CN113529406A - BaFe12O19-Ni0.8Zn0.2Fe2O4Preparation method of barium titanate wave-absorbing coating agent - Google Patents
BaFe12O19-Ni0.8Zn0.2Fe2O4Preparation method of barium titanate wave-absorbing coating agent Download PDFInfo
- Publication number
- CN113529406A CN113529406A CN202110804962.2A CN202110804962A CN113529406A CN 113529406 A CN113529406 A CN 113529406A CN 202110804962 A CN202110804962 A CN 202110804962A CN 113529406 A CN113529406 A CN 113529406A
- Authority
- CN
- China
- Prior art keywords
- bafe
- barium titanate
- wave
- coating agent
- preparation
- 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
Links
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 44
- 239000011248 coating agent Substances 0.000 title claims abstract description 42
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims description 5
- 239000004744 fabric Substances 0.000 claims abstract description 34
- 229920000742 Cotton Polymers 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000006229 carbon black Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 45
- 239000011701 zinc Substances 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 19
- 150000003839 salts Chemical class 0.000 claims description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002562 thickening agent Substances 0.000 claims description 5
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 239000011358 absorbing material Substances 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 238000003980 solgel method Methods 0.000 abstract description 2
- 229910002771 BaFe12O19 Inorganic materials 0.000 abstract 1
- 239000002159 nanocrystal Substances 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000004753 textile Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Soft Magnetic Materials (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention relates to the field of new materials, in particular to BaFe12O19‑Ni0.8Zn0.2Fe2O4A preparation method of a barium titanate wave-absorbing coating agent; with BaFe12O19Being a hard magnet, Ni0.8Zn0.2Fe2O4Separately preparing BaFe for soft magnet by sol-gel method12O19‑Ni0.8Zn0.2Fe2O4The nano-crystal composite powder and the barium titanate powder are respectively calcined in a muffle furnace to obtain BaFe12O19‑Ni0.8Zn0.2Fe2O4And barium titanate wave-absorbing material. Finally, BaFe12O19‑Ni0.8Zn0.2Fe2O4The novel viscous wave-absorbing coating finishing agent is prepared from materials such as ferrite, barium titanate, carbon black, an adhesive, water and the like, and is used for coating finishing of pure cotton fabrics.
Description
Technical Field
The invention relates to the field of new materials, in particular to BaFe12O19-Ni0.8Zn0.2Fe2O4A preparation method of barium titanate wave-absorbing coating agent.
Background
The existing developed wave-absorbing materials comprise magnetic materials, carbon materials, conductive high molecular polymers, ceramic materials and the like. Among the above materials, the magnetic material has the disadvantages of high density, high processing cost, easy corrosion, etc., despite the advantages of low cost, high thermal stability, good mechanical properties, etc.; the single conductive high molecular polymer and carbon material has the advantages of wide absorption band and low production cost, but has the defects of poor stability, narrow absorption band and low absorption strength; the ceramic material has good mechanical property and thermophysical property, small density and good wave-absorbing property, and can effectively absorb the energy of radar waves, so that the single wave-absorbing material can hardly meet the requirements of novel wave-absorbing materials, and the development direction of the microwave-absorbing material is to compound different materials.
In recent years, researchers at home and abroad are devoted to research and development of wave-absorbing materials. Wave-absorbing materials such as ferrite, carbonyl iron, ceramics, etc. have been widely studied, and in order to further improve the attenuation properties of incident electromagnetic waves, the electromagnetic properties of the base composite material can be optimized by adding a secondary magnetic component or a dielectric component. At present, the research on the composite wave-absorbing material has been greatly developed. However, in order to obtain satisfactory electromagnetic wave absorbing properties, the application of wave absorbing coatings has attracted increasing researchers' interest, for example, in understanding the absorption mechanism of the interface and studying the physical/chemical properties of the interface, and the properties thereofImpact on the absorption properties. And then, revealing the interaction among the components in the composite material coating and the influence of the components on the electromagnetic wave absorption effect, thereby preparing the novel electromagnetic wave absorbing coating material meeting the requirements. The novel coating composite material with ideal components and optimal performance has wide application prospect in the field of microwave absorption. The BaFe is prepared by compounding ceramic-based material barium titanate with dielectric property, carbon-based material carbon black and magnetic ferrite12O19-Ni0.8Zn0.2Fe2O4The barium titanate wave-absorbing coating agent is uniformly coated on the surface of cotton fabric, the wave-absorbing performance and other properties of the coated fabric are researched, and the barium titanate wave-absorbing coating agent accords with the development direction of the current textiles applied to development of stealth materials.
