CN103871540B - A kind of nickel bag glass conductive powder body and preparation method thereof for conductive rubber - Google Patents
A kind of nickel bag glass conductive powder body and preparation method thereof for conductive rubber Download PDFInfo
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- CN103871540B CN103871540B CN201410097073.7A CN201410097073A CN103871540B CN 103871540 B CN103871540 B CN 103871540B CN 201410097073 A CN201410097073 A CN 201410097073A CN 103871540 B CN103871540 B CN 103871540B
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 239000000843 powder Substances 0.000 title claims abstract description 133
- 239000011521 glass Substances 0.000 title claims abstract description 126
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000007747 plating Methods 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000126 substance Substances 0.000 claims abstract description 34
- 238000004140 cleaning Methods 0.000 claims abstract description 32
- 238000005530 etching Methods 0.000 claims abstract description 21
- 206010070834 Sensitisation Diseases 0.000 claims abstract description 20
- 230000008313 sensitization Effects 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 16
- 230000004913 activation Effects 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000003638 chemical reducing agent Substances 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 230000003213 activating effect Effects 0.000 claims description 10
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 10
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 9
- 239000008139 complexing agent Substances 0.000 claims description 9
- 238000005238 degreasing Methods 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 9
- 239000003381 stabilizer Substances 0.000 claims description 9
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 claims description 8
- 239000012493 hydrazine sulfate Substances 0.000 claims description 8
- 229910000377 hydrazine sulfate Inorganic materials 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical group [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 7
- 239000001632 sodium acetate Substances 0.000 claims description 7
- 235000017281 sodium acetate Nutrition 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 5
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical group [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 5
- 229910052763 palladium Inorganic materials 0.000 claims description 5
- -1 salt nickelous sulfate Chemical class 0.000 claims description 5
- 230000002000 scavenging effect Effects 0.000 claims description 5
- 239000000344 soap Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 239000001488 sodium phosphate Substances 0.000 claims description 5
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 5
- 239000001119 stannous chloride Substances 0.000 claims description 5
- 235000011150 stannous chloride Nutrition 0.000 claims description 5
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims description 3
- OQUFOZNPBIIJTN-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;sodium Chemical group [Na].OC(=O)CC(O)(C(O)=O)CC(O)=O OQUFOZNPBIIJTN-UHFFFAOYSA-N 0.000 claims 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000001788 irregular Effects 0.000 description 6
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- 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
- 238000007865 diluting Methods 0.000 description 4
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical group [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- PXHVJJICTQNCMI-OUBTZVSYSA-N nickel-60 atom Chemical compound [60Ni] PXHVJJICTQNCMI-OUBTZVSYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 229960002449 glycine Drugs 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 235000013905 glycine and its sodium salt Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 239000012811 non-conductive material Substances 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011238 particulate composite Substances 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
- 239000001230 potassium iodate Substances 0.000 description 1
- 229940093930 potassium iodate Drugs 0.000 description 1
- 235000006666 potassium iodate Nutrition 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 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 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Chemically Coating (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The invention discloses a kind of conductive rubber nickel bag glass conductive powder body and preparation method thereof, belong to electromagnetic shielding conductive powder body material field, the surface that described nickel bag glass conductive powder body is coated on 15% ~ 40% glass powder by 60% ~ 85% nickel forms, and its preparation method comprises glass powder alkali cleaning oil removing, the alligatoring of glass powder acid etching, glass powder sensitization, glass powder activation and glass powder chemical nickel plating. Preparation technology of the present invention, raw material composition is simple, is suitable for large-scale production, and the nickel bag glass conductive powder body making has good capability of electromagnetic shielding, is suitable for making the conductive rubber product of anti-electromagnetic interference and water vapor seal. The resistivity of the conductive rubber of making of the present invention is less than 0.15 Ω cm, has good mechanical property simultaneously, can meet the business application of middle and high end completely.
Description
Technical field
The invention belongs to a kind of electromagnetic shielding conductive powder body material, be specifically related to a kind of conductive rubber nickel bag glass conductionPowder and preparation method thereof.
