CN101701335A - Formula and processes of chemically plating tin and nickel on surface of mineral crystal whisker of calcium magnesium silicate - Google Patents
Formula and processes of chemically plating tin and nickel on surface of mineral crystal whisker of calcium magnesium silicate Download PDFInfo
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- CN101701335A CN101701335A CN200910216280A CN200910216280A CN101701335A CN 101701335 A CN101701335 A CN 101701335A CN 200910216280 A CN200910216280 A CN 200910216280A CN 200910216280 A CN200910216280 A CN 200910216280A CN 101701335 A CN101701335 A CN 101701335A
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- magnesium silicate
- calcium magnesium
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- whisker
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Abstract
The invention relates to preparation of a conducting mineral crystal whisker material which can be used for special fields, such as electromagnetic wave shielding, wave absorption, hiding, resistance of static electricity and the like, in particular to a formula and processes of chemically plating tin and nickel on a surface of a mineral crystal whisker of calcium magnesium silicate. The pretreatment process before the process of chemically plating tin and nickel on the surface of the mineral crystal whisker of calcium magnesium silicate mainly comprises degreasing, coarsening, sensitization, activation and the like. The formula of chemically plating tin and nickel mainly comprises tin dichloride, nickel sulfate, sodium hypophosphite and lactic acid; and the processes of chemically plating tin and nickel have the characteristics that the pH value is 2-6, the plating temperature is 60-100 DEG C, the plating time is 0.5-5 hours, and the drying temperature is 60-120 DEG C. The invention has the advantages of simplicity, convenience and easy operation and control; the technical parameters of the prepared conducting mineral crystal whisker of calcium magnesium silicate plated with tin and nickel are satisfactory, and the invention can be widely used for chemically plating tin and nickel on the surface of non-metallic powder.
Description
One, technical field
The invention belongs to the electroless plating technology field, preparation--the zinc-plated nickel prescription of-calcium magnesium silicate mineral whisker surface chemistry and the technology of the conductive mineral crystal whisker materials of special dimensions such as being specifically related to a kind ofly to can be used for electromagnetic wave shielding, inhaling ripple, be stealthy and antistatic.
Two, background technology
Whisker is a kind of filamentary material with certain length-to-diameter ratio that grows into the monocrystalline form, because its diameter is little, length-to-diameter ratio is big, the atom high-sequential, so whisker has the favorable mechanical mechanical property, its intensity height (intensity approaches the theoretical value of perfect crystal), Young's modulus height, the hardness height, high temperature resistant and fine corrosion resistance.Also can give performances such as some special magnetics of whisker, electricity and optics by modification.Therefore, Preparation of Whiskers, application and study on the modification thereof have become a big focus of Materials Science and Engineering area research.
Because be subjected to the restriction of raw material and production cost, the price of whisker is generally higher.The calcium magnesium silicate whisker is to be raw material with the natural tremolite in somewhere, Sichuan～diopside mineral, the silicate whisker material of a kind of novel acicular structure that is prepared from by hydrothermal growth process etc. [Sun Chuanmin. prepare calcium magnesium silicate whisker [J] with the natural mineral tremolite. Chengdu University of Technology's journal (natural science edition), 2005,32 (1): 65～71].Because raw material sources are extensive, preparation technology and equipment are simple, calcium magnesium silicate whisker with low cost, and respond well as composite material reinforcement body, but its electroconductibility is relatively poor, has influenced the use range of this whisker to a certain extent.
Electroless plating is a kind of environmental protection and surface metalation method of modifying cheaply.Electroless plating Sn, Ni calcium magnesium silicate conductive mineral Preparation of Whiskers principle are: with the calcium magnesium silicate whisker is matrix, utilize reductive agent with metal ion such as Sn, Ni chemical reduction in the solution on the calcium magnesium silicate whisker surface that is catalytic activity, under the situation that does not have extrinsic current to pass through, make it to form metal plating, thereby obtain plating Sn, Ni calcium magnesium silicate conductive mineral whisker.
