CN1176873C - Continuous chemical powder plating method and apparatus - Google Patents
Continuous chemical powder plating method and apparatusInfo
- Publication number
- CN1176873C CN1176873C CNB03115963XA CN03115963A CN1176873C CN 1176873 C CN1176873 C CN 1176873C CN B03115963X A CNB03115963X A CN B03115963XA CN 03115963 A CN03115963 A CN 03115963A CN 1176873 C CN1176873 C CN 1176873C
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- 239000000843 powder Substances 0.000 title claims abstract description 63
- 238000007747 plating Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000126 substance Substances 0.000 title claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 60
- 230000002829 reductive effect Effects 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 40
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 19
- 238000007772 electroless plating Methods 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 206010070834 Sensitisation Diseases 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 6
- 230000008313 sensitization Effects 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 4
- 229940038773 trisodium citrate Drugs 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 229960004249 sodium acetate Drugs 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims description 3
- 241000220317 Rosa Species 0.000 claims description 2
- 239000000872 buffer Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000006174 pH buffer Substances 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 claims description 2
- 235000019263 trisodium citrate Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000029219 regulation of pH Effects 0.000 abstract 2
- 239000012266 salt solution Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 239000002131 composite material Substances 0.000 description 7
- 239000008187 granular material Substances 0.000 description 7
- 238000010276 construction Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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Abstract
The present invention discloses a continuous chemical plating method for powder and a device thereof. The device comprises a first container filled with suspension prepared from powder and a solution L1 and a second container filled with a solution L2, wherein a mechanical agitator or an ultrasonic generator is arranged in the first container, and the solution L1 and the solution L2 respectively are a main salt reduction solution, a reduction solution main salt solution, a plating solution pH regulation solution or a pH regulation solution plating solution. The first container and the second container are respectively connected with a mixing chamber through respective pipes and metering pumps, the mixing chamber is connected to a coil pipe arranged in the ultrasonic generator through a pipe, and the coil pipe is connected to a third container through a pipe. After the solution in the first container and the solution in the second container are proportionally mixed, the chemical plating reaction of the solutions is carried out through the coil pipe placed in the ultrasonic generator. When the continuous chemical plating method for powder of the present invention is compared with general chemical plating for powder, the uniformity of the thickness of a metallic layer of the surface of powder is enhanced because the continuous chemical plating method for powder and the device thereof are used. In addition, continuous chemical plating processes are also realized, the labor intensity is reduced, and the uniformity of production efficiency and product quality is enhanced. The present invention can be used for chemical plating to which ultrasonic waves are applied, and the present invention is also suitable for conventional chemical plating.
Description
Technical field
The present invention relates to a kind of continuous powdery chemical plating method and device thereof.
Background technology
Electroless plating is to utilize appropriate reductant that the solution metal ion is reduced on the surface of tool catalytic activity selectively to separate out, and forms a kind of chemical treatment method of metal plating.In the powder surface electroless plating, can obtain composite granules such as metallic cover pottery, polymer, metal, in fields such as electrocondution slurry, electrical contact material, stealth material, sintex, hot spray powder, be widely used.
During powder electroless, the homogeneity of metallic cover is a crucial difficult problem.Adopt the method for low-temperature ultrasonic electroless plating, solved powder, especially cladding uniformity problem (number of patent application 01116714.9) during the superfine powder electroless plating preferably.But the used container of this method is less, still has the uneven problem of different powder surface metal thickness when producing in batches.This is that inhomogeneous as the coating of initial metal, then these powders that coated can preferentially be grown up fast because electroless plating is self-catalyzed reaction.And the amount of plating bath is many when producing in batches, therefore can provide the amount of metal ion of separating out many, thereby make the non-uniform phenomenon of metallic cover more serious.
Powder electroless carries out in small containers usually, adds a certain amount of powder in plating bath, makes it to react, and question response finishes back separation solution and powder, this method can only performance period the production of formula.Day the present invention a kind of new electroless plating technology " method of dripping ", and designed a kind of specific equipment, applied for relevant patent (the clear 62-30885 of special Open (1987), the flat 1-242782 of special Open (1989), special fair 2-25431 (1990)).It is at first powder to be made suspension in the aqueous solution, and quantitative respectively adding become owner of salt and reduced liquid in this container while stirring.Its main purpose is the self-decomposition that prevents plating bath.From this method, can't solve the homogeneity of metallic cover when producing in batches at all, and can not realize serialization production.