Background technology
Metallic nickel cladded type micro particulate materials is the composite particulate material that a class has nucleocapsid structure, and it has not only keptThe coat of metal and be wrapped by particle main feature separately, also shows by complex effect that each component interaction producesExcellent comprehensive performance, has application at numerous areas such as metallurgy, mechanical aviations, and wherein, glass nickel plating is exactly a kind of nickel whereinCoated powder material. Glass nickel plating is to adopt specific processing method to obtain layer of metal coating on glass basis surface, makes itHave the advantage of glass and nickel metal concurrently. Glass after nickel plating has metal appearance and good heat conduction, conduction and braze ability,Electronic applications has important application. Chemical plating is to realize the metallized a kind of important means of non-metal material surface. Due to nothingNeed additional power source, its not only can conduction metal material surface obtain coating, but also can Inorganic Non-metallic Materials,The surface deposition of the non-conductive material such as macromolecular material goes out metal or alloy coating, is therefore widely used in nonmetallic materialsIn surface metal metallization processes. Glass powder nickel plating can be used as the filler of electromagnetic shielding material conductive rubber, with conventionally usedSilver powder, silver-bearing copper powder, silver-colored aluminium powder, the conductive fillers such as pure nickel powder are compared, and can solve conductive filler density large, the asking of cost costlinessTopic, and non-corrosive, not oxidizable, because bi-material is metal and nonmetal, so just avoid in a lot of application scenariosThere is the possibility of electrochemical corrosion, thereby make conductive rubber product can keep permanent anti-electromagnetic interference and anti-steam to sealDual-use function.
Summary of the invention
The present invention proposes in order to overcome the shortcoming existing in prior art, its objective is a kind of conductive rubber is providedWith nickel bag glass conductive powder body and preparation method thereof.
Technical scheme of the present invention is:
A kind of nickel bag glass conductive powder body for conductive rubber, the component of described powder and percentage by weight are:
Nickel 60% ~ 85%
Glass powder 15% ~ 40%.
Described glass powder be shaped as spherical or irregular sheet, the average grain diameter of glass powder is 10～60 microns.
Described nickel is coated on the surface of glass powder.
A preparation method for nickel bag glass conductive powder body for conductive rubber, comprises the following steps:
(I) glass powder alkali cleaning oil removing
At 50 DEG C, with degreasing fluid, glass powder is carried out to alkali cleaning oil removing, scavenging period is 10～15 minutes;
The alligatoring of (II) glass powder acid etching
To cleaning with clear water through the glass powder of alkali cleaning oil removing, then service property (quality) mark is 20% hydrofluoric acid,At 20 DEG C, carry out acid etching alligatoring, etching period 30 minutes;
The sensitization of (III) glass powder
To cleaning with clear water through the glass powder of acid etching alligatoring, the stannous chloride that then working concentration is 30g/LCarry out sensitization processing, sensitization time is 3～5 minutes;
The activation of (IV) glass powder
To after the glass powder of sensitization cleans with clear water, then at 30 DEG C, use activating solution to activate,Soak time is 10 minutes;
(V) glass powder chemical nickel plating
Glass powder through overactivation is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, at 40 DEG CWater bath condition under, glass powder is added in chemical nickel-plating liquid, fully stir with electromagnetic mixer, and use pH regulator solutionRegulate pH value to 4.5 ~ 9, react 2 hours, till reacting completely, and with distilled water cleaning 5 minutes; After finishing, nickel plating uses clear waterNickel plating powder is rinsed to neutral, after oven dry, obtain conductive rubber nickel bag glass conductive powder body.
In described step (I), component and each concentration of component of degreasing fluid are respectively:
Sodium phosphate 50g/L
Sodium carbonate 30g/L
NaOH 25g/L
Soap powder is appropriate.
In described step (IV), component and each concentration of component of activating solution are respectively:
Palladium bichloride 0.5g/L
Concentrated hydrochloric acid 10mL/L.
In described step (V), chemical nickel-plating liquid comprises main salt and reducing agent, also comprises complexing agent, buffer and stabilizing agentIn one or more.
In described step (V), pH regulator solution is hydrochloric acid solution or Ammonia.
Described main salt is nickelous sulfate; Described reducing agent is at least one in sodium hypophosphite or hydrazine sulfate; Described complexing agentIt is natrium citricum; Described buffer is sodium acetate; Described stabilizing agent is plumbi nitras.
