CN106086828B - Preparation method of ZnOw whisker surface composite layer - Google Patents
Preparation method of ZnOw whisker surface composite layer Download PDFInfo
- Publication number
- CN106086828B CN106086828B CN201610628952.7A CN201610628952A CN106086828B CN 106086828 B CN106086828 B CN 106086828B CN 201610628952 A CN201610628952 A CN 201610628952A CN 106086828 B CN106086828 B CN 106086828B
- Authority
- CN
- China
- Prior art keywords
- znow
- whiskers
- concentration
- iron
- deposition
- 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.)
- Active
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 72
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 27
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 claims abstract description 21
- 239000002105 nanoparticle Substances 0.000 claims abstract description 19
- 238000005234 chemical deposition Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000011777 magnesium Substances 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 18
- 230000008021 deposition Effects 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 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
- 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
- 239000011572 manganese Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- 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
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 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
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 229910000147 aluminium phosphate 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
- 235000019795 sodium metasilicate Nutrition 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
- QDMGKUOANLJICG-UHFFFAOYSA-N [Mg].[N+](=O)(O)[O-] Chemical compound [Mg].[N+](=O)(O)[O-] QDMGKUOANLJICG-UHFFFAOYSA-N 0.000 claims description 3
- VJGJZVCKMKGZKS-UHFFFAOYSA-N iron;oxalic acid;hydrate Chemical compound O.[Fe].OC(=O)C(O)=O VJGJZVCKMKGZKS-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-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
- 239000011258 core-shell material Substances 0.000 abstract 2
- 229910052596 spinel Inorganic materials 0.000 abstract 1
- 239000011029 spinel Substances 0.000 abstract 1
- 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 description 4
- 238000000034 method Methods 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
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000010586 diagram Methods 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
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 235000019794 sodium silicate Nutrition 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer 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
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 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 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 has the advantages of wide frequency band, good wave-absorbing property of compatibility and excellent magnetic hysteresis and eddy current loss of the nickel nano-particles.
Description
Technical field
The present invention relates to absorbing material technical field, particularly a kind of preparation method of ZnOw whiskers surface composite layer.
Background technology
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
Outside, in military field, the stealth technology requirement of weaponry is also higher and higher, thus, research and develop a kind of high performance absorbing material
It is of great significance.Four pin ZnOw whiskers have unique microwave absorbing property as a kind of polar monomer, it is with the needle-shaped knot in corner
Structure, has larger dielectric loss in wave process is inhaled, and four pin ZnOw whiskers have piezoelectric effect, can be by incoming electromagnetic wave energy
It is converted into electric energy or other energy and disappears so as to achieve the purpose that to make electromagnetic wave to dissipate.But four pins prepared in the prior art
The low frequency microwave absorbing property of ZnOw whiskers can be poor, it is impossible to effectively meets low-frequency band absorbing property.
The content of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of preparation method of ZnOw whiskers surface composite layer,
The preparation method includes nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano particle and four pin ZnOw whiskers
Surface Fe and nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structure composite bed, preparation method of the present invention cause nickel core@
MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle dispersion is distributed in the metal iron layer on four pin ZnOw whiskers surfaces, fully
Played four pin ZnOw whiskers has the characteristics that larger dielectric loss when as absorbing material, and has gathered spinel-type
MnxMgyZn1-x-yFe2O4The excellent magnetic hysteresis of broadband and the microwave absorbing property of good compatibility and nano nickel particles that ferrite has
And the advantages of eddy-current loss.
The technical solution adopted by the present invention to solve the technical problems is：A kind of preparation side of ZnOw whiskers surface composite layer
Method, is made of following preparation process：
Step 1：Nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano particle；
Step 2：The chemical deposition of four pin ZnOw whiskers surface local iron；
Step 3：Four pin ZnOw whiskers Surface Fes and nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle
Composite codeposition.
