CN103757616A - Chemical plating alkaline composite plating solution used for preparing magnetic abrasive and preparation method of chemical plating alkaline composite plating solution - Google Patents
Chemical plating alkaline composite plating solution used for preparing magnetic abrasive and preparation method of chemical plating alkaline composite plating solution Download PDFInfo
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- CN103757616A CN103757616A CN201410018439.7A CN201410018439A CN103757616A CN 103757616 A CN103757616 A CN 103757616A CN 201410018439 A CN201410018439 A CN 201410018439A CN 103757616 A CN103757616 A CN 103757616A
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Abstract
The invention discloses a chemical plating alkaline composite plating solution used for preparing a magnetic abrasive and belongs to the field of chemical plating. The plating solution comprises 1-10g/L of abrasive particles, 20-30g/L of main salt, 20-40g/L of reducing agent, 95-155g/L of complexing agent, 40-60g/L of buffering agent and 1-2mg/L of stabilizing agent. A preparation method comprises the following steps of: pretreating diamond micro-powder; preparing the main salt and the complexing agent into a mixed solution; preparing a reducing agent solution and adding the reducing agent into the mixed solution under the condition of stirring; then adding the stabilizing agent and diamond micro-powder obtained in the step (1); and adjusting PH of the solution obtained in the step (4) to 8-10 by utilizing strong ammonia water. Compared with conventional acidic chemical plating, the plating solution has the advantages that the hardness of low-phosphorous nickel plating layer prepared by utilizing the plating solution is greatly improved, the holding force of the plating layer to particulates is strengthened, and thermal shock experiment verifies that the binding force of the plating layer and matrix is excellent so that the service life of the prepared magnetic abrasive is prolonged.
Description
Technical field
The present invention relates to electroless plating field, particularly a kind of alkalescence of the electroless plating for the preparation of magnetic abrasive Composite Coatings plating solution and preparation method thereof.
Background technology
Chemical nickel plating is by adding suitable reductive agent in solution, making nickel ion be reduced into metallic nickel, and in the process of plating piece surface deposition.Concrete reaction equation is:
separating out of the generation of this process simultaneous hydrogen and phosphorus.In this chemical reaction process, the Second Phase Particle adding has very strong chemical stability, does not participate in from start to finish any chemical reaction in plating process, and its change procedure belongs to physical change.Second Phase Particle stir and the effect low suspension of tensio-active agent in plating solution, be accompanied by Ni atom and P atom codeposition on plating piece surface.
The fine and close solidity to corrosion of coating that electroless plating obtains is good, and thickness of coating is even, and without significantly fringing effect, hardness is high; It has high rigidity by changing matrix metal and disperse particles, can obtaining, wear resistance, self-lubricating, thermotolerance, solidity to corrosion or special decorative coating, at aspects such as aviation, machinery, chemical industry, metallurgy and nuclear industry, is widely used.
The core of chemical plating nickel technology is composition and the performance of plating solution, so it is worth noting the improvement of plating solution itself in chemical nickel plating development most.Present stage, chemical nickel plating can be divided into acid chemical plating nickel and alkaline chemical nickel-plating, the service temperature high (plating temperature, more than 75 ℃, obtains suitable plating speed generally more than 80 ℃) of general acidic nickel plating, and energy consumption is large, and plating solution is unstable; The service temperature of alkalescence nickel plating is low, but plating speed is slower, and needs the volatile ammoniacal liquor of a large amount of employing as PH conditioning agent, poor working environment.Therefore probe into the main direction that cost performance is high, plating speed plating solution very fast, that have steady-working state is still current plating solution exploitation.
Chinese invention patent mandate publication number CN1248786C has proposed a kind of chemical nickel-plating solution of acidity, adopt alkali metal hydroxide, alkaline earth metal hydroxides as the PH conditioning agent of plating solution, with expectation, regulate and to maintain the PH of plating solution stable, the plating solution of alkali metal containing oxyhydroxide is also more easily processed than the plating solution containing ammoniacal liquor.Although this plating solution need not adopt ammoniacal liquor, but whole complex operation, plating temperature is more than 80 ℃, but before adopting alkali metal hydroxide to regulate PH need plating solution to cool to below 60 ℃, after PH conditioning agent to be added, again plating solution is warmed up to plating temperature, time-consuming, and be not easy to production operation.
