CN106854453A - A kind of preparation method of lamellar composite absorbing material - Google Patents
A kind of preparation method of lamellar composite absorbing material Download PDFInfo
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- CN106854453A CN106854453A CN201611163699.9A CN201611163699A CN106854453A CN 106854453 A CN106854453 A CN 106854453A CN 201611163699 A CN201611163699 A CN 201611163699A CN 106854453 A CN106854453 A CN 106854453A
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Abstract
A kind of preparation method of lamellar composite absorbing material, is prepared for being taken on (001) direction the sheet BaFe of growth by molten-salt growth method first12O19Powder, Ti is corroded secondly by HF3AlC2Obtain the Ti of class graphene-structured3C2Powder, eventually passes casting molding processes, obtains lamellar composite absorbing material.The present invention uses casting molding processes, simple to operate, short preparation period, is capable of achieving increasingly automated, and production efficiency is high, reduces cost, and the material for preparing is uniformly dispersed, and compactness and has good uniformity.
Description
Technical field
The invention belongs to material science, it is related to a kind of preparation method of lamellar composite absorbing material.
Background technology
With developing rapidly for modern magnetoelectricity technology, various electromagnetic equipment applications it is increasingly extensive, electromagnetic radiation has turned into
Human lives and work public hazards, electromagnetic interference and electromagnetic pollution produced by it damaged high frequency electronic equipment working environment and
Human habitat, high performance absorbing material has become one of emphasis of current electromagnetic material area research and exploitation.
Additionally, in modern war, electromagnetic wave absorbing material is reducing or eliminating radar, ultrared detection, to reach the stealthy aspect in battlefield
Have a wide range of applications, receive the great attention of countries in the world.It can be seen that research has high-performance biological wave-absorbing material to the mankind
Daily life and military building-up all have urgent practical value.Absorbing material traditional at present cannot meet current anti-electricity
Thin, light, wide, the strong requirement of magnetic disturbance and military stealth technology to radio-radar absorber, high-performance composite wave-suction material grinds
Studying carefully and developing has turned into current important research direction.
Barium ferrite has the advantages that preparation process is simple, with low cost, to absorb strong, absorption band wide, and its frequency
Characteristic is good (its relative permeability is larger, and relative dielectric constant is smaller), is adapted to make matching layer, and frequency band side is widened in low frequency
Face, with good application potential.Class grapheme material refers to then the tow -dimensions atom comprising other elements with graphene-structured
Crystal or compound.Class Graphene has excellent physicochemical properties, and its component is adjustable, appropriate control and reconciles its group
Dividing can obtain the two-dimensional layer nano crystal material with property, be that it has established good in the application of field of nanometer technology
Good basis.Class Graphene is fast-developing at this stage, be mainly applied to both at home and abroad nano adsorber, electrochemical sensor,
The fields such as lithium ion battery, ultracapacitor and hydrogen storage.Class Graphene density is small, electrical conductivity is high, heat endurance is good, is potential
Dielectric loss type absorbent；The barium ferrite of laminated structure absorbs strong, absorption band magnetocrystalline anisotropy field, nature wide, high
Resonant frequency is high, is good magnetic loss type absorbent.But preparation method is complicated in the prior art, and prepared sorbing material
Absorption property still await further raising.
The content of the invention
It is an object of the invention to provide a kind of preparation method of lamellar composite absorbing material, the method operation letter
Single, with low cost, obtained Radar Absorbing Properties of Composites is preferable.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of lamellar composite absorbing material, absolute ethyl alcohol, butanone and olein are carried out once
Ball milling, is well mixed, and is subsequently adding polyvinyl butyral resin, polyethylene glycol and dibutyl phthalate (DBP), carries out secondary ball milling,
It is well mixed, it is subsequently adding sheet BaFe12O19Powder and through hydrofluoric acid corrode after Ti3C2Powder, is cast after ball milling, is obtained
To lamellar composite absorbing material；Wherein, sheet BaFe12O19Powder and through hydrofluoric acid corrode after Ti3C2The mass ratio of powder
(0.5~1):(5~6).