Summary of the invention
The object of the present invention is to provide a kind of continuous powdery chemical plating method and device thereof, improve the homogeneity of metallic cover thickness between different powders and realized the serialization of electroless plating process.
The technical solution used in the present invention is as follows:
1, principle
When considering on the different powder surfaces metallic cover thickness evenness, the ideal method is around each powder corresponding with it plating bath amount to be arranged, and so many metal ions can only be provided from this plating bath.For this reason, adopt special equipment, mixing zone and reaction zone are set, and make the solution that contains powder, in specific time, pass through reaction zone, as shown in Figure 1 with small amount.Like this, respectively at time t1, t2, t3 ... solution L1, L2, the L3 of ti input pipe ... between the Li, because the restriction of caliber, the mixing of each solution is controlled in the as far as possible little scope, and the metal that the result just can make powder surface separate out only limits to this small quantity solution metal ion.
2, method
1) at first container pack into powder and solution L
1Suspension, stir or ultrasonic generator by mechanical stirrer, make powder that sedimentation not take place;
2) the solution L that in second container, packs into
2
3) L
1/ L
2Be respectively main saline solution/(reduced liquid+pH adjusts liquid), (reduced liquid+pH adjusts liquid)/main saline solution, reduced liquid/(main saline solution+pH adjusts liquid) or pH adjust liquid/(main saline solution+reduced liquid);
4) volume pump by separately respectively with two kinds of solution in first container and second container, the input mixing section, the pH value that makes mixed solution in proportion is 4.5～13.5;
5) under the ultrasonic wave radiation, flow through coil pipe from the mixed solution of mixing section output by the coil pipe that places ultrasonic generator and carry out electroless plating reaction;
6) powder after reaction finishes and plating bath flow out from outlet and enter the 3rd container;
Powder is aluminum oxide or silicon oxide or the titanium carbide or the stannic oxide powder of nanometer or micron-scale;
Metallic cover is handled and is used bath composition:
Main salt: single nickel salt or rose vitriol or copper sulfate or Silver Nitrate 10～50 grams per liters
Reductive agent: formaldehyde 2～50 grams per liters of inferior sodium phosphate or 38% concentration
Complexing agent: Trisodium Citrate or disodium ethylene diamine tetraacetate or
Ammoniacal liquor 10～66 grams per liters of 25% concentration
PH buffer reagent: boric acid or sodium-acetate 0～50 grams per liter
Dispersion agent: 0～100 milliliter/liter of methyl alcohol
Stablizer: yellow prussiate of potash 0～50 mg/litre
PH regulator agent: sodium hydroxide or sulfuric acid 2～30 grams per liters
Water adds to into 1 liter
Wherein, main saline solution is made up of main salt, complexing agent, pH buffer reagent, stablizer and water, and reduced liquid is made up of reductive agent, dispersion agent and water, and pH adjusts liquid and is made up of pH regulator agent and water.
3, in the aluminum oxide or silicon oxide or titanium carbide or stannic oxide powder adding preprocessing solution with nanometer or micron-scale, under the room temperature, apply ultrasonication respectively, clean the back oven dry at alligatoring, sensitization, activation stage;
The preparation method:
Metallic cover is handled the medicine of forming with plating bath be mixed with solution L1 and L2 respectively, nanometer that will be pretreated or micro-powder add first container that contains solution L1 then, solution L2 are put into second container, L
1/ L
2Be respectively main saline solution/(reduced liquid+pH adjusts liquid), (reduced liquid+pH adjusts liquid)/main saline solution, reduced liquid/(main saline solution+pH adjusts liquid) or pH adjust liquid/(main saline solution+reduced liquid).It is 4.5～13.5 that two kinds of solution mix back pH, coats in temperature is 20～60 ℃, ultrasonic wave, gained powder in the 3rd container is separated with plating bath, and through cleaning and the aftertreatment of oven dry gets final product.
4, device
It comprises: first container of dress suspension, mechanical stirrer or ultrasonic generator are housed in first container, adorn second container of general solution, first container and second container connect the mixing section mixing section through separately pipe, separately volume pump respectively and are connected to the coil pipe of the ultrasonic generator of packing into through pipe, and coil pipe inserts the 3rd container through pipe.