Preferably, the step 1 is specially：
1. prepare reaction solution：It is that analytically pure manganese acetate, magnesium nitrate and ferrous acetate are added in deionized water by concentration, shape
Into the mixing that manganese acetate concentration is 50-280g/L, nitric acid magnesium density is 80-320g/L and ferrous acetate concentration is 35-410g/L
Liquid, then to the phosphoric acid, analytically pure disodium hydrogen phosphate and potassium permanganate that 60% is sequentially added in mixed liquor, forms 60% phosphorus
The reaction solution that acid concentration is 60-90mL/L, disodium hydrogen phosphate concentration is 15-40g/L and potassium permanganate concentration is 60-160g/L.
2. prepare nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle：Nano nickel particles are added into deionization
Water, it is 10%-40% to make its percentage by weight, disperses to form stable nickel nanometer when 1-1.5 is small at room temperature with ultrasonic wave
Grain deionized water dispersion；The reaction solution of the foregoing preparations of 50-120mL and 1L nano nickel particles deionized water dispersions are filled
Point mixing, reaction 1-1.5 it is small when after filtering drying, obtained granular powder is nickel core MnxMgyZn1-x-yFe2O4Ferrite
Shell structural nano particle.
Preferably, the step 2 is specially：
1. it is equipped with chemical sinking effusion：It is analytically pure ferrous acetate by concentration, praseodynium iron, three oxalic acid hydrate iron ammoniums
Added with sodium sulfite and ferrous acetate, praseodynium iron, three oxalic acid hydrate iron ammoniums and sodium sulfite are formed in deionized water
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 whiskers surface local iron：Four pin ZnOw whiskers are added into deionized water, make its heavy
The percentage of amount is 30-60%, disperses to form four stable pin ZnOw whisker deionizations when 0.5-1 is small at room temperature with ultrasonic wave
Aqueous dispersion A；Take dispersion 300-500mL to add in chemical sinking effusion described in 500mL and be sufficiently mixed, react 10-
The local deposition of four pin ZnOw whisker surface metal iron is realized after 30 minutes.
Preferably, the step 3 is specially：
1. prepare deposition basal liquid：It is analytically pure ferric nitrate by concentration, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, sulphur
Sour hydrogen sodium and sodium metasilicate, which add, forms ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, niter cake and silicon in deionized water
The concentration of sour 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 whiskers surfaces：By surface local deposition metal four pin ZnOw whiskers add
Deionized water, it is 50%-80% to make its percentage by weight, disperses to form stable four in 10-20 minutes with ultrasonic wave at room temperature
Pin ZnOw whisker deionized water dispersions B；Take dispersion 500mL and 500mL deposition basal liquids to be sufficiently mixed, be co-deposited
Filtering drying is crossed after when 0.5-2 is small, i.e., forms iron and nickel core MnxMgyZn1-x-yFe2O4 iron oxygen on four pin ZnOw whiskers surfaces
Solid shell structure composite bed.
The positive effect of the present invention：Four pin ZnOw whiskers Surface Fes prepared according to the methods of the invention and nickel core@
MnxMgyZn1-x-yFe2O4Ferrite shell structure composite bed, the complex dielectric permittivity on the one hand having given full play to four pin ZnOw whiskers are empty
Portion has bigger numerical within the specific limits, has the characteristics that larger dielectric loss when as absorbing material, on the other hand ties
Spinel-type Mn is closedxMgyZn1-x-yFe2O4The broadband and the microwave absorbing property of good compatibility and nickel nanometer that ferrite has
The advantages of grain excellent magnetic hysteresis and eddy-current loss, thus the four pin ZnOw whiskers Surface Fes and nickel core@Mn preparedxMgyZn1-x- yFe2O4Ferrite shell structure composite bed is the absorbing material for having excellent broadband and high-absorbility.
Brief description of the drawings
Fig. 1 is the flow diagram of composite bed preparation method of the present invention；
Fig. 2 is the structure diagram of composite bed of the present invention.
Embodiment
Below in conjunction with the accompanying drawings to a preferred embodiment of the present invention will be described in detail.
Referring to figs. 1 to Fig. 2, the preferred embodiment of the present invention provides a kind of preparation method of ZnOw whiskers surface composite layer, by
Following preparation process composition：
Step 1：Nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano particle；
Step 2：The chemical deposition of four pin ZnOw whiskers surface local iron；
Step 3：Four pin ZnOw whiskers Surface Fes and nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle
Composite codeposition.
