CN102296286A - Long-acting nano-micron composite layer synthetic solution and preparation method thereof - Google Patents
Long-acting nano-micron composite layer synthetic solution and preparation method thereof Download PDFInfo
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Abstract
The invention relates to long-acting nano-micron composite layer synthetic solution and a preparation method thereof. The synthetic solution is prepared from a main salt, a reducer, a main complexing agent, an auxiliary complexing agent, a buffer a, a buffer b, silicon carbide, magnesium oxide, a cationic surfactant, a nonionic surfactant, rare earth, a stabilizer, a promoter and deionized water. Compared with the normal conventional chemical composite plating solution, the synthetic solution has the advantages of high plating speed, stable performance of plating solution, no pollution and high economy. The synthetic solution can be recycled by only periodically replenishing loss; and the binding force of the synthetic solution and a matrix reaches up to over 400MPa, is 200MPa higher than that of the common alkaline self-decomposition plating solution and is 300Mpa higher than that of electroplating.
Description
Technical field
The present invention relates to the cermet field, particularly relate to the technology of the compound plating of a kind of sintering metal.
Background technology
As everyone knows, metal especially metal alloy has superior physical and mechanical properties, as certain rigidity, and remarkable toughness and ductility, compactness, shock resistance, resistance to pressure.And pottery has very high hardness, superior wear resistance, corrosion-resistant etc.Both combinations be inevitable advantage two combine into one, separately shortcoming is dropped to MIN way, that is exactly the compound plating of sintering metal chemistry.Composite bed ceramal synthetic technology is to be transformed on the basis of autocatalysis nickel-phosphorus alloy.Autocatalytic plating is a kind of newer Technology.
Chinese patent " generation fluid for environmental protective Nano composite reinforced abrasion resistant coating ", the patent No.: 200610086886.1.Disclose a kind of generation fluid for environmental protective Nano composite reinforced abrasion resistant coating, this coating Generation Liquid does not rely on electrical forces just can generate one deck on the metal part surface and receives the scuff-resistant coating that micron hard ceramic forms by nickel phosphorus.This invention is compared with durionise has the advantages that cost is low, power consumption is low, free from environmental pollution, particularly high-performance nano pottery is coprecipitated goes in the alloy layer lattice, strengthened the comprehensive wear resisting property of coating greatly, improved more than 3-5 times than durionise layer wear resistance.Alternative durionise layer carries out surface Hardening Treatment to metal part.But this liquid is when using four to five cycles, and bad stability, easily decomposition, plating bath are lacked work-ing life.
Summary of the invention
The present invention aims to provide a kind of high speed, the long-acting micron composite bed of receiving energy-conservation, stable, additional use capable of circulation synthesizes liquid.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of long-acting synthetic liquid of micron composite bed of receiving is formed fully by the following raw materials in parts by weight numeral system:
Main salt 20～40g, reductive agent 20～40g, main complexing agent 20～40g, auxiliary complex-former 20～40g, buffer reagent a10～30g, buffer reagent b10～30mL, silicon carbide 8～20g, magnesium oxide 0～1g, cats product 0.1～1g, nonionogenic tenside 0.1～1g, rare earth 0.01～0.1g, stablizer 0.1～20mg, promotor 0.1～20g, deionized water 800～1500mL.
Above-mentioned main salt is to choose any one kind of them in single nickel salt, nickelous hypophosphite, nickelous chloride, nickel acetate, the nickel sulfamic acid; Above-mentioned reductive agent is to choose any one kind of them in sodium hypophosphite, sodium borohydride, dimethyamine borane, the diethylamine borane.
Above-mentioned cats product is to choose any one kind of them in cetyl trimethylammonium bromide, polymine, the perfluoroalkyl trimethyl ammonium chloride; Nonionogenic tenside is to choose any one kind of them in polyoxyethylene glycol, the fluorine carbon type nonionogenic tenside.
