CN105295303B - Resin, the composite block material of ferrite and MXenes, preparation method and application - Google Patents
Resin, the composite block material of ferrite and MXenes, preparation method and application Download PDFInfo
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- CN105295303B CN105295303B CN201510757001.5A CN201510757001A CN105295303B CN 105295303 B CN105295303 B CN 105295303B CN 201510757001 A CN201510757001 A CN 201510757001A CN 105295303 B CN105295303 B CN 105295303B
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Abstract
The invention discloses the composite block materials of a kind of resin, ferrite and MXenes, and wherein ferrite molecule, which is dispersed in the lamellar structure of MXenes, forms powder granule, and powder granule, which is dispersed in resin, forms block materials.The advantages of on the one hand composite block material has both Ferrite Material and MXenes, with good conductivity, certain conductivity can be still kept when temperature is less than 260K, there is good impedance matching performance simultaneously, therefore it can be applied as absorbing material, be particularly suitable for applying under cryogenic；On the other hand, resin is introduced in the composite block material, powder granule is dispersed in resin and is formed, has the characteristics that be easy to processing and forming, simultaneously because the solidification temperature of resin is low compared with the sintering temperature of powder granule, therefore efficiently solve the problems such as powder granule is oxidizable at high temperature.
Description
Technical field
The present invention relates to technical field of composite materials, more particularly to a kind of resin, ferrite and MXenes composite block
Material, preparation method and application.
Background technology
With the rapid development of electronics and information industry, the mobile communication equipments such as laptop, mobile phone, tablet computer are a large amount of
It is universal, it has almost been covered to each family, and as a part indispensable in daily life.But with these channel radios
Letter equipment and high-frequency electron device dosage sharply increase, electromagnetic interference (Electromagnetic interference) phenomenon
It also grows in intensity with electromagnetic pollution problem.
Ferrite Material is double composite dielectrics, not only ohmic loss, polarization loss, ion and electricity with general dielectric material
Sub-resonance is lost, and also has the distinctive domain wall resonance loss of ferrite, magnetic moment natural resonance loss and particle resonant loss, because
This, ferrite is as a kind of absorbing material, in each electron-like member device such as electromagnetism interference antenna, filter, inductance element
It is widely used in part.But the density of Ferrite Material is relatively high, insulator is translated under low temperature, and exist
The brittleness problems of ceramic material, it is special in high-order mode absorber (accelerator) and space weapon equipment etc. that these factors limit it
The application in field (aerospace).
Two-dimentional transition metal carbide or carbonitride, i.e. MXenes are by Gogotsi and Barsoum et al. 2011
The new material with two-dimensional slice structure that year cooperation is found, is generally available Mn+1XnTzIt indicates, wherein M refers to magnesium-yttrium-transition metal
(such as Ti, Zr, Hf, V, Nb, Ta, Cr, Sc), X refer to C or/and N, and n is generally 1-3, TzRefer to surface group (such as O2-、OH-、F-、
NH3、NH4 +Deng).Currently, MXenes is typically derived from ternary layered cermet Mn+1AXn(M is transition metal element to phase, and A is
Major element, X are C and/or N, and n is generally 1~3, abbreviation MAX phases), by the way that weaker A bits element will be combined in MAX phases (such as
The atoms such as Al, Si) extraction obtain.Similar with graphene, MXenes has excellent electrical and thermal conductivity, higher specific surface
Product.Moreover, MXenes naturally has multilayer " class accordion " structure, it is not easy to reunite；Meanwhile the abundant group energy that surface carries
Suitable ligand enough as iron/nickel cobalt plasma.