The present invention is further improved, sheet BaFe12O19Powder and through hydrofluoric acid corrode after Ti3C2The total matter of powder
Amount is the total of absolute ethyl alcohol, butanone, olein, polyvinyl butyral resin, polyethylene glycol and dibutyl phthalate (DBP)
The 30%~80% of quality；During curtain coating, 200~250 μm of the height of scraper is cast.
Further improvement of the invention is that the mass ratio of absolute ethyl alcohol, butanone and olein is (2~6):(5
~8):(1~3).
The present invention is further improved, the matter of polyvinyl butyral resin, polyethylene glycol and dibutyl phthalate (DBP)
Amount is than being (0.2~0.6):(0.1~0.5):(0.1~0.5).
The present invention is further improved, sheet BaFe12O19Powder is prepared by procedure below：
1) according to chemical general formula BaFe12O19In mol ratio, by BaCO3With Fe2O3Mixing, adds NaCl by ball
Mill is well mixed, then dries, crosses 60 mesh sieves, obtains mixed powder A1；Wherein, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:(1~2)；
2) by step 1) obtained by mixed powder A1In 1000~1200 DEG C of 2~4h of pre-burning, washing obtains BaFe12O19
The precursor B of powder1；
3) by Fe2O3、BaCl·2H2O and BaFe12O19The precursor B of powder1, after wet-milling, mixed slurry is obtained, then will
Mixed slurry crosses 60 mesh sieves after drying, and obtains mixed powder C1, then by mixed powder C12~8h, water are calcined in 1000~1200 DEG C
Wash, obtain the sheet BaFe on (001) direction with orientation12O19Powder.
Of the invention further improvement be, step 1) in the rotating speed of ball milling be 500~600r/min, the time of ball milling is
15~20h；Dry temperature is 60~100 DEG C, and the time is 4~8h；BaCl·2H2The quality of O is Fe2O32~3 times of quality,
BaFe12O19The precursor B of powder1Quality be BaCl2H2O、Fe2O3And BaFe12O19The precursor B of powder1Gross mass
5%-15%.
Further improvement of the invention is, through the Ti after hydrofluoric acid corrosion3C2Powder is prepared by procedure below：Massage
You compare Ti:Al:TiC=1.0:1.2:2.0, by Ti, Al and TiC, ball milling mixing is uniform, is sintered in atmosphere furnace after drying, so
After corroding by hydrofluoric acid, the Ti after corroding through hydrofluoric acid is obtained3AlC2Powder.
Of the invention further improvement is to be protected using nitrogen during sintering, and the temperature of sintering is 1350 DEG C, sintering when
Between be 1~4h.
Further improvement of the invention is to be heated to 1350 DEG C with the heating rate of 6~8 DEG C/min.
Further improvement of the invention is that corrosion detailed process is：Product after 2~5g is sintered is immersed in 60~
In the hydrofluoric acid solution of 100mL, 2~6h of stirring makes corrosion completely, is then centrifuged for separating, and washing is until centrifuged supernatant pH value is
5~6, then by 24~48h of gained solid sample drying at room temperature.
Compared with prior art, the device have the advantages that：The BaFe of laminated structure in the present invention12O19Absorb it is strong,
Absorption band magnetocrystalline anisotropy field wide, high, natural resonant frequency are high, are good magnetic loss type absorbents.By Ti3AlC2
Corrosion treatment in ceramic powder immersion HF, can be prepared into two-dimentional Ti3C2Material, the material has excellent physicochemical properties, very
Good heat conductivility and electric conductivity, and its component is adjustable, appropriate control and reconciles its component and can obtain with particularity
The two-dimensional layer of energy, is conducive to electromagnetic wave in layer and layer reflection loss；The present invention comprehensively utilizes the advantage of the two, using the tape casting
Prepare Ti3C2/BaFe12O19Composite.The present invention uses casting technique, and material dispersion is uniform and thickness of film is homogeneous, and
And casting slurry nontoxicity used is prepared, human body will not be damaged.Present device is simple, and process stabilizing can be continuous
Operation, production efficiency is high, is capable of achieving increasingly automated, reduces cost, material compactness and has good uniformity, and the side of preparation
Method is simple.Obtained flaky powder BaFe of the invention12O19With class graphene-structured Ti3C2Powder is carried out in organic carrier slurry
The arrangement of in-plane, the good absorbing material of orientation is obtained by drying.
