CN106753238A - A kind of preparation method of lamination Wave suction composite material - Google Patents

A kind of preparation method of lamination Wave suction composite material Download PDF

Info

Publication number
CN106753238A
CN106753238A CN201611163166.0A CN201611163166A CN106753238A CN 106753238 A CN106753238 A CN 106753238A CN 201611163166 A CN201611163166 A CN 201611163166A CN 106753238 A CN106753238 A CN 106753238A
Authority
CN
China
Prior art keywords
powder
bafe
preparation
composite material
ball milling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201611163166.0A
Other languages
Chinese (zh)
Inventor
林营
刘潇
戴菁菁
杨海波
韩宁
王幸
孙雨佳
高淑雅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201611163166.0A priority Critical patent/CN106753238A/en
Publication of CN106753238A publication Critical patent/CN106753238A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/24—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of indefinite length
    • B29C41/32—Making multilayered or multicoloured articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure

Abstract

A kind of preparation method of lamination Wave suction composite material, is prepared for (001) Ba by molten-salt growth method first3Co2Fe24O41Flaky powder, Ba is prepared by sol-gal process3Co2Fe24O41Graininess powder, Ti is prepared by etch3C2MXene nano-sheet powders, the first tunic and Ti3C2It is to be effectively superimposed by superficial film adhesion between MXene films, after flow casting molding, the excellent lamination composite wave-suction material of absorbing property is obtained.The present invention uses casting technique, and material dispersion is uniform and thickness of film is homogeneous, and it is non-toxic to prepare casting slurry used, and human body will not be damaged.Present device is simple, and process stabilizing can be operated continuously, and production efficiency is high, is capable of achieving increasingly automated, reduces cost, material compactness and has good uniformity, and preparation method is simple.

