CN102296286B - 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 a kind of technology of sintering metal Composite Coatings.
Background technology
As everyone knows, metal especially metal alloy has superior physical and mechanical properties, as certain hardness, 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 sintering metal chemistry Composite Coatings.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 generates liquid and does not rely on electrical forces just can receive by nickel phosphorus the scuff-resistant coating that micron hard ceramic forms at generation one deck on the metal part surface.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 enters in the alloy layer lattice, greatly strengthened the comprehensive wear resisting property of coating, 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, bad stability, easily decompose, plating solution is short work-ing life.
Summary of the invention
The present invention aims to provide the long-acting nano-micron composite layer synthetic solution of a kind of high speed, energy-conservation, stable, additional use capable of circulation.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of long-acting nano-micron composite layer synthetic solution forms by the following raw materials in parts by weight numeral system is standby:
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, nickel sulfamic acid; Above-mentioned reductive agent is to choose any one kind of them in sodium hypophosphite, sodium borohydride, dimethyamine borane, diethylamine borane.
Above-mentioned cats product is to choose any one kind of them in cetyl trimethylammonium bromide, polymine, perfluoroalkyl trimethyl ammonium chloride; Nonionogenic tenside is to choose any one kind of them in polyoxyethylene glycol, fluorine carbon type nonionogenic tenside.
Above-mentioned rare earth is to choose any one kind of them in ceric sulfate, rehenic acid ammonium, Cadmium Sulphate; The aforementioned stable agent is to choose any one kind of them in Potassium Iodate, thiocarbamide, Sodium Fluoride, lead nitrate or two kinds; Above-mentioned promotor is to choose any one kind of them in aspartic acid, Sodium Fluoride, aminocarboxylic acid.
Above-mentioned main complexing agent is choose any one kind of them in citric acid, lactic acid, oxyacetic acid, oxysuccinic acid, propionic acid, succinic acid, Padil or make up; Above-mentioned auxiliary complex-former is choose any one kind of them in sodium tetraborate, Trisodium Citrate, Seignette salt, Soduxin, quadrol or make up.
Above-mentioned buffer reagent a chooses any one kind of them in sodium-acetate, anhydrous sodium sulphate, borax, NaOH, Sodium Tetraborate; Buffer reagent b chooses any one kind of them in Glacial acetic acid, glycine, succinic acid, boric acid.
A kind of preparation method of long-acting nano-micron composite layer synthetic solution comprises the steps:
A. silicon carbide activation treatment: soaked 5～90 minutes with trisodium phosphate solution, then add deionized water to clean to pH=4～8, the deionized water more than silicon carbide was sucked after precipitation until 20～90 minutes, be made into the silicon carbide mixed solution, be called for short A liquid, standby;
B. magnesium oxide with hydrofluoric acid etch 5～90 minutes, then adds deionized water to wash away hydrofluoric acid, cleans to pH=4～8, the deionized water more than magnesium oxide is sucked after precipitation until 20～90 minutes, is made into the magnesium oxide mixed solution, is called for short B liquid, and is standby;
C. add in deionized water and become owner of salt, it is fully dissolved, after stirring evenly impurity screening, be made into C liquid standby;
D. add reductive agent in deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into D liquid standby;
E. add in deionized water and become owner of complexing agent, it is fully dissolved, after stirring evenly impurity screening, be made into E liquid standby;
F. add auxiliary complex-former in deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into F liquid standby;
G. add buffer reagent a in deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into G liquid standby;
H. with sodium hydroxide solution or ammonia soln, the pH value of buffer reagent b is transferred to 4.4～5.1, be made into H liquid standby;
I. add cats product in deionized water, it is fully dissolved, stir evenly, be made into I liquid standby;
J. add nonionogenic tenside in deionized water, it is fully dissolved, stir evenly, be made into J liquid standby;
K. add rare earth in deionized water, it is fully dissolved, stir evenly, be made into K liquid standby;
L. add stablizer in deionized water, it is fully dissolved, stir evenly, be made into L liquid standby;
M. add promotor in deionized water, it is fully dissolved, stir evenly, be made into M liquid standby;
