CN105776892A - Magnetic Ag-plated glass bead and preparing method thereof - Google Patents
Magnetic Ag-plated glass bead and preparing method thereof Download PDFInfo
- Publication number
- CN105776892A CN105776892A CN201610067823.5A CN201610067823A CN105776892A CN 105776892 A CN105776892 A CN 105776892A CN 201610067823 A CN201610067823 A CN 201610067823A CN 105776892 A CN105776892 A CN 105776892A
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- China
- Prior art keywords
- magnetic
- plating
- glass microballoon
- parts
- obtains
- Prior art date
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Links
- 239000011521 glass Substances 0.000 title claims abstract description 132
- 239000011324 bead Substances 0.000 title abstract description 10
- 238000000034 method Methods 0.000 title abstract description 6
- 229910018104 Ni-P Inorganic materials 0.000 claims abstract description 24
- 229910018536 Ni—P Inorganic materials 0.000 claims abstract description 24
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 23
- 239000000956 alloy Substances 0.000 claims abstract description 23
- 238000007747 plating Methods 0.000 claims description 76
- 239000000243 solution Substances 0.000 claims description 47
- 238000003756 stirring Methods 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 36
- 239000007864 aqueous solution Substances 0.000 claims description 32
- 239000012153 distilled water Substances 0.000 claims description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 27
- 238000002360 preparation method Methods 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 20
- 239000010410 layer Substances 0.000 claims description 19
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 18
- 239000011229 interlayer Substances 0.000 claims description 18
- 239000003381 stabilizer Substances 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 15
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 13
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 13
- 235000002906 tartaric acid Nutrition 0.000 claims description 13
- 239000011975 tartaric acid Substances 0.000 claims description 13
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 230000009467 reduction Effects 0.000 claims description 9
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- ZKDNBOAOTQCXLM-UHFFFAOYSA-N 2,3-dihydroxybutanedioic acid;potassium;sodium Chemical compound [Na].[K].OC(=O)C(O)C(O)C(O)=O ZKDNBOAOTQCXLM-UHFFFAOYSA-N 0.000 claims description 2
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 2
- 101150003085 Pdcl gene Proteins 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 description 11
- 235000011167 hydrochloric acid Nutrition 0.000 description 8
- 239000000696 magnetic material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000011026 diafiltration Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 235000011083 sodium citrates Nutrition 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 3
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical class [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005426 magnetic field effect Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3607—Coatings of the type glass/inorganic compound/metal
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3644—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3668—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties
- C03C17/3676—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties specially adapted for use as electromagnetic shield
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/31—Pre-treatment
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
- C03C2218/324—De-oxidation
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
The invention relates to a magnetic Ag-plated glass bead and a preparing method thereof.The magnetic Ag-plated glass bead comprises a glass bead core, a Ni-P alloy middle layer is arranged on the outer surface of the glass bead core, an Ag layer is arranged on the outer surface of the Ni-P alloy middle layer, and the diameter of the glass bead core ranges from 30 micrometers to 60 micrometers.The preparing method of the magnetic Ag-plated glass bead comprises the following steps that firstly, a glass bead body is pretreated; secondly, the Ni-P alloy middle layer is prepared; thirdly, a magnetic glass bead body is pretreated; fourthly, the Ag layer is prepared.
Description
Technical field
The invention belongs to field of material engineering technology, be specifically related to a kind of magnetic plating Ag glass micro-
Pearl and preparation method thereof.
Background technology
In polymer base electro-magnetic screen composite material, for making composite have sufficiently high leading
Electricity rate reflects or electromagnetic wave absorption, it will usually doses in nonconducting polymeric matrix and has
The metal powder material of high conductivity, these metal powders are referred to as conducting filler.Work as conductive fill
When body doses certain mark (" diafiltration " threshold value), the specific insulation of composite can be dashed forward
The most acutely decline, " diafiltration " phenomenon occurs；Further, continue to increase when the filling fraction of electric conductor
Added-time, the specific insulation of composite quickly can tend towards stability, now the conduction of material internal
Path is the most perfect, is further added by conducting filler and also will not significantly improve the electric conductivity of material
Can, the deadweight of composite can be increased on the contrary and reduce its mechanical property.Therefore, reduction is compound
" diafiltration " threshold value of material is to improving the combination property of shielding composite and reducing cost
Highly beneficial.And reduce material " diafiltration " threshold value the best way and select conductance exactly very
High and that performance is sufficiently stable metal Ag powder.