The inventor of the invention specially provides the invention through long-time research and practice in order to expand the application field of textiles and research the application of the wave-absorbing material in the stealth material of the textiles.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides BaFe12O19-Ni0.8Zn0.2Fe2O4The barium titanate wave-absorbing coating agent is used for researching the application of textiles as the stealth material field.
In order to solve the problems, the invention adopts the following technical scheme:
BaFe12O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent comprises the following steps:
S1、BaFe12O19-Ni0.8Zn0.2Fe2O4preparing ferrite: putting Ba metal salt, Fe metal salt, Ni metal salt and Zn metal salt into citric acid aqueous solution, stirring the solution at 70-80 ℃ to form transparent solution, adding ethylene glycol, adding ammonia water after stirring, adjusting the pH value to 6-7, stirring the solution at 75 ℃ to form gel with certain viscosity, and drying the gel at 120 ℃ to form dry gel; sintering the dried xerogel to obtain BaFe12O19-Ni0.8Zn0.2Fe2O4A ferrite;
s2, preparation of barium titanate: stirring tetrabutyl titanate liquid and barium acetate liquid to form gel, precipitating and drying, and calcining the dried gel to obtain barium titanate powder;
S3、BaFe12O19-Ni0.8Zn0.2Fe2O4preparation of barium titanate wave-absorbing coating agent: first, BaFe obtained in step S112O19-Ni0.8Zn0.2Fe2O4Mixing ferrite with barium titanate powder obtained from S2, carbon black, binder, thickener and water, and stirring to obtain BaFe12O19-Ni0.8Zn0.2Fe2O4Barium titanate wave-absorbing coating agent.
Further, in the step S1, the mass ratio of the Ba metal salt to the Fe metal salt to the Ni metal salt to the Zn metal salt to the citric acid aqueous solution is 5:103 to 104:3.9 to 4:1: 15.333.
Further, the metal salts of Ba, Fe, Ni and Zn are barium nitrate, ferric nitrate nonahydrate, nickel nitrate hexahydrate and zinc nitrate hexahydrate.
Further, the xerogel sintering procedure in step S1: presintering at 400 deg.C in a program-controlled furnace, and calcining at 1100 deg.C.
Further, the dried gel is sintered, naturally cooled and then ground to obtain black powder as BaFe in step S112O19-Ni0.8Zn0.2Fe2O4Ferrite.
Further, the mass ratio of the tetrabutyl titanate liquid to the barium acetate liquid in the step S2 is 1: 0.75-0.76.
Further, the calcination in step S2 is performed in a programmed furnace.
BaFe12O19-Ni0.8Zn0.2Fe2O4Barium titanate wave-absorbing coating agent, wherein the coating finishing agent is prepared by adopting the preparation method.
BaFe12O19-Ni0.8Zn0.2Fe2O4The barium titanate wave-absorbing coating agent is applied, the coating finishing agent prepared by the preparation method is used for carrying out coating finishing on cotton fabrics, the cotton fabrics are aired at room temperature and then are pre-dried at 90 ℃, baked at 120 ℃ and naturally cooled to obtain coated fabrics.
Further, the cotton fabric is medium-thick cotton fabric.