N. E liquid slowly added F liquid and constantly stir, being made into N liquid standby;
O. N liquid slowly added G liquid and constantly stir, being made into O liquid standby;
P. O liquid slowly added C liquid and constantly stir, being made into P liquid standby;
Q. H liquid slowly added P liquid and constantly stir, being made into Q liquid standby;
R. L liquid, M liquid slowly added D liquid and constantly stir, being made into R liquid standby;
S. B, I, J, K are added A and continuous stirring to be made into S liquid standby;
T. R liquid slowly added Q liquid and constantly stir, being made into T liquid standby;
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 plating 10～90 minutes, slowly add S liquid and constantly stir, continuing 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 nano-micron composite layer synthetic solution forms by the following raw materials in parts by weight numeral system is standby:
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 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, and environment-friendly high-efficiency, good economy performance.Only need the cycle to replenish loss, take 5 hours as a cycle, main salt replenishes 1～20g/L, and reductive agent replenishes 1～20g/L.As radix, in every one cycle of increase, the corresponding 1～20g that adds gets final product.Other auxiliary substance fills into 0.1%～10% of standard formula amount with each cycle and gets final product.In the plating process, per hour replenish pure water, the maintenance solution capacity is 1000mL.Up to more than 400MPa, exceed 200MPa than common alkaline self-decomposition plating solution with basal body binding force, exceed 300Mpa than the bonding force of electroplating.
The present invention is further described below in conjunction with embodiment:
Embodiment
Embodiment 1
A kind of long-acting nano-micron composite layer synthetic solution forms by the following raw materials in parts by weight numeral system is standby:
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 preparation method of long-acting nano-micron composite layer synthetic solution:
A. silicon carbide activation treatment: soaked 10 minutes with 5% trisodium phosphate solution 20mL, then add the 300mL deionized water to clean to pH=4～8, the deionized water more than silicon carbide was sucked after precipitation until 30 minutes, be made into the silicon carbide mixed solution, be called for short A liquid standby;
B. magnesium oxide with 1% hydrofluoric acid 2mL etch 10 minutes, then adds the 80mL deionized water to wash away hydrofluoric acid, cleans to pH=4～8, the deionized water more than magnesium oxide is sucked after precipitation until 30 minutes, is made into the magnesium oxide mixed solution, is called for short B liquid standby;
C. add single nickel salt in the 100mL deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into C liquid standby;
D. add sodium hypophosphite in the 100mL deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into D liquid standby;
E. add citric acid in the 100mL deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into E liquid standby;
F. add Trisodium Citrate, sodium tetraborate in the 100mL deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into F liquid standby;
G. add anhydrous sodium sulphate in the 50mL deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into G liquid standby;
H. with 20% sodium hydroxide solution or ammonia soln, the pH value of Glacial acetic acid is transferred to 4.4～5.1, be made into H liquid standby;
I. add cetyl trimethylammonium bromide in the 5mL deionized water, it is fully dissolved, stir evenly, be made into I liquid standby;
J. add polyoxyethylene glycol in the 25mL deionized water, it is fully dissolved, stir evenly, be made into J liquid standby;
K. add ceric sulfate in the 5mL deionized water, it is fully dissolved, stir evenly, be made into K liquid standby;
L. add Potassium Iodate in the 5mL deionized water, it is fully dissolved, stir evenly, be made into L liquid standby;
M. add Sodium Fluoride in the 5mL deionized water, it is fully dissolved, stir evenly, be made into M liquid standby;
N. E liquid slowly added F liquid and constantly stir, being made into N liquid standby;
O. N liquid slowly added G liquid and constantly stir, being made into O liquid standby;
P. O liquid slowly added C liquid and constantly stir, being made into P liquid standby;
Q. H liquid slowly added P liquid and constantly stir, being made into Q liquid standby;
R. L liquid, M liquid slowly added D liquid and constantly stir, being made into R liquid standby;
S. B, I, J, K are added A and continuous stirring to be made into S liquid standby;
T. R liquid slowly added Q liquid and constantly stir, being made into T liquid standby;
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 plating 10～90 minutes, slowly add S liquid and constantly stir, continuing plating 3-6 hour.