In recent years, lightweight, green cheap to some, the material that is prone to processing carried out surface gold
Genusization replaces costliness and the excessive Ag powder of density, it has also become of conductive filler development
Important trend.Fact proved, plating Ag glass microballoon complies fully with as the substitute of pure Ag powder
Technology and the requirement in market.But, along with making rapid progress of science and technology, current electromagnetic shielding
The development of material fast forwards through to the requirement of more Gao Gengxin and target, wherein to " widescreen
Cover " the requirement most challenge of effect.This means to have improved merely the conductance of composite
Requirement can not be met, it is necessary to the function that another imparting composite is new while meeting high conductivity
Strengthen its shield effectiveness；And the introducing of magnetic material is by the electromagnetic shielding for improving composite
Performance injects new vitality.Because under the effect of electromagnetic wave, the magnetization of magnetic material presents dynamic
State process, the most not only also exists the magnetic hystersis loss not available for common dielectric, there is also
By energy loss produced by the effects such as magnetic aftereffect, domain wall resonance, natural resonance, and these are not
The electromagnetic wave of different frequency range it is respectively acting on again with the magnetic loss of mechanism.Such as, at 10kHz～
In the intermediate frequency range of 1MHz, magnetic material can occur dimensional resonance and magnetic force resonance phenomenon；?
In the high frequency stage of 1～100MHz, magnetic material will appear from domain wall resonance or relaxation；?
In 100MHz～10GHz uhf-range, magnetic material can occur natural resonance.Therefore, magnetic
The introducing of property material will strengthen the shield effectiveness of shielding material to a great extent and widens shielding
The shield ranges of material.
Summary of the invention
Goal of the invention: the problem that the present invention is directed to the existence of above-mentioned prior art makes improvement, i.e. originally
First purpose of disclosure of the invention is open a kind of magnetic plating Ag glass microballoon.The present invention's
Second purpose is to disclose the preparation method of a kind of magnetic plating Ag glass microballoon.
Technical scheme: a kind of magnetic plating Ag glass microballoon, including glass microballoon core, in institute
The outer surface stating glass microballoon core is provided with a Ni-P alloy interlayer, in the middle of Ni-P alloy
The outer surface of layer is provided with Ag layer,
A diameter of 30～60 μm of described glass microballoon core.
Further, the thickness of described Ni-P alloy interlayer is 1～3 μm.
Further, the thickness of described Ag layer is 1～3 μm.
