CN107740074A - Ce Ni Mo P/Go Composite electroless deposit layers that a kind of ultrasonic wave aids in double complexing agents and preparation method thereof - Google Patents
Ce Ni Mo P/Go Composite electroless deposit layers that a kind of ultrasonic wave aids in double complexing agents and preparation method thereof Download PDFInfo
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- CN107740074A CN107740074A CN201711012857.5A CN201711012857A CN107740074A CN 107740074 A CN107740074 A CN 107740074A CN 201711012857 A CN201711012857 A CN 201711012857A CN 107740074 A CN107740074 A CN 107740074A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1662—Use of incorporated material in the solution or dispersion, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1664—Process features with additional means during the plating process
- C23C18/1666—Ultrasonics
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Abstract
Ce Ni Mo P/Go Composite electroless deposit layers aided in the invention discloses a kind of ultrasonic wave with double complexing agents and preparation method thereof.Present invention ultrasonic wave added in Ce Ni Mo P/Go Composite electroless deposit liquid by mild steel, Ce Ni Mo P/Go Composite electroless deposit layers are obtained in surface of low-carbon steel.Contain nickel sulfate hexahydrate, sodium molybdate, sodium hypophosphite, trisodium citrate, lactic acid, lead acetate cerium, graphene oxide and lauryl sodium sulfate in every liter of composite deposition liquid.The present invention matches somebody with somebody the trisodium citrate used in formula of liquid and the double complexing agent systems of lactic acid, is advantageous to accelerate the deposition of coating and improves performance；The catalysis of cerium itself is advantageous to the deposition reaction of plating solution with reproducibility.The composite sedimentary layer prepared by this method can effectively improve the performances such as the decay resistance of mild steel, case hardness, wearability, and can effectively solve the problem that face checking, the problems such as voidage is big.
Description
Technical field
The invention belongs to technical field of inorganic material, more particularly to a kind of Ce-Ni-Mo-P/Go Composite electroless deposits layer and
Its preparation method.
Background technology
Chemical plating is also referred to as autocatalytic plating, is to make in the case of without impressed current by the reducing agent properly worked as in plating solution
Metal ion is reduced into metal, and deposits to a kind of coating method of piece surface.Compared with other surfaces treatment technology, chemistry
Plating does not need additional power source, easy to operate, technique is simple, coating is uniform, porosity is low and outward appearance is good, and can plastics,
Deposited on a variety of nonmetal basal bodies such as ceramics, glass, and with excellent covering property, high adhesive force, it is excellent anticorrosive and
Anti-wear performance and excellent functional performance.
Chemical nickel plating, which is developed so far, have been approximately passed through 50 years, and the composition from most original plating solution is nickel salt, reducing agent, plating solution pole
It is unstable, no actual application value, it is made up of to plating solution nickel salt, reducing agent, complexing agent, the stability of plating solution increases, and enters
The practical sexual stage is entered, then has been made up of to plating solution nickel salt, reducing agent, complexing agent and stabilizer, the stability of plating solution further carries
Height, the industrial applications stage is entered, plating solution is by nickel salt, reducing agent, complexing agent, stabilizer, accelerator, buffering till now
Agent, brightener, wetting agent etc., the performance of plating solution further improve, commercial Application further genralrlization.With electroplating process phase
Than chemical nickel plating industrial applications initially as replacement Hard Chromium Coating, developing into corrosion resistance, wearability, anti-electromagnetism later
The functional coatings such as wave screen is covered, compact disk and obtain extensive use.Compared with electroplating technology, the coating of chemical nickel plating acquisition
Have many good qualities：Coating is uniform, and structure is compacted fine and closely woven, good corrosion resistance；Hardness is higher, has good wearability；Operation letter
Just, it is easy to grasp, slot allocation is very easy with adjusting；Plating solution service life is grown；Pollute low, nickel utilization rate height etc..
Graphene is because of its unique two-dimensional structure and comes by each in excellent electricity, optics, warm blood and mechanical performance, this year
The concern of big scientific research institution, have become the hot research problem in the fields such as chemistry, physics.A large amount of theoretical and experimental study tables
Bright, graphene and its derivative are in nano-device, semi-conducting material, biology sensor, information storage, solar cell and hydrogen storage
The fields such as material have potential significant application value.
Rare earth because it has the physical characteristics such as excellent photoelectromagnetic, can it is different with other materials component property, kind is numerous
More new materials, its most significant function are exactly to increase substantially the quality and performance of other products.Ce is as rare earth element
Middle abundance highest, key player is play in rare earth field.Because its own has certain catalysis and reproducibility, to changing
It is highly beneficial to learn coating.