Embodiment 2
A kind of raw material optimal components ratio of long-acting nano-micron composite layer synthetic solution 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, and take plating 5 hours as a cycle, main salt replenishes 1～20g/L, and reductive agent replenishes 1～20g/L.As radix, in every one cycle of increase, the corresponding 1～20g that adds gets final product.Other auxiliary substance fills into 0.5%～3% of standard formula amount with each cycle and gets final product.In the plating process, per hour replenish pure water, the maintenance solution capacity is 1000mL.
Claims (8)
1. long-acting nano-micron composite layer synthetic solution is characterized in that: comprising that the following raw materials in parts by weight numeral system is standby forms:
0.01～0.1g, stablizer 0.1～20mg, promotor 0.1～20g, deionized water 800～1500mL choose any one kind of them in 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, ceric sulfate, rehenic acid ammonium, Cadmium Sulphate;
Above-mentioned main complexing agent is choose any one kind of them in citric acid, lactic acid, oxyacetic acid, oxysuccinic acid, propionic acid, succinic acid, Padil or make up; Above-mentioned auxiliary complex-former is choose any one kind of them in sodium tetraborate, Trisodium Citrate, Seignette salt, Soduxin, quadrol or make up;
Above-mentioned buffer reagent a chooses any one kind of them in sodium-acetate, anhydrous sodium sulphate, borax, NaOH, Sodium Tetraborate; Buffer reagent b chooses any one kind of them in Glacial acetic acid, glycine, succinic acid, boric acid.
2. a kind of long-acting nano-micron composite layer synthetic solution 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, nickel sulfamic acid; Above-mentioned reductive agent is to choose any one kind of them in sodium hypophosphite, sodium borohydride, dimethyamine borane, diethylamine borane.
3. a kind of long-acting nano-micron composite layer synthetic solution 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, perfluoroalkyl trimethyl ammonium chloride; Nonionogenic tenside is to choose any one kind of them in polyoxyethylene glycol, fluorine carbon type nonionogenic tenside.
4. a kind of long-acting nano-micron composite layer synthetic solution according to claim 1, it is characterized in that: the aforementioned stable agent is to choose any one kind of them in Potassium Iodate, thiocarbamide, Sodium Fluoride, lead nitrate or two kinds; Above-mentioned promotor is to choose any one kind of them in aspartic acid, Sodium Fluoride, aminocarboxylic acid.
5. the preparation method of a long-acting nano-micron composite layer synthetic solution, is characterized in that: comprise the steps:
A. silicon carbide activation treatment: soaked 5～90 minutes with trisodium phosphate solution, then add deionized water to clean to pH=4～8, the deionized water more than silicon carbide was sucked after precipitation until 20～90 minutes, be made into the silicon carbide mixed solution, be called for short A liquid, standby;
B. magnesium oxide with hydrofluoric acid etch 5～90 minutes, then adds deionized water to wash away hydrofluoric acid, cleans to pH=4～8, the deionized water more than magnesium oxide is sucked after precipitation until 20～90 minutes, is made into the magnesium oxide mixed solution, is called for short B liquid, and is standby;
C. add in deionized water and become owner of salt, it is fully dissolved, after stirring evenly impurity screening, be made into C liquid standby;
D. add reductive agent in deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into D liquid standby;
E. add in deionized water and become owner of complexing agent, it is fully dissolved, after stirring evenly impurity screening, be made into E liquid standby;
F. add auxiliary complex-former in deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into F liquid standby;
G. add buffer reagent a in deionized water, it is fully dissolved, after stirring evenly impurity screening, be made into G liquid standby;
H. with sodium hydroxide solution or ammonia soln, the pH value of buffer reagent b is transferred to 4.4～5.1, be made into H liquid standby;