Above-mentioned rare earth is to choose any one kind of them in ceric sulfate, rehenic acid ammonium, the Cadmium Sulphate; The aforementioned stable agent is to choose any one kind of them in Potassium Iodate, thiocarbamide, Sodium Fluoride, the lead nitrate or two kinds; Above-mentioned promotor is to choose any one kind of them in aspartic acid, Sodium Fluoride, the aminocarboxylic acid.
Above-mentioned main complexing agent is to choose any one kind of them in citric acid, lactic acid, oxyacetic acid, oxysuccinic acid, propionic acid, Succinic Acid, the Padil or make up; Above-mentioned auxiliary complex-former is to choose any one kind of them in sodium tetraborate, Trisodium Citrate, Seignette salt, Soduxin, the quadrol or make up.
Above-mentioned buffer reagent a chooses any one kind of them in sodium-acetate, anhydrous sodium sulphate, borax, NaOH, the Sodium Tetraborate; Buffer reagent b chooses any one kind of them in Glacial acetic acid, glycine, Succinic Acid, the boric acid.
A kind of long-acting preparation method who receives the synthetic liquid of micron composite bed comprises the steps:
A. silicon carbide activation treatment: soaked 5～90 minutes with trisodium phosphate solution, add deionized water again and clean, treat that 20～90 minutes post precipitations are inhaled the deionized water more than the silicon carbide, be made into the silicon carbide mixed solution, be called for short A liquid to pH=4～8, standby;
B. magnesium oxide adds deionized water flush away hydrofluoric acid then with hydrofluoric acid etch 5～90 minutes, cleans to pH=4～8, treats that 20～90 minutes post precipitations go the suction of the deionized water more than the magnesium oxide, is made into the magnesium oxide mixed solution, is called for short B liquid, and is standby;
C. in deionized water, add and become owner of salt, it is fully dissolved, stir evenly impurity screening after, it is standby to be made into C liquid;
D. in deionized water, add reductive agent, it fully dissolved, stir evenly impurity screening after, it is standby to be made into D liquid;
E. in deionized water, add and become owner of complexing agent, it is fully dissolved, stir evenly impurity screening after, it is standby to be made into E liquid;
F. in deionized water, add auxiliary complex-former, it fully dissolved, stir evenly impurity screening after, it is standby to be made into F liquid;
G. in deionized water, add buffer reagent a, it fully dissolved, stir evenly impurity screening after, it is standby to be made into G liquid;
H. with sodium hydroxide solution or ammonia soln the pH value of buffer reagent b is transferred to 4.4～5.1, it is standby to be made into H liquid;
I. add cats product in deionized water, it is fully dissolved, stir evenly, it is standby to be made into I liquid;
J. add nonionogenic tenside in deionized water, it is fully dissolved, stir evenly, it is standby to be made into J liquid;
K. add rare earth in deionized water, it is fully dissolved, stir evenly, it is standby to be made into K liquid;
L. add stablizer in deionized water, it is fully dissolved, stir evenly, it is standby to be made into L liquid;
M. add promotor in deionized water, it is fully dissolved, stir evenly, it is standby to be made into M liquid;
N. E liquid is slowly added F liquid and constantly stir, it is standby to be made into N liquid;
O. N liquid is slowly added G liquid and constantly stir, it is standby to be made into O liquid;
P. O liquid is slowly added C liquid and constantly stir, it is standby to be made into P liquid;
Q. H liquid is slowly added P liquid and constantly stir, it is standby to be made into Q liquid;
R. L liquid, M liquid are slowly added D liquid and constantly stir, it is standby to be made into R liquid;
S. it is standby B, I, J, K adding A and continuous stirring to be made into S liquid;
T. R liquid is slowly added Q liquid and constantly stir, it is standby to be made into T liquid;
U. with deionized water T liquid is diluted to volume 1000mL;
V. the pH value with sulfuric acid, sodium hydroxide solution or ammonia soln adjusting T liquid is 4.4～5.1, puts into coating bath and gets final product plating.