Further, the present invention is prepared for the sheet BaFe with orientation by molten-salt growth method12O19Powder, is corroded by HF
Ti3AlC2Obtain the Ti of class graphene-structured3C2Powder, eventually passes casting molding processes, obtains that there is preferably orientation to have Jie concurrently
Electricity, the sorbing material of magnetic loss function.
Brief description of the drawings
Fig. 1 is BaFe prepared by molten-salt growth method12O19The XRD of powder.
Fig. 2 is Ti3AlC2Powder utilizes the XRD of the corrosion product after HF corrosion treatments 2h.
Fig. 3 is BaFe prepared by molten-salt growth method of the present invention12O19The SEM figures of powder.
Fig. 4 is Ti3AlC2Powder is schemed using the SEM of the corrosion product after HF corrosion treatments 2h.
Fig. 5 is stratiform Ti prepared by the tape casting3C2/BaFe12O19The SEM figures of composite wave-suction material.
Fig. 6 is stratiform Ti prepared by the tape casting3C2/BaFe12O19Composite wave-suction material thickness is the reflection loss of 3.0mm
Figure.
Fig. 7 is stratiform Ti prepared by the tape casting3C2/BaFe12O19Composite wave-suction material thickness is the reflection loss of 4.5mm
Figure.
Fig. 8 is stratiform Ti prepared by the tape casting3C2/BaFe12O19Composite wave-suction material thickness is the reflection loss of 5.0mm
Figure.
Specific embodiment
By specific embodiment, the present invention is described in detail below in conjunction with the accompanying drawings.
Sheet Ba in the present invention2Fe12O19Powder is in (001) direction oriented growth.The temperature of hot pressing is 60 in the present invention
~80 DEG C, pressure is 0.5~1MPa, and the dwell time is 30s~1min.
Embodiment 1
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 600r/min, and Ball-milling Time is 15h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:2, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1000 DEG C into phase after compound after ball milling is dried, and being incubated 4h makes oxide fully carry out fused salt
Reaction.
Step 3：The ultrasonic disperse in water is removed by what the product obtained after reaction was placed in, washing is dried, and obtains BaFe12O19
Presoma.Wherein the temperature of deionized water is 80 DEG C, and ultrasonic time 15min is washed 5 times, 80 DEG C of dry temperature.
Step 4：By Fe2O3、BaCl·2H2O and BaFe12O19The precursor B of powder1, after wet-milling, mixed slurry is obtained, so
60 mesh sieves are crossed after mixed slurry is dried afterwards, mixed powder C is obtained1；Wherein, BaFe12O19The precursor B of powder1Quality be
BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H25%, BaCl of O gross masses2·2H2O is preparation Ba2Fe12O19Piece
Fused salt used by shape, it is Fe that it adds quality2O32 times of quality.
Step 5：By mixed powder C18h is incubated at 1100 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in the ultrasonic disperse in water, is washed, dried.It is wherein used go from
The temperature of sub- water is 80 DEG C, and ultrasonic time 15min is washed 5 times, and 80 DEG C of dry temperature obtains sheet BaFe12O19Powder.
Step 7：Ti in molar ratio:Al:TiC=1.0:1.2:2.0, weigh Ti, Al and TiC that total amount is 20g, Ran Hou
Ball milling is carried out in ball mill, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains equal
Even powder simultaneously dries it at 50 DEG C；
Step 8：Dry batch mixing is protected with nitrogen, 1350 DEG C is heated to the heating rate of 7 DEG C/min, be incubated 4h,
Obtain Ti3AlC2Powder.