The step 1 is specially：
1. prepare reaction solution：It is that analytically pure manganese acetate, magnesium nitrate and ferrous acetate are added in deionized water by concentration, shape
Into the mixed liquor that manganese acetate concentration is 70g/L, nitric acid magnesium density is 220g/L and ferrous acetate concentration is 60g/L, then to mixed
60% phosphoric acid, analytically pure disodium hydrogen phosphate and potassium permanganate is sequentially added in conjunction liquid, the phosphoric acid concentration for forming 60% is
80mL/L, the reaction solution that disodium hydrogen phosphate concentration is 40g/L and potassium permanganate concentration is 110g/L.
2. prepare nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle：Nano nickel particles are added into deionization
Water, make its percentage by weight be 30%, at room temperature with ultrasonic wave disperse 1 it is small when form stable nano nickel particles deionized water
Dispersion；The reaction solution of the foregoing preparations of 80mL and 1L nano nickel particles deionized water dispersions are sufficiently mixed, reaction 1.5
Filtering drying after hour, obtained granular powder is nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle.
The step 2 is specially：
1. it is equipped with chemical sinking effusion：It is analytically pure ferrous acetate by concentration, praseodynium iron, three oxalic acid hydrate iron ammoniums
Added with sodium sulfite and ferrous acetate, praseodynium iron, three oxalic acid hydrate iron ammoniums and sodium sulfite are formed in deionized water
Concentration is respectively the chemical sinking effusion of 60g/L, 130g/L, 20g/L, 40g/L.
2. the chemical deposition of four pin ZnOw whiskers surface local iron：Four pin ZnOw whiskers are added into deionized water, make its heavy
The percentage of amount is 40%, at room temperature with ultrasonic wave disperse 1 it is small when form four stable pin ZnOw whisker deionized waters and disperse
System A；Take dispersion 400mL to add in chemical sinking effusion described in 500mL and be sufficiently mixed, reaction is realized after twenty minutes
The local deposition of four pin ZnOw whisker surface metal iron.
The step 3 is specially：
1. prepare deposition basal liquid：It is analytically pure ferric nitrate by concentration, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, sulphur
Sour hydrogen sodium and sodium metasilicate, which add, forms ferric nitrate, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, niter cake and silicon in deionized water
The concentration of sour 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 whiskers surfaces：By surface local deposition metal four pin ZnOw whiskers add
Deionized water, it is 70% to make its percentage by weight, disperses to form within 15 minutes stable four pin ZnOw crystalline substances at room temperature with ultrasonic wave
Must deionized water dispersion B；Dispersion 500mL and 500mL deposition basal liquids are taken to be sufficiently mixed, when co-deposition 1.5 is small
Filtering drying is crossed afterwards, i.e., forms iron and nickel core@MnxMgyZn1-x-yFe2O4 ferrite shell structures on four pin ZnOw whiskers surfaces
Composite bed.
By phase homogenous quantities ZnOw whiskers Surface Fe manufactured in the present embodiment and nickel core MnxMgyZn1-x-yFe2O4Ferrite shell
Structure composite layer absorbing material and the common four pins ZnOw whiskers of phase homogenous quantities add coating, add common four pins ZnOw coating
It is 10-18GHz to inhale the wide experimental result of wavestrip, and adds ZnOw whiskers Surface Fe and nickel core@manufactured in the present embodiment
MnxMgyZn1-x-yFe2O4The wide experimental result of suction wavestrip of ferrite shell structure composite bed absorbing material coating is 3-18GHz.It is aobvious
So, the ZnOw whiskers Surface Fe and nickel core@Mn prepared according to the present inventionxMgyZn1-x-yFe2O4Ferrite shell structure composite bed inhales ripple
Material combines spinel-type MnxMgyZn1-x-yFe2The broadband and the microwave absorbing property of good compatibility and nickel that O4 ferrites have
The advantages of nano particle excellent magnetic hysteresis and eddy-current loss, have the absorbing property of excellent broadband and high-absorbility.