After the plating 10～90 minutes, slowly add S liquid and constantly stir continuation plating 3-6 hour.
Above-mentioned trisodium phosphate solution concentration is 0.5～50%, and volume is 10～100mL; Above-mentioned hydrofluoric acid solution concentration is 0.5～50%, and volume is 1～50mL; Above-mentioned concentration of sodium hydroxide solution is 0.5～50%; Above-mentioned ammonia soln concentration is 0.5～50%; Above-mentioned sulphuric acid soln concentration is 2:1.
Above-mentioned deionized water temperature is 50～70 ℃.
A kind of long-acting synthetic liquid of micron composite bed of receiving is formed fully by the following raw materials in parts by weight numeral system:
Main salt: single nickel salt 25g, reductive agent: sodium hypophosphite 24g, main complexing agent: citric acid 30g, auxiliary complex-former: Trisodium Citrate 10g+ sodium tetraborate 20g, buffer reagent a: anhydrous sodium sulphate 15g or sodium-acetate 15g, buffer reagent b: Glacial acetic acid 20mL, silicon carbide 10g, magnesium oxide 0.5g, cats product: cetyl trimethylammonium bromide 0.3g, nonionogenic tenside: polyoxyethylene glycol 0.6g, rare earth: ceric sulfate 0.01g, stablizer: Potassium Iodate 2mg, promotor: Sodium Fluoride 0.6g, 70 ℃ of deionized water 900～1200mL.
The beneficial effect of this patent is:
1, the present invention compares with the chemical composite plating bath of normal conventional, has that plating speed is high, plating solution performance is stable.
2, the present invention is at the composite bed of sediment-filled phase stack pile, and this synthetic liquid can be saved the time more than one times.
3, the synthetic liquid of the present invention is non-maintaining, pollution-free, can be recycled environment-friendly high-efficiency, good economy performance.Only need the cycle to replenish loss, with 5 hours be one-period, main salt replenishes 1～20g/L, reductive agent replenishes 1～20g/L.As radix, every increase one-period, the corresponding 1～20g that adds gets final product.Other auxiliary substance is mended into 0.1%～10% of standard formula amount with each cycle and is got final product.In the plating process, per hour replenish pure water, the maintenance solution capacity is 1000mL.With basal body binding force up to more than the 400MPa, exceed 200MPa than common alkaline self-decomposition plating bath, exceed 300Mpa than galvanized bonding force.
The present invention is further described below in conjunction with embodiment:
Embodiment
Embodiment 1
A kind of long-acting synthetic liquid of micron composite bed of receiving is formed fully by the following raw materials in parts by weight numeral system:
Single nickel salt 40g, sodium hypophosphite 40g, citric acid 40g, Trisodium Citrate 20g+ sodium tetraborate 20g, anhydrous sodium sulphate 10g or sodium-acetate 10g, Glacial acetic acid 10mL, silicon carbide 8g, magnesium oxide 0.3g, cetyl trimethylammonium bromide 0.8g, polyoxyethylene glycol 0.8g, ceric sulfate 0.08g, Potassium Iodate 10mg, Sodium Fluoride 10g, 50 ℃ of deionized water 1000mL.