Step 9：By gained Ti in step 83AlC2Powder takes 4g and is immersed in the hydrofluoric acid of 70mL (concentration of hydrofluoric acid is
49%, buy in Chemical Reagent Co., Ltd., Sinopharm Group) in, using magnetic agitation, mixing speed is 500r/min, carries out corruption
Erosion reaction 4h, centrifugation is washed up to centrifuged supernatant pH value is between 5~6, by gained solid sample drying at room temperature 32h,
Ti after corroding through hydrofluoric acid3C2Powder；
Step 10：Weighing 4g absolute ethyl alcohols, 6g butanone, 2g oleins carries out a ball milling.
Step 11：Then to addition 0.4g polyvinyl butyral resins, the poly- second two of 0.3g in the product after ball milling in step 10
Alcohol and 0.2g dibutyl phthalate (DBP)s, carry out secondary ball milling.
Step 12：To addition 0.8g sheets BaFe in the product being added to after step 11 ball milling12O19Powder and 5.5g are through hydrogen
Ti after fluoric acid corrosion3C2Powder, the ball milling 2h in the case where rotating speed is 280r/min.
Step 13：The slurry that step 12 is mixed, is cast, and the height for being cast scraper is 220 μm, obtains stratiform
Ti3C2/BaFe12O19Composite wave-suction material.
By composite wave-suction material through hot pressing after, the temperature of specific hot pressing is 70 DEG C, and pressure is 0.6MPa, pressurize 45smin
After tested.
It will be seen from figure 1 that BaFe prepared by molten-salt growth method12O19Without dephasign generation, the diffracted intensity in (001) face strengthens,
Show that crystal grain there occurs that preferred orientation grows.
From figure 3, it can be seen that the BaFe that molten-salt growth method is prepared12O19Crystal grain is 500 μm~100 μm or so of the length of side, thickness 10
μm or so slab-like, surface is smooth and smooth, and crystal grain there occurs obvious preferred orientation growth.
From fig. 5, it can be seen that by the sheet BaFe after casting technique treatment12O19Crystal grain orientations at one layer above,
Stratiform Ti3C2One layer below, it is tightly combined between layers.
From fig. 6, it can be seen that stratiform Ti3C2/BaFe12O19Composite wave-suction material thickness is 3.0mm, in 6.1GHz, most
Big reflection loss -21.9dB.
From figure 7 it can be seen that stratiform Ti3C2/BaFe12O19Composite wave-suction material thickness is 4.0mm, in 3.9GHz, most
Big reflection loss -18.4dB.
From figure 8, it is seen that stratiform Ti3C2/BaFe12O19Composite wave-suction material thickness is 5.0mm, in 3.5GHz, most
Big reflection loss -22.8dB.
Embodiment 2
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 600r/min, and Ball-milling Time is 15h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:2, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1200 DEG C into phase after compound after ball milling is dried, and being incubated 4h makes oxide fully carry out fused salt
Reaction.
Step 3：The ultrasonic disperse in water is removed by what the product obtained after reaction was placed in, washing is dried, and obtains BaFe12O19
Presoma.Wherein the temperature of deionized water is 100 DEG C, and ultrasonic time 20min is washed 5 times, 90 DEG C of dry temperature.
Step 4：By Fe2O3、BaCl·2H2O and BaFe12O19The precursor B of powder1, after wet-milling, mixed slurry is obtained, so
60 mesh sieves are crossed after mixed slurry is dried afterwards, mixed powder C is obtained1；Wherein, BaFe12O19The precursor B of powder1Quality be
BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H210%, BaCl of O gross masses2·2H2O is preparation Ba2Fe12O19
Fused salt used by sheet, it is Fe that it adds quality2O31.5 times of quality.
Step 5：By mixed powder C110h is incubated at 1150 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in the ultrasonic disperse in water, is washed, dried.It is wherein used go from
The temperature of sub- water is 80 DEG C, and ultrasonic time 15min is washed 5 times, and 80 DEG C of dry temperature obtains sheet BaFe12O19Powder.
Step 7：Ti in molar ratio:Al:TiC=1.0:1.2:2.0, weigh total amount and weigh Ti, Al and TiC for 25g, so
Ball milling is carried out in ball mill afterwards, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h is obtained
Obtain uniform powder and it is dried at 40 DEG C.