Compared with the prior art, the invention has the beneficial effects that:
(1) the operation is simple, the steps are few, and the requirement on experimental conditions is low;
(2) the application of the wave-absorbing material in the field of textiles is widened;
(3) can be widely applied to preparing multi-component wave-absorbing coating agents;
(4) the method can be applied to the finishing of wave-absorbing coatings of various fabrics;
(5) the invention respectively prepares BaFe by utilizing a simple sol-gel method12O19-Ni0.8Zn0.2Fe2O4Ferrite and barium titanate wave-absorbing material, and then BaFe is prepared12O19-Ni0.8Zn0.2Fe2O4The barium titanate wave-absorbing coating agent is used for coating finishing on cotton fabrics by adjusting different mass ratios, so that the coated fabrics have a wave-absorbing effect, and the application of the stealth material in textile materials is realized.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Step a, BaFe12O19-Ni0.8Zn0.2Fe2O4Preparing ferrite: adding Ba, Fe, Ni and Zn metal salts in a mass ratio of 5: 103-104: 3.9-4: 1 into 15.333g of citric acid aqueous solution, stirring at 70-80 ℃ to obtain a transparent solution, and then adding the transparent solutionThen adding 8.14mL of ethylene glycol, stirring, adding ammonia water, adjusting the pH value to 6-7, stirring at 75 ℃ to form gel with certain viscosity, and drying at 120 ℃ to form dry gel. Finally, pre-sintering the dried gel in a program control furnace at 400 ℃, roasting at 1100 ℃ for a certain time, naturally cooling, and grinding to obtain black powder, namely BaFe12O19-Ni0.8Zn0.2Fe2O4Ferrite.
Step b, preparation of barium titanate: stirring tetrabutyl titanate liquid and barium acetate liquid in a mass ratio of 1: 0.75-0.76 at a certain temperature for a certain time to form gel, then precipitating for a certain time and drying, calcining the dried gel in a program-controlled furnace at 850 ℃ for a certain time, naturally cooling and grinding to obtain white powder, namely the barium titanate powder.
BaFe12O19-Ni0.8Zn0.2Fe2O4Preparation of barium titanate wave-absorbing coating agent: firstly, BaFe prepared in the above way12O19-Ni0.8Zn0.2Fe2O4Mixing ferrite, barium titanate powder, carbon black, an adhesive, a thickening agent and deionized water, uniformly stirring, then performing coating finishing on the cotton fabric, drying the cotton fabric at room temperature, pre-drying the cotton fabric at 90 ℃, baking the cotton fabric at 120 ℃ for a certain time, naturally cooling the cotton fabric, and taking out the coated fabric.
Example 1
0.5g of Ba (NO)3)2，10.3g Fe(NO3)3·9H2O，0.39g Ni(NO3)2·6H2O and 0.1gZn (NO)3)2·6H2And (3) putting O into 15.333g of citric acid aqueous solution, stirring the mixture at 75 ℃ to obtain a transparent solution, then adding 8.14mL of ethylene glycol, stirring the solution, then adding ammonia water, adjusting the pH value to 6-7, stirring the solution at 75 ℃ to obtain gel with certain viscosity, and drying the gel at 120 ℃ to obtain dry gel. Finally, pre-sintering the dried gel in a program control furnace at 400 ℃ for 3h, roasting at 1100 ℃ for 2h, naturally cooling, and grinding to obtain black powder, namely BaFe12O19-Ni0.8Zn0.2Fe2O4Ferrite.
31.3g of tetrabutyl titanate liquid, 23.475g of barium acetate were weighed. Dissolving weighed tetrabutyl titanate in 30mL of ethanol, stirring by using a strong magnetic stirrer to fully mix, dropwise adding 30mL of 1moL/L hydrochloric acid, and continuously stirring to prepare solution A; and dissolving barium acetate in 70mL of deionized water, fully dissolving the barium acetate in a water bath at 40 ℃, taking out the barium acetate from the water bath, and cooling to room temperature to obtain a solution B after the barium acetate is fully dissolved. And then placing the solution A in a water bath at 40 ℃, and dropwise adding the solution B into the solution A until the solution A is completely dripped. Then stirring by a magnetic stirrer to form sol after 30min, and then putting the sol into an oven to be dried after being settled for 4h at room temperature. And calcining the dried gel in a program-controlled furnace at 850 ℃ for 4h, naturally cooling, and grinding to obtain white powder, namely barium titanate powder.
Firstly, BaFe prepared in the above way12O19-Ni0.8Zn0.2Fe2O4Mixing ferrite, barium titanate powder, carbon black, an adhesive, a thickening agent and deionized water, uniformly stirring, then performing coating finishing on the cotton fabric, drying the cotton fabric at room temperature, pre-drying the cotton fabric at 90 ℃, baking the cotton fabric at 120 ℃ for a certain time, naturally cooling the cotton fabric, and taking out the coated fabric.