A kind of long-acting preparation method who receives the synthetic liquid of micron composite bed:
A. silicon carbide activation treatment: soaked 10 minutes with 5% trisodium phosphate solution 20mL, add the 300mL deionized water again and clean to pH=4～8, treat that 30 minutes post precipitations are inhaled the deionized water more than the silicon carbide, be made into the silicon carbide mixed solution, it is standby to be called for short A liquid;
B. magnesium oxide adds 80mL deionized water flush away hydrofluoric acid then with 1% hydrofluoric acid 2mL etch 10 minutes, cleans to pH=4～8, treats that 30 minutes post precipitations go the suction of the deionized water more than the magnesium oxide, is made into the magnesium oxide mixed solution, and it is standby to be called for short B liquid;
C. in the 100mL deionized water, add single nickel salt, it fully dissolved, stir evenly impurity screening after, it is standby to be made into C liquid;
D. in the 100mL deionized water, add sodium hypophosphite, it fully dissolved, stir evenly impurity screening after, it is standby to be made into D liquid;
E. in the 100mL deionized water, add citric acid, it fully dissolved, stir evenly impurity screening after, it is standby to be made into E liquid;
F. in the 100mL deionized water, add Trisodium Citrate, sodium tetraborate, it fully dissolved, stir evenly impurity screening after, it is standby to be made into F liquid;
G. in the 50mL deionized water, add anhydrous sodium sulphate, it fully dissolved, stir evenly impurity screening after, it is standby to be made into G liquid;
H. with 20% sodium hydroxide solution or ammonia soln the pH value of Glacial acetic acid is transferred to 4.4～5.1, it is standby to be made into H liquid;
I. add cetyl trimethylammonium bromide in the 5mL deionized water, it is fully dissolved, stir evenly, it is standby to be made into I liquid;
J. add polyoxyethylene glycol in the 25mL deionized water, it is fully dissolved, stir evenly, it is standby to be made into J liquid;
K. add ceric sulfate in the 5mL deionized water, it is fully dissolved, stir evenly, it is standby to be made into K liquid;
L. add Potassium Iodate in the 5mL deionized water, it is fully dissolved, stir evenly, it is standby to be made into L liquid;
M. add Sodium Fluoride in the 5mL deionized water, it is fully dissolved, stir evenly, it is standby to be made into M liquid;
N. E liquid is slowly added F liquid and constantly stir, it is standby to be made into N liquid;
O. N liquid is slowly added G liquid and constantly stir, it is standby to be made into O liquid;
P. O liquid is slowly added C liquid and constantly stir, it is standby to be made into P liquid;
Q. H liquid is slowly added P liquid and constantly stir, it is standby to be made into Q liquid;
R. L liquid, M liquid are slowly added D liquid and constantly stir, it is standby to be made into R liquid;
S. it is standby B, I, J, K adding A and continuous stirring to be made into S liquid;
T. R liquid is slowly added Q liquid and constantly stir, it is standby to be made into T liquid;
U. with deionized water T liquid is diluted to volume 1000mL;
V. the pH value with sulfuric acid, sodium hydroxide solution or ammonia soln adjusting T liquid is 4.4～5.1, puts into coating bath and gets final product plating.
After the plating 10～90 minutes, slowly add S liquid and constantly stir continuation plating 3-6 hour.
Embodiment 2
A kind of long-acting raw material optimal components ratio of receiving the synthetic liquid of micron composite bed is:
Single nickel salt 25g, sodium hypophosphite 24g, citric acid 30g, Trisodium Citrate 10g, sodium tetraborate 20g, anhydrous sodium sulphate 15g or sodium-acetate 15g, Glacial acetic acid 20mL, silicon carbide 10g, magnesium oxide 0.5g, cats product 0.3g, nonionogenic tenside 0.6g, ceric sulfate 0.01g, Potassium Iodate 2mg, Sodium Fluoride 0.6g, 70 ℃ of deionized water 1000mL.Synthetic liquid and preparation method thereof is undertaken by embodiment 1 step.About plating workpiece area 03dm2/L～1.5dm2/L.
This embodiment only needs the cycle to replenish loss, 5 hours is one-period with plating, and main salt replenishes 1～20g/L, and reductive agent replenishes 1～20g/L.As radix, every increase one-period, the corresponding 1～20g that adds gets final product.Other auxiliary substance is mended into 0.5%～3% of standard formula amount with each cycle and is got final product.In the plating process, per hour replenish pure water, the maintenance solution capacity is 1000mL.