Step 8：Dry batch mixing is protected with nitrogen, 1350 DEG C is heated to the heating rate of 6 DEG C/min, be incubated 1h,
Obtain Ti3AlC2Powder.
Step 9：By gained Ti in step 83AlC2Powder takes 2g and is immersed in the hydrofluoric acid of 60mL (concentration of hydrofluoric acid is
49%, buy in Chemical Reagent Co., Ltd., Sinopharm Group) in, using magnetic agitation, mixing speed is 500r/min, carries out corruption
Erosion reaction 2h, centrifugation is washed up to centrifuged supernatant pH value is between 5~6, by gained solid sample drying at room temperature 24h,
Ti after corroding through hydrofluoric acid3C2Powder；
Step 10：Weighing 2g absolute ethyl alcohols, 5g butanone, 1g oleins carries out a ball milling.
Step 11：Then to addition 0.2g polyvinyl butyral resins, the poly- second two of 0.1g in the product after ball milling in step 10
Alcohol and 0.1g dibutyl phthalate (DBP)s, carry out secondary ball milling.
Step 12：To addition 0.5g sheets BaFe in the product being added to after step 11 ball milling12O19Powder and 5g are through hydrogen fluorine
Ti after acid corrosion3C2Powder, the ball milling 2h in the case where rotating speed is 280r/min.
Step 13：The slurry that step 12 is mixed, is cast, and is cast 200 μm of the height of scraper, obtains stratiform
Ti3C2/BaFe12O19Composite wave-suction material.
By composite wave-suction material through hot pressing after, the temperature of specific hot pressing is 60 DEG C, and pressure is 0.5MPa, pressurize 30smin
After tested.
Figure it is seen that after HF corrosion, the enhancing of 29 ° of θ ≈ or so (002) face diffraction maximum intensity, this is in Ti3C2's
PDF cards are consistent.
From fig. 4, it can be seen that Ti3C2The very thin thickness of layer, and synusia spacing is big, one end is presented and opens becoming for one end contraction
Gesture.
Embodiment 3
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 500r/min, and Ball-milling Time is 18h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:1, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1200 DEG C into phase after compound after ball milling is dried, and being incubated 3h makes oxide fully carry out fused salt
Reaction.
Step 3：The ultrasonic disperse in water is removed by what the product obtained after reaction was placed in, washing is dried, and obtains BaFe12O19
Presoma.Wherein the temperature of deionized water is 90 DEG C, and ultrasonic time 15min is washed 5 times, dry temperature 60 C.
Step 4：By Fe2O3、BaCl·2H2O and BaFe12O19The precursor B of powder1, after wet-milling, mixed slurry is obtained, so
60 mesh sieves are crossed after mixed slurry is dried afterwards, mixed powder C is obtained1；Wherein, BaFe12O19The precursor B of powder1Quality be
BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H25%, BaCl of O gross masses2·2H2O is preparation Ba2Fe12O19Piece
Fused salt used by shape, it is Fe that it adds quality2O31 times of quality.
Step 5：By mixed powder C16h is incubated at 1100 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in the ultrasonic disperse in water, is washed, dried.It is wherein used go from
The temperature of sub- water is 100 DEG C, and ultrasonic time 15min is washed 5 times, and dry temperature 60 C obtains sheet BaFe12O19Powder.
Step 7：Ti in molar ratio:Al:TiC=1.0:1.2:2.0, weigh Ti, Al and TiC that total amount is 12g, Ran Hou
Ball milling is carried out in ball mill, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains equal
Even powder simultaneously dries it at 60 DEG C；
Step 8：Dry batch mixing is protected with nitrogen, 1350 DEG C is heated to the heating rate of 6 DEG C/min, be incubated 4h,
Obtain Ti3AlC2Powder.