In described chemical nickel-plating liquid, the concentration of main salt nickelous sulfate is 25g/L ~ 38g/L; Reducing agent in described chemical nickel-plating liquidThe concentration of sodium hypophosphite is 25g/L ~ 33g/L, and the concentration of hydrazine sulfate is 10g/L; Described Complexing Agent in Electroless Nickel Deposition Baths citric acidThe concentration of sodium is 38mg/L; In described chemical nickel-plating liquid, the concentration of buffer sodium acetate is 10g/L; In described chemical nickel-plating liquidThe concentration of stabilizing agent plumbi nitras is 1mg/L ~ 3mg/L.
The invention has the beneficial effects as follows:
Nickel bag glass conductive powder body and preparation method thereof for a kind of conductive rubber provided by the invention, preparation technology, raw materialComposition is simple, is suitable for large-scale production, and the nickel bag glass conductive powder body making has good capability of electromagnetic shielding, is applicable toFor making the conductive rubber product of anti-electromagnetic interference and water vapor seal. The resistivity of the conductive rubber of making of the present invention is less than0.15 Ω cm has good mechanical property simultaneously, can meet the business application of middle and high end completely.
Brief description of the drawings
Fig. 1 is the ESEM of the irregular foliated glass conducting powder of conductive rubber nickel bag prepared of the embodiment of the present invention 1Figure;
Fig. 2 is the scanning electron microscope (SEM) photograph of the conductive rubber nickel bag globular glass conducting powder prepared of the embodiment of the present invention 2.
Detailed description of the invention
Below in conjunction with drawings and the specific embodiments to the present invention a kind of nickel bag glass conductive powder body and system thereof for conductive rubberPreparation Method is elaborated:
A kind of nickel bag glass conductive powder body for conductive rubber, the component of described powder and percentage by weight are:
Nickel 60% ~ 85%
Glass powder 15% ~ 40%.
Described glass powder be shaped as spherical or irregular sheet, the average grain diameter of glass powder is 10～60 microns.
Described nickel is coated on the surface of glass powder.
A preparation method for nickel bag glass conductive powder body for conductive rubber, comprises the following steps:
(I) glass powder alkali cleaning oil removing
At 50 DEG C, with degreasing fluid, glass powder is carried out to alkali cleaning oil removing, scavenging period is 10～15 minutes;
The alligatoring of (II) glass powder acid etching
To cleaning with clear water through the glass powder of alkali cleaning oil removing, then service property (quality) mark is 20% hydrofluoric acid,At 20 DEG C, carry out acid etching alligatoring, etching period 30 minutes;
The sensitization of (III) glass powder
To cleaning with clear water through the glass powder of acid etching alligatoring, the stannous chloride that then working concentration is 30g/LCarry out sensitization processing, sensitization time is 3～5 minutes;
The activation of (IV) glass powder
To after the glass powder of sensitization cleans with clear water, then at 30 DEG C, use activating solution to activate,Soak time is 10 minutes;
(V) glass powder chemical nickel plating
Glass powder through overactivation is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, at 40 DEG CWater bath condition under, glass powder is added in chemical nickel-plating liquid, fully stir with electromagnetic mixer, and use pH regulator solutionRegulate pH value to 4.5 ~ 9, react 2 hours, till reacting completely, and with distilled water cleaning 5 minutes; After finishing, nickel plating uses clear waterNickel plating powder is rinsed to neutral, after oven dry, obtain conductive rubber nickel bag glass conductive powder body.
In described step (I), component and each concentration of component of degreasing fluid are respectively:
Sodium phosphate 50g/L
Sodium carbonate 30g/L
NaOH 25g/L
Soap powder is appropriate.
In described step (IV), component and each concentration of component of activating solution are respectively:
Palladium bichloride 0.5g/L
Concentrated hydrochloric acid 10mL/L.
In described step (V), chemical nickel-plating liquid comprises main salt and reducing agent, also comprises complexing agent, buffer and stabilizing agentIn one or more.
In described step (V), pH regulator solution is hydrochloric acid solution or Ammonia.
Described main salt is nickelous sulfate; Described reducing agent is at least one in sodium hypophosphite or hydrazine sulfate; Described complexing agentIt is natrium citricum; Described buffer is sodium acetate; Described stabilizing agent is plumbi nitras.