It is above-described to be merely a preferred embodiment of the present invention, it should be understood that the explanation of above example is simply used
Understand the method and its core concept of the present invention in help, the protection domain being not intended to limit the present invention is all the present invention's
Any modification for being made within thought and principle, equivalent substitution etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of preparation method of ZnOw whiskers surface composite layer, it is characterised in that be made of following preparation process：
Step 1：Nickel core@MnxMgyZn1-x-yFe2O4The preparation of ferrite shell structural nano particle；
Step 2：The chemical deposition of four pin ZnOw whiskers surface local iron；
Step 3：Four pin ZnOw whiskers Surface Fes and nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle it is compound
It is co-deposited；
The step 1 is specially：
1. prepare reaction solution：It is that analytically pure manganese acetate, magnesium nitrate and ferrous acetate are added in deionized water by concentration, is formed mixed
Liquid is closed, then to the phosphoric acid, analytically pure disodium hydrogen phosphate and potassium permanganate that 60% is sequentially added in mixed liquor, forms reaction
Liquid；
2. prepare nickel core@MnxMgyZn1-x-yFe2O4Ferrite shell structural nano particle：Nano nickel particles are added into deionized water,
It is 10%-40% to make its percentage by weight, disperses to form stable nano nickel particles when 1-1.5 is small at room temperature with ultrasonic wave
Ion aqueous dispersion；The reaction solution of the foregoing preparations of 50-120mL and 1L nano nickel particles deionized waters dispersion is fully mixed
Close, reaction 1-1.5 it is small when after filtering drying, obtained granular powder is nickel core MnxMgyZn1-x-yFe2O4Ferrite shell knot
Structure nano particle；
The step 2 is specially：
1. it is equipped with chemical sinking effusion：It is analytically pure ferrous acetate, praseodynium iron, three oxalic acid hydrate iron ammoniums and Asia by concentration
Sodium sulphate adds in deionized water and forms chemical sinking effusion；
2. the chemical deposition of four pin ZnOw whiskers surface local iron：Four pin ZnOw whiskers are added into deionized water, make its weight
Percentage is 30-60%, disperses to form four stable pin ZnOw whisker deionization moisture when 0.5-1 is small at room temperature with ultrasonic wave
Granular media system A；Take dispersion 300-500mL to add in chemical sinking effusion described in 500mL and be sufficiently mixed, 10-30 points of reaction
The local deposition of four pin ZnOw whisker surface metal iron is realized after clock；
The step 3 is specially：
1. prepare deposition basal liquid：It is analytically pure ferric nitrate by concentration, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, hydrogen sulfate
Sodium and sodium metasilicate, which are added in deionized water, forms deposition basal liquid；
2. the composite codeposition on four pin ZnOw whiskers surfaces：By surface local deposition metal four pin ZnOw whiskers add go from
Sub- water, it is 50%-80% to make its percentage by weight, disperses to form four stable pins in 10-20 minutes with ultrasonic wave at room temperature
ZnOw whisker deionized water dispersions B；Take dispersion 500mL and 500mL deposition basal liquids to be sufficiently mixed, be co-deposited
Filtering drying after when 0.5-2 is small, i.e., form iron and nickel core MnxMgyZn on four pin ZnOw whiskers surfaces1-x-yFe2O4 ferrite shells
Structure composite layer.