The useful effect that the present invention has is:
It is compared with general powder electroless, owing to adopt a kind of continuous powdery chemical plating method and device thereof, has improved the homogeneity of metallic cover thickness between different powders.In addition, also realized the serialization of electroless plating process, reduced labour intensity, improved the consistence of production efficiency and quality product.The present invention can be used for applying hyperacoustic electroless plating, also is applicable to conventional electroless plating.
Description of drawings
Fig. 1 is a continuous powdery electroless plating schematic diagram;
Fig. 2 is the structural representation of apparatus of the present invention.
Embodiment
As shown in Figure 2, the present invention includes powder and solution L are housed
1First container 1, mechanical stirrer or ultrasonic generator 3 are housed in first container 1, solution L is housed
2Second container, 2, the first containers 1 and second container 2 connect mixing section 6 through pipe separately, volume pump 4,5 separately respectively, mixing section 6 is connected to the coil pipe 7 of the ultrasonic generator 8 of packing into through pipe, coil pipe 7 inserts the 3rd container 9 through pipe.
1, plating bath is divided into two portions, a part is powder and solution L
1, another part is solution L
2Pack in container 1 and 2.
2, solution L
1/ L
2Be respectively main saline solution/(reduced liquid+pH adjusts liquid), (reduced liquid+pH adjusts liquid)/main saline solution, reduced liquid/(main saline solution+pH adjusts liquid) or pH adjust liquid/(main saline solution+reduced liquid).
3, the suspension in the container 1 stirs by mechanical stirrer 3 or ultrasonic generator, makes powder that sedimentation not take place.
4, two solution are passed through volume pump 4 and 5, quantitatively import mixing section 6 according to a certain percentage, make two kinds of solution in the microcosmic scope, realize mixing.
5, mixing section can be static mixer, the mixing tank that also can constitute with twisted tube and high speed rotating atomizing mixer etc.
6, mixed solution is exported from mixing section, and by the coil pipe 7 of certain diameter, certain-length, coil pipe places ultrasonic generator 8.Under ultrasonic irradiation, plating bath flows through coil pipe with certain flow velocity, in specific time, carries out electroless plating reaction.Coil pipe can be a glass, also can be inflexible plastics class material.
7, powder and plating bath after reaction finishes flow out from outlet, enter container 9.
In this process, the caliber of coil pipe plays a decisive role to the phase mutual interference that prevents mixed solution, thereby guarantees the homogeneity of each batch powder clad metal thickness; The length of flow and coil pipe has determined the time of reaction.By aforesaid device, can also realize the full-automatic operation of whole process.
Embodiment 1
1) caliber is 20 millimeters, 7.2 liters/hour of flow velocitys, and 12 meters of ultrasonic wave inner disc pipe ranges, then the time of solution under ultrasonic irradiation is 90 minutes, per hour the raw material powder scale of construction is 648 grams.
2) volume pump power, specification: 600W, 10 liters/hour
3) ultrasonic power, frequency are: 300W, 20～40KHz
4) composite granule: 720 Grams Per Hours (metal content is in weight percent 10%)
5) solution composition: nano alumina powder jointed, be of a size of 10～20nm.Powder after sensitization, activation adds sulfur acid cobalt 35 grams per liters, and Trisodium Citrate 15 grams per liters in the main salts solution of boric acid 40 grams per liters, stir and form suspension L
1Another solution L
2By inferior sodium phosphate 20 grams per liters, and a certain amount of NaOH forms the pH value 10.5 of mixed solution.The gained composite granule is even compound cobalt/aluminum oxide powder under the nano-scale through the projection electron microscopic observation.
Embodiment 2
1) caliber is 20 millimeters, 35 liters/hour of flow velocitys, and 60 meters of ultrasonic wave inner disc pipe ranges, the time of solution under ultrasonic irradiation is 90 minutes, per hour the raw material powder scale of construction is 3240 grams.