I. add cats product in deionized water, it is fully dissolved, stir evenly, be made into I liquid standby;
J. add nonionogenic tenside in deionized water, it is fully dissolved, stir evenly, be made into J liquid standby;
K. add rare earth in deionized water, it is fully dissolved, stir evenly, be made into K liquid standby;
L. add stablizer in deionized water, it is fully dissolved, stir evenly, be made into L liquid standby;
M. add promotor in deionized water, it is fully dissolved, stir evenly, be made into M liquid standby;
N. E liquid slowly added F liquid and constantly stir, being made into N liquid standby;
O. N liquid slowly added G liquid and constantly stir, being made into O liquid standby;
P. O liquid slowly added C liquid and constantly stir, being made into P liquid standby;
Q. H liquid slowly added P liquid and constantly stir, being made into Q liquid standby;
R. L liquid, M liquid slowly added D liquid and constantly stir, being made into R liquid standby;
S. B, I, J, K are added A and continuous stirring to be made into S liquid standby;
T. R liquid slowly added Q liquid and constantly stir, being made into T liquid standby;
U. with deionized water, T liquid is diluted to volume 1000mL;
The pH value of V. regulating T liquid with sulfuric acid or sodium hydroxide solution, ammonia soln is 4.4～5.1, puts into coating bath and gets final product plating;
After plating 10～90 minutes, slowly add S liquid and constantly stir, continuing plating 3-6 hour;
Above-mentioned main complexing agent is choose any one kind of them in citric acid, lactic acid, oxyacetic acid, oxysuccinic acid, propionic acid, succinic acid, Padil or make up; Above-mentioned auxiliary complex-former is choose any one kind of them in sodium tetraborate, Trisodium Citrate, Seignette salt, Soduxin, quadrol or make up;
Above-mentioned buffer reagent a chooses any one kind of them in sodium-acetate, anhydrous sodium sulphate, borax, NaOH, Sodium Tetraborate; Buffer reagent b chooses any one kind of them in Glacial acetic acid, glycine, succinic acid, boric acid.
6. the preparation method of a kind of long-acting nano-micron composite layer synthetic solution according to claim 5, 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.
7. the preparation method of a kind of long-acting nano-micron composite layer synthetic solution according to claim 5, it is characterized in that: above-mentioned deionized water temperature is 50～70 ℃.
8. a kind of long-acting nano-micron composite layer synthetic solution according to claim 1 is characterized in that: form by the following raw materials in parts by weight numeral system is standby:
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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| CN105063696A (en) * | 2015-08-07 | 2015-11-18 | 昆山—邦泰汽车零部件制造有限公司 | Manufacturing method of abrasion-proof automotive hardware |
| CN105063530A (en) * | 2015-08-07 | 2015-11-18 | 昆山—邦泰汽车零部件制造有限公司 | Method for manufacturing high-hardness automobile hardware |
| CN105063581A (en) * | 2015-08-07 | 2015-11-18 | 昆山—邦泰汽车零部件制造有限公司 | Method for manufacturing high-tenacity automobile hardware |
| CN105543814A (en) * | 2015-11-24 | 2016-05-04 | 中国科学院兰州化学物理研究所 | Ni-P-(MoS2-CaF2) composite plating solution, and application thereof on surface of carbon steel |
| CN107475698B (en) * | 2017-06-23 | 2020-04-10 | 安庆师范大学 | Preparation method of Ni-Cr-B-P of stripping layer of ultrathin copper foil |
| CN109030148B (en) * | 2018-07-27 | 2020-09-29 | 中南大学 | Preparation method of iron-based alloy powder EBSD detection sample |
| CN110055522A (en) * | 2019-04-28 | 2019-07-26 | 祝亚琴 | A kind of chemical nickel plating solution additive |
| CN110158129B (en) * | 2019-05-27 | 2020-06-05 | 广州三孚新材料科技股份有限公司 | Pre-penetrant composition, pre-penetrant, copper plating pretreatment method, and cyanide-free copper plating method |
| CN111074250B (en) * | 2020-02-13 | 2021-05-28 | 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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