Described main salt can also be any one in nickel chloride or nickel acetate; Described reducing agent can also be sodium borohydrideOr one or more in amido borine; Described complexing agent can also be glycolic, citric acid, lactic acid, malic acid, propionic acid,One or more in glycine or aminoacetic acid; Described buffer can also be a kind of or several in ammonium chloride or ammonium borateKind; Described stabilizing agent can also be one or more in heavy metal lead salt, thiocarbamide, Potassiumiodate or maleic acid.
In described chemical nickel-plating liquid, the concentration of main salt nickelous sulfate is 25g/L ~ 38g/L; Reducing agent in described chemical nickel-plating liquidThe concentration of sodium hypophosphite is 25g/L ~ 33g/L, and the concentration of hydrazine sulfate is 10g/L; Described Complexing Agent in Electroless Nickel Deposition Baths citric acidThe concentration of sodium is 38mg/L; In described chemical nickel-plating liquid, the concentration of buffer sodium acetate is 10g/L; In described chemical nickel-plating liquidThe concentration of stabilizing agent plumbi nitras is 1mg/L ~ 3mg/L.
Embodiment 1
A kind of nickel bag glass conductive powder body for conductive rubber, the component of described powder and percentage by weight are:
Nickel 85%
Glass 15%.
The average grain diameter of described glass is 10 microns, glass powder be shaped as irregular sheet.
Described nickel is coated on the surface of glass powder.
A preparation method for nickel bag glass conductive powder body for conductive rubber, comprises the following steps:
(I) glass powder alkali cleaning oil removing
The preparation of alkali cleaning degreasing fluid: take the sodium phosphate of 25 grams and the sodium carbonate of 15 grams, the NaOH of 12.5 grams, and 4Gram soap powder admixed together, and with distilled water diluting to 500ml, mix and stir evenly rear stand-by.
The average grain diameter of getting 10 grams is the irregular foliated glass powder of 10 microns, at 50 DEG C with the oil removing of above-mentioned preparationLiquid carries out alkali cleaning oil removing to glass powder, and scavenging period is 15 minutes;
The alligatoring of (II) glass powder acid etching
To cleaning with clear water through the glass powder of alkali cleaning oil removing, then service property (quality) mark is 20% hydrofluoric acid,At 20 DEG C, carry out acid etching alligatoring, etching period 30 minutes;
The sensitization of (III) glass powder
To cleaning with clear water through the glass powder of acid etching alligatoring, the stannous chloride that then working concentration is 30g/LCarry out sensitization processing, sensitization time is 3 minutes;
The activation of (IV) glass powder
The preparation of activating solution: take the palladium bichloride of 0.25 gram, and 5mL concentrated hydrochloric acid is admixed together, and uses distilled water dilutingTo 500ml, mix and stir evenly rear stand-by;
To after the glass powder of sensitization cleans with clear water, then at 30 DEG C, use the activating solution of above-mentioned preparationActivate, soak time is 10 minutes;
(V) glass powder chemical nickel plating
The preparation of chemical nickel-plating liquid:
Prepare by the ratio that in nickel bag glass conductive powder body, nickeliferous weight is 85% in conductive rubber; Take 379 gramsMain salt nickelous sulfate, the reducing agent sodium hypophosphite of 379 grams, the reducing agent hydrazine sulfate of 152 grams, the buffer sodium acetate and 20 of 152 gramsMilligram stabilizing agent plumbi nitras, dissolves with a small amount of distilled water respectively; After nickelous sulfate dissolves completely, under constantly stirring toWherein add successively sodium hypophosphite solution and hydrazine sulfate solution, and continuous vigorous stirring; Then add lead nitrate solution, acetic acidSodium solution; Then with distilled water diluting to 15 liter, finally with hydrochloric acid solution, the pH value of solution is adjusted to 4.5, and uses filter mistakeStand-by after filter.
Glass powder through overactivation is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, at 40 DEG CWater bath condition under, glass powder is added in chemical nickel-plating liquid, fully stir with electromagnetic mixer, and use hydrochloric acid solutionRegulate pH value to 4.5 left and right, react 2 hours, till reacting completely, and with distilled water cleaning 5 minutes; After nickel plating is complete, use clear waterPowder is rinsed to neutral, after oven dry, obtain conductive rubber nickel bag glass conductive powder body.