A kind of 2. preparation method of ZnOw whiskers surface composite layer according to claim 1, it is characterised in that：The mixing
Manganese acetate concentration is 50-280g/L in liquid, and nitric acid magnesium density is 80-320g/L, and ferrous acetate concentration is 35-410g/L, described
60% phosphoric acid concentration is 60-90mL/L in reaction solution, and disodium hydrogen phosphate concentration is 15-40g/L, and potassium permanganate concentration is 60-
160g/L。
A kind of 3. preparation method of ZnOw whiskers surface composite layer according to claim 1, it is characterised in that：The chemistry
In deposition liquid ferrous acetate, praseodynium iron, the concentration of three oxalic acid hydrate iron ammoniums and sodium sulfite be respectively 35-80g/L,
90-270g/L、5-30g/L、20-50g/L。
A kind of 4. preparation method of ZnOw whiskers surface composite layer according to claim 1, it is characterised in that：The deposition
Ferric nitrate in basal liquid, ferrous acetate, ferric ammonium ethylene diamine tetraacetate, the concentration of niter cake and sodium metasilicate are respectively 130-
280g/L, 90-320g/L, 5-20g/L, 10-45mL/L and 160-310g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610628952.7A CN106086828B (en) | 2016-08-03 | 2016-08-03 | Preparation method of ZnOw whisker surface composite layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610628952.7A CN106086828B (en) | 2016-08-03 | 2016-08-03 | Preparation method of ZnOw whisker surface composite layer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106086828A CN106086828A (en) | 2016-11-09 |
| CN106086828B true CN106086828B (en) | 2018-04-13 |
Family
ID=57453878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610628952.7A Active CN106086828B (en) | 2016-08-03 | 2016-08-03 | Preparation method of ZnOw whisker surface composite layer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106086828B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1209135A1 (en) * | 2000-11-28 | 2002-05-29 | Minebea Co., Ltd. | Production process of recycled Mn-Zn ferrite |
| CN1655296A (en) * | 2003-02-14 | 2005-08-17 | 美蓓亚株式会社 | Electromagnetic wave absorber formed of Mn-Zn ferrite |
| CN101928985A (en) * | 2010-07-23 | 2010-12-29 | 北京航空航天大学 | Quadrilateral zinc oxide/ nickel ferrite material and preparation method thereof |
| CN105274555A (en) * | 2015-11-12 | 2016-01-27 | 中国海洋大学 | NiO@PANI@ZnO three-dimensional nano composite material and preparation method thereof |
| CN105374491A (en) * | 2014-08-18 | 2016-03-02 | 南京理工大学 | Fe3O4@SiO2@ZnO ternary heterostructure core-shell nanoparticle and preparation method therefor |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2806528B2 (en) * | 1988-05-28 | 1998-09-30 | 富士電気化学株式会社 | Magnesium-zinc ferrite material for radio wave absorber |
| JP2001053483A (en) * | 1999-08-04 | 2001-02-23 | Fuji Elelctrochem Co Ltd | Nickel-zinc based ferrite electronic wave absorber |
| JP2002338339A (en) * | 2001-05-17 | 2002-11-27 | Fdk Corp | Method for manufacturing oxide magnetic material |
-
2016
- 2016-08-03 CN CN201610628952.7A patent/CN106086828B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1209135A1 (en) * | 2000-11-28 | 2002-05-29 | Minebea Co., Ltd. | Production process of recycled Mn-Zn ferrite |
| CN1655296A (en) * | 2003-02-14 | 2005-08-17 | 美蓓亚株式会社 | Electromagnetic wave absorber formed of Mn-Zn ferrite |
| CN101928985A (en) * | 2010-07-23 | 2010-12-29 | 北京航空航天大学 | Quadrilateral zinc oxide/ nickel ferrite material and preparation method thereof |
| CN105374491A (en) * | 2014-08-18 | 2016-03-02 | 南京理工大学 | Fe3O4@SiO2@ZnO ternary heterostructure core-shell nanoparticle and preparation method therefor |
| CN105274555A (en) * | 2015-11-12 | 2016-01-27 | 中国海洋大学 | NiO@PANI@ZnO three-dimensional nano composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| "Nanocrystalline spinel ferrite (MFe2O4, M=Ni,Co,Mn,Mg,Zn) powders prepared by a simple aloe vera plant-extracted solution hydrothermal route";Santi Phumying et al.;《Materials Research Bulletin》;20130228;第48卷;第2060-2065页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106086828A (en) | 2016-11-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Facile synthesis of ultrasmall Fe3O4 nanoparticles on MXenes for high microwave absorption performance | |
| Lv et al. | A brief introduction to the fabrication and synthesis of graphene based composites for the realization of electromagnetic absorbing materials | |
