CN106086828A - Preparation method of novel ZnOw whisker surface composite layer - Google Patents
Preparation method of novel ZnOw whisker surface composite layer Download PDFInfo
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- CN106086828A CN106086828A CN201610628952.7A CN201610628952A CN106086828A CN 106086828 A CN106086828 A CN 106086828A CN 201610628952 A CN201610628952 A CN 201610628952A CN 106086828 A CN106086828 A CN 106086828A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 64
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 27
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 27
- 238000005234 chemical deposition Methods 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 239000011777 magnesium Substances 0.000 claims description 23
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 16
- 230000008021 deposition Effects 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- 239000008187 granular material Substances 0.000 claims description 12
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 12
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 9
- 238000002604 ultrasonography Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- XNSQZBOCSSMHSZ-UHFFFAOYSA-K azane;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxymethyl)amino]acetate;iron(3+) Chemical compound [NH4+].[Fe+3].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O XNSQZBOCSSMHSZ-UHFFFAOYSA-K 0.000 claims description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229940071125 manganese acetate Drugs 0.000 claims description 6
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- 235000010265 sodium sulphite Nutrition 0.000 claims description 5
- 238000002242 deionisation method Methods 0.000 claims description 4
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims description 3
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 241001614291 Anoplistes Species 0.000 claims 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 1
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 claims 1
- 229910052938 sodium sulfate Inorganic materials 0.000 claims 1
- 235000011152 sodium sulphate Nutrition 0.000 claims 1
- 239000011358 absorbing material Substances 0.000 abstract description 8
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 239000011258 core-shell material Substances 0.000 abstract 2
- 229910052596 spinel Inorganic materials 0.000 abstract 1
- 239000011029 spinel Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000011572 manganese Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention relates to a preparation method of a novel ZnOw whisker surface composite layer, which is characterized in that Mn is deposited on the surface of metallic nickel nano particlesxMgyZn1‑x‑yFe2O4Ferrite, thereby forming core-shell structured nanoparticles; then carrying out composite codeposition of core-shell structure nanoparticles on the basis of realizing local chemical deposition of metallic iron on the surface of the four-needle ZnOw whisker, thereby preparing iron and nickel core @ Mn on the surface of the four-needle ZnOw whiskerxMgyZn1‑x‑yFe2O4The ferrite shell structure composite layer fully exerts the characteristic that the four-needle ZnOw whisker has larger dielectric loss when used as a wave-absorbing material, and combines spinel MnxMgyZn1‑x‑yFe2O4The ferrite hasThe wave-absorbing property of wide frequency band and good compatibility, and the excellent magnetic hysteresis and eddy current loss of the nickel nano-particles.
Description
Technical field
The present invention relates to absorbing material technical field, the preparation side of a kind of novel ZnOw whisker surface composite layer
Method.
Background technology
Along with the development of science and technology, it is increasingly severe that the electromagnetism good fortune that radio and television, communication and electric power produce penetrates pollution；This
Outward, in military field, the stealth technology of weaponry requires more and more higher, thus, research and develop a kind of high performance absorbing material
Significant.Four pin ZnOw whiskers have the microwave absorbing property of uniqueness as a kind of polar monomer, and it has corner needle-like knot
Structure, has bigger dielectric loss in inhaling wave process, and four pin ZnOw whiskers has piezoelectric effect, can be by incoming electromagnetic wave energy
It is converted into electric energy or other energy thus reaches the purpose making electromagnetic wave dissipation disappear.But, four pins of preparation in prior art
The low frequency microwave absorbing property of ZnOw whisker can be poor, it is impossible to effectively meets low-frequency band absorbing property.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides the preparation side of a kind of novel ZnOw whisker surface composite layer
Method, this preparation method includes nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano granule and four pin ZnOw are brilliant
Must Surface Fe and nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structure composite bed, preparation method of the present invention makes nickel
Core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle dispersion is distributed in the metal iron layer on four pin ZnOw whisker surfaces, fills
Distribution has been waved four pin ZnOw whiskers and has been had the feature of bigger dielectric loss when as absorbing material, and has gathered spinel-type
MnxMgyZn1-x-yFe2O4Broadband that ferrite has and the good microwave absorbing property of compatibility and the excellent magnetic hysteresis of nano nickel particles
Advantage with eddy-current loss.
The technical solution adopted for the present invention to solve the technical problems is: the system of a kind of novel ZnOw whisker surface composite layer
Preparation Method, is made up of following preparation process:
Step one: nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano granule；
Step 2: the chemical deposition of four pin ZnOw whisker surface local ferrum；
Step 3: four pin ZnOw whisker Surface Fes and nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano granule
Composite codeposition.