The preparation method of a kind of magnetic plating Ag glass microballoon, comprises the following steps:
(1) pretreated glass microballon
(11) first with the Na that concentration is 5～40wt%2CO3Glass microballoon is carried out by the aqueous solution
Clean, then with the aqueous hydrochloric acid solution of 2～10wt%, glass microballoon is carried out, finally use
Glass microballoon is carried out by the industrial alcohol aqueous solution of 60～70wt%；
(12) glass microballoon that step (11) obtains is put into the hydrofluoric acid water of 0.1～3wt%
Solution is carried out be roughened etching processing 5～15 minutes；
(13) glass microballoon obtaining step (12) puts into SnCl2Mixing water with HCl
In solution, stir 10～40 minutes；
(14) glass microballoon that step (13) obtains is put into concentration be 0.02～
0.1wt%PdCl2In aqueous solution, stir 10～40 minutes；
(2) Ni-P alloy interlayer is prepared
(21) preparation plating solution
By 2～8 parts of NiCl2·6H2O, 1～5 part of sodium citrate, 0.1～1 part of tartaric acid
Potassium sodium is dissolved in 50～150 parts of distilled water, then to take 50～150 parts of concentration be 3～5wt%
NaH2PO2·H2The O aqueous solution is added thereto, and is added thereto to 6～9 parts of concentration the most again
It is 25～28wt% ammoniacal liquor, after stirring, i.e. obtains plating solution；
(22) plating
The glass microballoon that step (14) obtains is put in the plating solution that step (21) obtains,
With 2～5 DEG C of min under stirring-1Heating rate be heated to 70 DEG C after be incubated
20～40min, filter, after distilled water washing, prepare magnetic glass microballon；
(3) pretreatment magnetic glass microballon
(31) by 1～5 part of SnCl2, 2～8 parts of concentrated hydrochloric acid and 5～30 parts of polyethylene glycol
2000 are dissolved in 50～150 parts of distilled water, stir and i.e. obtain cleaning fluid；
(32) the magnetic glass microballon that step (22) obtains is put into step (31) to obtain
Cleaning fluid in, stir 20～40min, filter, then wash after 2～3 times with distilled water
Obtain magnetic glass microballon；
(33) the magnetic glass microballon that step (32) obtains is put into concentration be 0.02～
The PdCl of 0.1wt%2In the aqueous solution, stir 10～30min, filter, then wash with distillation
Wash 2～3 times and obtain magnetic glass microballon；
(4) Ag layer is prepared
(41) preparation plating solution
By 1～5 part of AgNO3It is dissolved in 100 parts of distilled water with 1～5 part of compound stabilizer,
Adding the ammoniacal liquor that 3～9 parts of concentration is 25～28wt%, stirring is completely dissolved to precipitation and get final product
To plating solution；
(42) complex reducing agent preparation
0.5～3 part of hydrazine hydrate is dissolved in 40～60 parts of methyl alcohol formation complex reducing agent molten
Liquid；
(43) plating
The magnetic glass microballon that step (33) obtains is put into the plating that step (41) obtains
Liquid stirs, then drips the composite reduction agent solution that step (42) obtains, instead
Filter after answering 10～30min, wash, i.e. obtain magnetic plating Ag glass microballoon after drying.
Further, in the mixed aqueous solution in step (13), SnCl2Concentration be 1～8wt%,
The concentration of HCl is 5～15wt%.
Further, the compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric acid
Mixture, the mass ratio of tartaric acid, EDTA and thiocarbamide is (0.5～6): (0.1～2):
(0.03～0.1).
Beneficial effect: the invention discloses a kind of magnetic plating Ag glass microballoon and preparation method thereof
Have the advantages that
1, in silver plating process, owing to using compound stabilizer, therefore plating solution is sufficiently stable,
Place the longer time and also undergo no deterioration within the scope of wider temperature, being of value to industrialization
Produce；
2, in silver plating process, the reproducibility of complex reducing agent is relatively strong, when both shortening reaction
Between, ensure again silver coating compactness；
3, silver-plated glass beads has certain magnetic.
Accompanying drawing explanation
Fig. 1 be a kind of magnetic disclosed by the invention plating Ag glass microballoon stereoscan photograph；
Fig. 2 be a kind of magnetic disclosed by the invention plating Ag glass microballoon XRD spectrum；
Fig. 3 is the magnetic hysteresis regression curve of a kind of magnetic disclosed by the invention plating Ag glass microballoon.
Detailed description of the invention:
Below the detailed description of the invention of the present invention is described in detail.
Specific embodiment 1
A kind of magnetic plating Ag glass microballoon, including glass microballoon core, at glass microballoon core
Outer surface be provided with a Ni-P alloy interlayer, the outer surface at Ni-P alloy interlayer is provided with
Ag layer,
A diameter of 30 μm of glass microballoon core.
Further, the thickness of Ni-P alloy interlayer is 1 μm.
Further, the thickness of Ag layer is 1 μm.