2) volume pump power, specification: 3000W, 50 liters/hour
3) ultrasonic power, frequency are: 1500W, 20～40KHz
4) composite granule: 6480 Grams Per Hours (metal content is in weight percent 50%)
5) solution composition: micron titanium carbide powder is of a size of 0.8～1.2 μ m.Powder after sensitization, activation adds and contains inferior sodium phosphate 15 grams per liters, reaches a certain amount of H
2SO
4Reduced liquid L
1In, stir and form suspension; Another solution is single nickel salt 30 grams per liters, Trisodium Citrate 17 grams per liters, the main saline solution L of sodium-acetate 15 grams per liters
2, the pH value 4.5 of mixed solution.The result is by scanning electron microscopic observation, and nickel evenly is coated on the carbonized titanium powder surface.
Embodiment 3
1) caliber is 20 millimeters, 7.2 liters/hour of flow velocitys, and 12 meters of ultrasonic wave inner disc pipe ranges, the time of solution under ultrasonic irradiation is 30 minutes, per hour the raw material powder scale of construction is 648 grams.
2) volume pump power, specification: 600W, 10 liters/hour
3) ultrasonic power, frequency are: 300W, 20～40KHz
4) composite granule: 1296 Grams Per Hours (metal content is in weight percent 50%)
5) solution composition: micron stannic oxide powder is of a size of 1～5 μ m.Powder after sensitization, activation adds and contains formaldehyde 6 grams per liters, the reduced liquid L that methyl alcohol is 2.2 milliliters/liter
1In, stir and form suspension; Another solution L
2By Silver Nitrate 17.5 grams per liters, ammoniacal liquor 35 grams per liters, sodium hydroxide 2 grams per liters are formed.The gained composite granule evenly is compounded in the powder of putty powder surface through scanning electron microscopic observation for Ag.
Embodiment 4
1) caliber is 10 millimeters, 35 liters/hour of flow velocitys, and 60 meters of ultrasonic wave inner disc pipe ranges, the time of solution under ultrasonic irradiation is 30 minutes, per hour the raw material powder scale of construction is 324 grams.
2) volume pump power, specification: 3000W, 50 liters/hour
3) ultrasonic power, frequency are: 1500W, 20～40KHz
4) composite granule: 3240 Grams Per Hours (metal content is in weight percent 90%)
5) solution composition: the micron silica powder is of a size of 5～10 μ m.Powder after sensitization, activation adds the pH value that contains sodium hydroxide 20 grams per liters and adjusts liquid L
1In, stir and form suspension; Another solution is by copper sulfate 44 grams per liters, disodium ethylene diamine tetraacetate 66 grams per liters, yellow prussiate of potash 10 mg/litre, 24 milliliters/liter in formaldehyde, the plating bath L that methyl alcohol is 100 milliliters/liter
2Form, mix the pH value 13.0 of back solution.The gained powder is through scanning electron microscopic observation, and copper evenly is coated on the silica powder surface.
Claims (4)
1. continuous powdery chemical plating method is characterized in that:
1) at first container pack into powder and solution L
1The suspension of making stirs or ultrasonic generator by mechanical stirrer, makes powder that sedimentation not take place;
2) the solution L that in second container, packs into
2
3) solution L
1/ L
2Be respectively main saline solution/(reduced liquid+pH adjusts liquid), (reduced liquid+pH adjusts liquid)/main saline solution, reduced liquid/(main saline solution+pH adjusts liquid) or pH adjust liquid/(main saline solution+reduced liquid);
4) volume pump by separately respectively with two kinds of solution in first container and second container, the input mixing section, the pH value that makes mixed solution in proportion is 4.5～13.5;
5) under the ultrasonic wave radiation, flow through coil pipe from the mixed solution of mixing section output by the coil pipe that places ultrasonic generator and carry out electroless plating reaction;
6) powder after reaction finishes and plating bath flow out from outlet and enter the 3rd container;
Powder is aluminum oxide or silicon oxide or the titanium carbide or the stannic oxide powder of nanometer or micron-scale;
Metallic cover is handled and is used bath composition:
Main salt: single nickel salt or rose vitriol or copper sulfate or Silver Nitrate 10～50 grams per liters
Reductive agent: formaldehyde 2～50 grams per liters of inferior sodium phosphate or 38% concentration
Complexing agent: Trisodium Citrate or disodium ethylene diamine tetraacetate or
Ammoniacal liquor 10～66 grams per liters of 25% concentration
PH buffer reagent: boric acid or sodium-acetate 0～50 grams per liter
Dispersion agent: 0～100 milliliter/liter of methyl alcohol
Stablizer: yellow prussiate of potash 0～50 mg/litre
PH regulator agent: sodium hydroxide or sulfuric acid 2～30 grams per liters
Water adds to into 1 liter
Wherein, main saline solution is made up of main salt, complexing agent, pH buffer reagent, stablizer and water, and reduced liquid is made up of reductive agent, dispersion agent and water, and pH adjusts liquid and is made up of pH regulator agent and water.