Fig. 1 is the ESEM of the irregular foliated glass conducting powder of conductive rubber nickel bag prepared of the embodiment of the present invention 1Figure.
Embodiment 2
A kind of nickel bag glass conductive powder body for conductive rubber, the component of described powder and percentage by weight are:
Nickel 60%
Glass 40%.
The average grain diameter of described glass is 60 microns, glass powder be shaped as spherical shape.
Described nickel is coated on the surface of glass powder.
A preparation method for nickel bag glass conductive powder body for conductive rubber, comprises the following steps:
(I) glass powder alkali cleaning oil removing
The preparation of alkali cleaning degreasing fluid: take the sodium phosphate of 25 grams and the sodium carbonate of 15 grams, the NaOH of 12.5 grams, and 4Gram soap powder admixed together, and with distilled water diluting to 500ml, mix and stir evenly rear stand-by.
The average grain diameter of getting 10 grams is the globular glass powder of 60 microns, at 50 DEG C with the degreasing fluid of above-mentioned preparation to glassGlass powder carries out alkali cleaning oil removing, and scavenging period is 10 minutes;
The alligatoring of (II) glass powder acid etching
To cleaning with clear water through the glass powder of alkali cleaning oil removing, then service property (quality) mark is 20% hydrofluoric acid,At 20 DEG C, carry out acid etching alligatoring, etching period 30 minutes;
The sensitization of (III) glass powder
To cleaning with clear water through the glass powder of acid etching alligatoring, the stannous chloride that then working concentration is 30g/LCarry out sensitization processing, sensitization time is 5 minutes;
The activation of (IV) glass powder
The preparation of activating solution: take the palladium bichloride of 0.25 gram, and 5mL concentrated hydrochloric acid is admixed together, and uses distilled water dilutingTo 500ml, mix and stir evenly rear stand-by;
To after the glass powder of sensitization cleans with clear water, then at 30 DEG C, use the activating solution of above-mentioned preparationActivate, soak time is 10 minutes;
(V) glass powder chemical nickel plating
The preparation of chemical nickel-plating liquid:
Prepare by the ratio that in nickel bag glass conductive powder body, nickeliferous weight is 60% in conductive rubber; Take 268 gramsMain salt nickelous sulfate, the reducing agent sodium hypophosphite of 234 grams, the complexing agent natrium citricum of 268 milligrams and 20 milligrams of stabilizing agent plumbi nitras,Dissolve with a small amount of distilled water respectively; After nickelous sulfate dissolves completely, under constantly stirring, add wherein sodium hypophosphiteSolution, and continuous vigorous stirring; Then add sodium citrate solution, lead nitrate solution; Then with distilled water diluting to 7 liter,Finally with ammonium hydroxide, the pH value of solution is adjusted to 9, and stand-by after filtering with filter.
Glass powder through overactivation is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, at 40 DEG CWater bath condition under, glass powder is added in chemical nickel-plating liquid, fully stir with electromagnetic mixer, and use ammonium hydroxideSolution regulates pH value to 9 left and right, reacts 2 hours, and till reacting completely, and with distilled water cleaning 5 minutes; The complete rear use of nickel plating is clearWater rinses powder to neutral, obtains conductive rubber nickel bag glass conductive powder body after oven dry.
Fig. 2 is the scanning electron microscope (SEM) photograph of the conductive rubber nickel bag globular glass conducting powder prepared of the embodiment of the present invention 2.
Embodiment 3
The nickel bag glass conductive powder body that embodiment 1 and embodiment 2 are made is put into banbury according to the proportioning of table 1 and is carried outMix and make silica-based conductive rubber material.
The silica-based conductive rubber composition that the nickel bag glass conductive powder body that table 1 embodiment 1～2 makes is raw material
By the silica-based nickel bag glass conductive rubber making, thick by within 10 minutes, making 2mm 170 DEG C of mold pressings, 12mm ×The rectangular sheet of 12mm, records after resistance, and calculates its resistivity, shown in result (in table 2), and the silica-based conductive rubber tool makingThere are good electric conductivity and mechanical property.