Example 2
0.5g of Ba (NO)3)2，10.4g Fe(NO3)3·9H2O，0.4g Ni(NO3)2·6H2O and 0.1gZn (NO)3)2·6H2And (3) putting O into 15.333g of citric acid aqueous solution, stirring the mixture at 75 ℃ to obtain a transparent solution, then adding 8.14mL of ethylene glycol, stirring the solution, then adding ammonia water, adjusting the pH value to 6-7, stirring the solution at 75 ℃ to obtain gel with certain viscosity, and drying the gel at 120 ℃ to obtain dry gel. Finally, pre-sintering the dried gel in a program control furnace at 400 ℃ for 3h, roasting at 1100 ℃ for 2h, naturally cooling, and grinding to obtain black powder, namely BaFe12O19-Ni0.8Zn0.2Fe2O4Ferrite.
31.3g of tetrabutyl titanate liquid, 23.788g of barium acetate were weighed. Dissolving weighed tetrabutyl titanate in 30mL of ethanol, stirring by using a strong magnetic stirrer to fully mix, dropwise adding 30mL of 1moL/L hydrochloric acid, and continuously stirring to prepare solution A; and dissolving barium acetate in 70mL of deionized water, fully dissolving the barium acetate in a water bath at 40 ℃, taking out the barium acetate from the water bath, and cooling to room temperature to obtain a solution B after the barium acetate is fully dissolved. And then placing the solution A in a water bath at 40 ℃, and dropwise adding the solution B into the solution A until the solution A is completely dripped. Then stirring by a magnetic stirrer to form sol after 30min, and then putting the sol into an oven to be dried after being settled for 4h at room temperature. And calcining the dried gel in a program-controlled furnace at 850 ℃ for 4h, naturally cooling, and grinding to obtain white powder, namely barium titanate powder.
Firstly, BaFe prepared in the above way12O19-Ni0.8Zn0.2Fe2O4Mixing ferrite, barium titanate powder, carbon black, an adhesive, a thickening agent and deionized water, uniformly stirring, then performing coating finishing on the cotton fabric, drying the cotton fabric at room temperature, pre-drying the cotton fabric at 90 ℃, baking the cotton fabric at 120 ℃ for a certain time, naturally cooling the cotton fabric, and taking out the coated fabric.
Although only the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art, and all changes are encompassed in the scope of the present invention.
Claims (10)
1. BaFe12O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent is characterized by comprising the following steps:
S1、BaFe12O19-Ni0.8Zn0.2Fe2O4preparing ferrite: putting Ba metal salt, Fe metal salt, Ni metal salt and Zn metal salt into citric acid aqueous solution, stirring the solution at 70-80 ℃ to form transparent solution, adding ethylene glycol, adding ammonia water after stirring, adjusting the pH value to 6-7, stirring the solution at 75 ℃ to form gel with certain viscosity, and drying the gel at 120 ℃ to form dry gel; will be provided withSintering the dried xerogel to obtain BaFe12O19-Ni0.8Zn0.2Fe2O4A ferrite;
s2, preparation of barium titanate: stirring tetrabutyl titanate liquid and barium acetate liquid to form gel, precipitating and drying, and calcining the dried gel to obtain barium titanate powder;
S3、BaFe12O19-Ni0.8Zn0.2Fe2O4preparation of barium titanate wave-absorbing coating agent: first, BaFe obtained in step S112O19-Ni0.8Zn0.2Fe2O4Mixing ferrite with barium titanate powder obtained from S2, carbon black, binder, thickener and water, and stirring to obtain BaFe12O19-Ni0.8Zn0.2Fe2O4Barium titanate wave-absorbing coating agent.
2. BaFe according to claim 112O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent is characterized by comprising the following steps: in the step S1, the mass ratio of the Ba metal salt, the Fe metal salt, the Ni metal salt, the Zn metal salt and the citric acid aqueous solution is 5: 103-104: 3.9-4: 1: 15.333.
3. BaFe according to claim 212O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent is characterized by comprising the following steps: ba. The Fe, Ni and Zn metal salts are barium nitrate, ferric nitrate nonahydrate, nickel nitrate hexahydrate and zinc nitrate hexahydrate.