Claims (10)
1. the long-acting micron composite bed of receiving synthesizes liquid, and it is characterized in that: this synthetic liquid contains following raw material and is prepared from by weight:
Main salt 20～40g, reductive agent 20～40g, main complexing agent 20～40g, auxiliary complex-former 20～40g, buffer reagent a10～30g, buffer reagent b10～30mL, silicon carbide 8～20g, magnesium oxide 0～1g, cats product 0.1～1g, nonionogenic tenside 0.1～1g, rare earth 0.01～0.1g, stablizer 0.1～20mg, promotor 0.1～20g, deionized water 800～1500mL.
2. a kind of long-acting synthetic liquid of micron composite bed of receiving according to claim 1, it is characterized in that: above-mentioned main salt is to choose any one kind of them in single nickel salt, nickelous hypophosphite, nickelous chloride, nickel acetate, the nickel sulfamic acid; Above-mentioned reductive agent is to choose any one kind of them in sodium hypophosphite, sodium borohydride, dimethyamine borane, the diethylamine borane.
3. a kind of long-acting synthetic liquid of micron composite bed of receiving according to claim 1, it is characterized in that: above-mentioned cats product is to choose any one kind of them in cetyl trimethylammonium bromide, polymine, the perfluoroalkyl trimethyl ammonium chloride; Nonionogenic tenside is to choose any one kind of them in polyoxyethylene glycol, the fluorine carbon type nonionogenic tenside.
4. a kind of long-acting synthetic liquid of micron composite bed of receiving according to claim 1, it is characterized in that: above-mentioned rare earth is to choose any one kind of them in ceric sulfate, rehenic acid ammonium, the Cadmium Sulphate; The aforementioned stable agent is to choose any one kind of them in Potassium Iodate, thiocarbamide, Sodium Fluoride, the lead nitrate or two kinds; Above-mentioned promotor is to choose any one kind of them in aspartic acid, Sodium Fluoride, the aminocarboxylic acid.
5. a kind of long-acting synthetic liquid of micron composite bed of receiving according to claim 1 is characterized in that: above-mentioned main complexing agent is to choose any one kind of them in citric acid, lactic acid, oxyacetic acid, oxysuccinic acid, propionic acid, Succinic Acid, the Padil or make up; Above-mentioned auxiliary complex-former is to choose any one kind of them in sodium tetraborate, Trisodium Citrate, Seignette salt, Soduxin, the quadrol or make up.
6. a kind of long-acting synthetic liquid of micron composite bed of receiving according to claim 1, it is characterized in that: above-mentioned buffer reagent a chooses any one kind of them in sodium-acetate, anhydrous sodium sulphate, borax, NaOH, the Sodium Tetraborate; Buffer reagent b chooses any one kind of them in Glacial acetic acid, glycine, Succinic Acid, the boric acid.
7. a long-acting preparation method who receives the synthetic liquid of micron composite bed is characterized in that: comprise the steps:
A. silicon carbide activation treatment: soaked 5～90 minutes with trisodium phosphate solution, add deionized water again and clean, treat that 20～90 minutes post precipitations are inhaled the deionized water more than the silicon carbide, be made into the silicon carbide mixed solution, be called for short A liquid to pH=4～8, standby;
B. magnesium oxide adds deionized water flush away hydrofluoric acid then with hydrofluoric acid etch 5～90 minutes, cleans to pH=4～8, treats that 20～90 minutes post precipitations go the suction of the deionized water more than the magnesium oxide, is made into the magnesium oxide mixed solution, is called for short B liquid, and is standby;
C. in deionized water, add and become owner of salt, it is fully dissolved, stir evenly impurity screening after, it is standby to be made into C liquid;
D. in deionized water, add reductive agent, it fully dissolved, stir evenly impurity screening after, it is standby to be made into D liquid;
E. in deionized water, add and become owner of complexing agent, it is fully dissolved, stir evenly impurity screening after, it is standby to be made into E liquid;