2. a kind of continuous powdery chemical plating method according to claim 1 is characterized in that:
1) in the aluminum oxide or silicon oxide or titanium carbide or stannic oxide powder adding preprocessing solution with nanometer or micron-scale, under the room temperature, applies ultrasonication respectively, clean the back oven dry at alligatoring, sensitization, activation stage;
2) preparation method: metallic cover is handled the medicine of forming with plating bath be mixed with solution L respectively
1And L
2, nanometer that will be pretreated or micro-powder add and contain solution L then
1First container, with solution L
2Put into second container, it is 4.5～13.5 that two kinds of solution mix back pH, coats in temperature is 20～60 ℃, ultrasonic wave, gained powder in the 3rd container is separated with plating bath, and through cleaning and the aftertreatment of oven dry gets final product.
3. the device that is used for the described a kind of continuous powdery chemical plating method of claim 1, it is characterized in that it comprises: first container (1) of dress suspension, mechanical stirrer or ultrasonic generator (3) are housed in first container (1), adorn second container (2) of general solution, first container (1) connects mixing section (6) through pipe separately, volume pump (4,5) separately respectively with second container (2), mixing section (6) is connected to the coil pipe (7) of the ultrasonic generator of packing into (8) through pipe, and coil pipe (7) inserts the 3rd container (9) through pipe.
4. the device of a kind of continuous powdery chemical plating method according to claim 3 is characterized in that: said mixing section (6) is static mixer or the mixing tank or the high speed rotating atomizing mixer that are made of twisted tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03115963XA CN1176873C (en) | 2003-03-20 | 2003-03-20 | Continuous chemical powder plating method and apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03115963XA CN1176873C (en) | 2003-03-20 | 2003-03-20 | Continuous chemical powder plating method and apparatus |
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| Publication Number | Publication Date |
|---|---|
| CN1440951A CN1440951A (en) | 2003-09-10 |
| CN1176873C true CN1176873C (en) | 2004-11-24 |
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|---|---|---|---|
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|---|---|---|---|---|
| JP2014005531A (en) * | 2012-01-17 | 2014-01-16 | Dowa Electronics Materials Co Ltd | Silver-coated copper alloy powder and method for producing the same |
| CN104060245B (en) * | 2014-06-10 | 2017-03-15 | 上海交通大学 | Super-hydrophobic nano silver structure Raman strengthens base material and preparation method thereof |
| CN104498916B (en) * | 2014-11-24 | 2017-04-26 | 广西大学 | Method used for preparing aluminium-doped zinc oxide thin film via electroless deposition |
| CN104846411B (en) * | 2015-04-27 | 2017-08-25 | 北京航空航天大学 | The method and its product of flower-like nanometer metal cobalt are prepared using anodic oxidation aluminium formwork |
| CN106077623B (en) * | 2016-07-19 | 2018-06-12 | 廖川金 | A kind of preparation method for being evenly coated copper-coated iron composite powder |
| CN106435541B (en) * | 2016-09-26 | 2019-02-19 | 四川大学 | A kind of aluminum grain refiner and preparation method thereof based on titanium carbonitride |
| CN106898748A (en) * | 2017-03-17 | 2017-06-27 | 成都新柯力化工科技有限公司 | A kind of preparation method of the ternary lithium nickel cobalt manganese battery electrode material of core-shell structure |
| CN107267965B (en) * | 2017-07-31 | 2019-04-02 | 北京矿冶研究总院 | Continuous type powder chemical plating device |
| CN110802224A (en) * | 2018-08-06 | 2020-02-18 | 三菱电机株式会社 | Preparation method of silver-nickel-tin oxide composite powder and silver-nickel-tin oxide electrical contact material |
| CN114737175B (en) * | 2022-06-13 | 2022-08-12 | 常州金襄新材料科技有限公司 | Silver-coated copper powder continuous conveying device |
-
2003
- 2003-03-20 CN CNB03115963XA patent/CN1176873C/en not_active Expired - Fee Related
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