4. BaFe according to claim 112O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent is characterized by comprising the following steps: the xerogel sintering procedure in step S1: presintering at 400 deg.C in a program-controlled furnace, and calcining at 1100 deg.C.
5. BaFe according to claim 112O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent is characterized by comprising the following steps: sintering the xerogel, naturally cooling and grinding to obtain black powder serving as BaFe in step S112O19-Ni0.8Zn0.2Fe2O4Ferrite.
6. BaFe according to claim 112O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent is characterized by comprising the following steps: in the step S2, the mass ratio of the tetrabutyl titanate liquid to the barium acetate liquid is 1: 0.75-0.76.
7. BaFe according to claim 112O19-Ni0.8Zn0.2Fe2O4The preparation method of the barium titanate wave-absorbing coating agent is characterized by comprising the following steps: the calcination in step S2 is performed in a programmed furnace.
8. BaFe12O19-Ni0.8Zn0.2Fe2O4Barium titanate wave-absorbing coating agent, which is characterized in that: the coating finish is prepared by the preparation method as claimed in any one of claims 1 to 7.
9. BaFe12O19-Ni0.8Zn0.2Fe2O4The application of the barium titanate wave-absorbing coating agent is characterized in that: coating finishing is carried out on the cotton fabric by using the coating finishing agent prepared by the preparation method according to any one of claims 1 to 7, the cotton fabric is pre-dried at 90 ℃ after being dried at room temperature, and is baked at 120 ℃, and the coated fabric is obtained after natural cooling.
10. BaFe according to claim 912O19-Ni0.8Zn0.2Fe2O4Barium titanate getterUse of a wave coating agent, characterized in that: the cotton fabric is medium-thick cotton fabric.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110804962.2A CN113529406A (en) | 2021-07-16 | 2021-07-16 | BaFe12O19-Ni0.8Zn0.2Fe2O4Preparation method of barium titanate wave-absorbing coating agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110804962.2A CN113529406A (en) | 2021-07-16 | 2021-07-16 | BaFe12O19-Ni0.8Zn0.2Fe2O4Preparation method of barium titanate wave-absorbing coating agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113529406A true CN113529406A (en) | 2021-10-22 |
Family
ID=78128367
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110804962.2A Pending CN113529406A (en) | 2021-07-16 | 2021-07-16 | BaFe12O19-Ni0.8Zn0.2Fe2O4Preparation method of barium titanate wave-absorbing coating agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113529406A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070003757A1 (en) * | 2005-06-28 | 2007-01-04 | Fujikura Kasei Co., Ltd. | Radio Wave Absorbing Coating Composition and Coated Object Therewith |
| CN101712837A (en) * | 2009-11-30 | 2010-05-26 | 浙江师范大学 | High-efficiency broadband wave-absorbing coating material and use method |
| US20130056673A1 (en) * | 2011-09-06 | 2013-03-07 | Chung-Shan Institute of Science and Technology, Armaments, Bureau, Ministry of National Defense | Electromagnetic Wave-Absorbing Material |
| CN103467079A (en) * | 2013-08-28 | 2013-12-25 | 西北工业大学 | Preparation method for grapheme/Ni0.8Zn0.2Ce0.06Fe1.94O4 nano wave-absorbing material |
| JP2015172152A (en) * | 2014-03-12 | 2015-10-01 | 株式会社西澤 | Electromagnetic wave-absorbing coating agent, sheet coated with the same, and method for producing the same |
| CN112095351A (en) * | 2020-08-25 | 2020-12-18 | 东华大学 | Frequency band-adjustable integrated multilayer wave-absorbing planar fabric and preparation method thereof |
-
2021
- 2021-07-16 CN CN202110804962.2A patent/CN113529406A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070003757A1 (en) * | 2005-06-28 | 2007-01-04 | Fujikura Kasei Co., Ltd. | Radio Wave Absorbing Coating Composition and Coated Object Therewith |
| CN101712837A (en) * | 2009-11-30 | 2010-05-26 | 浙江师范大学 | High-efficiency broadband wave-absorbing coating material and use method |