Preferably, described step one particularly as follows:
1. reactant liquor is prepared: be that analytically pure manganese acetate, magnesium nitrate and ferrous acetate add in deionized water by concentration, shape
Becoming manganese acetate concentration is 50-280g/L, magnesium nitrate concentration is 80-320g/L and ferrous acetate concentration is the mixing of 35-410g/L
Liquid, with being sequentially added into the phosphoric acid of 60%, analytically pure disodium hydrogen phosphate and potassium permanganate in backward mixed liquor, forms the phosphorus of 60%
Acid concentration is 60-90mL/L, disodium hydrogen phosphate concentration is 15-40g/L and potassium permanganate concentration is the reactant liquor of 60-160g/L.
2. nickel core@Mn is preparedxMgyZn1-x-yFe2O4Ferrite shell structural nano granule: nano nickel particles is added deionization
Water so that it is percentage by weight is 10%-40%, at room temperature disperses 1-1.5 hour to form stable nickel nanometer with ultrasound wave
Grain deionized water dispersion；The reactant liquor of aforementioned for 50-120mL preparation is filled with 1L nano nickel particles deionized water dispersion
Dividing mixing, filtering drying after reacting 1-1.5 hour, obtained granular powder is nickel core@MnxMgyZn1-x-yFe2O4Ferrite
Shell structural nano granule.
Preferably, described step 2 particularly as follows:
1. chemical sinking effusion it is equipped with: be analytically pure ferrous acetate, praseodynium ferrum, three oxalic acid hydrate ferrum ammoniums by concentration
Add with sodium sulfite and deionized water is formed ferrous acetate, praseodynium ferrum, three oxalic acid hydrate ferrum ammoniums and sodium sulfite
Concentration is respectively the chemical sinking effusion of 35-80g/L, 90-270g/L, 5-30g/L, 20-50g/L.
2. the chemical deposition of four pin ZnOw whisker surface local ferrum: four pin ZnOw whiskers are added deionized water so that it is weight
The percentage ratio of amount is 30-60%, at room temperature disperses 0.5-1 hour to form four stable pin ZnOw whisker deionizations with ultrasound wave
Aqueous dispersion A；Take this dispersion 300-500mL add in chemical sinking effusion described in 500mL and be sufficiently mixed, react 10-
The local deposition of four pin ZnOw whisker surface metal ferrum is i.e. realized after 30 minutes.
Preferably, described step 3 particularly as follows:
1. preparation deposition basal liquid: be analytically pure ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, sulfur by concentration
Acid hydrogen sodium and sodium silicate add formation ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, sodium bisulfate and silicon in deionized water
The concentration of acid sodium is respectively the deposition basis of 130-280g/L, 90-320g/L, 5-20g/L, 10-45mL/L and 160-310g/L
Liquid.
2. the composite codeposition on four pin ZnOw whisker surfaces: the four pin ZnOw whiskers on surface local deposition metal are added
Deionized water so that it is percentage by weight is 50%-80%, at room temperature disperses 10-20 minute to form stable four with ultrasound wave
Pin ZnOw whisker deionized water dispersion B；Take this dispersion 500mL with 500mL deposition basal liquid to be sufficiently mixed, codeposition
Cross filtering drying after 0.5-2 hour, i.e. form ferrum and nickel core@MnxMgyZn1-x-yFe2O4 ferrum oxygen on four pin ZnOw whisker surfaces
Solid shell structure composite bed.
The positive effect of the present invention: four pin ZnOw whisker Surface Fe and nickel core@prepared according to the methods of the invention
MnxMgyZn1-x-yFe2O4Ferrite shell structure composite bed, the complex dielectric permittivity on the one hand having given full play to four pin ZnOw whiskers is empty
Portion has bigger numerical within the specific limits, has the feature of bigger dielectric loss when as absorbing material, on the other hand knot
Close spinel-type MnxMgyZn1-x-yFe2O4Broadband that ferrite has and the good microwave absorbing property of compatibility and nickel nanometer
The excellent magnetic hysteresis of grain and the advantage of eddy-current loss, thus four pin ZnOw whisker Surface Fes of preparation and nickel core@MnxMgyZn1-x- yFe2O4Ferrite shell structure composite bed is the absorbing material with excellent broadband and high-absorbility.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of composite bed preparation method of the present invention；
Fig. 2 is the structural representation of composite bed of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings to a preferred embodiment of the present invention will be described in detail.