Chinese invention patent mandate publication number CN101709492B has proposed a kind of chemical plating fluid of alkalescence, and this plating solution forms simple, and preparation is convenient, but need to add a large amount of ammoniacal liquor to maintain plating solution PH.In this patent, the add-on of ammoniacal liquor is 90～100ml/L, and the ammoniacal liquor of high density being hankered being easy to volatilization the PH of plating solution is changed adding, and then affects coating performance.
Chinese patent application, application number is CN10320775A, has proposed a kind of method that acidic bath is prepared magnetic abrasive.Adopt the plating solution in the method, can obtain plating speed faster, but the coating that plating temperature is high and coating hardness obtains with alkali plating solution is compared a certain distance in addition.
The magnetic abrasive using is at present mainly to be made by mull technique or sintering process.Specifically, these two kinds of methods are all that ferromagnetic phase and abrasive particle are mixed mutually by bonding or sinter bonded and arrived together, by broken, screening, obtain magnetic abrasive.These two kinds of method costs are lower, can large-scale application, and the life-span of the abrasive material of gained also can be accepted, but abrasive material is after fragmentation, and the bonding strength of matrix and abrasive particle reduces, and affects life-span and the processing effect to workpiece surface of abrasive material.Therefore this patent adopts the mode of Ni-P, Composite Coatings last layer nickel-phosphorus coating on iron-based body, and abrasive particle is co-deposited to it matrix surface, reaches the object that extends the abrasive material life-span.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of alkali electroless plating solution, the magnetic abrasive that ground, time-saving and efficiency a kind of matrix of preparation and abrasive particle bonding strength are high.
Technical scheme of the present invention is: a kind of alkalescence of the electroless plating for the preparation of magnetic abrasive composite plating bath, comprise abrasive particle, main salt, reductive agent, complexing agent, buffer reagent, stablizer and deionized water, and the concentration of each component is:
Abrasive particle: 1～10g/L;
Main salt: 20～30g/L;
Reductive agent: 20～40g/L;
Complexing agent: 95～155g/L;
Buffer reagent: 40-60ml/L;
Stablizer: 1～2mg/L.
This electroless plating alkalescence composite plating bath also comprises accelerator and tensio-active agent, and its concentration is:
Accelerator: 5～8g/L;
Tensio-active agent: 10～20mg/L.
Described abrasive particle is the diadust of particle diameter 5～10 μ m; Described main salt is nickel salt; Described reductive agent is sodium hypophosphite; Described complexing agent is that Trisodium Citrate, ammonium sulfate and boric acid mix, and wherein, the concentration of Trisodium Citrate is that the concentration of 60～80g/L, ammonium sulfate is that the concentration of 20～40g/L, boric acid is 15～35g/L.
Described accelerator is succinic acid, and described stablizer is thiocarbamide, and described tensio-active agent is sodium lauryl sulphate, and described buffer reagent is ammoniacal liquor and 10wt% sulphuric acid soln; Solid-state pharmaceutical chemicals purity is analytical pure above.
The preparation method of described electroless plating alkalescence composite plating bath, comprises the steps:
(1) diadust pre-treatment: the diadust that by particle diameter is 5～10 μ m soaks and disperses, cleans, is placed in basic solution and boil through organic solvent, rinses, and is placed in 50%-65% concentrated nitric acid and boils, and rinses, and dries.
(2) preparation mixing solutions: main salt and complexing agent are mixed with to mixing solutions.
(3) preparation reductant solution adds in the mixing solutions of step (2) under agitation condition.
(4) to adding stablizer in step (3), adding the diadust obtaining in step (1) again.
(5), with PH to 8～10 of strong aqua regulating step (4) solution, obtain the electroless plating alkalescence composite plating bath for the preparation of magnetic abrasive.
In the electroless plating alkalescence composite plating bath finally obtaining, diadust: 1～10g/L, main salt: 20～30g/L, reductive agent: 20～40g/L, complexing agent: 95～155g/L, buffer reagent: 40-60ml/L, stablizer: 1～2mg/L.