Currently, being concentrated mainly on energy storage side for the application study of two-dimentional transition metal carbide or carbon nitride material
To.For example, M.Naguib etc. reports V2CTzElectrode material as lithium ion battery has excellent specific discharge capacity, and
Can still be kept after charge and discharge 140 times good stability (M.Naguib et al, J.Am.Chem.Soc., 2013,
135,15966).M.Lukatskaya et al. then has studied lamella Ti3C2TxAs the electrode active material of ultracapacitor, hair
Now as 1M MgSO4As electrolyte, 1A g are used-1The specific capacitance of the material is up to 400Fcm when testing electric current-3
(M.Lukatskaya,et al,Science,2013,341,1502).Recently, M.W.Barsoum etc. is delivered on Nature
Recent posts is shown, with claylike Ti3C2TzThe ultracapacitor of preparation has 900F/cm3Volumetric capacitance, the value is non-
Very close to ruthenium oxide hydration (1000-1500F/cm3), (M.Ghidiu et al, Nature, 2014,516,78).Other application
In field, Zhou Aiguo etc. has studied the Ti activated through NaOH3C2Tz nanometer sheets find the absorption behavior of heavy metal in sewage
323K, under pH=5.8~6.2, the material is to the maximum adsorption capacity of Pb (II) up to 140mg g-1(Q.Peng et al,
J.Am.Chem.Soc.,2014,136,4113).The carrier material that MXenes also can be used as Pt nano-particles rises in fuel cell
Catalytic action (Y.P.Gao et al, Solid State Sciences, 2014,35,62.), its same Cu2The composite material of O can
To promote the decomposition (X.H.Xie et al, Chem.Commun., 2013,49,10112.) of ammonium perchlorate.In addition MXenes exists
Polymethylacrylic acid N, N- dimethylamino ethyl esters (PDMAEMA) branch are connected to by the application aspect in the field of polymers, Chen etc.
V2CTzIn nanometer sheet, it can obtain with CO2Temperature stimuli-responsive can hybrid material (Chen, J., et al.,
Chem.Commun.,2015,51,314)。
Macromolecule resin material has plasticity strong, and production cost is low, the features such as being easy to processing and forming, in lightweight electricity
Magnetic shielding material field shows good application prospect.For example, polyetherimide (PEI) is a kind of high-performance polymer tree
Fat, it not only has high glass transition temperature, also possesses excellent flame retardant property and mechanical performance, therefore is to prepare high-performance to gather
Close the best matrix selection of the composite microporous foaming electromagnetic shielding material of object.
Invention content
The present invention provides the composite block materials of a kind of resin, ferrite and MXenes, by resin and powder granule group
At, and powder granule is dispersed in resin；The powder granule is made of ferrite and MXenes, ferrite molecule
It is dispersed in the lamellar structure of MXenes.
In the composite block material, the quality of resin and powder granule is adjustable, according to actual needs, the quality of resin
The percentage composition for accounting for the composite block material gross mass is adjustable in 5%~99.8% range.
In the powder granule, the quality of Ferrite Material and MXenes are adjustable, according to actual needs, the matter of MXenes
The percentage composition that amount accounts for the powder granule gross mass is adjustable in 0.1~99.9% range, and Ferrite Material accounts for the powder
The degree of grain gross mass is adjustable in 0.1~99% range.
The Ferrite Material is unlimited, including chemical formula is MeFe2O4、AFe12O19、R3Fe5O12Etc. systems ferrite
Material.Wherein Me elements can be a kind of element in the elements such as Ni, Mn, Zn, Cu, Co, Fe, Li, Mg, Cr, Ca, Ba or two kinds
The combination of the above element；Element A can be a kind of element in the elements such as Ba, Co, Ni, Mn, Zn, Cu, Fe, Li, Mg, Cr, Ca
Or the combination of two or more elements；R element can be in the rare earth elements such as Y, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu
A kind of combination of element or two or more elements.
The preparation method of the MXenes is unlimited, can be by by ternary layered cermet Mn+1AXn(M is transition to phase
Metallic element, A are major element, and X is C and/or N, and n is generally 1~3) plain (such as Al, Si original of the weaker A bits of middle combination
Son) it extracts out and is made.
The resin includes but not limited to polyimide resin (PEI), polystyrene resin, polymethylacrylic acid tree
The arbitrary combination of one or more of fat, makrolon, acrylic resin, epoxy resin, phenolic resin etc..
The present invention also provides a kind of methods preparing the composite block material, and this method comprises the following steps：
Resin is dissolved in solvent, resin solution is configured；The powder granule is scattered in homogeneous solvent, powder is obtained
Particle solution；Resin solution is uniformly mixed with powder granule solution, standing, deaeration are simultaneously evenly applied to carrier surface, are closing
Solvent volatilizees under the conditions of suitable temperature and humidity, after cured cleaning removal excess of solvent, and then vacuum is dry at 30~200 DEG C
Dry 0.1~100h, you can obtain the composite block material.
The preparation method of the powder granule is unlimited, including chemical coprecipitation, solid-phase ball milling method, sol-gel method, from
Propagating combustion, co-precipitation-hydro-thermal method etc..
The solvent is unlimited, including dimethylformamide (DMF), toluene or dimethylbenzene etc..
The drying temperature is preferably 80~150 DEG C.