Description

A kind of preparation method of lamination Wave suction composite material
Technical field
The invention belongs to material science, it is related to a kind of preparation method of lamination Wave suction composite material.
Background technology
With developing rapidly for electronic technology, radar and the communication technology, electromagenetic wave radiation has turned into after noise pollution, air Another big public hazards after pollution, water pollution, solid waste pollution.The electromagnetic interference (EMI) that electromagenetic wave radiation is produced not only can The normal operation of various electronic equipments is influenceed, and also has harm to the healthy of the mankind.Therefore, electricity of good performance is developed Electromagnetic wave shielding material, evolution electromagnetic environment have very urgent scientific meaning and reality need.Traditional absorbing material has to be inhaled The shortcomings of wave energy power is weak, density big, suction wave frequency band is narrow, it is impossible to meet the requirement of novel wave-absorbing material " thin, light, wide, strong ".Cause This, while improving and optimizating traditional absorbing material, does one's utmost to explore the focus that advanced composite material (ACM) is current absorbing material research. Composite is that the trend of modern material development realizes that performance complement and optimization are expected preparative by the compound of multiple material function The excellent material of energy.
Absorbing material needs to meet two principles：Impedance matching, electromagnetic wave incident is maximum to energy during material surface Into material internal；Attenuation characteristic, the electromagnetic wave into material needs rapid effective decay.Ferrite is research using more It is extensive a kind of, the research of inorganic magnetic and the multiple correlation of organic matter a lot, its single ferritic reflection loss Small, frequency bandwidth is narrow, and in order to improve its absorbing property, the method mainly taken is that chemically composited method (has two or more Ferrite or ferrite and conductive bluk recombination), its preparation technology is complicated, easily occurs chemical reaction in recombination process, Interfacial effect is complicated, and absorption property is poor.
The content of the invention
It is an object of the invention to provide a kind of preparation method of lamination Wave suction composite material, the composite wave-suction material has Excellent absorbing property, maximum reflection loss reaches -32.2dB, and preparation process is simple.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of lamination Wave suction composite material, comprises the following steps：
Step 1：By random Ba2Co2Fe12O22Powder and (001) BaFe12O19Flaky powder is 1 according to mol ratio:1 mixes Close, it is fused-salt medium to use NaCl, at 1250~1300 DEG C, 6~10h of insulation makes oxide carry out abundant fused salt reaction, obtains (001)Ba3Co2Fe24O41Flaky powder；
Step 2：By solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carry out secondary ball milling, It is subsequently adding (001) Ba3Co2Fe24O41Flaky powder and graininess Ba3Co2Fe24O41Powder, is cast, and obtains ground floor Film；Wherein, by mass percentage, graininess Ba3Co2Fe24O41The mass percent of powder is 5%~35%, (001) Ba3Co2Fe24O41The mass percent of flaky powder is 65%~95%；
Step 3：By solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carry out secondary ball milling, It is subsequently adding Ti3C2- MXene nanometer sheets, are cast on the first tunic, obtain lamination Wave suction composite material.
Further improvement of the invention is that solvent is absolute ethyl alcohol, and dispersant is butanone mixed with olein Compound；Binding agent is polyvinyl butyral resin, and plasticizer is the mixture of dibutyl phthalate (DBP) and polyethylene glycol.
Further improvement of the invention is that the mass ratio of absolute ethyl alcohol, butanone and olein is (1~3):(2 ~3):(0.05~1.5)；The mass ratio of polyvinyl butyral resin, dibutyl phthalate (DBP) and polyethylene glycol for (2.5~ 3.0):1:1, the gross mass of solvent, dispersant, bonding agent and plasticizer and (001) Ba in step 13Co2Fe24O41Flaky powder With graininess Ba3Co2Fe24O41The total mass ratio of powder is 7:3；Solvent, dispersant, bonding agent and plasticizer is total in step 2 Quality and Ti3C2The mass ratio of-MXene nanometer sheets is 8:2.
The present invention is further improved, 200-250 μm of the height of scraper when being cast in step 2, when being cast in step 3 230-280 μm of the height of scraper.
The present invention is further improved, the random Ba2Co2Fe12O22Powder is prepared by procedure below：
By chemical formula formula by Ba2Co2Fe12O22Analytically pure CoO, BaCO3、Fe2O3It is mixed by 20~24h of ball milling after preparation Close uniform, then dry, sieve, briquetting, then through 1230~1270 DEG C of pre-burnings 3~6 hours, blocks of solid is obtained, then by block Shape solid crosses 120 mesh sieves and obtains Ba after crushing2Co2Fe12O22Powder.
The present invention is further improved, (001) BaFe12O19Flaky powder is prepared by procedure below：
Step 1：Will be according to BaFe12O19In mol ratio weigh BaCO respectively3、Fe2O3And fused salt ball milling mixing is equal It is even, 2~4h is then incubated at 1150~1200 DEG C, obtain BaFe12O19Presoma；
Step 2：By Fe2O3And BaCl2·2H2O mixes, and is subsequently adding BaFe12O19Presoma, after ball milling mixing is uniform, 6~10h is incubated at 1200~1250 DEG C, the BaFe that there is orientation in (001) direction is obtained12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder；Wherein, BaFe12O19The quality of presoma is Fe2O3And BaCl2·2H2The 5~10% of O gross masses； BaCl2·2H2The addition of O is Fe2O32~3 times of quality.
Further improvement of the invention is that fused salt is NaCl in step 1, and the quality of NaCl is BaCO3With Fe2O3Total matter 1~2 times of amount.
The present invention is further improved, graininess Ba3Co2Fe24O41Powder is prepared by procedure below：
According to chemical general formula Ba3Co2Fe24O41, barium nitrate, five water cobalt nitrates, nine water ferric nitrates are added in ultra-pure water, Add citric acid and be configured to solution, stirred at 80 DEG C, be then dropwise added drop-wise in solution ammoniacal liquor, make pH=7, stir 3~6h is mixed, colloidal sol is formed, dried, obtain black xerogel；Then 3~6h is calcined at 1230~1260 DEG C, graininess is obtained Ba3Co2Fe24O41Powder；Wherein, the amount of total material of the amount of the material of citric acid and barium ions, cobalt ions and iron ion It is identical；The ratio of barium nitrate, the gross mass of five water cobalt nitrates and nine water ferric nitrates and ultra-pure water is 20g：(40-60)mL.
The present invention is further improved, Ti3C2- MXene nanometer sheets are prepared by procedure below：Ti in molar ratio: Al:TiC=1.0:1.2:2.0, Ti, Al and TiC are weighed, after being well mixed, it is heated to the heating rate of 5~8 DEG C/min 1300~1360 DEG C, and 3~6h is incubated, obtain Ti3AlC2Powder, by gained Ti3AlC2Powder take 4~7g be immersed in 60~ In the hydrofluoric acid of 80mL, 3~6h of corrosion reaction is carried out, obtain the Ti after corroding through hydrofluoric acid3C2Powder.