The using method of described plating solution is that the container that this plating solution is housed is placed on magnetic stirring apparatus, and the loading ratio of getting magneticsubstance is 0.5～1.5dm
2/ L, joins magneticsubstance in plating solution, and the Heating temperature of setting magnetic stirring apparatus is 45～85 ℃, and the rotating speed 50～200r/min of magnetic force rotor, by particular case plating one hour to several hours.
Effect of the present invention and benefit are: the present invention adopts Trisodium Citrate, ammonium sulfate and boric acid that complex ability is very strong as complexing agent, has improved the stability of alkali plating solution; Ammonium sulfate can form buffer system stabilizing solution PH with ammoniacal liquor, contributes to guarantee that the homogeneous of quality of coating is constant; Boric acid can improve coating sedimentation rate as accelerator with succinic acid.Compare with existing acidic bath, the plating temperature of this plating solution can be low to moderate 44 ℃, at 60 ℃, just can have satisfied plating speed, and economy is fine.Compare with existing alkali plating solution, ammoniacal liquor add-on is 40～60ml/L, than consumption in existing patent reduced near half.Phosphorus content in coating is lower than 5%, and coating initial state Vickers' hardness can be up to 650HV, and after heat treatment hardness is higher, and coating can meet the requirement of magnetically grinding to the hold of abrasive particle, and the magnetic abrasive life-span of preparation is improved.
Accompanying drawing explanation
Accompanying drawing is composite deposite surface topography.
Embodiment
Below in conjunction with technical scheme, describe specific embodiments of the invention in detail.
Embodiment 1
(1) choose each concentration of component: single nickel salt is that 30g/L, sodium hypophosphite are that 30g/L, Trisodium Citrate are that 60g/L, ammonium sulfate are that 30g/L, boric acid are that 35g/L, succinic acid are that 6.5g/L, sodium lauryl sulphate are that 15mg/L, thiocarbamide are that 1mg/L, abrasive material are 5g/L, by liquor capacity 500ml, takes each component; Abrasive material is diadust, and purity is 99%; Other material purities are analytical pure;
(2) diadust pre-treatment: by particle diameter, be 10 μ m diadust through acetone soak and in ultrasonic cleaner, disperse 30min, the sodium hydroxide solution that cleans, be placed in 1mol/L boils, rinse, be placed in 50%-65% concentrated nitric acid and boil, rinse, dry;
(3) preparation mixing solutions: main salt and complexing agent are dissolved in and are mixed with mixing solutions in deionized water;
(4) reductive agent is dissolved in the water, under agitation condition, adds in the mixing solutions of step (3);
(5) to solution in step (4), add stablizer, add the diadust obtaining in 5g/L step (1) again;
(6) use the PH to 10 of strong aqua regulating step (5) solution.
The using method of plating solution is that the container that this plating solution is housed is placed on magnetic stirring apparatus, gets the loading of magneticsubstance than being 1dm
2/ L, joins magneticsubstance in plating solution, and the Heating temperature of setting magnetic stirring apparatus is 50 ℃, magnetic force rotor turn 150r/min, plating one hour.
Embodiment 2
(1) choose each concentration of component: single nickel salt is that 20g/L, sodium hypophosphite are that 20g/L, Trisodium Citrate are that 80g/L, ammonium sulfate are that 40g/L, boric acid are that 15g/L, succinic acid are that 7g/L, sodium lauryl sulphate are that 10mg/L, thiocarbamide are that 2mg/L, abrasive material are 10g/L, by liquor capacity 500ml, takes each component; Abrasive material is diadust, and purity is 99%; Other material purities are analytical pure;
(2) diadust pre-treatment: by particle diameter, be 10 μ m diadust through acetone soak and in ultrasonic cleaner, disperse 30min, the sodium hydroxide solution that cleans, be placed in 1.5mol/L boils, rinse, be placed in 50%-65% concentrated nitric acid and boil, rinse, dry;
(3) preparation mixing solutions: main salt and complexing agent are dissolved in and are mixed with mixing solutions in deionized water;
(4) reductive agent is dissolved in the water, under agitation condition, adds in the mixing solutions of step (3);
(5) to solution in step (4), add stablizer, add the diadust obtaining in 10g/L step (1) again;
(6) use the PH to 8 of strong aqua regulating step (5) solution.