Step 9：By gained Ti in step 83AlC2Powder takes 5g and is immersed in the hydrofluoric acid of 100mL (concentration of hydrofluoric acid is
49%, buy in Chemical Reagent Co., Ltd., Sinopharm Group) in, using magnetic agitation, mixing speed is 500r/min, carries out corruption
Erosion reaction 6h, centrifugation is washed up to centrifuged supernatant pH value is between 5~6, by gained solid sample drying at room temperature 48h,
Ti after corroding through hydrofluoric acid3C2Powder；
Step 10：Weighing 6g absolute ethyl alcohols, 8g butanone, 3g oleins carries out a ball milling.
Step 11：Then to addition 0.6g polyvinyl butyral resins, the poly- second two of 0.5g in the product after ball milling in step 10
Alcohol and 0.5g dibutyl phthalate (DBP)s, carry out secondary ball milling.
Step 12：To addition 1g sheets BaFe in the product being added to after step 11 ball milling12O19Powder and 6g Ti3C2Powder
Body, the ball milling 2h in the case where rotating speed is 280r/min.
Step 13：The slurry that step 12 is mixed, is cast, and is cast 250 μm of the height of scraper, obtains stratiform
Ti3C2/BaFe12O19Composite wave-suction material.
Embodiment 4
A kind of preparation method of lamellar composite absorbing material, comprises the following steps：
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 500r/min, and Ball-milling Time is 15h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:1, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1000 DEG C into phase after compound after ball milling is dried, and being incubated 4h makes oxide fully carry out fused salt
Reaction.
Step 3：The ultrasonic disperse in water is removed by what the product obtained after reaction was placed in, washing is dried, and obtains BaFe12O19
Presoma.Wherein the temperature of deionized water is 90 DEG C, and ultrasonic time 15min is washed 8 times, 100 DEG C of dry temperature.
Step 4：By Fe2O3、BaCl·2H2O and BaFe12O19The precursor B of powder1, after wet-milling, mixed slurry is obtained, so
60 mesh sieves are crossed after mixed slurry is dried afterwards, mixed powder C is obtained1；Wherein, BaFe12O19The precursor B of powder1Quality be
BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H215%, BaCl of O gross masses2·2H2O is preparation Ba2Fe12O19
Fused salt used by sheet, it is Fe that it adds quality2O32 times of quality.
Step 5：By mixed powder C18h is incubated at 1000 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in the ultrasonic disperse in water, is washed, dried.It is wherein used go from
The temperature of sub- water is 100 DEG C, and ultrasonic time 15min is washed 5 times, and dry temperature 60 C obtains sheet BaFe12O19Powder.
Step 7：Ti in molar ratio:Al:TiC=1.0:1.2:2.0, weigh Ti, Al and TiC that total amount is 12g, Ran Hou
Ball milling is carried out in ball mill, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains equal
Even powder simultaneously dries it at 60 DEG C；
Step 8：Dry batch mixing is protected with nitrogen, 1350 DEG C is heated to the heating rate of 7 DEG C/min, be incubated 2h,
Obtain Ti3AlC2Powder.
Step 9：By gained Ti in step 83AlC2Powder takes 5g and is immersed in the hydrofluoric acid of 100mL (concentration of hydrofluoric acid is
49%, buy in Chemical Reagent Co., Ltd., Sinopharm Group) in, using magnetic agitation, mixing speed is 500r/min, carries out corruption
Erosion reaction 6h, centrifugation is washed up to centrifuged supernatant pH value is between 5~6, by gained solid sample drying at room temperature 48h,
Ti after corroding through hydrofluoric acid3C2Powder；
Step 10：Weighing 6g absolute ethyl alcohols, 8g butanone, 3g oleins carries out a ball milling.
Step 11：Then to addition 0.6g polyvinyl butyral resins, the poly- second two of 0.5g in the product after ball milling in step 10
Alcohol and 0.5g dibutyl phthalate (DBP)s, carry out secondary ball milling.
Step 12：To addition 1g sheets BaFe in the product being added to after step 11 ball milling12O19Powder and 6g Ti3C2Powder
Body, the ball milling 2h in the case where rotating speed is 280r/min.
Step 13：The slurry that step 12 is mixed, is cast, and is cast 250 μm of the height of scraper, obtains stratiform
Ti3C2/BaFe12O19Composite wave-suction material.