Referring to figs. 1 through Fig. 2, the preferred embodiment of the present invention provides the preparation side of a kind of novel ZnOw whisker surface composite layer
Method, is made up of following preparation process:
Step one: nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano granule；
Step 2: the chemical deposition of four pin ZnOw whisker surface local ferrum；
Step 3: four pin ZnOw whisker Surface Fes and nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano granule
Composite codeposition.
Described step one particularly as follows:
1. reactant liquor is prepared: be that analytically pure manganese acetate, magnesium nitrate and ferrous acetate add in deionized water by concentration, shape
Becoming manganese acetate concentration is 70g/L, magnesium nitrate concentration is 220g/L and ferrous acetate concentration is the mixed liquor of 60g/L, with backward mixed
Closing and be sequentially added into the phosphoric acid of 60%, analytically pure disodium hydrogen phosphate and potassium permanganate in liquid, the phosphoric acid concentration of formation 60% is
80mL/L, disodium hydrogen phosphate concentration are 40g/L and potassium permanganate concentration is the reactant liquor of 110g/L.
2. nickel core@Mn is preparedxMgyZn1-x-yFe2O4Ferrite shell structural nano granule: nano nickel particles is added deionization
Water so that it is percentage by weight is 30%, at room temperature disperses 1 hour to form stable nano nickel particles deionized water with ultrasound wave
Dispersion；The reactant liquor of aforementioned for 80mL preparation is sufficiently mixed with 1L nano nickel particles deionized water dispersion, reacts 1.5
Filtering drying after hour, obtained granular powder is nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano granule.
Described step 2 particularly as follows:
1. chemical sinking effusion it is equipped with: be analytically pure ferrous acetate, praseodynium ferrum, three oxalic acid hydrate ferrum ammoniums by concentration
Add with sodium sulfite and deionized water is formed ferrous acetate, praseodynium ferrum, three oxalic acid hydrate ferrum ammoniums and sodium sulfite
Concentration is respectively the chemical sinking effusion of 60g/L, 130g/L, 20g/L, 40g/L.
2. the chemical deposition of four pin ZnOw whisker surface local ferrum: four pin ZnOw whiskers are added deionized water so that it is weight
The percentage ratio of amount is 40%, at room temperature disperses 1 hour to form four stable pin ZnOw whisker deionized water dispersions with ultrasound wave
System A；Take this dispersion 400mL add in chemical sinking effusion described in 500mL and be sufficiently mixed, i.e. realize after reacting 20 minutes
The local deposition of four pin ZnOw whisker surface metal ferrum.
Described step 3 particularly as follows:
1. preparation deposition basal liquid: be analytically pure ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, sulfur by concentration
Acid hydrogen sodium and sodium silicate add formation ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, sodium bisulfate and silicon in deionized water
The concentration of acid sodium is respectively the deposition basal liquid of 150g/L, 240g/L, 5g/L, 25mL/L and 170g/L.
2. the composite codeposition on four pin ZnOw whisker surfaces: the four pin ZnOw whiskers on surface local deposition metal are added
Deionized water so that it is percentage by weight is 70%, at room temperature disperses to form four stable pin ZnOw 15 minutes with ultrasound wave brilliant
Must deionized water dispersion B；Take this dispersion 500mL with 500mL deposition basal liquid to be sufficiently mixed, co-deposit 1.5 hours
Rear filtering drying of crossing, i.e. forms ferrum and nickel core@MnxMgyZn1-x-yFe2O4 ferrite shell structure on four pin ZnOw whisker surfaces
Composite bed.
ZnOw whisker Surface Fe prepared by equal in quality the present embodiment and nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell
Structure composite layer absorbing material adds coating with the common four pin ZnOw whiskers of equal in quality, adds common four pin ZnOw coating
Inhaling wavestrip width experimental result is 10-18GHz, and adds ZnOw whisker Surface Fe and nickel core@prepared by the present embodiment
MnxMgyZn1-x-yFe2O4The suction wavestrip width experimental result of ferrite shell structure composite bed absorbing material coating is 3-18GHz.Aobvious
So, the ZnOw whisker Surface Fe prepared according to the present invention and nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structure composite bed inhales ripple
Material combines spinel-type MnxMgyZn1-x-yFe2O4Broadband that ferrite has and the good microwave absorbing property of compatibility and nickel
Magnetic hysteresis that nano-particle is excellent and the advantage of eddy-current loss, have the absorbing property of excellent broadband and high-absorbility.
Above-described only the preferred embodiments of the present invention, the explanation of it should be understood that above example is simply used
In helping to understand method and the core concept thereof of the present invention, the protection domain being not intended to limit the present invention, all the present invention's
Any amendment of being made within thought and principle, equivalent etc., should be included within the scope of the present invention.