As a kind of preferred structure, in the powder granule, lamella knot of the ferrite molecule growth in situ in MXenes
In structure.For this purpose, the present invention prepares the powder granule with the preferred structure using coprecipitation, specifically comprise the following steps：
Appropriate MXenes is dissolved in dispersion liquid, finely dispersed MXenes solution is made；
The raw material that Ferrite Material is carried out according to the amount of the substance of respective element in Ferrite Material chemical formula is prepared；
The raw material of Ferrite Material is mixed with MXenes solution, obtains mixed solution one；
Mixed solution one is instilled in alkaline solution, obtains mixed solution two, the pH value for adjusting mixed solution two is 7~
12, under agitation mixed solution two react at a temperature of 20~90 DEG C, reaction product cleaning, drying, obtain iron oxygen
The powder granule of body material and MXenes.
The dispersion liquid is unlimited, including but not limited to the one of sodium lignin sulfonate, neopelex or oleyl amine
Kind solution etc..
The reaction time is preferably 10min~120min.
The alkaline solution is unlimited, including sodium hydroxide, potassium hydroxide, ammonia spirit etc..
In conclusion the present invention is compound by Ferrite Material and MXenes progress, nano level ferrite molecule is dispersed in
Powder granule is constituted in the MXenes lamellar structures of submicron order, which, which is dispersed in resin, forms composite block
Material, the composite block material have the following advantages that：
(1) the advantages of having both Ferrite Material and MXenes.On the one hand, MXenes lamellar structures form conductive network, make
The composite block material has good conductivity, and certain conductivity can be still kept when temperature is less than 260K；It is another
Aspect, the composite block material have good impedance matching performance.Therefore, which can be used as absorbing material
And applied in all kinds of electronic components such as electromagnetism interference antenna, filter, inductance element, it is particularly suitable in cryogenic conditions
Lower application.For example, can work under the liquid nitrogen cryogenics of 80K, so as to apply based on energy recovery type accelerator from
By in electronic laser light source, meeting low temperature requirements of such accelerator to high-order mode suppressor absorbing material；It can apply
Deep sea submarine is met when submarine is in deep sea low temperature, the absorbing material energy in Radome part in Radome part
Enough normal performance purposes；It can apply in outer space electricity consumption magnetic screen device, meet when electromagnetic shielding device is in the outer space
When in low temperature, absorbing material therein can normally play purposes；And it applies in other such as electronic devices, electromagnetism interference
In device etc., meet when such device is in room temperature or low temperature, absorbing material therein can normally play purposes, with full
Requirement of the foot in actual production life under specific condition.
(2) obtained from be sintered powder granule compared with composite block material, composite block material of the invention
Resin is introduced, powder granule is dispersed in resin and is formed, on the one hand has the characteristics that be easy to processing and forming, another party
Face efficiently solves powder granule easy oxygen at high temperature since the solidification temperature of resin is low compared with the sintering temperature of powder granule
The problems such as change.
(3) due to including the MXenes with multilayer " class accordion " structure, density drop in the composite block material
It is low, light weight, and be not easy to reunite, so as to widen the application field as absorbing material.
(4) mass fraction of resin, Ferrite Material and MXenes are adjustable, therefore can be adjusted according to practical application request
Absorbing property.
(5) can the composite block material be molded or is processed into according to the actual application the device of required shape and size
Part.
(6) preferably, using coprecipitation, the surface group of MXenes is made full use of, by Ferrite Material ion source
Position is adsorbed in MXenes sheet of material structures, coprecipitation in-situ preparation ferrite molecule is then utilized, to make ferrite
On the one hand molecule growth in situ strengthens the combination of ferrite molecule and MXenes lamellar structures in the lamellar structure of MXenes
Power, the performance for being on the other hand conducive to the composite block material are stablized.
Description of the drawings
Fig. 1 is the photo in kind of composite block material obtained in the embodiment of the present invention 1；
Fig. 2 is MXenes-20wt.%Ni obtained in the embodiment of the present invention 10.5Zn0.5Fe2O4The XRD of powder granule is composed；
Fig. 3 is MXenes-20wt.%Ni in the embodiment of the present invention 10.5Zn0.5Fe2O4The SEM photograph of powder granule.
Specific implementation mode
The specific implementation mode of the present invention is described further with embodiment below in conjunction with attached drawing, it should be pointed out that
Embodiment described below is intended to be convenient for the understanding of the present invention, and does not play any restriction effect to it.
