CN102965647A - Laser nanocrystallization method of Ni-W-P and Ni-P dual-alloy coating - Google Patents
Laser nanocrystallization method of Ni-W-P and Ni-P dual-alloy coating Download PDFInfo
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Abstract
The invention belongs to metal surface modification in industrial production, and in particular relates to a laser nanocrystallization method of a Ni-W-P and Ni-P dual-alloy coating. The laser nanocrystallization method of the Ni-W-P and Ni-P dual-alloy coating is characterized by comprising the following steps of: 1, carrying out chemical precipitation to obtain a Ni-W-P and Ni-P dual-alloy coating; and 2, carrying out laser induction to obtain a Ni-W-P and Ni-P nanocrystallized dual-alloy coating. According to the method, laser induction dual-coating crystallization is carried out directly in air to prepare a nanocrystalline material, thus the maneuverability is provided for the practical production, more importantly, the obtained nanocrystallized dual-alloy coating has texture characteristics such as specific grain size and crystallization degree, so that the bonding force of the coating with a metal matrix can be improved, and the property of the matrix is not influenced, and therefore, respective advantages of different coatings are given a full play, and surface properties of the material are greatly improved.
Description
(1) technical field
The invention belongs to the metal surface modification in the industrial production, particularly a kind of Ni-W-P, Ni-P pairing gold plate laser nano method.
(2) background technology
Electroless plating Ni-P base alloy Annealing Crystallization is a kind of method of preparation nanocrystalline material, formed nanocrystalline coating, and the wear resistance that it is good and solidity to corrosion mostly appear under the higher temperature.Wherein the Ni-W-P alloy layer after the annealing shows the wear-resisting and corrosion resisting property that is better than the Ni-P alloy layer, but the bonding force of Ni-P coating and metallic matrix then is higher than Ni-W-P coating.Will effectively improve the metallic surface performance, single coating is not ideal enough.Yet preparation Ni-P and Ni-W-P pairing gold plate when carrying out the high temperature annealing crystallization, may lose because of the diffusion of atom the meaning of two coating.In addition, also may because of the change of its weave construction, cause its mechanical property greatly to reduce to heat sensitive base material high temperature annealing.
(3) summary of the invention
The present invention is in order to remedy the deficiencies in the prior art, a kind of Ni-W-P, Ni-P pairing gold plate laser nano method are provided, the method can improve the bonding force of coating and metallic matrix, is unlikely again the performance of sacrificing its matrix, and can brings into play to greatest extent different coating advantage separately.
The present invention is achieved through the following technical solutions:
A kind of Ni-W-P, Ni-P pairing gold plate laser nano method, its special character is: may further comprise the steps:
(1) electroless plating: the base material of cleaning is placed plating in the coating bath that the Ni-P plating bath is housed, and the Ni-P bath temperature is 80-90 ℃, and the pH value is 4-5, takes out, and washed with de-ionized water obtains Ni-P coating; Then Ni-P coating is changed over to the coating bath plating that another fills the Ni-W-P plating bath, the Ni-W-P bath temperature is 90-98 ℃, and pH value 9-10 takes out, and rinses well with the water that flows and obtains Ni-W-P, Ni-P pairing gold plate;
(2) induced with laser: adopt semiconductor laser scan N i-W-P, Ni-P pairing gold plate, sweep velocity is 7-14mm/s, obtains the pairing gold plate of Ni-W-P, Ni-P nanometer.
Electroplate liquid formulation in Ni-W-P of the present invention, the Ni-P pairing gold plate laser nano method, step (1):
Contain in every liter of Ni-P plating bath:
Single nickel salt 20-25 g
Inferior sodium phosphate 20-24 g
Trisodium Citrate 6-10 g
Cadmium Sulphate 0.002-0.004 g
Lactic acid 11-15ml
Cerous compounds 0.003-0.008g;
Contain in every liter of Ni-W-P plating bath:
Single nickel salt 19-23 g
Inferior sodium phosphate 19-22 g
Trisodium Citrate 15-18 g
Citric acid 7-9 g
Ammonium chloride 13-15 g
Sodium wolframate 4-10 g
Cerous compounds 0.003-0.008g.