Plating Sn, Ni calcium magnesium silicate conductive mineral whisker can be used as the functional stuffing of electrically conducting coating, are used for electromagnetic wave shielding, inhale ripple, stealthy and antistatic field.Calcium magnesium silicate mineral whisker surface chemical plating Sn, Ni technology are expected to improve the comprehensive exploitation of non-metallic minerals and utilize level that a kind of new technological method is provided for improving the added value of calcium magnesium silicate whisker.
At present, have about the disclosed patent of calcium magnesium silicate mineral whisker: the preparation method of the silicon-calcium-magnesium whisker (patent No.: ZL200410081355.4; Grant number: CN1327045C).By retrieval, do not find to adopt chemical plating method to prepare the patent application or the bibliographical information of tin-nickel plating calcium magnesium silicate whisker.
Three, summary of the invention
The purpose of this invention is to provide a kind of prescription and technology for preparing the zinc-plated nickel of zinc-plated nickel calcium magnesium silicate conductive mineral whisker----calcium magnesium silicate mineral whisker surface chemistry at the zinc-plated nickel of calcium magnesium silicate mineral whisker surface chemistry.Mainly be that calcium magnesium silicate mineral whisker is after pre-treatment such as oil removing, alligatoring, sensitization, activation, utilize reductive agent with Sn, the chemical reduction of Ni metal ion in the solution on the calcium magnesium silicate whisker surface that is catalytic activity, under the situation that does not have extrinsic current to pass through, make it to form metal plating, thereby make the calcium magnesium silicate conductive mineral whisker that the surface contains Sn, Ni, improve the chemical ingredients of calcium magnesium silicate whisker on the one hand, improve the conductivity of calcium magnesium silicate whisker on the other hand.
For solving the problems of the technologies described above, the present invention adopts following technical proposals:
1, the zinc-plated nickel liquid formula of calcium magnesium silicate mineral whisker surface chemistry is as follows:
Tin protochloride 20～50g/L
Single nickel salt 5～20g/L
Inferior sodium phosphate 25～60g/L
Lactic acid 60～100g/L
2, the pretreatment technology step of calcium magnesium silicate mineral whisker is as follows:
(1) uses the acetone oil removing, and wash with distilled water;
(2) it is in 0.5～5% the silane coupler solution, flood 2-20 minute that the calcium magnesium silicate mineral whisker step (1) handled immerses concentration, filters, and dries;
(3) the calcium magnesium silicate whisker immersion concentration of step (2) being handled is that the salpeter solution of 40-65% carries out roughening treatment processing 10～60 minutes, and the temperature maintenance of salpeter solution is at 40～80 ℃;
(4) it is 5～20g/L SnCl that the calcium magnesium silicate whisker of step (3) being handled immerses concentration
22H
2Carrying out sensitization in O and the 10～30g/LHCl mixing solutions handles;
(5) the calcium magnesium silicate whisker that step (4) was handled is at 0.1～2g/L PdCl
2With carry out activation treatment in 1～20mL/L HCl mixing solutions.
3, the zinc-plated nickel processing step of calcium magnesium silicate mineral whisker surface chemistry is as follows:
(1) by the described tin-nickel plating prescription of claim 1, uses the dissolved in distilled water tin protochloride respectively, single nickel salt, inferior sodium phosphate and lactic acid;
(2) consoluet tin protochloride and nickel sulfate solution are mixed after, join in the lactic acid solution, stir;
(3) the ortho phosphorous acid sodium solution is slowly added the solution that step (2) is prepared, and dilution cause volume required, with salt acid for adjusting pH value to 2～6;
(4) calcium magnesium silicate mineral whisker after will handling by the described pretreatment technology of claim 2 is put into the plating bath that step (3) prepared and is carried out tin-nickel plating, 60～100 ℃ of plating temperatures, plating time 0.5～5 hour;
(5) with above-mentioned prepared zinc-plated nickel calcium magnesium silicate conductive mineral whisker oven dry, 60～120 ℃ of bake out temperatures.
The calcium magnesium silicate conductive mineral whisker of method for preparing with X-ray energy spectrometer test surfaces chemical ingredients, contains Sn 10～30wt%, Ni 2～10wt% through the densification of microscopic examination coating.Special dimensions such as this conductive mineral whisker can be used for electromagnetic wave shielding, inhales ripple, stealthy and antistatic.