| Li et al. | Synthesis of u-channelled spherical Fe x (Co y Ni 1− y) 100− x Janus colloidal particles with excellent electromagnetic wave absorption performance | |
| CN103450845B (en) | Preparation method of wave-absorbing material | |
| Hekmatara et al. | Synthesis and microwave absorption characterization of SiO 2 coated Fe 3 O 4–MWCNT composites | |
| Shu et al. | Size-morphology control, surface reaction mechanism and excellent electromagnetic wave absorption characteristics of Fe3O4 hollow spheres | |
| CN103342982A (en) | Hollow spherical ferroferric oxide/graphene composite wave-absorbing material and preparation method thereof | |
| Wang et al. | Magnetic and microwave absorption properties of Ni microcrystals with hierarchical branch-like and flowers-like shapes | |
| CN108795379A (en) | A kind of preparation method of three-dimensional netted multi-walled carbon nanotube/Ni ferrite composite wave-suction material | |
| CN100355939C (en) | Method for cladding honeycomb metal cobalt or cobalt alloy on nickel or nickel alloy powder surface | |
| Han et al. | Complex permeability and microwave absorbing properties of planar anisotropy carbonyl-iron/Ni0. 5Zn0. 5Fe2O4 composite in quasimicrowave band | |
| JP2014029024A (en) | Iron cobalt ternary alloy nanoparticles with silica shells | |
| CN107418513A (en) | A kind of grapheme foam loading nanometer Fe3O4Magnetic particle composite wave-suction material and preparation method thereof | |
| Li et al. | Tunable magnetic coupling and dipole polarization of core-shell Magnéli Ti4O7 ceramic/magnetic metal possessing broadband microwave absorption properties | |
| CN101941076A (en) | Method for preparing multilayer hollow metal microspheres for electromagnetic wave absorbing material | |
| Liao et al. | Fabrication of one-dimensional CoFe 2/C@ MoS 2 composites as efficient electromagnetic wave absorption materials | |
| CN103390479B (en) | A kind of inorganic compounding micropowder of high electromagnet shield effect and preparation method thereof | |
| Wang et al. | State of the art and prospects of Fe3O4/carbon microwave absorbing composites from the dimension and structure perspective | |
| CN102568733A (en) | Thin-filmed compound broadband anti-electromagnetic interference magnetic powder and preparation method thereof | |
| Zheng et al. | Bimetallic nanocubes embedded in biomass-derived porous carbon to construct magnetic/carbon dual-mechanism layered structures for efficient microwave absorption | |
| Maleki et al. | Facile hydrothermal synthesis and microwave absorption of halloysite/polypyrrole/Fe3O4 | |
| Wu et al. | Porous Fe hollow structures with optimized impedance matching as highly efficient, ultrathin, and lightweight electromagnetic wave absorbers | |
| Zeng et al. | Enhanced dielectric loss and magnetic loss properties of copper oxide-nanowire-covered carbon fiber composites by porous nickel film | |
| CN106086828B (en) | Preparation method of ZnOw whisker surface composite layer | |
| He et al. | Magnetic needles enable tunable microwave absorption from S to Ku band via collective orientation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191118 Address after: 313000 1-B, building 1, No. 656, Qixing Road, high tech Zone, Wuxing District, Huzhou City, Zhejiang Province Patentee after: Huzhou Qiqi Electromechanical Technology Co.,Ltd. Address before: 100000 Beijing Haidian District Huayuan Road No. 2 peony building 4 floor 1424 room Patentee before: Beijing Zhonglian Technology Service Co.,Ltd. Effective date of registration: 20191118 Address after: 100000 Beijing Haidian District Huayuan Road No. 2 peony building 4 floor 1424 room Patentee after: Beijing Zhonglian Technology Service Co.,Ltd. Address before: 100144 Beijing City, Shijingshan District Jin Yuan Zhuang Road No. 5 Patentee before: NORTH CHINA University OF TECHNOLOGY |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210425 Address after: Haimen City Jiangsu city of Nantong province is more than 226100 Zhenan Bridge Village nine Group No. 101 Patentee after: Haimen Chuanghao Industrial Design Co.,Ltd. Address before: 313000 1-B, building 1, No. 656, Qixing Road, high tech Zone, Wuxing District, Huzhou City, Zhejiang Province Patentee before: Huzhou Qiqi Electromechanical Technology Co.,Ltd. |