Compared with prior art, the device have the advantages that：The present invention is prepared for (001) by molten-salt growth method first Ba3Co2Fe24O41Flaky powder, Ba is prepared by sol-gal process3Co2Fe24O41Graininess powder, is prepared by etch Ti3C2- MXene nano-sheet powders, wherein, (001) Ba3Co2Fe24O41The mass percent of flaky powder accounts for the 10% of total amount, 0.1(001)Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41Film (i.e. the first tunic) and Ti3C2It is by surface between-MXene films Membranous layer binding force is effectively superimposed, and after flow casting molding, 0.1 (001) excellent Ba of absorbing property is obtained3Co2Fe24O41- 0.9Ba3Co2Fe24O41/Ti3C2- MXene lamination composite wave-suction materials.The present invention uses casting technique, material dispersion it is uniform and The thickness of film is homogeneous, and prepares casting slurry nontoxicity used, and human body will not be damaged.Present device is simple, Process stabilizing, can operate continuously, and production efficiency is high, achievable increasingly automated, reduce cost, material compactness and uniformity Well, and preparation method is simple.
It is an object of the invention to provide 0.1 (001) Ba of one kind3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2-MXene Absorbing material its preparation method, the uniformity of the obtained curtain coating thick film of the present invention preferably makes flaky powder uniformly tile On casting films band.The saturation magnetization of composite is 7.15emu/g, and remanent magnetization is 1.57emu/g, inhales ripple material The thickness of material is 2mm, and preferably, the absorption band width that absorption maximum can reach below -32.2dB, -10dB is absorbing property 7GHz。
Further, sheet Ba is prepared using molten-salt growth method in the present invention3Co2Fe24O41, prepared by a step etch Ti3C2- MXene nanometer sheets, 0.1 (001) Ba is prepared beneficial to later stage the tape casting3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- Mxene lamination thick films.Absorbing material good dispersion prepared by the method, thickness is uniform, and compactness is good and can generate on a large scale.
Brief description of the drawings
Fig. 1 is (001) Ba prepared by molten-salt growth method3Co2Fe24O41Flaky powder, the XRD obtained by 1300 DEG C of sintering.
Fig. 2 is Ba prepared by sol-gal process3Co2Fe24O41Powder, the XRD obtained by 1250 DEG C of sintering.
Fig. 3 is Ti3C2The XRD of-MXene nano-sheet powders.
Fig. 4 is 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene curtain coating gained composites SEM schemes.
Fig. 5 is 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene curtain coating gained composites Hysteresis curve.
Fig. 6 is 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene, when thickness is 2mm, is cast institute Obtain the reflection loss figure of composite.
Fig. 7 is 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene, when thickness is 3mm, is cast institute Obtain the reflection loss figure of composite.
Fig. 8 is 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene, when thickness is 3.5mm, curtain coating The reflection loss figure of gained composite.
Specific embodiment
By specific embodiment, the present invention is described in detail below in conjunction with the accompanying drawings.
In the present invention it is compressing be specifically the casting films that will fold as in mould, after the demoulding, by thick film lamination, hot pressing Cyclization, 180 DEG C of heating-up temperature, pressurize 0.5~1MPa, 30~60s of pressurize.
Embodiment 1
One kind (001) Ba3Co2Fe24O41Flaky powder fills random powder and Ti3C2- Mxene nanometer sheets lamination is inhaled ripple and is answered The preparation method of condensation material, it is characterised in that the chemical expression of the absorbing material is 0.1 (001) Ba3Co2Fe24O41- 0.9Ba3Co2Fe24O41/Ti3C2-MXene。
Above-mentioned 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2The preparation method of-MXene absorbing materials, Comprise the following steps：
(1) by BaCO3, Fe2O3, after NaCl electronic balances are accurately weighed, it is placed in ball grinder, it is sufficiently mixed It is even, take out dry for standby.Wherein BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:1, BaCO3With Fe2O3Amount press According to by chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, the rotating speed of ball mill It is 500r/min, ball milling 18h, to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh sieves to temperature in an oven.
(2) raw material that will be prepared obtains BaFe in 1150 DEG C of pre-burning 4h12O19Presoma, is then entered with the ultra-pure water of heat Row washing, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2·2H2O and BaFe12O19Presoma ball milling mixing is uniform, then in 1200 DEG C of calcinings 10h, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing, filtering is dried to obtain sheet (001) BaFe12O19Flaky powder, It is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2·2H2The addition of O is Fe2O32 times of quality；BaFe12O19Forerunner The quality of body is BaCl2·2H2O、Fe2O3And BaFe12O19The 5% of presoma gross mass.
(4) by chemical general formula Ba2Co2Fe12O22, by BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, placement The ball milling 24h in ball grinder, then dries, sieving, and then briquetting is incubated 6h into phase at 1230 DEG C, crosses 120 mesh sieve, obtains To random Ba2Co2Fe12O22Powder, is designated as Co2Y。
The random Ba that will be obtained2Co2Fe12O22Powder and above-mentioned (001) BaFe for preparing12O19Powder is according to mol ratio It is 1:1 mixing, adds NaCl, and electric stirring mixing 12h, the quality that NaCl is added is equal to random Ba2Co2Fe12O22Powder with (001)BaFe12O19Powder quality summation, being incubated 10h at 1250 DEG C makes oxide carry out abundant fused salt reaction, then with heat Ultra-pure water is washed, and until sodium chloride is washed clean, filtering is dried, and obtains (001) Ba3Co2Fe24O41Flaky powder.
(5) according to chemical general formula Ba3Co2Fe24O41, barium nitrate, five water cobalt nitrates, nine water ferric nitrates are added to ultra-pure water In, add citric acid and be configured to solution, stirred at 80 DEG C, then ammoniacal liquor is dropwise added drop-wise in solution, make pH= 7,3~6h is stirred, colloidal sol is formed, dry, obtain black xerogel；Then 6h is calcined at 1230 DEG C, obtains graininess Ba3Co2Fe24O41Powder；Wherein, the amount of total material of the amount of the material of citric acid and barium ions, cobalt ions and iron ion It is identical；The ratio of barium nitrate, the gross mass of five water cobalt nitrates and nine water ferric nitrates and ultra-pure water is 20g：40mL.
(6) Ti in molar ratio:Al:TiC=1.0:1.2:2.0, Ti, Al and TiC that total amount is 15g are weighed, then in ball Ball milling is carried out in grinding machine, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains uniform Powder simultaneously dries it at 50 DEG C；Dry batch mixing is protected with nitrogen, 1300 are heated to the heating rate of 5 DEG C/min DEG C, 6h is incubated, obtain Ti3AlC2Powder.