Ni-W-P of the present invention, Ni-P pairing gold plate laser nano method, the base material cleaning process in the step (1) is:
Base material is placed oil removing, rust cleaning medicament, and the pressure rotated flowing liquid that produces by chemical industry vortex pump, swirler cleans, and uses afterwards rich O
3Water is sheared turbulent flow and is cleaned; Place acidic activated liquid, it is acidic activated to carry out magnetic field, uses afterwards rich O
3Water is sheared turbulent flow and is cleaned; Place 70-90 ℃ deionized water to soak, change in the presoak at last and soak.Contain vinyl carbinol polyoxy alkyl oxide 1-10ml, trisodium phosphate 12-25g, trolamine 1-6ml, alkyl phosphate 1-10g, Starso 10-20g, ethylene glycol butyl ether 0.5-2ml, Sodium Benzoate 0.05-2g in wherein every liter of oil removing, the rust cleaning medicament; Contain oxalic acid 10-20g, phosphoric acid 5-15ml, ammonium bifluoride 1-10g, hydrogen peroxide 10-20ml, Sodium Benzoate 0.5-2g, wetting agent 0.5-2g in every liter of acidic activated liquid; Contain ammoniacal liquor 0.1-1.0 ml in every liter of presoak, Palladous chloride 0.0001-0.0002g, disodium ethylene diamine tetraacetate 0.0001-0.0002g.
Semiconductor laser power is 1.5kW in Ni-W-P of the present invention, the Ni-P pairing gold plate laser nano method, step (2), and beam spot size is the rectangle of 2.5mm * 3.5mm, and laser power is 150W, sweep velocity 8-10mm/s.
The thickness of Ni-P and Ni-W-P coating is respectively 16-18 μ m and 14-16 μ m in Ni-W-P of the present invention, the Ni-P pairing gold plate laser nano method, step (1), and the total thickness of Ni-P and Ni-W-P pairing gold plate is 30-34 μ m.
The invention has the beneficial effects as follows: the present invention designed with the electroless plating Ni-P noncrystalline alloy as with the transition layer of metallic matrix; the Ni-W-P alloy of mixed crystal attitude is as the Ni-W-P on top layer; Ni-P pairing gold plate; and employing need not argon shield; directly in air, carry out the new way of two coating crystallization (the not melting) preparation of induced with laser nanocrystalline material; this coating for metal surfaces laser nano technology directly carries out not only providing operability for actual production in air; the more important thing is that two coating of nanometer can improve the bonding force of coating and metallic matrix; be unlikely again the performance of sacrificing its matrix; and can bring into play to greatest extent different coating advantage separately, greatly improve the surface property of material.
(4) description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing.
Accompanying drawing 1 is laser scanning overlapping region synoptic diagram.
(5) embodiment
Embodiment 1:
1. the preparation of electroless plating Ni-W-P, Ni-P pairing gold plate
(1) plating bath forms
Contain in every liter of Ni-P plating bath: single nickel salt 20 g, inferior sodium phosphate 24 g, Trisodium Citrate 10 g, Cadmium Sulphate 0.002 g, lactic acid: 13ml, cerous compounds 0.003g;
Contain in every liter of Ni-W-P plating bath: single nickel salt 23 g, inferior sodium phosphate 19 g, Trisodium Citrate 17 g, citric acid 7g, ammonium chloride 15 g, sodium wolframate 10 g, cerous compounds 0.003g.
(2) base material plating technology
Cleaning before copper plating is processed: adopt the chemical combined disposable oil removing of eddy current, rust cleaning, be about to base material and place oil removing, rust cleaning medicament (prepare 1 liter of oil removing, the medicament that eliminates rust need vinyl carbinol polyoxy alkyl oxide 10ml, trisodium phosphate 25g, trolamine 5ml, alkyl phosphate 10g, Starso 15g, ethylene glycol butyl ether 0.5ml, Sodium Benzoate 2g to add water and make), produce the pressure rotated flowing liquid by chemical industry vortex pump, swirler, then efficient greasy dirt and corrosion of removing substrate surface use rich O
3Water is sheared turbulent flow and is cleaned, and utilizes rich O
3Water forms the Re(Reynolds number through swirler)〉5000 shearing turbulent flow, remove fast the residual dirt of substrate surface; Use acidic activated liquid (prepare 1 liter of acidic activated liquid need oxalic acid 10g, phosphatase 11 5ml, ammonium bifluoride 5g, hydrogen peroxide 10ml, Sodium Benzoate 2g, wetting agent 2g to add water make), under Actions of Gradient Magnetic Field, efficiently activate substrate surface, use again rich O
3Water is sheared turbulent flow and is cleaned, and removes the acid residue of substrate surface; Carry out at last pre-preg, soak 2min in 80 ℃ deionized water, changing 1 liter of presoak of presoak immersion 3min(preparation over to needs ammoniacal liquor 1.0ml, Palladous chloride 0.0002g, disodium ethylene diamine tetraacetate 0.0001g).