The present invention has following characteristics:
1, the tin-nickel plating calcium magnesium silicate conductive mineral whisker that is provided has the favorable conductive characteristic, shows to contain Sn 10～30wt%, Ni 2～10wt%.
2, compare with function solenoid fillers such as the sphere of using always, sheets, tin-nickel plating calcium magnesium silicate mineral conductive mineral whisker is a kind of micron order whiskers body crystal whisker materials, and improvement is coated with the layer function skeleton good action.
3, tin-nickel plating calcium magnesium silicate conductive mineral Preparation of Whiskers is all carried out at low temperatures, and save energy is easy to use.
4, tin-nickel plating calcium magnesium silicate conductive mineral Preparation of Whiskers method simple, convenient, be easy to operate and control, use conventional equipment fully, can be widely used on the non-metallic powder in the tin-nickel plating process, investment is little, risk is less, is convenient to promote.
Four, embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention; the person skilled in the art of this area can make some nonessential improvement and adjustment according to the content of foregoing invention.
Embodiment 1
With the calcium magnesium silicate mineral whisker is base material, use the acetone oil removing, and wash with distilled water, immerse concentration and be in 1.5% the silane coupler solution, flood filtration 10 minutes, oven dry, the concentration that immerses 60 ℃ is that 50% salpeter solution roughening treatment was handled 30 minutes, washing, and immersing concentration is 10g/L SnCl
22H
2Carry out sensitization in O and the 20g/L HCl mixing solutions and handle, immersing concentration is 0.3g/L PdCl
2With carry out activation treatment in the 1.5mL/L HCl mixing solutions.Immersed in 90 ℃ of plating baths plating then 40 minutes, electroplate liquid formulation is tin protochloride 30g/L, single nickel salt 10g/L, inferior sodium phosphate 35g/L, lactic acid 90g/L, pH value 4.2.Obtain the zinc-plated nisiloy of surface chemistry acid calcium magnesium mineral conductive mineral whisker, after with 100 ℃ it being dried, use microscopic examination, the coating densification.
Embodiment 2
With the calcium magnesium silicate mineral whisker is base material, use the acetone oil removing, and wash with distilled water, immerse concentration and be in 2% the silane coupler solution, flood filtration 8 minutes, oven dry, the concentration that immerses 55 ℃ is that 60% salpeter solution roughening treatment was handled 35 minutes, washing, and immersing concentration is 12g/L SnCl
22H
2Carry out sensitization in O and the 25g/L HCl mixing solutions and handle, immersing concentration is 0.2g/L PdCl
2With carry out activation treatment in the 2mL/L HCl mixing solutions.Immersed in 88 ℃ of plating baths plating then 60 minutes, electroplate liquid formulation is tin protochloride 40g/L, single nickel salt 12g/L, and inferior sodium phosphate 40g/L, lactic acid 95g/L, pH value 5, bake out temperature is 95 ℃.Obtain the zinc-plated nisiloy of surface chemistry acid calcium magnesium mineral conductive mineral whisker, after with 95 ℃ it being dried, use microscopic examination, the coating densification.
Embodiment 3
With the calcium magnesium silicate mineral whisker is base material, use the acetone oil removing, and wash with distilled water, immerse concentration and be in 1% the silane coupler solution, flood filtration 15 minutes, oven dry, the concentration that immerses 50 ℃ is that 55% salpeter solution roughening treatment was handled 40 minutes, washing, and immersing concentration is 8g/L SnCl
22H
2Carry out sensitization in O and the 15g/L HCl mixing solutions and handle, immersing concentration is 0.5g/L PdCl
2With carry out activation treatment in the 2mL/L HCl mixing solutions.Immersed in 93 ℃ of plating baths plating then 60 minutes, electroplate liquid formulation is tin protochloride 40g/L, single nickel salt 14g/L, inferior sodium phosphate 45g/L, lactic acid 95g/L, pH value 4.5.Bake out temperature is 100 ℃.Obtain the zinc-plated nisiloy of surface chemistry acid calcium magnesium mineral conductive mineral whisker, after with 100 ℃ it being dried, use microscopic examination, the coating densification.