(7) gained Ti3AlC2Powder takes 4g and is immersed in the hydrofluoric acid of 60mL (concentration of hydrofluoric acid is 49%, is bought in traditional Chinese medicines Chemical reagent Co., Ltd of group) in, using magnetic agitation, mixing speed is 500r/min, carries out corrosion reaction 3h, centrifugation point From washing, by gained solid sample drying at room temperature 31h, obtains rotten through hydrofluoric acid up to centrifuged supernatant pH value is between 5~6 Ti after erosion3C2Powder.
(8) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add (001) Ba3Co2Fe24O41Flaky powder and graininess Ba3Co2Fe24O41Powder, is cast, the height of scraper during curtain coating 200 μm, obtain the first tunic；Wherein, by mass percentage, graininess Ba3Co2Fe24O41The mass percent of powder is 90%, (001) Ba3Co2Fe24O41The mass percent of flaky powder is 10%, solvent, dispersant, bonding agent and plasticizer Gross mass and Ba3Co2Fe24O41The mass ratio of powder is 7:3.
(9) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add Ti3C2- MXene nanometer sheets, are cast on the first tunic, 230 μm of the height of scraper during curtain coating, are obtained lamination and are inhaled ripple Composite；Wherein, the gross mass of solvent, dispersant, bonding agent and plasticizer with through hydrofluoric acid corrode after Ti3C2Powder Mass ratio is 8:2.
Solvent is absolute ethyl alcohol in step (8) and (9), and dispersant is the mixture of butanone and olein；Bond Agent is polyvinyl butyral resin, and plasticizer is the mixture of dibutyl phthalate (DBP) and polyethylene glycol.
Specifically, the mass ratio of absolute ethyl alcohol, butanone and olein is 1:2:0.05；Polyvinyl butyral resin, The mass ratio of dibutyl phthalate (DBP) and polyethylene glycol is 2.5:1:1.
(10) after the demoulding, dry, by thick film lamination, hot pressing cyclization, 180 DEG C of heating-up temperature, pressurization 0.5MPa, pressurize 60s.
It will be seen from figure 1 that the Ba for preparing3Co2Fe24O41Without dephasign generation, the oriented growth on (001) direction.
Figure it is seen that the Ba for preparing3Co2Fe24O41Random powder is generated without dephasign.
From figure 3, it can be seen that Ti after the corrosion for preparing3C2Without dephasign generation.
As can be seen from Figure 4, (001) Ba3Co2Fe24O41Template grains are 5~10 μm or so of sheet, Ba3Co2Fe24O41At random Powder grain size is 80nm~100nm or so, Ba3Co2Fe24O41Content is less, Ti after corrosion3C2Into laminar structured, it is combined Material compactness is good.
From fig. 5, it can be seen that the saturation magnetization of composite is 5.05emu/g, remanent magnetization is 1.08emu/g, coercive field is 355.89Oe.
From fig. 6, it can be seen that thickness of composite material is 2mm, and in 8.7GHz, maximum reflection loss -33.2dB, -10dB Following absorption band width is 3.4GHz (6.8~10.2GHz)
From figure 7 it can be seen that thickness of composite material is 3mm, and in 5.4GHz, maximum reflection loss -24.3dB, -10dB Following absorption band width is 2.3GHz (4.5~6.8GHz).
From figure 8, it is seen that thickness of composite material is 4mm, and in 16.5GHz, maximum reflection loss -28.7dB, -10dB Following absorption band width is 7.1GHz (3.2~5.8GHz) and (13.5~18GHz).
Embodiment 2
One kind (001) Ba3Co2Fe24O41Flaky powder fills its random powder and Ti3C2- Mxene nanometer sheets lamination inhales ripple The preparation method of composite, it is characterised in that the chemical expression of the absorbing material is 0.1 (001) Ba3Co2Fe24O41- 0.9Ba3Co2Fe24O41/Ti3C2-Mxene。
Above-mentioned 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2The preparation method of-Mxene absorbing materials, Comprise the following steps：
(1) by raw material BaCO3, Fe2O3, after NaCl electronic balances are accurately weighed, it is placed in ball grinder, it is fully mixed Close uniform, take out dry for standby.Wherein raw material BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:1.4, BaCO3With Fe2O3Amount according to by chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, ball The rotating speed of grinding machine is 500r/min, ball milling 18h, and to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh to temperature in an oven Sieve.
(2) raw material that will be prepared obtains BaFe in 1170 DEG C of pre-burning 3.5h12O19Presoma.Then with the ultra-pure water of heat Washed, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2·2H2O and BaFe12O19Presoma ball milling mixing is uniform, then calcines 9h at 1220 DEG C Obtain sheet (001) BaFe12O19Flaky powder, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing, filtering is dried to obtain Sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2·2H2The addition of O is Fe2O32.2 times of quality；BaFe12O19The quality of presoma is BaCl2·2H2O、Fe2O3And BaFe12O19Presoma gross mass 7%.
(4) by chemical general formula Ba2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, Ball milling 23h in ball grinder is placed on, is then dried, sieved, then briquetting is incubated 5h into phase at 1240 DEG C, crosses 120 mesh sieves Son, obtains random Ba2Co2Fe12O22Powder, is designated as Co2Y, the random Ba that will be obtained2Co2Fe12O22Powder is prepared with above-mentioned (001)BaFe12O19(as template) is 1 according to mol ratio:1 mixing, adds NaCl electric stirring mixing 14h, NaCl addition Quality be equal to Ba2Co2Fe12O22Powder and (001) BaFe12O191.2 times of flaky powder quality summation, at 1270 DEG C, insulation 9h makes oxide carry out abundant fused salt reaction, is then washed with the ultra-pure water of heat, until sodium chloride is washed clean, mistake Filter, dries, and obtains (001) Ba3Co2Fe24O41Flaky powder.
(5) according to chemical general formula Ba3Co2Fe24O41, barium nitrate, five water cobalt nitrates, nine water ferric nitrates are added to ultra-pure water In, add citric acid and be configured to solution, stirred at 80 DEG C, then ammoniacal liquor is dropwise added drop-wise in solution, make pH= 7,3~6h is stirred, colloidal sol is formed, dry, obtain black xerogel；Then 5h is calcined at 1240 DEG C, obtains graininess Ba3Co2Fe24O41Powder；Wherein, the amount of total material of the amount of the material of citric acid and barium ions, cobalt ions and iron ion It is identical；The ratio of barium nitrate, the gross mass of five water cobalt nitrates and nine water ferric nitrates and ultra-pure water is 20g：60mL.
(6) Ti in molar ratio:Al:TiC=1.0:1.2:2.0, Ti, Al and TiC that total amount is 20g are weighed, then in ball Ball milling is carried out in grinding machine, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains uniform Powder simultaneously dries it at 50 DEG C；Dry batch mixing is protected with nitrogen, 1320 are heated to the heating rate of 6 DEG C/min DEG C, 5h is incubated, obtain Ti3AlC2Powder.
(7) gained Ti3AlC2Powder takes 5g and is immersed in the hydrofluoric acid of 60mL (concentration of hydrofluoric acid is 49%, is bought in traditional Chinese medicines Chemical reagent Co., Ltd of group) in, using magnetic agitation, mixing speed is 500r/min, carries out corrosion reaction 5h, centrifugation point From washing, by gained solid sample drying at room temperature 32h, obtains rotten through hydrofluoric acid up to centrifuged supernatant pH value is between 5~6 Ti after erosion3C2Powder.