The electroless plating operation: the base material after the cleaning enters coating bath (the Ni-P bath temperature is 85 ℃, pH value 5), takes out behind the plating 1h, uses washed with de-ionized water; Then change another coating bath (the Ni-W-P bath temperature is 98 ℃, pH value 9) over to, take out behind the plating 1h, rinse well with the water that flows, check and accept (hot blast drying detects surface quality, warehouse-in).
By above-mentioned electroless copper deposition operation, the thickness of Ni-P and Ni-W-P coating is respectively 16-18 μ m and 14-16 μ m, and the chemical ingredients of two coating is determined such as table 1 by energy spectrum analysis.
The chemical ingredients of table 1 coating
| ? | Ni(weight percent %) | P(weight percent %) | W(weight percent %) |
| Ni-P | 90.7-90.5 | 9.3-9.5 | - |
| Ni-W-P | 89.1-88.8 | 6.0-6.2 | 4.9-5.0 |
2. laser induced chemical deposition Ni-W-P, Ni-P pairing gold plate nanometer technique
Adopt the semiconductor laser of 1.5kW continuous wavelength, the laser work parameter is: beam spot size is the rectangle of 2.5mm * 3.5mm, power 150W, and the sweep velocity scope is preferably 8-10mm/s between 7-14mm/s.
Scanning process is: the Ni-W-P, the Ni-P pairing gold plate that prepare are placed under the laser irradiation, bundle spot minor face carries out the single track shuttle-scanning at coating surface along its long limit in air, scan track has overlapping, shown in the first track in the accompanying drawing 1 and the second track, the hot spot scan track overlaps 0.5mm each other.
3. tissue signature and the performance of laser induced chemical deposition Ni-W-P, Ni-P pairing gold plate nanometer
(1) pairing gold plate laser nano degree
Under different scanning speed, the Ni that two coating laser crystallizations form reaches Ni mutually
3The mutually shared volume fraction of P is as shown in table 2.
Table 2 pair coating laser nano degree
In the table 2, in 10 to 8mm/s sweep velocity scope, Ni-P and Ni-W-P coating nanometer degree reach respectively 60-71% and 79-84%(percent by volume), and two coating laser nano top layer Ni-W-P has higher crystallization degree than transition layer Ni-P, but formed Ni
3It is similar that P accounts for the volume fraction of coating separately mutually, is approximately 26-28% for Ni-P coating, is approximately about 16% for Ni-W-P coating.The pairing gold plate that the laser crystallization parameter of the present invention's design is processed, this tissue signature of acquisition is the most reasonable.
(2) grain-size of pairing gold plate laser nano
Under different scanning speed, the grain-size of the two coating of laser nanoization is as shown in table 3.
The grain-size of the two coating of table 3 laser nanoization
In the table 3, Crystallization Phases Ni and Ni
3The crystal grain of P all is no more than 60nm.
(3) hardness of pairing gold plate laser nano and wear resistance
Under different scanning speed, the mechanical property of the two coating of laser nanoization is as shown in table 4.
The mechanical property of the two coating of table 4 laser nanoization
In the table 4, the hardness of the two coating of laser nanoization is higher than plated state (not laser nano) coating, wear rate not only is lower than plated state coating, and is lower than single Ni-W-P coating, illustrates that this coating for metal surfaces laser nano technology has special advantage for improving the material surface performance.
Laser scanning speed changes to 8mm/s from 10, is equivalent to Heating temperature and raises, and the crystallization degree of coating increases, and the grain-size of coating increases, but all surpasses nano level.The Ni of large-size
3The P phase factor increases the contact area with friction pair, and is conducive to improve the surface strengthening effect, therefore, and the wear rate of coating when sweep velocity is 8 mm/s (Ni-P, 4.8 * 10
-15m
3/ Nm; Ni-W-P, 1.5 * 10
-15m
3/ wear rate (Ni-P, 4.0 * 10 when Nm) being 10mm/s a little less than sweep velocity
-15m
3/ Nm; Ni-W-P, 1.3 * 10
-15m
3/ Nm), namely showed more better wear resistance.