The preparation method of a kind of magnetic plating Ag glass microballoon, comprises the following steps:
(1) pretreated glass microballon
(11) it is first the Na of 5wt% by concentration2CO3Glass microballoon is carried out by the aqueous solution,
With the aqueous hydrochloric acid solution of 2wt%, glass microballoon is carried out again, finally with 60wt%'s
Glass microballoon is carried out by the industrial alcohol aqueous solution；
(12) hydrofluoric acid that the glass microballoon that step (11) obtains is put into 0.1wt% is water-soluble
Liquid is carried out be roughened etching processing 5 minutes；
(13) glass microballoon obtaining step (12) puts into SnCl2Mixing water with HCl
In solution, stir 10 minutes；
(14) glass microballoon that step (13) obtains being put into concentration is 0.02wt%PdCl2
In aqueous solution, stir 10 minutes；
(2) Ni-P alloy interlayer is prepared
(21) preparation plating solution
By 2 parts of NiCl2·6H2O, 1 part of sodium citrate, 0.1 part of sodium potassium tartrate tetrahydrate are dissolved in
In 50 parts of distilled water, then to take 50 parts of concentration be the NaH of 3wt%2PO2·H2The O aqueous solution adds
Entering wherein, being added thereto to 6 parts of concentration the most again is 25wt% ammoniacal liquor, after stirring
I.e. obtain plating solution；
(22) plating
The glass microballoon that step (14) obtains is put in the plating solution that step (21) obtains,
With 2 DEG C of min under stirring-1Heating rate be heated to 70 DEG C after be incubated 20min,
Filter, after distilled water washing, prepare magnetic glass microballon；
(3) pretreatment magnetic glass microballon
(31) by 1 part of SnCl2, 2 parts of concentrated hydrochloric acids and 5 parts of polyethylene glycol 2000s are dissolved in
In 50 parts of distilled water, stir and i.e. obtain cleaning fluid；
(32) the magnetic glass microballon that step (22) obtains is put into step (31) to obtain
Cleaning fluid in, stir 20min, filter, then wash after 2 times with distilled water and obtain magnetic
Property glass microballoon；
(33) the magnetic glass microballon that step (32) obtains being put into concentration is 0.02wt%
PdCl2In the aqueous solution, stir 10min, filter, then obtain for 2 times with distilled water washing
Magnetic glass microballon；
(4) Ag layer is prepared
(41) preparation plating solution
By 3 parts of AgNO3It is dissolved in 100 parts of distilled water with 3.86 parts of compound stabilizers, adds
Entering 3 parts of concentration is the ammoniacal liquor of 25wt%, and stirring is completely dissolved to precipitation and i.e. obtains plating solution；
(42) complex reducing agent preparation
1.5 parts of hydrazine hydrates are dissolved in 55 parts of methyl alcohol formation composite reduction agent solution；
(43) plating
The magnetic glass microballon that step (33) obtains is put into the plating that step (41) obtains
Liquid stirs, then drips the composite reduction agent solution that step (42) obtains, instead
Filter after answering 10min, wash, i.e. obtain magnetic plating Ag glass microballoon after drying.
Further, in the mixed aqueous solution in step (13), SnCl2Concentration be 1wt%,
The concentration of HCl is 5wt%.
Further, the compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric acid
Mixture, the mass ratio of tartaric acid, EDTA and thiocarbamide is 3:0.8:0.06.
The magnetic plating Ag glass microballoon prepared is characterized.
As shown in Figure 1, the surface of magnetic plating Ag glass microballoon has densification, clad complete.
As shown in Figure 2, magnetic plating Ag glass microballoon is amorphous state, the crystalline substance of Ni-P alloy-layer
Change degree is the lowest, but the diffraction peak intensity of Ag layer is higher and to a certain degree wideization occurs,
Illustrate that the grain size being deposited on compound particle outermost Ag particle is the least.
From the figure 3, it may be seen that hysteresis occurs under magnetic plating Ag glass microballoon outside magnetic field effect,
There is magnetic.