(8) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add (001) Ba3Co2Fe24O41Flaky powder and graininess Ba3Co2Fe24O41Powder, is cast, the height of scraper during curtain coating 210 μm, obtain the first tunic；Wherein, by mass percentage, graininess Ba3Co2Fe24O41The mass percent of powder is 90%, (001) Ba3Co2Fe24O41The mass percent of flaky powder is 10%, solvent, dispersant, bonding agent and plasticizer Gross mass and Ba3Co2Fe24O41The mass ratio of powder is 7:3.
(9) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add Ti3C2- MXene nanometer sheets, are cast on the first tunic, during curtain coating 240 μm of the height of scraper obtain lamination inhale ripple answer Condensation material.Wherein, the gross mass of solvent, dispersant, bonding agent and plasticizer with through hydrofluoric acid corrode after Ti3C2The matter of powder Amount is than being 8:2.
Solvent is absolute ethyl alcohol in step (8) and (9), and dispersant is the mixture of butanone and olein；Bond Agent is polyvinyl butyral resin, and plasticizer is the mixture of dibutyl phthalate (DBP) and polyethylene glycol.
Specifically, the mass ratio of absolute ethyl alcohol, butanone and olein is 2:2.5:1；Polyvinyl butyral resin, neighbour The mass ratio of phthalic acid dibutylester and polyethylene glycol is 2.8:1:1.
(10) after the demoulding, dry, by thick film lamination, hot pressing cyclization, 180 DEG C of heating-up temperature, pressurization 0.6MPa, pressurize 50s.
0.1 (001) Ba for preparing is proved after tested3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene inhales ripple material Material, template uniformly spreads over Ba3Co2Fe24O41In matrix, there is excellent absorbing property in the range of 2-18GHz.
Embodiment 3
One kind (001) Ba3Co2Fe24O41Flaky powder fills Ba3Co2Fe24O41The absorbing material and its system of granular base Preparation Method, it is characterised in that the chemical expression of the absorbing material is 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/ Ti3C2-MXene。
Above-mentioned 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2The preparation method of-MXene absorbing materials, Comprise the following steps：
(1) by raw material BaCO3, Fe2O3, after NaCl electronic balances are accurately weighed, it is placed in ball grinder, it is fully mixed Close uniform, take out dry for standby.Wherein raw material BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:1.6, BaCO3With Fe2O3Amount according to by chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, ball The rotating speed of grinding machine is 500r/min, ball milling 18h, and to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh to temperature in an oven Sieve.
(2) raw material that will be prepared obtains BaFe in 1180 DEG C of pre-burning 3h12O19Presoma.Then entered with the ultra-pure water of heat Row washing, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2·2H2O and BaFe12O19Presoma ball milling mixing is uniform, then calcines 8h at 1240 DEG C Obtain sheet (001) BaFe12O19Flaky powder, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing, filtering is dried, obtained Sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2·2H2The addition of O is Fe2O32.6 times of quality；BaFe12O19The quality of presoma is BaCl2·2H2O、Fe2O3And BaFe12O19Presoma gross mass 8%.
(4) by chemical general formula Ba2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, Ball milling 21h in ball grinder is placed on, is then dried, sieved, then briquetting is incubated 4h into phase at 1250 DEG C, crosses 120 mesh sieves Son, obtains random Ba2Co2Fe12O22Powder, is designated as Co2Y, the random Ba that will be obtained2Co2Fe12O22Powder is prepared with above-mentioned (001)BaFe12O19Powder is 1 according to mol ratio:1 mixing, adds NaCl electric stirring mixing 16h, the quality that NaCl is added Equal to random Ba2Co2Fe12O22Powder and (001) BaFe12O191.4 times of powder quality summation, at 1260 DEG C, insulation 8h makes oxygen Compound carries out abundant fused salt reaction, is then washed with the ultra-pure water of heat, and until sodium chloride is washed clean, filtering is dried, Obtain (001) Ba3Co2Fe24O41Flaky powder.
(5) according to chemical general formula Ba3Co2Fe24O41, barium nitrate, five water cobalt nitrates, nine water ferric nitrates are added to ultra-pure water In, add citric acid and be configured to solution, stirred at 80 DEG C, then ammoniacal liquor is dropwise added drop-wise in solution, make pH= 7,3~6h is stirred, colloidal sol is formed, dry, obtain black xerogel；Then 4h is calcined at 1250 DEG C, obtains graininess Ba3Co2Fe24O41Powder；Wherein, the amount of total material of the amount of the material of citric acid and barium ions, cobalt ions and iron ion It is identical；The ratio of barium nitrate, the gross mass of five water cobalt nitrates and nine water ferric nitrates and ultra-pure water is 20g：40mL.
(6) Ti in molar ratio:Al:TiC=1.0:1.2:2.0, Ti, Al and TiC that total amount is 24g are weighed, then in ball Ball milling is carried out in grinding machine, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains uniform Powder simultaneously dries it at 50 DEG C；Dry batch mixing is protected with nitrogen, 1350 are heated to the heating rate of 7 DEG C/min DEG C, 4h is incubated, obtain Ti3AlC2Powder.
(7) gained Ti3AlC2Powder takes 6g and is immersed in the hydrofluoric acid of 70mL (concentration of hydrofluoric acid is 49%, is bought in traditional Chinese medicines Chemical reagent Co., Ltd of group) in, using magnetic agitation, mixing speed is 500r/min, carries out corrosion reaction 5.5h, centrifugation Separate, washing is until centrifuged supernatant pH value between 5~6, gained solid sample drying at room temperature 33h is obtained through hydrofluoric acid Ti after corrosion3C2Powder.
(8) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add (001) Ba3Co2Fe24O41Flaky powder and graininess Ba3Co2Fe24O41Powder, is cast, the height of scraper during curtain coating 230 μm, obtain the first tunic；Wherein, by mass percentage, graininess Ba3Co2Fe24O41The mass percent of powder is 90%, (001) Ba3Co2Fe24O41The mass percent of flaky powder is 10%, solvent, dispersant, bonding agent and plasticizer Gross mass and Ba3Co2Fe24O41The mass ratio of powder is 7:3.
(9) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add Ti3C2- MXene nanometer sheets, are cast on the first tunic, 260 μm of the height of scraper during curtain coating, are obtained lamination and are inhaled ripple Composite；Wherein, the gross mass of solvent, dispersant, bonding agent and plasticizer with through hydrofluoric acid corrode after Ti3C2Powder Mass ratio is 8:2.
Solvent is absolute ethyl alcohol in step (8) and (9), and dispersant is the mixture of butanone and olein；Bond Agent is polyvinyl butyral resin, and plasticizer is the mixture of dibutyl phthalate (DBP) and polyethylene glycol.
Specifically, the mass ratio of absolute ethyl alcohol, butanone and olein is 3:31.5；Polyvinyl butyral resin, neighbour The mass ratio of phthalic acid dibutylester and polyethylene glycol is 3:1:1.
(10) after the demoulding, dry, by thick film lamination, hot pressing cyclization, 180 DEG C of heating-up temperature, pressurization 0.8MPa, pressurize 40s.