Claims (3)
1. the zinc-plated nickel prescription of calcium magnesium silicate mineral whisker surface chemistry is characterized in that with the calcium magnesium silicate mineral whisker being matrix, and it is carried out tin-nickel plating, and the tin-nickel plating liquid formula is as follows:
Tin protochloride 20～50g/L
Single nickel salt 5～20g/L
Inferior sodium phosphate 25～60g/L
Lactic acid 60～100g/L
2. the zinc-plated nickel preprocessing technology of a kind of calcium magnesium silicate mineral whisker surface chemistry according to claim 1, technology comprises pre-treatment such as calcium magnesium silicate mineral whisker oil removing, alligatoring, sensitization, activation, it is characterized in that the pretreatment technology step is as follows:
(1) uses the acetone oil removing, and wash with distilled water;
(2) it is in 0.5～5% the silane coupler solution, flood 2-20 minute that the calcium magnesium silicate mineral whisker step (1) handled immerses concentration, filters, and dries;
(3) the calcium magnesium silicate whisker immersion concentration of step (2) being handled is that the salpeter solution of 40-65% carries out roughening treatment processing 10～60 minutes, and the temperature maintenance of salpeter solution is at 40～80 ℃;
(4) it is 5～20g/L SnCl that the calcium magnesium silicate whisker of step (3) being handled immerses concentration
22H
2Carrying out sensitization in O and the 10～30g/LHCl mixing solutions handles;
(5) the calcium magnesium silicate whisker that step (4) was handled is at 0.1～2g/L PdCl
2With carry out activation treatment in 1～20mL/L HCl mixing solutions.
3. according to claim 1 and the zinc-plated nickel technology of 2 described a kind of calcium magnesium silicate mineral whisker surface chemistries, it is characterized in that the zinc-plated nickel processing step of calcium magnesium silicate mineral whisker surface chemistry is as follows:
(1) by the described tin-nickel plating prescription of claim 1, uses the dissolved in distilled water tin protochloride respectively, single nickel salt, inferior sodium phosphate and lactic acid;
(2) consoluet tin protochloride and nickel sulfate solution are mixed after, join in the lactic acid solution, stir;
(3) the ortho phosphorous acid sodium solution is slowly added the solution that step (2) is prepared, and dilution cause volume required, with salt acid for adjusting pH value to 2～6;
(4) calcium magnesium silicate mineral whisker after will handling by the described pretreatment technology of claim 2 is put into the plating bath that step (3) prepared and is carried out tin-nickel plating, 60～100 ℃ of plating temperatures, plating time 0.5～5 hour.
(5) with above-mentioned prepared zinc-plated nickel calcium magnesium silicate conductive mineral whisker oven dry, 60～120 ℃ of bake out temperatures.
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| CN200910216280A CN101701335A (en) | 2009-11-20 | 2009-11-20 | Formula and processes of chemically plating tin and nickel on surface of mineral crystal whisker of calcium magnesium silicate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011107A (en) * | 2010-12-24 | 2011-04-13 | 杭州东方表面技术有限公司 | Chemical nickel-phosphorus alloy plating solution capable of obtaining high-solderability plating layer |
| CN102277566A (en) * | 2011-08-12 | 2011-12-14 | 淮阴师范学院 | Method for preparing rod-like nickel powder by chemical nickel plating on surface of potassium titanate whisker |
-
2009
- 2009-11-20 CN CN200910216280A patent/CN101701335A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011107A (en) * | 2010-12-24 | 2011-04-13 | 杭州东方表面技术有限公司 | Chemical nickel-phosphorus alloy plating solution capable of obtaining high-solderability plating layer |
| CN102011107B (en) * | 2010-12-24 | 2012-07-11 | 杭州东方表面技术有限公司 | Chemical nickel-phosphorus alloy plating solution capable of obtaining high-solderability plating layer |
| CN102277566A (en) * | 2011-08-12 | 2011-12-14 | 淮阴师范学院 | Method for preparing rod-like nickel powder by chemical nickel plating on surface of potassium titanate whisker |
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Open date: 20100505 |