The nickel bag glass, silicon-based conductive rubber testing experiment result that table 2 the present invention makes
Nickel bag glass conductive powder body and preparation method thereof for a kind of conductive rubber provided by the invention, preparation technology, raw materialComposition is simple, is suitable for large-scale production, and the nickel bag glass conductive powder body making has good capability of electromagnetic shielding, is applicable toFor making the conductive rubber product of anti-electromagnetic interference and water vapor seal. The resistivity of the conductive rubber of making of the present invention is less than0.15 Ω cm has good mechanical property simultaneously, can meet the business application of middle and high end completely.
Claims (7)
1. a preparation method for nickel bag glass conductive powder body for conductive rubber, is characterized in that: comprise the following steps:
(I) glass powder alkali cleaning oil removing
At 50 DEG C, with degreasing fluid, glass powder is carried out to alkali cleaning oil removing, scavenging period is 10～15 minutes;
The alligatoring of (II) glass powder acid etching
To cleaning with clear water through the glass powder of alkali cleaning oil removing, then service property (quality) mark is 20% hydrofluoric acid, 20At DEG C, carry out acid etching alligatoring, etching period 30 minutes;
The sensitization of (III) glass powder
To cleaning with clear water through the glass powder of acid etching alligatoring, the stannous chloride that then working concentration is 30g/L carries outSensitization processing, sensitization time is 3～5 minutes;
The activation of (IV) glass powder
To after the glass powder of sensitization cleans with clear water, then at 30 DEG C, use activating solution to activate, activationTime is 10 minutes;
(V) glass powder chemical nickel plating
Glass powder through overactivation is cleaned with clear water, then use chemical nickel-plating liquid to carry out nickel plating, at the water of 40 DEG CUnder bath condition, glass powder is added in chemical nickel-plating liquid, fully stir with electromagnetic mixer, and regulate with pH regulator solutionPH value to 4.5 ~ 9, react 2 hours, till reacting completely, and with distilled water clean 5 minutes; Nickel plating finishes will plate with clear water afterwardsNickel by powder rinses to neutral, obtains conductive rubber nickel bag glass conductive powder body after oven dry.
2. the preparation method of nickel bag glass conductive powder body for a kind of conductive rubber according to claim 1, is characterized in that:In described step (I), component and each concentration of component of degreasing fluid are respectively:
Sodium phosphate 50g/L
Sodium carbonate 30g/L
NaOH 25g/L
Soap powder is appropriate.
3. the preparation method of nickel bag glass conductive powder body for a kind of conductive rubber according to claim 1, is characterized in that:In described step (IV), component and each concentration of component of activating solution are respectively:
Palladium bichloride 0.5g/L
Concentrated hydrochloric acid 10mL/L.
4. the preparation method of nickel bag glass conductive powder body for a kind of conductive rubber according to claim 1, is characterized in that:In described step (V), chemical nickel-plating liquid comprises main salt and reducing agent, also comprises the one in complexing agent, buffer and stabilizing agentOr several.
5. the preparation method of nickel bag glass conductive powder body for a kind of conductive rubber according to claim 1, is characterized in that:In described step (V), pH regulator solution is hydrochloric acid solution or Ammonia.
6. the preparation method of nickel bag glass conductive powder body for a kind of conductive rubber according to claim 4, is characterized in that:Described main salt is nickelous sulfate; Described reducing agent is at least one in sodium hypophosphite or hydrazine sulfate; Described complexing agent is citric acidSodium; Described buffer is sodium acetate; Described stabilizing agent is plumbi nitras.
7. the preparation method of nickel bag glass conductive powder body for a kind of conductive rubber according to claim 4, is characterized in that:In described chemical nickel-plating liquid, the concentration of main salt nickelous sulfate is 25g/L ~ 38g/L; Reducing agent sodium hypophosphite in described chemical nickel-plating liquidConcentration be 25g/L ~ 33g/L, the concentration of hydrazine sulfate is 10g/L; The concentration of described Complexing Agent in Electroless Nickel Deposition Baths natrium citricumFor 38mg/L; In described chemical nickel-plating liquid, the concentration of buffer sodium acetate is 10g/L; Stabilizing agent nitre in described chemical nickel-plating liquidThe concentration of lead plumbate is 1mg/L ~ 3mg/L.
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