Embodiment 1：
In the present embodiment, resin is polyetherimide resin (PEI), Ferrite Material Ni0.5Zn0.5Fe2O4, MXenes
Material is Ti3C2Tx.The Ferrite Material constitutes powder granule, in powder granule, the matter of Ferrite Material with MXenes materials
It is 80% to measure the mass percentage that percentage composition is 20%, MXenes, chemical representation MXenes-20wt.%
Ni0.5Zn0.5Fe2O4.Also, powder granule, which is dispersed in resin, forms composite block material, and the quality of powder granule accounts for this
The 5% of composite block material gross mass, the quality of resin account for the 95% of the composite block material gross mass.
The specific preparation method of above-mentioned composite block material is as follows：
(1) 0.5gTi is weighed3C2TxIt is dissolved in the supersaturated solution of sodium lignin sulfonate, ultrasonication 45min, is made and divides
Dissipate uniform MXenes solution；
(2) Ferrite Material Ni is pressed at room temperature0.5Zn0.5Fe2O4Molar ratio Ni2+:Zn2+:Fe3+=0.5:0.5:2 claim
Take Ni (NO3)2·6H2O、Zn(NO3)2·6H2O and Fe (NO3)3·9H2O is added in MXenes solution, obtains mixed solution one,
Wherein Ferrite Material accounts for Ferrite Material and Ti3C2TxThe mass percentage of gross mass is 20%；
(3) according to a certain ratio, a certain amount of sodium hydroxide solution is configured, mixed solution one is instilled with the flow velocity of 0.3L/h
In the sodium hydroxide solution, mixed solution two is obtained, the pH value for adjusting mixed solution two is 10.5, and with the rotating speed of 1000rpm
Stirring, mixed solution two reacts 60min at a temperature of 70 DEG C；Gained slurry is washed with deionized 5 times after the completion of reaction, is connect
It and is dried at 80 DEG C, obtain MXenes-20wt.%Ni0.5Zn0.5Fe2O4Powder granule；
(4) suitable PEI is dissolved in dimethylformamide (DMF), configures PEI/DMF solution；It will be prepared in step (3)
Obtained MXenes-20wt.%Ni0.5Zn0.5Fe2O4It is molten to obtain powder granule in suitable DMF for powder granule ultrasonic disperse
Liquid；Gained powder granule solution is mixed with PEI/DMF solution, it is 5 to make the mass ratio of powder granule and PEI：95, ultrasound,
It is dispersed with stirring 60min, is then allowed to stand 10h, vacuum defoamation, obtains mixed solution, and the mixed solution is evenly applied to totally
Glass pane surface；
(5) glass plate is placed under 25 DEG C and 70% damp condition, the solvent volatilization in mixed solution, after cured by it
It immerses in deionized water and removes extra DMF, be then dried in vacuo 12h at 100 DEG C, you can obtain as shown in Figure 1 compound
Block materials.
To the MXenes-20wt.%Ni being prepared in above-mentioned steps (3)0.5Zn0.5Fe2O4The object of powder body material mutually carries out
Analysis is measured, obtains XRD spectrums as shown in Figure 2, as can be seen from Figure 2：With Ni0.5Zn0.5Fe2O4After compound, MXenes is still kept
Original phase structure, there is TiO2Dephasign generates.
Fig. 3 is the MXenes-20wt.%Ni0.5Zn0.5Fe2O4The SEM photograph of powder, as can be seen from Figure 3：
Ni0.5Zn0.5Fe2O4Growth in situ forms class accordion structure in the lamellar structure of MXenes.
Embodiment 2：
In the present embodiment, resin is polyetherimide resin (PEI), Ferrite Material Ni0.5Zn0.5Fe2O4, MXenes
Material is Ti3C2Tx.The Ferrite Material constitutes powder granule, in powder granule, the matter of Ferrite Material with MXenes materials
It is 2% to measure the mass percentage that percentage composition is 98%, MXenes, chemical representation Ni0.5Zn0.5Fe2O4- 2wt.%
MXenes.Also, powder granule, which is dispersed in resin, forms composite block material, and the quality of powder granule accounts for the composite block
The 20% of body material gross mass, the quality of resin account for the 80% of the composite block material gross mass.