F. in deionized water, add auxiliary complex-former, it fully dissolved, stir evenly impurity screening after, it is standby to be made into F liquid;
G. in deionized water, add buffer reagent a, it fully dissolved, stir evenly impurity screening after, it is standby to be made into G liquid;
H. with sodium hydroxide solution or ammonia soln the pH value of buffer reagent b is transferred to 4.4～5.1, it is standby to be made into H liquid;
I. add cats product in deionized water, it is fully dissolved, stir evenly, it is standby to be made into I liquid;
J. add nonionogenic tenside in deionized water, it is fully dissolved, stir evenly, it is standby to be made into J liquid;
K. add rare earth in deionized water, it is fully dissolved, stir evenly, it is standby to be made into K liquid;
L. add stablizer in deionized water, it is fully dissolved, stir evenly, it is standby to be made into L liquid;
M. add promotor in deionized water, it is fully dissolved, stir evenly, it is standby to be made into M liquid;
N. E liquid is slowly added F liquid and constantly stir, it is standby to be made into N liquid;
O. N liquid is slowly added G liquid and constantly stir, it is standby to be made into O liquid;
P. O liquid is slowly added C liquid and constantly stir, it is standby to be made into P liquid;
Q. H liquid is slowly added P liquid and constantly stir, it is standby to be made into Q liquid;
R. L liquid, M liquid are slowly added D liquid and constantly stir, it is standby to be made into R liquid;
S. it is standby B, I, J, K adding A and continuous stirring to be made into S liquid;
T. R liquid is slowly added Q liquid and constantly stir, it is standby to be made into T liquid;
U. with deionized water T liquid is diluted to volume 1000mL;
V. the pH value with sulfuric acid, sodium hydroxide solution or ammonia soln adjusting T liquid is 4.4～5.1, puts into coating bath and gets final product plating.
After the plating 10～90 minutes, slowly add S liquid and constantly stir continuation plating 3-6 hour.
8. a kind of long-acting preparation method who receives the synthetic liquid of micron composite bed according to claim 7, it is characterized in that: above-mentioned trisodium phosphate solution concentration is 0.5～50%, volume is 10～100mL; Above-mentioned hydrofluoric acid solution concentration is 0.5～50%, and volume is 1～50mL; Above-mentioned concentration of sodium hydroxide solution is 0.5～50%; Above-mentioned ammonia soln concentration is 0.5～50%; Above-mentioned sulphuric acid soln concentration is 2: 1.
9. a kind of long-acting preparation method who receives the synthetic liquid of micron composite bed according to claim 7, it is characterized in that: above-mentioned deionized water temperature is 50～70 ℃.
10. a kind of long-acting synthetic liquid of micron composite bed of receiving according to claim 1 is characterized in that: formed fully by the following raw materials in parts by weight numeral system:
Main salt: single nickel salt 25g; Reductive agent: sodium hypophosphite 24g; Main complexing agent: citric acid 30g; Auxiliary complex-former: Trisodium Citrate 10g+ sodium tetraborate 20g; Buffer reagent a: anhydrous sodium sulphate 15g or sodium-acetate 15g; Buffer reagent b: Glacial acetic acid 20mL; Silicon carbide 10g; Magnesium oxide 0.5g; Cats product: cetyl trimethylammonium bromide 0.3g; Nonionogenic tenside: polyoxyethylene glycol 0.6g; Rare earth: ceric sulfate 0.01g; Stablizer: Potassium Iodate 2mg; Promotor: Sodium Fluoride 0.6g; 70 ℃ of deionized water 900～1200mL.
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| CN110158129A (en) * | 2019-05-27 | 2019-08-23 | 广州三孚新材料科技股份有限公司 | Pre- bleeding agent composition, pre- bleeding agent, copper facing preprocess method and cyanide-free copper electroplating method |
| CN111074250A (en) * | 2020-02-13 | 2020-04-28 | 西安交通大学 | High-corrosion-resistance stable chemical nickel plating solution for aluminum alloy surface, and preparation method and application thereof |
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