Claims (7)
1. the preparation method of a novel ZnOw whisker surface composite layer, it is characterised in that be made up of following preparation process:
Step one: nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano granule；
Step 2: the chemical deposition of four pin ZnOw whisker surface local ferrum；
Step 3: four pin ZnOw whisker Surface Fes and nickel core@MnxMgyZn1-x-yFe2O4Being combined of ferrite shell structural nano granule
Codeposition.
The preparation method of a kind of novel ZnOw whisker surface composite layer the most according to claim 1, it is characterised in that: described
Step one particularly as follows:
1. prepare reactant liquor: be that analytically pure manganese acetate, magnesium nitrate and ferrous acetate add in deionized water by concentration, formed mixed
Close liquid, with backward mixed liquor is sequentially added into the phosphoric acid of 60%, analytically pure disodium hydrogen phosphate and potassium permanganate, form reaction
Liquid.
2. nickel core@Mn is preparedxMgyZn1-x-yFe2O4Ferrite shell structural nano granule: nano nickel particles is added deionized water,
Making its percentage by weight is 10%-40%, at room temperature disperses to form stable nano nickel particles 1-1.5 hour with ultrasound wave and goes
Ionized water dispersion；By the most mixed with 1L nano nickel particles deionized water dispersion for the reactant liquor of aforementioned for 50-120mL preparation
Closing, filtering drying after reacting 1-1.5 hour, obtained granular powder is nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell is tied
Structure nano-particle.
The preparation method of a kind of novel ZnOw whisker surface composite layer the most according to claim 2, it is characterised in that: described
In mixed liquor, manganese acetate concentration is 50-280g/L, and magnesium nitrate concentration is 80-320g/L, and ferrous acetate concentration is 35-410g/L,
In described reactant liquor, the phosphoric acid concentration of 60% is 60-90mL/L, and disodium hydrogen phosphate concentration is 15-40g/L, and potassium permanganate concentration is
60-160g/L。
The preparation method of a kind of novel ZnOw whisker surface composite layer the most according to claim 1, it is characterised in that: described
Step 2 particularly as follows:
1. chemical sinking effusion it is equipped with: be analytically pure ferrous acetate, praseodynium ferrum, three oxalic acid hydrate ferrum ammonium and Asias by concentration
Sodium sulfate adds formation chemical sinking effusion in deionized water.
2. the chemical deposition of four pin ZnOw whisker surface local ferrum: four pin ZnOw whiskers are added deionized water so that it is weight
Percentage ratio is 30-60%, at room temperature disperses 0.5-1 hour to form four stable pin ZnOw whisker deionization moisture with ultrasound wave
Prose style free from parallelism system A；Taking this dispersion 300-500mL add in chemical sinking effusion described in 500mL and be sufficiently mixed, reaction 10-30 divides
The local deposition of four pin ZnOw whisker surface metal ferrum is i.e. realized after clock.
The preparation method of a kind of novel ZnOw whisker surface composite layer the most according to claim 4, it is characterised in that: described
In chemical sinking effusion, the concentration of ferrous acetate, praseodynium ferrum, three oxalic acid hydrate ferrum ammoniums and sodium sulfite is respectively 35-80g/
L、90-270g/L、5-30g/L、20-50g/L。
The preparation method of a kind of novel ZnOw whisker surface composite layer the most according to claim 1, it is characterised in that: described
Step 3 particularly as follows:
1. preparation deposition basal liquid: be analytically pure ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, hydrogen sulfate by concentration
Sodium and sodium silicate add formation deposition basal liquid in deionized water.
2. the composite codeposition on four pin ZnOw whisker surfaces: by surface local deposition metal four pin ZnOw whiskers add go from
Sub-water so that it is percentage by weight is 50%-80%, at room temperature disperses 10-20 minute to form four stable pins with ultrasound wave
ZnOw whisker deionized water dispersion B；Take this dispersion 500mL with 500mL deposition basal liquid to be sufficiently mixed, codeposition
Cross filtering drying after 0.5-2 hour, i.e. form ferrum and nickel core@MnxMgyZn on four pin ZnOw whisker surfaces1-x-yFe2O4 ferrite
Shell structure composite bed.
The preparation method of a kind of novel ZnOw whisker surface composite layer the most according to claim 6, it is characterised in that: described
In deposition basal liquid, the concentration of ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, sodium bisulfate and sodium silicate is respectively 130-
280g/L, 90-320g/L, 5-20g/L, 10-45mL/L and 160-310g/L.
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