The specific preparation method of above-mentioned composite block material is as follows：
(1) 0.5g Ti are weighed3C2TxIt is dissolved in the supersaturated solution of sodium lignin sulfonate, ultrasonication 45min, is made and divides
Dissipate uniform MXenes solution；
(2) Ferrite Material Ni is pressed at room temperature0.5Zn0.5Fe2O4Molar ratio Ni2+:Zn2+:Fe3+=0.5:0.5:2 claim
Take Ni (NO3)2·6H2O、Zn(NO3)2·6H2O and Fe (NO3)3·9H2The MXenes solution configured in step (1) is added in O,
Mixed solution one is obtained, it is 2% that wherein MXenes, which accounts for Ferrite Material and the mass percentage of MXenes gross masses,；
(3) according to a certain ratio, a certain amount of sodium hydroxide solution is configured, mixed solution one is instilled with the flow velocity of 0.5L/h
In the sodium hydroxide solution, mixed solution two is obtained, the pH value for adjusting mixed solution two is 10.8, and with the rotating speed of 2000rpm
Stirring, mixed solution two react 60min at a temperature of 60 DEG C；Gained slurry is washed with deionized 3 times after the completion of reaction, is connect
It and is dried at 60 DEG C, obtain Ni0.5Zn0.5Fe2O4- 2wt.%MXenes powder granules；
(4) suitable PEI is dissolved in dimethylformamide (DMF), configures PEI/DMF solution；It will be prepared in step (3)
Obtained Ni0.5Zn0.5Fe2O4It is molten to obtain powder granule in suitable DMF for -2wt.%MXenes powder granules ultrasonic disperse
Liquid；Gained powder granule solution is mixed with PEI/DMF solution, it is 1 to make the mass ratio of powder granule and PEI：4, ultrasound is stirred
Dispersion 60min is mixed, 10h, vacuum defoamation is then allowed to stand, obtains mixed solution, and the mixed solution is evenly applied to clean
Glass pane surface；
(5) glass plate is placed under 25 DEG C and 70% damp condition, the solvent volatilization in mixed solution, after cured by it
It immerses in deionized water and removes extra DMF, be then dried in vacuo 12h at 100 DEG C, you can obtain similar to Figure 1 answer
Close block materials.
To the Ni being prepared in above-mentioned steps (3)0.5Zn0.5Fe2O4The object of -2wt.%Mxenes powder granules mutually carries out
Analysis is measured, similar XRD as shown in Figure 2 is obtained and composes, as can be seen from the figure：With Ni0.5Zn0.5Fe2O4After compound, MXenes
Original phase structure is still kept, there is a small amount of TiO2Dephasign generates.
Further with SEM to the Ni0.5Zn0.5Fe2O4- 2wt.%MXenes powder body material patterns are observed, and class can be obtained
It is similar to the photo of Fig. 3, it can be seen that Ni0.5Zn0.5Fe2O4Growth in situ forms class accordion knot in the lamellar structure of MXenes
Structure.
It is returned with the room temperature magnetic hysteresis for the composite block material being prepared in measuring physical properties systematic survey above-mentioned steps (5)
Line and alternating temperature conductivity, structure show：The composite block material still maintains preferable magnetic property；With pure iron ferrite phase
Than the room-temperature conductivity of the composite block material improves, and when temperature is less than 273K, which remains able to
Keep good conductivity, conductive energy.
Therefore, which has low-temperature conductive performance, absorbing material can be used as to be applied to below in low temperature
In the device used under environment：
(1) in the FEL light sources based on ERL, meet such accelerator and the low temperature of high-order mode suppressor absorbing material is wanted
It asks；
(2) it can apply in deep sea submarine Radome part, satisfaction is in when submarine in deep-sea under low temperature environment,
Absorbing material in Radome part can normally play purposes；
(3) it applies in outer space electricity consumption magnetic screen device, meets when the outer space is in low temperature ring with electromagnetic shielding device
Under border, absorbing material therein can normally play purposes；
(4) it applies in other such as electronic devices, anti-EMI materials etc., meets when the device is in low temperature environment
Under, absorbing material therein can normally play purposes.
Embodiment 3：
In the present embodiment, resin is epoxy resin (EP), Ferrite Material CoFe2O4, MXenes materials are V3C2Tx.It should
Ferrite Material constitutes powder granule with MXenes materials, and in powder granule, the mass percentage of Ferrite Material is
The mass percentage of 90%, MXenes are 10%, chemical representation CoFe2O4- 10wt.%MXenes.Also, powder
Even particulate dispersion forms composite block material in resin, and the quality of powder granule accounts for the composite block material gross mass
40%, the quality of resin accounts for the 60% of the composite block material gross mass.