| US20130056673A1 (en) * | 2011-09-06 | 2013-03-07 | Chung-Shan Institute of Science and Technology, Armaments, Bureau, Ministry of National Defense | Electromagnetic Wave-Absorbing Material |
| CN103467079A (en) * | 2013-08-28 | 2013-12-25 | 西北工业大学 | Preparation method for grapheme/Ni0.8Zn0.2Ce0.06Fe1.94O4 nano wave-absorbing material |
| JP2015172152A (en) * | 2014-03-12 | 2015-10-01 | 株式会社西澤 | Electromagnetic wave-absorbing coating agent, sheet coated with the same, and method for producing the same |
| CN112095351A (en) * | 2020-08-25 | 2020-12-18 | 东华大学 | Frequency band-adjustable integrated multilayer wave-absorbing planar fabric and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 刘侠侠等: "低温燃烧反应合成Ni_(0.25)Mn_(0.25)Zn_(0.50)Fe_2O_4铁氧体及其微波吸收性能的研究", 《人工晶体学报》 * |
| 梁慧敏等, 北京理工大学出版社 * |
| 罗道源等: ""(1-x)BaFe_(12)O_(19)/xBaTiO_3复合吸波材料的制备及微波吸收性能"，材料导报Ｂ研究篇，第26卷第12期，第30-33,40页", 《材料导报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109181639B (en) | SiC @ SiO2@ ferrite high-temperature wave-absorbing composite material and preparation method thereof | |
| CN104030667B (en) | Zirconium-doped barium ferrite wave-absorbing material and preparation method thereof | |
| CN104844182B (en) | Zirconium and titanium-co-doped barium ferrite wave-absorbing powder material and preparation method therefor | |
| CN104628372B (en) | A kind of niobium nickel co-doped barium ferrite wave-absorbing powder material and preparation method thereof | |
| CN111285671B (en) | Low-frequency wave-absorbing material and preparation method thereof | |
| CN103482969A (en) | Ferrite wave-absorbing material and preparation method thereof | |
| CN104529428A (en) | Manganese cerium doped nickel zinc ferrite nano wave absorbing powder and preparation method thereof | |
| CN101217861A (en) | A W-type ferrite electromagnetic-wave absorbent and the corresponding preparation method | |
| CN103848989A (en) | Preparation method of nickel-zinc ferrite/polyaniline composite material | |
| CN115109487B (en) | Preparation method of nickel ferrite-based/water-based polyacrylate wave-absorbing coating | |
| CN101100374A (en) | Ni-Zn ferrite fibre and preparing process thereof | |
| CN102153338A (en) | Seepage type barium titanate-nickel zinc ferrite composite ceramic wave absorption material and preparation method thereof | |
| CN110540735B (en) | Epoxy resin-based composite wave-absorbing material and preparation method and application thereof | |
| CN113816620B (en) | Dielectric fiber composite wave-absorbing material coated with molybdenum disulfide/iron-cobalt alloy/carbon on surface and preparation method thereof | |
| CN111748317A (en) | Petal-shaped ferric oxide-based composite wave absorbing agent and preparation method thereof and wave absorbing material | |
| CN105218807A (en) | Ferrite composite material that nano polyaniline is coated and preparation method thereof | |
| CN113529406A (en) | BaFe12O19-Ni0.8Zn0.2Fe2O4Preparation method of barium titanate wave-absorbing coating agent | |
| CN104671764A (en) | Niobium-doped barium ferrite wave-absorbing powder material and preparation method | |
| CN112280533B (en) | Preparation method of ternary composite wave-absorbing material with hollow structure | |
| CN107188553B (en) | Preparation method of wave-absorbing ferrite | |
| CN105174933A (en) | Preparation method for soft magnetic ferrite with high saturation magnetic induction strength and high magnetic permeability | |
| CN109837062A (en) | A kind of wave absorbing agent and preparation method thereof | |
| CN104058735B (en) | Iron-zirconium-tungsten complex ferrite and preparation method thereof | |
| CN114044540A (en) | A-site and B-site co-doped perovskite type electromagnetic wave-absorbing material and preparation method thereof | |
| CN113136726A (en) | Microwave absorbent based on cooperative coupling protection and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211022 |
|
| RJ01 | Rejection of invention patent application after publication |