0.1 (001) Ba for preparing is proved after tested3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene inhales ripple material Material, template is uniformly spread in random powder, has excellent absorbing property in the range of 2-18GHz.
Embodiment 4
One kind (001) Ba3Co2Fe24O41Flaky powder fills absorbing material of its random powder and preparation method thereof, and it is special Levy and be, the chemical expression of the absorbing material is 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2-MXene。
Above-mentioned 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2The preparation method of-MXene absorbing materials, Comprise the following steps：
(1) by raw material BaCO3, Fe2O3, after NaCl electronic balances are accurately weighed, it is placed in ball grinder, it is fully mixed Close uniform, take out dry for standby.Wherein raw material BaCO3, Fe2O3The mass ratio of quality summation and NaCl be 1:2, BaCO3With Fe2O3Amount according to by chemical general formula BaFe12O19Weighed；Material used by ball milling, ball, the mass ratio of alcohol is 1：2：1, ball The rotating speed of grinding machine is 500r/min, ball milling 18h, and to place 7h at 98 DEG C, taking-up mixed powder crosses 60 mesh to temperature in an oven Sieve.
(2) raw material that will be prepared obtains BaFe in 1200 DEG C of pre-burning 2h12O19Presoma.Then entered with the ultra-pure water of heat Row washing, until sodium chloride is washed clean.
(3) by Fe2O3、BaCl2·2H2O and BaFe12O19Presoma ball milling mixing is uniform, then calcines 6h at 1250 DEG C Obtain sheet (001) BaFe12O19Flaky powder, is subsequently adding the ultra-pure water of heat, and ultrasonic disperse, washing, filtering is dried, obtained Sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2·2H2The addition of O is Fe2O33 times of quality；BaFe12O19The quality of presoma is BaCl2·2H2O、Fe2O3And BaFe12O19Presoma gross mass 10%.
(4) by chemical general formula Ba2Co2Fe12O22, by raw material BaCO3, Fe2O3, CoO, after accurately being weighed with electronic balance, Ball milling 24h in ball grinder is placed on, is then dried, sieved, then briquetting is incubated 3h into phase at 1260 DEG C, crosses 120 mesh sieves Son, obtains sheet (001) BaFe12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder.Wherein, BaCl2·2H2O's Addition is Fe2O32 times of quality；BaFe12O19The quality of presoma is BaCl2·2H2O、Fe2O3And BaFe12O19Presoma The 5% of gross mass.Ba2Co2Fe12O22Powder and above-mentioned (001) BaFe for preparing12O19Powder is 1 according to mol ratio:1 powder Body, NaCl electric stirring mixing 16h, the quality that NaCl is added is equal to Ba2Co2Fe12O22Powder and (001) BaFe12O19Powder matter 2 times of amount summation, at 1300 DEG C, insulation 6h makes oxide carry out abundant fused salt reaction, is then washed with the ultra-pure water of heat, Until sodium chloride is washed clean, filtering is dried, and obtains (001) Ba3Co2Fe24O41Flaky powder.
(5) according to chemical general formula Ba3Co2Fe24O41, barium nitrate, five water cobalt nitrates, nine water ferric nitrates are added to ultra-pure water In, add citric acid and be configured to solution, stirred at 80 DEG C, then ammoniacal liquor is dropwise added drop-wise in solution, make pH= 7,3~6h is stirred, colloidal sol is formed, dry, obtain black xerogel；Then 3h is calcined at 1260 DEG C, obtains graininess Ba3Co2Fe24O41Powder；Wherein, the amount of total material of the amount of the material of citric acid and barium ions, cobalt ions and iron ion It is identical；The ratio of barium nitrate, the gross mass of five water cobalt nitrates and nine water ferric nitrates and ultra-pure water is 20g：40mL.
(6) Ti in molar ratio:Al:TiC=1.0:1.2:2.0, Ti, Al and TiC that total amount is 27g are weighed, then in ball Ball milling is carried out in grinding machine, drum's speed of rotation is 600r/min, expected:Ball:Ethanol=1:2:1 (mass ratio)；Ball milling 1h obtains uniform Powder simultaneously dries it at 50 DEG C；Dry batch mixing is protected with nitrogen, 1360 are heated to the heating rate of 8 DEG C/min DEG C, 3h is incubated, obtain Ti3AlC2Powder.
(7) gained Ti3AlC2Powder takes 7g and is immersed in the hydrofluoric acid of 70mL (concentration of hydrofluoric acid is 49%, is bought in traditional Chinese medicines Chemical reagent Co., Ltd of group) in, using magnetic agitation, mixing speed is 500r/min, carries out corrosion reaction 6h, centrifugation point From washing, by gained solid sample drying at room temperature 34h, obtains rotten through hydrofluoric acid up to centrifuged supernatant pH value is between 5~6 Ti after erosion3C2Powder.
(8) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add (001) Ba3Co2Fe24O41Flaky powder and graininess Ba3Co2Fe24O41Powder, is cast, the height of scraper during curtain coating 220 μm, obtain the first tunic；Wherein, by mass percentage, graininess Ba3Co2Fe24O41The mass percent of powder is 90%, (001) Ba3Co2Fe24O41The mass percent of flaky powder is 10%, solvent, dispersant, bonding agent and plasticizer Gross mass and Ba3Co2Fe24O41The mass ratio of powder is 7:3.
(9) by solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carries out secondary ball milling, then Add Ti3C2- MXene nanometer sheets, after the first tunic is air-dried 30min, are cast on the first tunic, are scraped during curtain coating 250 μm of the height of knife, obtains lamination Wave suction composite material；Wherein, the gross mass of solvent, dispersant, bonding agent and plasticizer with Ti after corroding through hydrofluoric acid3C2The mass ratio of powder is 8:2.
Solvent is absolute ethyl alcohol in step (8) and (9), and dispersant is the mixture of butanone and olein；Bond Agent is polyvinyl butyral resin, and plasticizer is the mixture of dibutyl phthalate (DBP) and polyethylene glycol.
Specifically, the mass ratio of absolute ethyl alcohol, butanone and olein is 3:3:1.5；Polyvinyl butyral resin, neighbour The mass ratio of phthalic acid dibutylester and polyethylene glycol is 3:1:1.
(10) after the demoulding, dry, by thick film lamination, hot pressing cyclization, 180 DEG C of heating-up temperature, pressurization 1MPa, pressurize 30s.
0.1 (001) Ba for preparing is proved after tested3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- MXene inhales ripple material Material, template is uniformly spread in random powder, has excellent absorbing property in the range of 2-18GHz.
The present invention prepares 0.1 (001) Ba by the tape casting3Co2Fe24O41-0.9Ba3Co2Fe24O41/Ti3C2- Mxene laminations Thick film.By organic matter and 0.1 (001) Ba3Co2Fe24O41-0.9Ba3Co2Fe24O41Powder, organic matter and Ti3C2- Mxene nanometers Piece distinguishes ball milling mixing, and lamination curtain coating, hot pressing is then discharged out organic matter.Prepared (001) using molten-salt growth method in the present invention Ba3Co2Fe24O41Flaky powder, using sol-gal process prepare Ba3Co2Fe24O41Graininess powder, existed using a step etch Corrode Ti in hydrofluoric acid3AlC2Prepare Ti3C2- Mxene nanometer sheets.The tape casting is used afterwards, prepares the thick film of directional profile, It is hot-forming.Equipment is simple, and production efficiency is high, and automatization level is high, and performance is uniform, you can the excellent and big rule of absorbing property are obtained The Ba of mould production3Co2Fe24O41/Ti3C2- Mxene nanometer sheet lamination Wave suction composite materials.