Embodiment 5
A kind of preparation method of lamellar composite absorbing material, comprises the following steps：
Step 1：The BaCO that total amount is 20g is accurately taken with electronic balance3、Fe2O3And NaCl, then ball milling mixing is uniform, its
In, the rotating speed of ball milling is 500r/min, and Ball-milling Time is 20h.NaCl is fused salt, BaCO3With Fe2O3Gross mass and NaCl
Mass ratio is 1:2, BaCO3With Fe2O3Amount according to chemical general formula BaFe12O19In mol ratio.
Step 2：At 1100 DEG C into phase after compound after ball milling is dried, and being incubated 2h makes oxide fully carry out fused salt
Reaction.
Step 3：The ultrasonic disperse in water is removed by what the product obtained after reaction was placed in, washing is dried, and obtains BaFe12O19
Presoma.Wherein the temperature of deionized water is 90 DEG C, and ultrasonic time 15min is washed 6 times, 100 DEG C of dry temperature.
Step 4：By Fe2O3、BaCl·2H2O and BaFe12O19The precursor B of powder1, after wet-milling, mixed slurry is obtained, so
60 mesh sieves are crossed after mixed slurry is dried afterwards, mixed powder C is obtained1；Wherein, BaFe12O19The precursor B of powder1Quality be
BaFe12O19The precursor B of powder1、Fe2O3With BaCl2H25%, BaCl of O gross masses2·2H2O is preparation Ba2Fe12O19Piece
Fused salt used by shape, it is Fe that it adds quality2O33 times of quality.
Step 5：By mixed powder C12h is incubated at 1200 DEG C makes oxide fully carry out fused salt reaction.
Step 6：The product obtained after reaction is placed in the ultrasonic disperse in water, is washed, dried.It is wherein used go from
The temperature of sub- water is 100 DEG C, and ultrasonic time 15min is washed 5 times, and dry temperature 60 C obtains sheet BaFe12O19Powder.
Step 7：Ti in molar ratio:Al:TiC=1.0:1.2:2.0, weigh Ti, Al and TiC that total amount is 12g, Ran Hou
Ball milling is carried out in ball mill, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains equal
Even powder simultaneously dries it at 60 DEG C；
Step 8：Dry batch mixing is protected with nitrogen, 1350 DEG C is heated to the heating rate of 8 DEG C/min, be incubated 1h,
Obtain Ti3AlC2Powder.
Step 9：By gained Ti in step 83AlC2Powder takes 5g and is immersed in the hydrofluoric acid of 100mL (concentration of hydrofluoric acid is
49%, buy in Chemical Reagent Co., Ltd., Sinopharm Group) in, using magnetic agitation, mixing speed is 500r/min, carries out corruption
Erosion reaction 6h, centrifugation is washed up to centrifuged supernatant pH value is between 5~6, by gained solid sample drying at room temperature 48h,
Ti after corroding through hydrofluoric acid3C2Powder；
Step 10：Weighing 6g absolute ethyl alcohols, 8g butanone, 3g oleins carries out a ball milling.
Step 11：Then to addition 0.6g polyvinyl butyral resins, the poly- second two of 0.5g in the product after ball milling in step 10
Alcohol and 0.5g dibutyl phthalate (DBP)s, carry out secondary ball milling.
Step 12：To addition 1g sheets BaFe in the product being added to after step 11 ball milling12O19Powder and 6g Ti3C2Powder
Body, the ball milling 2h in the case where rotating speed is 280r/min.
Step 13：The slurry that step 12 is mixed, is cast, and is cast 250 μm of the height of scraper, obtains stratiform
Ti3C2/BaFe12O19Composite wave-suction material.
Claims (10)
1. a kind of preparation method of lamellar composite absorbing material, it is characterised in that by absolute ethyl alcohol, butanone and olein
A ball milling is carried out, is well mixed, be subsequently adding polyvinyl butyral resin, polyethylene glycol and dibutyl phthalate (DBP), carried out
Secondary ball milling, is well mixed, and is subsequently adding sheet BaFe12O19Powder and through hydrofluoric acid corrode after Ti3C2Powder, ball milling is laggard
Row curtain coating, obtains lamellar composite absorbing material；Wherein, sheet BaFe12O19Powder and through hydrofluoric acid corrode after Ti3C2Powder
Mass ratio (0.5~1):(5~6).