Specific embodiment 2
A kind of magnetic plating Ag glass microballoon, including glass microballoon core, at glass microballoon core
Outer surface be provided with a Ni-P alloy interlayer, the outer surface at Ni-P alloy interlayer is provided with
Ag layer,
A diameter of 60 μm of glass microballoon core.
Further, the thickness of Ni-P alloy interlayer is 3 μm.
Further, the thickness of Ag layer is 3 μm.
The preparation method of a kind of magnetic plating Ag glass microballoon, comprises the following steps:
(1) pretreated glass microballon
(11) it is first the Na of 40wt% by concentration2CO3Glass microballoon is carried out clearly by the aqueous solution
Wash, then with the aqueous hydrochloric acid solution of 10wt%, glass microballoon is carried out, finally use 70wt%
The industrial alcohol aqueous solution glass microballoon is carried out；
(12) glass microballoon that step (11) obtains is put into the hydrofluoric acid aqueous solution of 3wt%
In carry out being roughened etching processing 15 minutes；
(13) glass microballoon obtaining step (12) puts into SnCl2Mixing water with HCl
In solution, stir 40 minutes；
(14) glass microballoon that step (13) obtains being put into concentration is 0.1wt%PdCl2
In aqueous solution, stir 40 minutes；
(2) Ni-P alloy interlayer is prepared
(21) preparation plating solution
By 8 parts of NiCl2·6H2O, 5 parts of sodium citrates, 1 part of sodium potassium tartrate tetrahydrate are dissolved in 150
In part distilled water, then to take 150 parts of concentration be the NaH of 5wt%2PO2·H2The O aqueous solution adds
Wherein, being added thereto to 9 parts of concentration the most again is 28wt% ammoniacal liquor, after stirring i.e.
Obtain plating solution；
(22) plating
The glass microballoon that step (14) obtains is put in the plating solution that step (21) obtains,
With 5 DEG C of min under stirring-1Heating rate be heated to 70 DEG C after be incubated 40min,
Filter, after distilled water washing, prepare magnetic glass microballon；
(3) pretreatment magnetic glass microballon
(31) by 5 parts of SnCl2, 8 parts of concentrated hydrochloric acids and 30 parts of polyethylene glycol 2000s are dissolved in
In 150 parts of distilled water, stir and i.e. obtain cleaning fluid；
(32) the magnetic glass microballon that step (22) obtains is put into step (31) to obtain
Cleaning fluid in, stir 40min, filter, then wash after 3 times with distilled water and obtain magnetic
Property glass microballoon；
(33) the magnetic glass microballon that step (32) obtains being put into concentration is 0.1wt%'s
PdCl2In the aqueous solution, stir 30min, filter, then obtain magnetic 3 times with distilled water washing
Property glass microballoon；
(4) Ag layer is prepared
(41) preparation plating solution
By 5 parts of AgNO3It is dissolved in 100 parts of distilled water with 5 parts of compound stabilizers, adds 9
Part concentration is the ammoniacal liquor of 28wt%, and stirring is completely dissolved to precipitation and i.e. obtains plating solution；
(42) complex reducing agent preparation
3 parts of hydrazine hydrates are dissolved in 60 parts of methyl alcohol formation composite reduction agent solution；
(43) plating
The magnetic glass microballon that step (33) obtains is put into the plating that step (41) obtains
Liquid stirs, then drips the composite reduction agent solution that step (42) obtains, instead
Filter after answering 30min, wash, i.e. obtain magnetic plating Ag glass microballoon after drying.
Further, in the mixed aqueous solution in step (13), SnCl2Concentration be 8wt%,
The concentration of HCl is 15wt%.
Further, the compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric acid
Mixture, the mass ratio of tartaric acid, EDTA and thiocarbamide is 3:0.1:0.03.
Specific embodiment 3
A kind of magnetic plating Ag glass microballoon, including glass microballoon core, at glass microballoon core
Outer surface be provided with a Ni-P alloy interlayer, the outer surface at Ni-P alloy interlayer is provided with
Ag layer,
A diameter of 40 μm of glass microballoon core.
