation method thereof |
| CN113423255A (en) * | 2021-06-09 | 2021-09-21 | 西北工业大学 | Core-shell structure Ti4O7Magnetic metal composite absorbent and preparation method thereof |
| CN113479940A (en) * | 2021-08-06 | 2021-10-08 | 南京冠旭新材料科技有限公司 | Carbon nanotube and carbonyl iron self-assembly wave absorbing agent and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109943285A (en) * | 2019-04-16 | 2019-06-28 | 贵州大学 | A kind of high-performance wave-absorbing material core-shell structure CoxFe3-xO4@MoS2Nano-complex and its synthetic method |
| CN109943285B (en) * | 2019-04-16 | 2021-09-17 | 贵州大学 | High-performance wave-absorbing material core-shell structure CoxFe3-xO4@MoS2Nano-composite and synthesis method thereof |
| CN110177449A (en) * | 2019-05-17 | 2019-08-27 | 同济大学 | A kind of carbon nanotube base Electromagnetic heating absorbing material and its preparation method and application |
| CN113381199A (en) * | 2020-03-10 | 2021-09-10 | 武汉理工大学 | Iron-cobalt/silicon-barium composite alloy particle temperature-resistant magnetic wave absorbing agent and preparation method thereof |
| CN113381199B (en) * | 2020-03-10 | 2022-08-16 | 武汉理工大学 | Iron-cobalt/silicon-barium composite alloy particle temperature-resistant magnetic wave absorbing agent and preparation method thereof |
| CN111303833A (en) * | 2020-03-12 | 2020-06-19 | 西安工程大学 | Preparation method of cobalt-iron alloy/porous carbon electromagnetic wave absorption composite material |
| CN111303833B (en) * | 2020-03-12 | 2022-12-16 | 西安工程大学 | Preparation method of cobalt-iron alloy/porous carbon electromagnetic wave absorption composite material |
| CN112892480A (en) * | 2021-01-20 | 2021-06-04 | 宜春惠众生物能源有限公司 | Porous biochar and preparation method thereof |
| CN113423254A (en) * | 2021-05-26 | 2021-09-21 | 西安理工大学 | Composite wave absorbing agent with electromagnetic wave absorbing performance and preparation method thereof |
| CN113423255A (en) * | 2021-06-09 | 2021-09-21 | 西北工业大学 | Core-shell structure Ti4O7Magnetic metal composite absorbent and preparation method thereof |
| CN113479940A (en) * | 2021-08-06 | 2021-10-08 | 南京冠旭新材料科技有限公司 | Carbon nanotube and carbonyl iron self-assembly wave absorbing agent and preparation method thereof |
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