The present invention mainly is hardness and the wear resistance that improvement is provided for the metallic surface, is particularly useful for bearing the surface modification of aluminium and the materials such as aluminium alloy, magnesium and magnesium alloy of high temperature.By designing special plating pre-treatment, electroplate liquid formulation and depositing operation, obtain the Amorphous Ni-P Alloy coating conduct of proper composition and the transition of matrix, improve its bonding strength; Obtain the mixed crystal attitude Ni-W-P coating of proper composition as the top layer; By formulating rational laser crystallization processing parameter, can make the excellent performance of pairing gold plate in its single alloy layer.Especially this coating for metal surfaces laser nano technology need not protective atmosphere, can directly carry out in air, and this provides operability for suitability for industrialized production.
Embodiment 2:
1. the preparation of electroless plating Ni-W-P, Ni-P pairing gold plate
(1) plating bath forms
Contain in every liter of Ni-P plating bath: single nickel salt 25 g, inferior sodium phosphate 20g, Trisodium Citrate 6 g, Cadmium Sulphate 0.004 g, lactic acid: 11ml, cerous compounds 0.008g;
Contain in every liter of Ni-W-P plating bath: single nickel salt 19 g, inferior sodium phosphate 22 g, Trisodium Citrate 18 g, citric acid 9 g, ammonium chloride 13 g, sodium wolframate 4 g, cerous compounds 0.008g.
(2) base material plating technology
Prepare 1 liter of oil removing, the rust cleaning medicament need vinyl carbinol polyoxy alkyl oxide 1ml, trisodium phosphate 12g, trolamine 6ml, alkyl phosphate 1g, Starso 20g, ethylene glycol butyl ether 2ml, Sodium Benzoate 0.05g to add water and make; Preparing 1 liter of acidic activated liquid needs oxalic acid 20g, phosphoric acid 5ml, ammonium bifluoride 10g, hydrogen peroxide 20ml, Sodium Benzoate 0.5g, wetting agent 0.5g to add water to make; Soak in 70-90 ℃ deionized water, change in the presoak and soak, need ammoniacal liquor 0.1ml and prepare 1 liter of presoak, Palladous chloride 0.0001g, disodium ethylene diamine tetraacetate 0.0002g add water and make.
The electroless plating operation: the Ni-P bath temperature is 90 ℃, pH value 4; The Ni-W-P bath temperature is 90 ℃, and the pH value is 10.
Other are identical with embodiment 1.
Embodiment 3:
1. the preparation of electroless plating Ni-W-P, Ni-P pairing gold plate
(1) plating bath forms
Contain in every liter of Ni-P plating bath: single nickel salt 22 g, inferior sodium phosphate 22 g, Trisodium Citrate 8 g, Cadmium Sulphate 0.003 g, lactic acid: 15ml, cerous compounds 0.006g;
Contain in every liter of Ni-W-P plating bath: single nickel salt 21 g, inferior sodium phosphate 20 g, Trisodium Citrate 15 g, citric acid 8 g, ammonium chloride 14 g, sodium wolframate 7 g, cerous compounds 0.006g.
(2) base material plating technology
Cleaning before copper plating is processed: prepare 1 liter of oil removing, the medicament that eliminates rust needs vinyl carbinol polyoxy alkyl oxide 5ml, trisodium phosphate 19g, trolamine 1ml, alkyl phosphate 5g, Starso 10g, ethylene glycol butyl ether 1.2ml, Sodium Benzoate 0.09g to add water and make; Preparing 1 liter of acidic activated liquid needs oxalic acid 15g, phosphatase 11 0ml, ammonium bifluoride 1g, hydrogen peroxide 15ml, Sodium Benzoate 1.3g, wetting agent 1.4g to add water to make; Preparing 1 liter of presoak needs ammoniacal liquor 0.5ml, and Palladous chloride 0.00015g, disodium ethylene diamine tetraacetate 0.00015g add water and make.
The electroless plating operation: the Ni-P bath temperature is 80 ℃, pH value 4.5; The Ni-W-P bath temperature is 94 ℃, pH value 9.5.
Other are identical with embodiment 1.