Further, the thickness of Ni-P alloy interlayer is 2 μm.
Further, the thickness of Ag layer is 2 μm.
The preparation method of a kind of magnetic plating Ag glass microballoon, comprises the following steps:
(1) pretreated glass microballon
(11) it is first the Na of 20wt% by concentration2CO3Glass microballoon is carried out clearly by the aqueous solution
Wash, then with the aqueous hydrochloric acid solution of 5wt%, glass microballoon is carried out, finally use 65wt%
The industrial alcohol aqueous solution glass microballoon is carried out；
(12) glass microballoon that step (11) obtains is put into the hydrofluoric acid aqueous solution of 1wt%
In carry out being roughened etching processing 10 minutes；
(13) glass microballoon obtaining step (12) puts into SnCl2Mixing water with HCl
In solution, stir 20 minutes；
(14) glass microballoon that step (13) obtains being put into concentration is 0.05wt%PdCl2
In aqueous solution, stir 20 minutes；
(2) Ni-P alloy interlayer is prepared
(21) preparation plating solution
By 5 parts of NiCl2·6H2O, 3 parts of sodium citrates, 0.5 part of sodium potassium tartrate tetrahydrate are dissolved in
In 100 parts of distilled water, then to take 100 parts of concentration be the NaH of 4wt%2PO2·H2The O aqueous solution
Being added thereto, being added thereto to 7 parts of concentration the most again is 26wt% ammoniacal liquor, stirs
After i.e. obtain plating solution；
(22) plating
The glass microballoon that step (14) obtains is put in the plating solution that step (21) obtains,
With 3 DEG C of min under stirring-1Heating rate be heated to 70 DEG C after be incubated 30min,
Filter, after distilled water washing, prepare magnetic glass microballon；
(3) pretreatment magnetic glass microballon
(31) by 3 parts of SnCl2, 5 parts of concentrated hydrochloric acids and 20 parts of polyethylene glycol 2000s are dissolved in
In 100 parts of distilled water, stir and i.e. obtain cleaning fluid；
(32) the magnetic glass microballon that step (22) obtains is put into step (31) to obtain
Cleaning fluid in, stir 30min, filter, then wash after 3 times with distilled water and obtain magnetic
Property glass microballoon；
(33) the magnetic glass microballon that step (32) obtains being put into concentration is 0.05wt%
PdCl2In the aqueous solution, stir 20min, filter, then obtain for 2 times with distilled water washing
Magnetic glass microballon；
(4) Ag layer is prepared
(41) preparation plating solution
By 1 part of AgNO3It is dissolved in 100 parts of distilled water with 1.07 parts of compound stabilizers, adds
Entering 6 parts of concentration is the ammoniacal liquor of 26wt%, and stirring is completely dissolved to precipitation and i.e. obtains plating solution；
(42) complex reducing agent preparation
0.5 part of hydrazine hydrate is dissolved in 40 parts of methyl alcohol formation composite reduction agent solution；
(43) plating
The magnetic glass microballon that step (33) obtains is put into the plating that step (41) obtains
Liquid stirs, then drips the composite reduction agent solution that step (42) obtains, instead
Filter after answering 20min, wash, i.e. obtain magnetic plating Ag glass microballoon after drying.
Further, in the mixed aqueous solution in step (13), SnCl2Concentration be 5wt%,
The concentration of HCl is 10wt%.
Further, the compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric acid
Mixture, the mass ratio of tartaric acid, EDTA and thiocarbamide is 3:2:0.1.
Specific embodiment 4
Roughly the same with specific embodiment 1, differ only in:
Step (41) is by 3 parts of AgNO3It is dissolved in 100 parts of distilled water with 3.78 parts of compound stabilizers
In, adding 3 parts of concentration is the ammoniacal liquor of 25wt%, and stirring is completely dissolved to precipitation and i.e. obtains plating solution；
Compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric mixture,
The mass ratio of tartaric acid, EDTA and thiocarbamide is 0.5:0.1:0.03.