The specific preparation method of above-mentioned composite block material is as follows：
(1) 0.5g V are weighed3C2TxIt is dissolved in the supersaturated solution of neopelex, ultrasonication 45min, makes
Obtain finely dispersed MXenes solution；
(2) Ferrite Material CoFe is pressed at room temperature2O4Molar ratio Co2+:Fe3+=1:2 weigh Co (NO3)2·6H2O and
Fe(NO3)3·9H2O is added the MXenes solution configured in step (1), obtains mixed solution one, wherein MXenes accounts for iron oxygen
Body material and the mass percentage of MXenes gross masses are 10%；
(3) according to a certain ratio, a certain amount of sodium hydroxide solution is configured, mixed solution one is instilled with the flow velocity of 0.5L/h
In the sodium hydroxide solution, mixed solution two is obtained, the pH value for adjusting mixed solution two is 9.5, and is stirred with the rotating speed of 1500rpm
It mixes, reacts 30min at a temperature of 80 DEG C；Gained slurry is washed with deionized 3 times after the completion of reaction, is then dried at 60 DEG C
It is dry, obtain CoFe2O4- 10wt.%MXenes powder granules；
(4) suitable EP is dissolved in DMF, is configured to EP/DMF solution；The CoFe that will be prepared in step (3)2O4-
10wt.%MXenes powder granules ultrasonic disperse obtains powder granule solution in suitable DMF；Gained powder granule is molten
Liquid is mixed with EP/DMF solution, and it is 2 to make the mass ratio of powder granule and EP：3, ultrasound is dispersed with stirring 60min, is then allowed to stand
12h, vacuum defoamation obtain mixed solution, and the mixed solution are evenly applied to clean glass pane surface；
(5) glass plate is placed under 30 DEG C and 60% damp condition, the solvent volatilization in mixed solution, after cured by it
It immerses in deionized water and removes extra DMF, be then dried in vacuo 10h at 120 DEG C, you can obtain similar to Figure 1 answer
Close block materials.
To the CoFe being prepared in above-mentioned steps (3)2O4The object of -10wt.%MXenes powder granules mutually measures point
Analysis obtains similar XRD as shown in Figure 2 and composes, as can be seen from the figure：With CoFe2O4After powder is compound, MXenes still keeps former
There is phase structure, there is a small amount of TiO2Dephasign generates.
Further with SEM to the CoFe2O4- 10wt.%MXenes powder body material patterns are observed, and can be similar to
The photo of Fig. 3, it can be seen that CoFe2O4Growth in situ forms class accordion structure in the lamellar structure of MXenes.
It is returned with the room temperature magnetic hysteresis for the composite block material being prepared in measuring physical properties systematic survey above-mentioned steps (5)
Line and alternating temperature conductivity, structure show：The composite block material still maintains preferable magnetic property；With pure iron ferrite phase
Than the room-temperature conductivity of the composite block material improves, and when temperature is less than 273K, which remains able to
Keep good conductivity, conductive energy.
Therefore, which has low-temperature conductive performance, absorbing material can be used as to be applied to below in low temperature
In the device used under environment：
(1) in the FEL light sources based on ERL, meet such accelerator and the low temperature of high-order mode suppressor absorbing material is wanted
It asks；
(2) it can apply in deep sea submarine Radome part, satisfaction is in when submarine in deep-sea under low temperature environment,
Absorbing material in Radome part can normally play purposes；
(3) it applies in outer space electricity consumption magnetic screen device, meets when the outer space is in low temperature ring with electromagnetic shielding device
Under border, absorbing material therein can normally play purposes；
(4) it applies in other such as electronic devices, anti-EMI materials etc., meets when the device is in low temperature environment
Under, absorbing material therein can normally play purposes.
Embodiment 4：
In the present embodiment, resin is acrylic resin (PP), Ferrite Material CoFe2O4, MXenes materials are V3C2Tx。
The Ferrite Material constitutes powder granule with MXenes materials, and in powder granule, the mass percentage of Ferrite Material is
The mass percentage of 50%, MXenes are 50%, chemical representation CoFe2O4- 50wt.%MXenes.Also, powder
Even particulate dispersion forms composite block material in resin, and the quality of powder granule accounts for the composite block material gross mass
50%, the quality of resin accounts for the 50% of the composite block material gross mass.