But there is presently no the phase of the Ce-Ni-Mo-P/Go Composite electroless deposit layer preparation methods on ultrasonic assistant
Close research.Now refer to more than comparison be Ni-Mo-P research, but it is related to ultrasonic and rare earth doped element and oxygen
Graphite alkene.
The content of the invention
For above-mentioned technical problem of the prior art, it is an object of the invention to provide a kind of ultrasonic wave and double complexing agents
Ce-Ni-Mo-P/Go Composite electroless deposit layers of auxiliary and preparation method thereof.The present invention is aided in using ultrasonic wave and double complexing agents
Prepared by method, it is resistance to that obtained Ce-Ni-Mo-P/Go Composite electroless deposit layers solve surface of low-carbon steel of the prior art
Burn into crocking resistance and the not high technical problem of hardness.
Technical scheme is specifically described as follows.
A kind of preparation method of ultrasonic wave and the Ce-Ni-Mo-P/Go Composite electroless deposit layers of double complexing agent auxiliary, specifically
Step is as follows：Surface of low-carbon steel is pre-processed first, pretreated mild steel is then put into Ce-Ni-Mo-P/Goization
Learn in composite deposition liquid, plate 1h at a temperature of 80~88 DEG C and with ultrasonic wave added, finally take out and dry, obtain Ce-Ni-
Mo-P/Go Composite electroless deposit layers；Wherein in Ce-Ni-Mo-P/Go Composite electroless deposits liquid, often heaving hydrops includes such as the following group
Into component：25~50g nickel sulfate hexahydrates, 1~3g sodium molybdates, 10~40g sodium hypophosphites, 10~50g trisodium citrates, 5~
15g lactic acid, 0.01~0.2g lead acetates, 0.1~5g ceriums, 1~5g graphene oxides, 0.04~0.06g lauryl sodium sulfate.
In the present invention, the pretreatment of mild steel includes first being polished with coated abrasive surface, and then acetone cleaning removes in ultrasonic wave
Oil, the step of the activation of last chlorohydric acid pickling.
In the present invention, the pH value of Ce-Ni-Mo-P/Go Composite electroless deposit liquid is adjusted between 8~9 with sodium hydroxide.
In the present invention, in Ce-Ni-Mo-P/Go Composite electroless deposit liquid, the component that hydrops includes forming as follows is often heaved：
30~45g nickel sulfate hexahydrates, 2~3g sodium molybdates, 20~30g sodium hypophosphites, 20~40g trisodium citrates, 8~12g lactic acid,
0.05~0.15g lead acetates, 2~4g ceriums, 2~4g graphene oxides, 0.04~0.06g lauryl sodium sulfate.
In the present invention, the mass ratio of trisodium citrate and lactic acid is 11:4~13:Between 4.
In the present invention, the intensity of ultrasonic wave is between 100~300W, and frequency is between 40~80KHz.
In the present invention, drying temperature is between 20~25 DEG C.
The present invention also provides the Ce-Ni-Mo-P/Go Composite electroless deposit layers that a kind of above-mentioned preparation method obtains；Coating is in
Ball-type nodular structure.
A kind of Ce-Ni-Mo-P/Go Composite electroless deposits liquid of the present invention, added in original Ni-Mo-P deposits liquid
Rare earth element ce and Go, therefore the Composite electroless deposit liquid is applied in the plating of carbon steel work-piece surface, the Ce- being ultimately formed
The wearability enhancing of Ni-Mo-P/Go Composite electroless deposit layers.By Rare-Earth Ce and GO performance, carbon steel surface is significantly improved
The wearability of layer, corrosion resistance and hardness.
In the present invention, in the preparation of Ce-Ni-Mo-P/Go Composite electroless deposits layer, passed by ultrasonic wave in liquid medium
Cavitation effect caused by sowing time and mechanical shearing effect, it can effectively disperse nanometer in the nano combined depositing operation of chemistry
Grain, crystal grain thinning, so as to ensure that nano-composite plate has good structure property, improve coating crystal orientation, increase coating is bright
Degree, improve hardness and corrosion resistance etc..
Compared to the prior art, Ce-Ni-Mo-P/Go of the invention Composite electroless deposit layer is stronger corrosion resistance
Can, its corrosion resistance shown is better than simple Ni-Mo-P alloy-layers.In addition, introducing ultrasonic wave in preparation process, refine
Coating surface crystal grain and the content and uniformity for improving graphite oxide GO in coating.The trisodium citrate of use is double with lactic acid
Complexing agent system, be advantageous to accelerate the deposition of coating and improve performance；The catalysis of cerium itself is advantageous to plating solution with reproducibility
Deposition reaction.Lead acetate is advantageous to improve the life-span of composite sedimentary layer；Therefore, the Ce-Ni-Mo-P/Goization being ultimately formed
Learning composite sedimentary layer has excellent decay resistance, rub resistance and high rigidity.