Specific embodiment 5
Roughly the same with specific embodiment 2, differ only in:
Compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric mixture,
The mass ratio of tartaric acid, EDTA and thiocarbamide is 0.5:2:0.1.
Specific embodiment 6
Roughly the same with specific embodiment 3, differ only in:
By 1 part of AgNO in step (41)3It is dissolved in 100 parts of distillations with 1.02 parts of compound stabilizers
In water, adding 6 parts of concentration is the ammoniacal liquor of 26wt%, and stirring is completely dissolved to precipitation and is i.e. plated
Liquid；
Compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric mixture,
The mass ratio of tartaric acid, EDTA and thiocarbamide is 6:0.1:0.03.
Specific embodiment 7
Roughly the same with specific embodiment 1, differ only in:
By 3 parts of AgNO in step (41)3It is dissolved in 100 parts of distillations with 3.43 parts of compound stabilizers
In water, adding 3 parts of concentration is the ammoniacal liquor of 25wt%, and stirring is completely dissolved to precipitation and is i.e. plated
Liquid；
Compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric mixture,
The mass ratio of tartaric acid, EDTA and thiocarbamide is 6:0.8:0.06.
Above embodiments of the present invention are elaborated.On but the present invention is not limited to
State embodiment, in the ken that art those of ordinary skill is possessed, also
Can make a variety of changes on the premise of without departing from present inventive concept.
Claims (6)
1. a magnetic plating Ag glass microballoon, it is characterised in that include glass microballoon core,
Outer surface at described glass microballoon core is provided with a Ni-P alloy interlayer, at Ni-P alloy
The outer surface in intermediate layer is provided with Ag layer, a diameter of 30～60 μm of described glass microballoon core.
A kind of magnetic plating Ag glass microballoon the most according to claim 1, it is characterised in that
The thickness of described Ni-P alloy interlayer is 1～3 μm.
A kind of magnetic plating Ag glass microballoon the most according to claim 1 and 2, its feature
Being, the thickness of described Ag layer is 1～3 μm.
4. the preparation method of a magnetic plating Ag glass microballoon, it is characterised in that include following
Step:
(1) pretreated glass microballon
(11) first with the Na that concentration is 5～40wt%2CO3Glass microballoon is carried out by the aqueous solution
Clean, then with the aqueous hydrochloric acid solution of 2～10wt%, glass microballoon is carried out, finally use
Glass microballoon is carried out by the industrial alcohol aqueous solution of 60～70wt%；
(12) glass microballoon that step (11) obtains is put into the hydrofluoric acid water of 0.1～3wt%
Solution is carried out be roughened etching processing 5～15 minutes；
(13) glass microballoon obtaining step (12) puts into SnCl2Mixing water with HCl
In solution, stir 10～40 minutes；
(14) glass microballoon that step (13) obtains is put into concentration be 0.02～
0.1wt%PdCl2In aqueous solution, stir 10～40 minutes；
(2) Ni-P alloy interlayer is prepared
(21) preparation plating solution
By 2～8 parts of NiCl2·6H2O, 1～5 part of sodium citrate, 0.1～1 part of tartaric acid
Potassium sodium is dissolved in 50～150 parts of distilled water, then to take 50～150 parts of concentration be 3～5wt%
NaH2PO2·H2The O aqueous solution is added thereto, and is added thereto to 6～9 parts of concentration the most again
It is 25～28wt% ammoniacal liquor, after stirring, i.e. obtains plating solution；
(22) plating
The glass microballoon that step (14) obtains is put in the plating solution that step (21) obtains,
With 2～5 DEG C of min under stirring-1Heating rate be heated to 70 DEG C after be incubated
20～40min, filter, after distilled water washing, prepare magnetic glass microballon；