Claims (9)

1. a kind of preparation method of lamination Wave suction composite material, it is characterised in that comprise the following steps：
Step 1：By random Ba2Co2Fe12O22Powder and (001) BaFe12O19Flaky powder is 1 according to mol ratio:1 mixing, uses NaCl is fused-salt medium, and at 1250~1300 DEG C, 6~10h of insulation makes oxide carry out abundant fused salt reaction, obtains (001) Ba3Co2Fe24O41Flaky powder；
Step 2：By solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carry out secondary ball milling, then Add (001) Ba3Co2Fe24O41Flaky powder and graininess Ba3Co2Fe24O41Powder, is cast, and obtains the first tunic；Its In, by mass percentage, graininess Ba3Co2Fe24O41The mass percent of powder is 5%~35%, (001) Ba3Co2Fe24O41The mass percent of flaky powder is 65%~95%；
Step 3：By solvent and dispersant, after carrying out a ball milling, bonding agent and plasticizer are added, carry out secondary ball milling, then Add Ti3C2- MXene nanometer sheets, are cast on the first tunic, obtain lamination Wave suction composite material.
2. the preparation method of a kind of lamination Wave suction composite material according to claim 1, it is characterised in that solvent is anhydrous Ethanol, dispersant is the mixture of butanone and olein；Binding agent is polyvinyl butyral resin, and plasticizer is adjacent benzene two The mixture of formic acid dibutylester and polyethylene glycol.
3. the preparation method of a kind of lamination Wave suction composite material according to claim 2, it is characterised in that absolute ethyl alcohol, Butanone is (1~3) with the mass ratio of olein:(2~3):(0.05~1.5)；Polyvinyl butyral resin, O-phthalic The mass ratio of sour dibutylester and polyethylene glycol is (2.5~3.0):1:1, solvent, dispersant, bonding agent and plasticizer in step 1 Gross mass and (001) Ba3Co2Fe24O41Flaky powder and graininess Ba3Co2Fe24O41The total mass ratio of powder is 7:3；Step The gross mass and Ti of solvent, dispersant, bonding agent and plasticizer in 23C2The mass ratio of-MXene nanometer sheets is 8:2.
4. the preparation method of a kind of lamination Wave suction composite material according to claim 1, it is characterised in that flowed in step 2 200-250 μm of the height of time delay scraper, 230-280 μm of the height of scraper when being cast in step 3.
5. the preparation method of a kind of lamination Wave suction composite material according to claim 1, it is characterised in that described random Ba2Co2Fe12O22Powder is prepared by procedure below：
By chemical formula formula by Ba2Co2Fe12O22Analytically pure CoO, BaCO3、Fe2O3Mix equal by 20~24h of ball milling after preparation It is even, then dry, sieve, briquetting, then through 1230~1270 DEG C of pre-burnings 3~6 hours, blocks of solid is obtained, it is then that bulk is solid Body crosses 120 mesh sieves and obtains Ba after crushing2Co2Fe12O22Powder.
6. the preparation method of a kind of lamination Wave suction composite material according to claim 1, it is characterised in that (001) BaFe12O19Flaky powder is prepared by procedure below：
Step 1：Will be according to BaFe12O19In mol ratio weigh BaCO respectively3、Fe2O3And fused salt ball milling mixing is uniform, so 2~4h is incubated at 1150~1200 DEG C afterwards, BaFe is obtained12O19Presoma；
Step 2：By Fe2O3And BaCl2·2H2O mixes, and is subsequently adding BaFe12O19Presoma, after ball milling mixing is uniform, 1200 6~10h is incubated at~1250 DEG C, the BaFe that there is orientation in (001) direction is obtained12O19Flaky powder, is designated as (001) BaFe12O19Flaky powder；Wherein, BaFe12O19The quality of presoma is Fe2O3And BaCl2·2H2The 5~10% of O gross masses； BaCl2·2H2The addition of O is Fe2O32~3 times of quality.
7. the preparation method of a kind of lamination Wave suction composite material according to claim 6, it is characterised in that melted in step 1 Salt is NaCl, and the quality of NaCl is BaCO3With Fe2O31~2 times of gross mass.
8. a kind of preparation method of lamination Wave suction composite material according to claim 1, it is characterised in that graininess Ba3Co2Fe24O41Powder is prepared by procedure below：
According to chemical general formula Ba3Co2Fe24O41, barium nitrate, five water cobalt nitrates, nine water ferric nitrates are added in ultra-pure water, then added Enter citric acid and be configured to solution, stirred at 80 DEG C, be then dropwise added drop-wise in solution ammoniacal liquor, make pH=7, stirring 3 ~6h, forms colloidal sol, dries, and obtains black xerogel；Then 3~6h is calcined at 1230~1260 DEG C, graininess is obtained Ba3Co2Fe24O41Powder；Wherein, the amount of total material of the amount of the material of citric acid and barium ions, cobalt ions and iron ion It is identical；The ratio of barium nitrate, the gross mass of five water cobalt nitrates and nine water ferric nitrates and ultra-pure water is 20g：(40-60)mL.
9. a kind of preparation method of lamination Wave suction composite material according to claim 1, it is characterised in that Ti3C2-MXene Nanometer sheet is prepared by procedure below：Ti in molar ratio:Al:TiC=1.0:1.2:2.0, Ti, Al and TiC are weighed, it is well mixed Afterwards, 1300~1360 DEG C are heated to the heating rate of 5~8 DEG C/min, and are incubated 3~6h, obtain Ti3AlC2Powder, by gained Ti3AlC2Powder takes 4~7g and is immersed in the hydrofluoric acid of 60~80mL, carries out 3~6h of corrosion reaction, obtains corroding through hydrofluoric acid Ti afterwards3C2Powder.
CN201611163166.0A 2016-12-15 2016-12-15 A kind of preparation method of lamination Wave suction composite material Pending CN106753238A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611163166.0A CN106753238A (en) 2016-12-15 2016-12-15 A kind of preparation method of lamination Wave suction composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611163166.0A CN106753238A (en) 2016-12-15 2016-12-15 A kind of preparation method of lamination Wave suction composite material