Brief description of the drawings
Fig. 1 is the SEM figures for the sample A that embodiment 2 obtains.
Fig. 2 is the SEM figures for the sample B that embodiment 4 obtains.
Fig. 3 is the SEM figures for the sample C that embodiment 6 obtains.
Embodiment
Technical scheme is described in detail with reference to embodiment.
Embodiment 1
A kind of Ce-Ni-Mo-P/Go Composite electroless deposits liquid, calculated by every liter of solution, it is formed and content is as follows：
By nickel sulfate hexahydrate, sodium molybdate, sodium hypophosphite, trisodium citrate, lactic acid, cerium, lead acetate, graphene oxide, ten
Sodium dialkyl sulfate is added sequentially to dissolve in deionized water, then adds sodium hydroxide and adjusts pH value to 9.5, that is, obtains Ce-
Ni-Mo-P/Go Composite electroless deposit liquid.
Embodiment 2
The Composite electroless deposit liquid of the gained of embodiment 1 is applied to surface of low-carbon steel to form Ce-Ni-Mo-P/Go chemistry
Composite sedimentary layer, specifically comprise the following steps：
(1) pretreatment of low-carbon steel workpiece surface, the surface of low-carbon steel workpiece is removed through 3,5, No. 7 coated abrasive workings successively
Dirt, then with acetone in the case where ultrasonic wave aids in clearly degreasing 1 minute, with deionized water rinsing 10 seconds；Then mass percent is used again
The chlorohydric acid pickling 15s of concentration 10%, with deionized water rinsing 10 seconds.
(2) the pretreated low-carbon steel workpiece of step 1 is put into the Ce-Ni-Mo-P/Go Composite electroless deposit liquid prepared
In, solution temperature is controlled at 85 DEG C, ultrasound intensity takes out in 150W, supersonic frequency after 60KHZ, 1h, is washed with deionized water
After net, dry up at normal temperatures, that is, obtain to surface and be coated with the sample A of Ce-Ni-Mo-P/Go Composite electroless deposit layers.Sample A SEM
Figure coating ball-type nodositas structure unobvious and has crack as shown in figure 1, result is shown.By test, its hardness only has
366HV, corrosion electric current density (3.5%NaCl) are 1.044 × 10-5A/cm2。
Embodiment 3
A kind of Ce-Ni-Mo-P/Go Composite electroless deposits liquid, calculated by every liter of solution, it is formed and content is as follows：
By nickel sulfate hexahydrate, sodium molybdate, sodium hypophosphite, trisodium citrate, lactic acid, cerium, lead acetate, graphene oxide, ten
Sodium dialkyl sulfate is added sequentially to dissolve in deionized water, then adds sodium hydroxide and adjusts pH value to 9.5, that is, obtains Ce-
Ni-Mo-P/Go Composite electroless deposit liquid.
Embodiment 4
The Composite electroless deposit liquid of the gained of embodiment 3 is applied to surface of low-carbon steel to form Ce-Ni-Mo-P/Go chemistry
Composite sedimentary layer, specifically comprise the following steps：
(1) pretreatment of low-carbon steel workpiece surface, the surface of low-carbon steel workpiece is removed through 3,5, No. 7 coated abrasive workings successively
Dirt, then with acetone in the case where ultrasonic wave aids in clearly degreasing 1 minute, with deionized water rinsing 10 seconds；Then mass percent is used again
The chlorohydric acid pickling 15s of concentration 10%, with deionized water rinsing 10 seconds.
(2) the pretreated low-carbon steel workpiece of step 1 is put into the Ce-Ni-Mo-P/Go Composite electroless deposit liquid prepared
In, solution temperature is controlled at 85 DEG C, ultrasound intensity takes out in 200W, supersonic frequency after 60KHZ, 1h, is washed with deionized water
After net, dry up at normal temperatures, that is, obtain to surface and be coated with the sample B of Ce-Ni-Mo-P/Go Composite electroless deposit layers.Sample B SEM
As shown in Fig. 2 result shows coating nodular structure spherical in shape.By test, its hardness has reached 886HV, corrosion electric current density
(3.5%NaCl) is 7.887 × 10-6A/cm2。
Embodiment 5
A kind of Ce-Ni-Mo-P/Go Composite electroless deposits liquid, calculated by every liter of solution, it is formed and content is as follows：
By nickel sulfate hexahydrate, sodium molybdate, sodium hypophosphite, trisodium citrate, lactic acid, cerium, lead acetate, graphene oxide, ten
Sodium dialkyl sulfate is added sequentially to dissolve in deionized water, then adds sodium hydroxide and adjusts pH value to 9.5, that is, obtains Ce-
Ni-Mo-P/Go Composite electroless deposit liquid.