(3) pretreatment magnetic glass microballon
(31) by 1～5 part of SnCl2, 2～8 parts of concentrated hydrochloric acid and 5～30 parts of polyethylene glycol
2000 are dissolved in 50～150 parts of distilled water, stir and i.e. obtain cleaning fluid；
(32) the magnetic glass microballon that step (22) obtains is put into step (31) to obtain
Cleaning fluid in, stir 20～40min, filter, then wash after 2～3 times with distilled water
Obtain magnetic glass microballon；
(33) the magnetic glass microballon that step (32) obtains is put into concentration be 0.02～
The PdCl of 0.1wt%2In the aqueous solution, stir 10～30min, filter, then wash with distillation
Wash 2～3 times and obtain magnetic glass microballon；
(4) Ag layer is prepared
(41) preparation plating solution
By 1～5 part of AgNO3It is dissolved in 100 parts of distilled water with 1～5 part of compound stabilizer,
Adding the ammoniacal liquor that 3～9 parts of concentration is 25～28wt%, stirring is completely dissolved to precipitation and get final product
To plating solution；
(42) complex reducing agent preparation
0.5～3 part of hydrazine hydrate is dissolved in 40～60 parts of methyl alcohol formation complex reducing agent molten
Liquid；
(43) plating
The magnetic glass microballon that step (33) obtains is put into the plating that step (41) obtains
Liquid stirs, then drips the composite reduction agent solution that step (42) obtains, instead
Filter after answering 10～30min, wash, i.e. obtain magnetic plating Ag glass microballoon after drying.
The preparation method of a kind of magnetic the most according to claim 4 plating Ag glass microballoon,
It is characterized in that, in the mixed aqueous solution in step (13), SnCl2Concentration be 1～8wt%,
The concentration of HCl is 5～15wt%.
The preparation method of a kind of magnetic the most according to claim 4 plating Ag glass microballoon,
It is characterized in that, the compound stabilizer in step (41) is thiocarbamide, EDTA and tartaric
Mixture, the mass ratio of tartaric acid, EDTA and thiocarbamide is (0.5～6): (0.1～2): (0.03～
0.1)。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107285643A (en) * | 2017-07-18 | 2017-10-24 | 合肥鼎亮光学科技有限公司 | A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely |
| CN111154172A (en) * | 2020-01-08 | 2020-05-15 | 江苏科麦特科技发展有限公司 | Shielding type plastic film and composite belt prepared from same |
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| CN103130421A (en) * | 2013-04-03 | 2013-06-05 | 中国兵器工业集团第五三研究所 | Nickel plating silvered glass bead and preparation method thereof |
| JP2013258138A (en) * | 2012-05-16 | 2013-12-26 | Hitachi Chemical Co Ltd | Conductive particle, anisotropic conductive adhesive film, and connection structure |
| CN104646663A (en) * | 2014-12-11 | 2015-05-27 | 薛世君 | Ag Cu coated powder preparation method |
| CN105273689A (en) * | 2014-07-18 | 2016-01-27 | 广东工业大学 | Novel multi-element structure composite conductive filling material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013258138A (en) * | 2012-05-16 | 2013-12-26 | Hitachi Chemical Co Ltd | Conductive particle, anisotropic conductive adhesive film, and connection structure |
| CN103130421A (en) * | 2013-04-03 | 2013-06-05 | 中国兵器工业集团第五三研究所 | Nickel plating silvered glass bead and preparation method thereof |
| CN105273689A (en) * | 2014-07-18 | 2016-01-27 | 广东工业大学 | Novel multi-element structure composite conductive filling material |
| CN104646663A (en) * | 2014-12-11 | 2015-05-27 | 薛世君 | Ag Cu coated powder preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107285643A (en) * | 2017-07-18 | 2017-10-24 | 合肥鼎亮光学科技有限公司 | A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely |
| CN111154172A (en) * | 2020-01-08 | 2020-05-15 | 江苏科麦特科技发展有限公司 | Shielding type plastic film and composite belt prepared from same |
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