Claims (6)
1. a Ni-W-P, Ni-P pairing gold plate laser nano method is characterized in that: may further comprise the steps:
Electroless plating: the base material of cleaning is placed plating in the coating bath that the Ni-P plating bath is housed, and the Ni-P bath temperature is 80-90 ℃, and the pH value is 4-5, takes out, and washed with de-ionized water obtains Ni-P coating; Then Ni-P coating is changed over to the coating bath plating that another fills the Ni-W-P plating bath, the Ni-W-P bath temperature is 90-98 ℃, and pH value 9-10 takes out, and rinses well with the water that flows and obtains Ni-W-P, Ni-P pairing gold plate;
Induced with laser: adopt semiconductor laser scan N i-W-P, Ni-P pairing gold plate, sweep velocity is 7-14mm/s, obtains the pairing gold plate of Ni-W-P, Ni-P nanometer.
2. Ni-W-P according to claim 1, Ni-P pairing gold plate laser nano method is characterized in that: electroplate liquid formulation in the step (1):
Contain in every liter of Ni-P plating bath:
Single nickel salt 20-25 g
Inferior sodium phosphate 20-24 g
Trisodium Citrate 6-10 g
Cadmium Sulphate 0.002-0.004 g
Lactic acid 11-15ml
Cerous compounds 0.003-0.008g;
Contain in every liter of Ni-W-P plating bath:
Single nickel salt 19-23 g
Inferior sodium phosphate 19-22 g
Trisodium Citrate 15-18 g
Citric acid 7-9 g
Ammonium chloride 13-15 g
Sodium wolframate 4-10 g
Cerous compounds 0.003-0.008g.
3. Ni-W-P according to claim 1, Ni-P pairing gold plate laser nano method, it is characterized in that: the base material cleaning process is in the step (1): base material is placed oil removing, rust cleaning medicament, the pressure rotated flowing liquid that produces by chemical industry vortex pump, swirler cleans, and uses afterwards rich O
3Water is sheared turbulent flow and is cleaned, and places acidic activated liquid again, and it is acidic activated to carry out magnetic field, uses afterwards rich O
3Water is sheared turbulent flow and cleaned, and is last, place 70-90 ℃ deionized water to soak after, change in the presoak and soak.
4. Ni-W-P according to claim 3, Ni-P pairing gold plate laser nano method is characterized in that: contain in every liter of oil removing, the rust cleaning medicament:
Vinyl carbinol polyoxy alkyl oxide 1-10ml
Trisodium phosphate 12-25g
Trolamine 1-6ml
Alkyl phosphate 1-10g
Starso 10-20g
Ethylene glycol butyl ether 0.5-2ml
Sodium Benzoate 0.05-2g;
Contain in every liter of acidic activated liquid:
Oxalic acid 10-20g
Phosphoric acid 5-15ml
Ammonium bifluoride 1-10g
Hydrogen peroxide 10-20ml
Sodium Benzoate 0.5-2g
Wetting agent 0.5-2g;
Contain in every liter of presoak:
Ammoniacal liquor 0.1-1.0 ml
Palladous chloride 0.0001-0.0002g
Disodium ethylene diamine tetraacetate 0.0001-0.0002g.
5. Ni-W-P according to claim 1, Ni-P pairing gold plate laser nano method, it is characterized in that: semiconductor laser power is 1.5kW in the step (2), beam spot size is the rectangle of 2.5mm * 3.5mm, and laser power is 150W, sweep velocity 8-10mm/s.
6. Ni-W-P according to claim 1, Ni-P pairing gold plate laser nano method is characterized in that: the thickness of Ni-P and Ni-W-P coating is respectively 16-18 μ m, 14-16 μ m in the step (1).
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| CN105112824A (en) * | 2015-08-22 | 2015-12-02 | 慈溪市龙山汽配有限公司 | Method for preparing vehicle guide rail |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104264133A (en) * | 2014-09-26 | 2015-01-07 | 合肥工业大学 | Piston ring friction surface costing for internal combustion engine facing to bio-oil application and preparation method of piston ring friction surface costing for internal combustion engine |
| CN104264133B (en) * | 2014-09-26 | 2017-04-12 | 合肥工业大学 | Piston ring friction surface costing for internal combustion engine facing to bio-oil application and preparation method of piston ring friction surface costing for internal combustion engine |
| CN105112824A (en) * | 2015-08-22 | 2015-12-02 | 慈溪市龙山汽配有限公司 | Method for preparing vehicle guide rail |
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