The using method of described embodiment plating solution is that the container that this plating solution is housed is placed on magnetic stirring apparatus, gets the loading of magneticsubstance than being 1.5dm
2/ L, joins magneticsubstance in plating solution, and the Heating temperature of setting magnetic stirring apparatus is 70 ℃, the rotating speed 200r/min of magnetic force rotor, plating one hour.
Embodiment 3
(1) choose each concentration of component: single nickel salt is that 25g/L, sodium hypophosphite are that 40g/L, Trisodium Citrate are that 70g/L, ammonium sulfate are that 20g/L, boric acid are that 25g/L, succinic acid are that 6g/L, sodium lauryl sulphate are that 15mg/L, thiocarbamide are that 1.5mg/L, abrasive material are 1g/L, by liquor capacity 500ml, takes each component; Abrasive material is diadust, and purity is 99%; Other material purities are analytical pure;
(2) diadust pre-treatment: by particle diameter, be 5 μ m diadust through acetone soak and in ultrasonic cleaner, disperse 30min, the sodium hydroxide solution that cleans, be placed in 1mol/L boils, rinse, be placed in 50%-65% concentrated nitric acid and boil, rinse, dry;
(3) preparation mixing solutions: main salt and complexing agent are dissolved in and are mixed with mixing solutions in deionized water;
(4) reductive agent is dissolved in the water, under agitation condition, adds in the mixing solutions of step (3);
(5) to solution in step (4), add stablizer, add the diadust obtaining in 1g/L step (1) again;
(6) use the PH to 9 of strong aqua regulating step (5) solution.
The using method of plating solution is that the container that this plating solution is housed is placed on magnetic stirring apparatus, gets the loading of magneticsubstance than being 0.5dm
2/ L, joins magneticsubstance in plating solution, and the Heating temperature of setting magnetic stirring apparatus is 80 ℃, the rotating speed 150r/min of magnetic force rotor, plating one hour.
Claims (10)
1. for the preparation of an electroless plating alkalescence composite plating bath for magnetic abrasive, it is characterized in that, this electroless plating alkalescence composite plating bath comprises abrasive particle, main salt, reductive agent, complexing agent, buffer reagent, stablizer and deionized water, and its concentration is:
Abrasive particle: 1～10g/L;
Main salt: 20～30g/L;
Reductive agent: 20～40g/L;
Complexing agent: 95～155g/L;
Buffer reagent: 40-60ml/L;
Stablizer: 1～2mg/L.
2. electroless plating alkalescence composite plating bath according to claim 1, is characterized in that, this electroless plating alkalescence composite plating bath also comprises accelerator and tensio-active agent, and its concentration is:
Accelerator: 5～8g/L;
Tensio-active agent: 10～20mg/L.
3. electroless plating according to claim 1 and 2 alkalescence composite plating bath, it is characterized in that, described complexing agent is that Trisodium Citrate, ammonium sulfate and boric acid mix, and wherein, the concentration of Trisodium Citrate is that the concentration of 60～80g/L, ammonium sulfate is that the concentration of 20～40g/L, boric acid is 15～35g/L.
4. electroless plating alkalescence composite plating bath according to claim 1 and 2, is characterized in that, described main salt is nickel salt.
5. electroless plating alkalescence composite plating bath according to claim 3, is characterized in that, described main salt is nickel salt.
6. according to the electroless plating alkalescence composite plating bath described in claim 1,2 or 5, it is characterized in that, described abrasive particle is the diadust of particle diameter 5～10 μ m; Described reductive agent is sodium hypophosphite.
7. the preparation method of electroless plating alkalescence composite plating bath described in claim 1,2 or 5, is characterized in that, step is as follows:
(1) diadust pre-treatment: the diadust that by particle diameter is 5～10 μ m soaks and disperses, cleans, is placed in basic solution and boil through organic solvent, rinses, and is placed in 50%-65% concentrated nitric acid and boils, and rinses, and dries;
(2) preparation mixing solutions: main salt and complexing agent are mixed with to mixing solutions;
(3) preparation reductant solution adds in the mixing solutions of step (2) under agitation condition;
(4) to adding stablizer in step (3), adding the diadust obtaining in step (1) again;
(5), with PH to 8～10 of strong aqua regulating step (4) solution, obtain the electroless plating alkalescence composite plating bath for the preparation of magnetic abrasive.