2. a kind of preparation method of lamellar composite absorbing material according to claim 1, it is characterised in that sheet
BaFe12O19Powder and through hydrofluoric acid corrode after Ti3C2Powder gross mass is absolute ethyl alcohol, butanone, olein, poly- second
The 30%~80% of the gross mass of enol butyral, polyethylene glycol and dibutyl phthalate (DBP)；During curtain coating, the height of scraper is cast
200~250 μm of degree.
3. the preparation method of a kind of lamellar composite absorbing material according to claim 1, it is characterised in that absolute ethyl alcohol,
The mass ratio of butanone and olein is (2~6):(5~8):(1~3).
4. the preparation method of a kind of lamellar composite absorbing material according to claim 1, it is characterised in that polyvinyl alcohol contracts
The mass ratio of butyraldehyde, polyethylene glycol and dibutyl phthalate (DBP) is (0.2~0.6):(0.1~0.5):(0.1~0.5).
5. a kind of preparation method of lamellar composite absorbing material according to claim 1, it is characterised in that sheet
BaFe12O19Powder is prepared by procedure below：
1) according to chemical general formula BaFe12O19In mol ratio, by BaCO3With Fe2O3Mixing, adds NaCl mixed by ball milling
Close uniform, then dry, cross 60 mesh sieves, obtain mixed powder A1；Wherein, BaCO3With Fe2O3Gross mass and NaCl quality
Than being 1:(1~2)；
2) by step 1) obtained by mixed powder A1In 1000~1200 DEG C of 2~4h of pre-burning, washing obtains BaFe12O19Powder
Precursor B1；
3) by Fe2O3、BaCl·2H2O and BaFe12O19The precursor B of powder1, after wet-milling, mixed slurry is obtained, then will mixing
Slurry crosses 60 mesh sieves after drying, and obtains mixed powder C1, then by mixed powder C12~8h is calcined in 1000~1200 DEG C, is washed,
Obtain the sheet BaFe on (001) direction with orientation12O19Powder.
6. a kind of preparation method of lamellar composite absorbing material according to claim 4, it is characterised in that step 1) in ball
The rotating speed of mill is 500~600r/min, and the time of ball milling is 15~20h；Dry temperature be 60~100 DEG C, the time be 4~
8h；BaCl·2H2The quality of O is Fe2O32~3 times of quality, BaFe12O19The precursor B of powder1Quality be BaCl
2H2O、Fe2O3And BaFe12O19The precursor B of powder1The 5%-15% of gross mass.
7. the preparation method of a kind of lamellar composite absorbing material according to claim 1, it is characterised in that rotten through hydrofluoric acid
Ti after erosion3C2Powder is prepared by procedure below：Ti in molar ratio:Al:TiC=1.0:1.2:2.0, by Ti, Al and TiC, ball
Mill is well mixed, is sintered in atmosphere furnace after drying, and after then corroding through hydrofluoric acid, obtains the Ti after corroding through hydrofluoric acid3AlC2
Powder.
8. the preparation method of a kind of lamellar composite absorbing material according to claim 7, it is characterised in that used during sintering
Nitrogen is protected, and the temperature of sintering is 1350 DEG C, and the time of sintering is 1~4h.
9. the preparation method of a kind of lamellar composite absorbing material according to claim 8, it is characterised in that with 6~8 DEG C/
The heating rate of min is heated to 1350 DEG C.
10. the preparation method of a kind of lamellar composite absorbing material according to claim 7, it is characterised in that corrosion is specific
Process is：Product after 2~5g is sintered is immersed in the hydrofluoric acid solution of 60~100mL, and 2~6h of stirring makes corrosion completely,
It is then centrifuged for separating, washing is 5~6 up to centrifuged supernatant pH value, then by 24~48h of gained solid sample drying at room temperature.
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