The specific preparation method of above-mentioned composite block material is as follows：
(1) 0.5g V are weighed3C2TxIt is dissolved in the supersaturated solution of neopelex, ultrasonication 45min, makes
Obtain finely dispersed MXenes solution；
(2) Ferrite Material CoFe is pressed at room temperature2O4Molar ratio Co2+:Fe3+=1:2 weigh Co (NO3)2·6H2O and
Fe(NO3)3·9H2O is added the MXenes solution configured in step (1), obtains mixed solution one, wherein MXenes accounts for iron oxygen
Body material and the mass percentage of MXenes gross masses are 50%；
(3) according to a certain ratio, a certain amount of sodium hydroxide solution is configured, mixed solution one is instilled with the flow velocity of 0.5L/h
In the sodium hydroxide solution, mixed solution two is obtained, the pH value for adjusting mixed solution two is 9.5, and is stirred with the rotating speed of 1500rpm
It mixes, reacts 30min at a temperature of 80 DEG C；Gained slurry is washed with deionized 3 times after the completion of reaction, is then dried at 60 DEG C
It is dry, obtain CoFe2O4- 50wt.%MXenes powder granules；
(4) suitable PP is dissolved in DMF, configures PP/DMF solution；The CoFe that will be prepared in step (3)2O4-
10wt.%MXenes powder granules ultrasonic disperse obtains powder granule solution in suitable DMF；Gained powder granule is molten
Liquid is mixed with PP/DMF solution, and it is 1 to make the mass ratio of powder granule and PP：1, ultrasound is dispersed with stirring 60min, is then allowed to stand
9h, vacuum defoamation obtain mixed solution, and the mixed solution are evenly applied to clean glass pane surface；
(5) glass plate is placed under 25 DEG C and 65% damp condition, the solvent volatilization in mixed solution, after cured by it
It immerses in deionized water and removes extra DMF, be then dried in vacuo 9h at 120 DEG C, you can obtain similar to Figure 1 compound
Block materials.
To the CoFe being prepared in above-mentioned steps (3)2O4The object of -50wt.%MXenes powder granules mutually measures point
Analysis obtains similar XRD as shown in Figure 2 and composes, as can be seen from the figure：With CoFe2O4After powder is compound, MXenes still keeps former
There is phase structure, there is a small amount of TiO2Dephasign generates.
Further with SEM to the CoFe2O4- 50wt.%MXenes powder body material patterns are observed, and can be similar to
The photo of Fig. 3, it can be seen that CoFe2O4Growth in situ forms class accordion structure in the lamellar structure of MXenes.
It is returned with the room temperature magnetic hysteresis for the composite block material being prepared in measuring physical properties systematic survey above-mentioned steps (5)
Line and alternating temperature conductivity, structure show：The composite block material still maintains preferable magnetic property；With pure iron ferrite phase
Than the room-temperature conductivity of the composite block material improves, and when temperature is less than 273K, which remains able to
Keep good conductivity, conductive energy.
Therefore, which has low-temperature conductive performance, absorbing material can be used as to be applied to below in low temperature
In the device used under environment：
(1) in the FEL light sources based on ERL, meet such accelerator and the low temperature of high-order mode suppressor absorbing material is wanted
It asks；
(2) it can apply in deep sea submarine Radome part, satisfaction is in when submarine in deep-sea under low temperature environment,
Absorbing material in Radome part can normally play purposes；
(3) it applies in outer space electricity consumption magnetic screen device, meets when the outer space is in low temperature ring with electromagnetic shielding device
Under border, absorbing material therein can normally play purposes；
(4) it applies in other such as electronic devices, anti-EMI materials etc., meets when the device is in low temperature environment
Under, absorbing material therein can normally play purposes.
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that the foregoing is merely
Specific embodiments of the present invention are not intended to restrict the invention, all any modifications made in the spirit of the present invention, benefit
Fill or similar fashion substitute etc., should all be included in the protection scope of the present invention.
Claims (10)
1. the composite block material of resin, ferrite and MXenes, it is characterized in that：It is made of resin and powder granule, and powder
Body even particulate dispersion is in resin；The powder granule is made of ferrite and MXenes, ferrite molecule growth in situ
In the lamellar structure of MXenes, which is prepared using coprecipitation, is specifically comprised the following steps：
Appropriate MXenes is dissolved in dispersion liquid, finely dispersed MXenes solution is made；
The raw material that Ferrite Material is carried out according to the amount of the substance of respective element in Ferrite Material chemical formula is prepared；
The raw material of Ferrite Material is mixed with MXenes solution, obtains mixed solution one；
Mixed solution one is instilled in alkaline solution, mixed solution two is obtained, the pH value for adjusting mixed solution two is 7~12,
Mixed solution two reacts at a temperature of 20~90 DEG C under stirring condition, and reaction product cleaning, drying obtain Ferrite Material
With the powder granule of MXenes；
The preparation method of the composite block material includes the following steps：
Resin is dissolved in solvent, resin solution is configured；
The powder granule is scattered in homogeneous solvent, powder granule solution is obtained；
Resin solution is uniformly mixed with powder granule solution, standing, deaeration are simultaneously evenly applied to carrier surface, in suitable temperature
Solvent volatilizees under degree and damp condition, and cleaning removal excess of solvent, is then dried in vacuo 0.1 at 80~200 DEG C after cured
~100h obtains the composite block material.
2. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：The quality of resin
Account for the 5%~99.8% of the composite block material gross mass.
3. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：The matter of MXenes
Amount accounts for the 0.1~99.9% of the powder granule gross mass.
4. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：The iron oxygen
Body material includes that chemical formula is MeFe2O4、AFe12O19Or R3Fe5O12The Ferrite Material of system, wherein Me elements be Ni, Mn,
The combination of a kind of element or two or more elements in Zn, Cu, Co, Fe, Li, Mg, Cr, Ca, Ba element；Element A be Ba, Co,
The combination of a kind of element or two or more elements in Ni, Mn, Zn, Cu, Fe, Li, Mg, Cr, Ca element；R element is rare earth member
The combination of a kind of element or two or more elements in plain Y, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.
5. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：Described
MXenes is by by ternary layered cermet Mn+1AXnIt is made in conjunction with weaker A bit elements extraction in phase；Wherein, M was
Metallic element is crossed, A is major element, and X is C and/or N, and n is 1~3.
6. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：The resin
Including polyimide resin, polystyrene resin, polymethacrylate resin, makrolon, acrylic resin, epoxy resin,
The combination of one or more of phenolic resin.
7. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：The dispersion
Liquid includes a kind of solution in sodium lignin sulfonate, neopelex or oleyl amine.
8. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：The reaction
Time is 10min~120min.
9. the composite block material of resin as described in claim 1, ferrite and MXenes, it is characterized in that：The alkalinity
Solution is sodium hydroxide, potassium hydroxide, ammonia spirit.
10. the composite block material of resin, ferrite and MXenes as described in any claim in claim 1 to 9 is made
For the application of absorbing material.
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| CN106854453A (en) * | 2016-12-15 | 2017-06-16 | 陕西科技大学 | A kind of preparation method of lamellar composite absorbing material |
| US20180338396A1 (en) * | 2017-05-16 | 2018-11-22 | Murata Manufacturing Co., Ltd. | Electronic component having electromagnetic shielding and method for producing the same |
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| CN108251054B (en) * | 2018-03-23 | 2021-03-23 | 中国工程物理研究院材料研究所 | Composite wave-absorbing material and preparation method thereof |
| CN108751995A (en) * | 2018-07-10 | 2018-11-06 | 中国科学院宁波材料技术与工程研究所 | Nanoparticle in-stiu coating MXenes composite materials, its preparation method and purposes |
| CN108821291B (en) * | 2018-07-10 | 2020-07-07 | 中国科学院宁波材料技术与工程研究所 | Novel ternary layered MAX phase material, and preparation method and application thereof |
| CN108822797B (en) * | 2018-07-10 | 2021-02-19 | 中南大学 | Titanium silicon carbon composite wave absorbing agent and preparation method and application thereof |
| CN110698817A (en) * | 2019-10-14 | 2020-01-17 | 嘉兴学院 | Wear-resistant anti-ultraviolet aging epoxy composite material and preparation method thereof |
| CN113115581B (en) * | 2021-04-13 | 2022-12-02 | 郑州大学 | Ti 3 C 2 T x Composite material and preparation method thereof |
| CN113423254B (en) * | 2021-05-26 | 2023-03-24 | 西安理工大学 | Composite wave absorbing agent with electromagnetic wave absorbing performance and preparation method thereof |
| CN115216863A (en) * | 2021-06-18 | 2022-10-21 | 哈尔滨工业大学 | CoFe 2 O 4 -TiO 2 Composite fiber and preparation method and application thereof |
| CN113845695B (en) * | 2021-10-12 | 2022-03-11 | 南京工业大学 | Ternary nano composite flame retardant, flame-retardant epoxy resin and preparation method thereof |
| CN113980359B (en) * | 2021-11-22 | 2023-10-20 | 北京化工大学 | Modified MXene-loaded metal oxide composite and preparation method and application thereof |
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