8. the preparation method of electroless plating alkalescence composite plating bath described in claim 3, is characterized in that, step is as follows:
(1) diadust pre-treatment: the diadust that by particle diameter is 5～10 μ m soaks and disperses, cleans, is placed in basic solution and boil through organic solvent, rinses, and is placed in 50%-65% concentrated nitric acid and boils, and rinses, and dries;
(2) preparation mixing solutions: main salt and complexing agent are mixed with to mixing solutions;
(3) preparation reductant solution adds in the mixing solutions of step (2) under agitation condition;
(4) to adding stablizer in step (3), adding the diadust obtaining in step (1) again;
(5), with PH to 8～10 of strong aqua regulating step (4) solution, obtain the electroless plating alkalescence composite plating bath for the preparation of magnetic abrasive.
9. the preparation method of electroless plating alkalescence composite plating bath described in claim 4, is characterized in that, step is as follows:
(1) diadust pre-treatment: the diadust that by particle diameter is 5～10 μ m soaks and disperses, cleans, is placed in basic solution and boil through organic solvent, rinses, and is placed in 50%-65% concentrated nitric acid and boils, and rinses, and dries;
(2) preparation mixing solutions: main salt and complexing agent are mixed with to mixing solutions;
(3) preparation reductant solution adds in the mixing solutions of step (2) under agitation condition;
(4) to adding stablizer in step (3), adding the diadust obtaining in step (1) again;
(5), with PH to 8～10 of strong aqua regulating step (4) solution, obtain the electroless plating alkalescence composite plating bath for the preparation of magnetic abrasive.
10. the preparation method of electroless plating alkalescence composite plating bath described in claim 6, it is characterized in that, step is as follows: (1) diadust pre-treatment: the diadust that by particle diameter is 5～10 μ m soaks and disperses, cleans, is placed in basic solution and boil through organic solvent, rinse, being placed in 50%-65% concentrated nitric acid boils, rinse, dry;
(2) preparation mixing solutions: main salt and complexing agent are mixed with to mixing solutions;
(3) preparation reductant solution adds in the mixing solutions of step (2) under agitation condition;
(4) to adding stablizer in step (3), adding the diadust obtaining in step (1) again;
(5), with PH to 8～10 of strong aqua regulating step (4) solution, obtain the electroless plating alkalescence composite plating bath for the preparation of magnetic abrasive.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104191385A (en) * | 2014-09-05 | 2014-12-10 | 南京航空航天大学 | Ferromagnetic diamond abrasive material prepared by means of wet method |
| CN104746054A (en) * | 2015-04-20 | 2015-07-01 | 南京航空航天大学 | Magnetic control based method for wet-process preparation of diamond magnetic abrasive |
| CN108716000A (en) * | 2018-06-05 | 2018-10-30 | 遵义市播州区铁厂创业刚玉有限责任公司 | A kind of plating magnetic abrasive material preparation method |
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| CN103320775A (en) * | 2013-06-03 | 2013-09-25 | 大连理工大学 | Magnetic abrasive preparation method |
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2014
- 2014-01-14 CN CN201410018439.7A patent/CN103757616A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103320775A (en) * | 2013-06-03 | 2013-09-25 | 大连理工大学 | Magnetic abrasive preparation method |
Non-Patent Citations (2)
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| 李金桂: "《防腐蚀表面工程技术》", 31 January 2003 * |
| 王立娟，等: "《木材表面化学镀》", 31 December 2013, 科学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104191385A (en) * | 2014-09-05 | 2014-12-10 | 南京航空航天大学 | Ferromagnetic diamond abrasive material prepared by means of wet method |
| CN104191385B (en) * | 2014-09-05 | 2016-05-18 | 南京航空航天大学 | Ferromagnetism diamond abrasive prepared by a kind of wet method |
| CN104746054A (en) * | 2015-04-20 | 2015-07-01 | 南京航空航天大学 | Magnetic control based method for wet-process preparation of diamond magnetic abrasive |
| CN108716000A (en) * | 2018-06-05 | 2018-10-30 | 遵义市播州区铁厂创业刚玉有限责任公司 | A kind of plating magnetic abrasive material preparation method |
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Application publication date: 20140430 |