Publications (1)

Publication Number Publication Date
CN106753238A true CN106753238A (en) 2017-05-31

Family

ID=58892691

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611163166.0A Pending CN106753238A (en) 2016-12-15 2016-12-15 A kind of preparation method of lamination Wave suction composite material

Country Status (1)

Country Link
CN (1) CN106753238A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110290691A (en) * 2019-07-17 2019-09-27 湖南工程学院 A kind of ferritic composite wave-suction material of sheet MXene Supported Co and preparation method thereof
CN110304632A (en) * 2018-03-20 2019-10-08 中国科学院金属研究所 Sheet MXene material and preparation method thereof and energy storage material
CN110591641A (en) * 2019-01-25 2019-12-20 陕西科技大学 Fe2O3@ MXene composite powder and preparation method thereof
CN112147724A (en) * 2020-08-28 2020-12-29 国家纳米科学中心 Mxene-based broadband and wide-angle perfect absorber and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295303A (en) * 2015-11-09 2016-02-03 中国科学院宁波材料技术与工程研究所 Composite bulk material of resin, ferrite and MXenes and preparation method and application thereof
CN105418072A (en) * 2015-11-09 2016-03-23 中国科学院宁波材料技术与工程研究所 Ferrite material and MXenes composite material and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295303A (en) * 2015-11-09 2016-02-03 中国科学院宁波材料技术与工程研究所 Composite bulk material of resin, ferrite and MXenes and preparation method and application thereof
CN105418072A (en) * 2015-11-09 2016-03-23 中国科学院宁波材料技术与工程研究所 Ferrite material and MXenes composite material and preparation method and application thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
MEIKANG HAN，等: "Ti3C2 MXenes with Modified Surface for High-Performance Electromagnetic Absorption and Shielding in the X-Band", 《ACS APPL.MATER.INTERFACES》 *
ROBERT C. PULLAR: "Hexagonal ferrites：A review of the synthesis, properties and applications of hexaferrite ceramics", 《PROGRESS IN MATERIALS SCIENCE》 *
ROBERT C.PULLAR，等: "Magnetic properties of randomly oriented BaM, SrM, Co2Y, Co2Z and Co2W hexagonal ferrite fibres", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 *
YUCHANG QING,等: "Titanium carbide (MXene) nanosheets as promising microwave absorbers", 《CERAMICS INTERNATIONAL》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110304632A (en) * 2018-03-20 2019-10-08 中国科学院金属研究所 Sheet MXene material and preparation method thereof and energy storage material
CN110591641A (en) * 2019-01-25 2019-12-20 陕西科技大学 Fe2O3@ MXene composite powder and preparation method thereof
CN110290691A (en) * 2019-07-17 2019-09-27 湖南工程学院 A kind of ferritic composite wave-suction material of sheet MXene Supported Co and preparation method thereof
CN112147724A (en) * 2020-08-28 2020-12-29 国家纳米科学中心 Mxene-based broadband and wide-angle perfect absorber and preparation method thereof
CN112147724B (en) * 2020-08-28 2022-03-15 国家纳米科学中心 Mxene-based broadband and wide-angle perfect absorber and preparation method thereof

Similar Documents

Publication Publication Date Title
CN106587978A (en) Wave absorbing material of Z-shaped ferrite flaky powder filled particulate powder and preparation method thereof
CN103740233B (en) A kind of millimeter wave wave-absorbing coating material and preparation method thereof
CN106753238A (en) A kind of preparation method of lamination Wave suction composite material
CN103304186B (en) Ferrite-base composite magnetic dielectric antenna substrate material and preparation method thereof
CN107734950B (en) Zinc ferrite@manganese dioxide@graphene composite wave-suction material and preparation method thereof
CN106673640A (en) Barium ferrite / zinc oxide composite wave-absorbing material and preparation method thereof
CN106587167B (en) A kind of preparation method of barium ferrite@ferroso-ferric oxide composite wave-suction materials
WO2006128333A1 (en) A spinel type composite metal oxide electrode material and a manufacture method of the same
CN106571455A (en) Silver loaded mesoporous silicon oxide coated ternary cathode material, and preparation method and applications thereof
CN104900869A (en) Preparation method of carbon-coated nickel-cobalt-aluminum ternary positive electrode material
CN108559445A (en) A kind of preparation method of the nano combined absorbing material of redox graphene/Mn ferrite
CN106118594A (en) A kind of preparation method of graphene oxide/ferriferrous oxide composite material
CN101521046B (en) Graphite sheet surface load magnetic alloy particle wave-absorbing material and preparation method thereof
CN108190876A (en) A kind of graphene composite absorber and preparation method thereof
CN107010675A (en) A kind of titanium silicon-carbon/Conjugate ferrite radio-radar absorber and preparation method
CN110668505B (en) Cobalt-containing two-dimensional accordion-shaped nanosheet material and preparation method and application thereof
CN106854453A (en) A kind of preparation method of lamellar composite absorbing material
CN105016395A (en) Nano ferrite material, and preparation method thereof
CN106587037A (en) Preparation method of Z-type ferrite and r-GO tape casting lamination microwave-absorbing composite material
CN104693690B (en) A kind of polyaniline/epoxide resin wave-absorbing composite material and preparation method
CN109437325B (en) Flower-shaped Y-shaped hexagonal ferrite-manganese dioxide nano powder and preparation method thereof
CN106633547B (en) A kind of Z- type ferrite flaky powder/PVDF Wave suction composite material and preparation method thereof
CN106278252A (en) A kind of bismuth titanates Bi4 Xprxti3 Xcoxo12ceramic material and preparation method thereof
CN103756635B (en) A kind of preparation method of mesopore silicon oxide foam-based composite wave-suction material
CN113059834B (en) Preparation method of pearl shell-imitated electromagnetic wave absorption film

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170531