Embodiment 6
The Composite electroless deposit liquid of the gained of embodiment 5 is applied to surface of low-carbon steel to form Ce-Ni-Mo-P/Go chemistry
Composite sedimentary layer, specifically comprise the following steps：
(1) pretreatment of low-carbon steel workpiece surface, the surface of low-carbon steel workpiece is removed through 3,5, No. 7 coated abrasive workings successively
Dirt, then with acetone in the case where ultrasonic wave aids in clearly degreasing 1 minute, with deionized water rinsing 10 seconds；Then mass percent is used again
The chlorohydric acid pickling 15s of concentration 10%, with deionized water rinsing 10 seconds.
(2) the pretreated low-carbon steel workpiece of step 1 is put into the Ce-Ni-Mo-P/Go Composite electroless deposit liquid prepared
In, solution temperature is controlled at 85 DEG C, ultrasound intensity takes out in 200W, supersonic frequency after 60KHZ, 1h, is washed with deionized water
After net, dry up at normal temperatures, that is, obtain to surface and be coated with the sample C of Ce-Ni-Mo-P/Go Composite electroless deposit layers.Sample C SEM
For figure as shown in figure 3, result is shown, coating is in ball-type nodular structure.By test, its hardness has reached 855HV, and corrosion current is close
It is 5.819 × 10 to spend (3.5%NaCl)-6A/cm2。
Claims (9)
1. the preparation method of a kind of ultrasonic wave and the Ce-Ni-Mo-P/Go Composite electroless deposit layers of double complexing agent auxiliary, its feature
It is, comprises the following steps that：Surface of low-carbon steel is pre-processed first, mild steel after pretreatment is then put into Ce-Ni-
It is ultrasonic at a temperature of 85~88 DEG C in Mo-P/Go Composite electroless deposit liquid, finally take out and dry, obtain Ce-Ni-Mo-P/
Go Composite electroless deposit layers；Wherein：In Ce-Ni-Mo-P/Go Composite electroless deposit liquid, often heaving hydrops includes what is formed as follows
Component：25~50g nickel sulfate hexahydrates, 1~3g sodium molybdates, 10~40g sodium hypophosphites, 10~50g trisodium citrates, 5~15g breasts
Acid, 0.01~0.2g lead acetates, 0.1~5g ceriums, 1~5g graphene oxides, 0.04~0.06g lauryl sodium sulfate.
2. preparation method as claimed in claim 1, it is characterised in that the pretreatment of mild steel includes first surface polishing degreasing,
The step of acetone cleans oil removing and finally activated with chlorohydric acid pickling in ultrasonic wave again.
3. preparation method as claimed in claim 1, it is characterised in that adjust Ce-Ni-Mo-P/Goization with sodium hydroxide solution
The pH value of composite deposition liquid is learned between 9~10.
4. preparation method as claimed in claim 1, it is characterised in that in Ce-Ni-Mo-P/Go Composite electroless deposit liquid, every liter
Deposition liquid includes the component formed as follows：30~45g nickel sulfate hexahydrates, 2~3g sodium molybdates, 20~30g sodium hypophosphites, 20~
40g trisodium citrates, 8~12g lactic acid, 0.05~0.15g lead acetates, 2~4g ceriums, 2~4g graphene oxides, 0.04~
0.06g lauryl sodium sulfate.
5. preparation method as claimed in claim 1, it is characterised in that the mass ratio of trisodium citrate and lactic acid is 11:4~
13:4。
6. preparation method as claimed in claim 1, it is characterised in that ultrasonic intensity is between 100~300W, and frequency is 40
Between~80KHz.
7. preparation method as claimed in claim 1, it is characterised in that drying temperature is between 20~25 DEG C.
A kind of 8. Ce-Ni-Mo-P/Go Composite electroless deposit layers that preparation method as described in one of claim 1-7 obtains.
9. Ce-Ni-Mo-P/Go Composite electroless deposits layer as claimed in claim 8, it is characterised in that coating is in ball-type tubercle
Structure.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441847A (en) * | 2018-05-29 | 2018-08-24 | 上海应用技术大学 | A kind of base steel super hydrophobic surface and preparation method thereof based on Ni-Mo-P chemical depositions |
| CN108677173A (en) * | 2018-05-29 | 2018-10-19 | 上海应用技术大学 | A kind of Ni-Mo-P/MoS of ultrasonic wave auxiliary2Composite electroless deposit layer and preparation method thereof |
| CN114855151A (en) * | 2022-05-09 | 2022-08-05 | 广东省科学院新材料研究所 | Chemical composite plating solution and preparation method thereof, and chemical composite plating layer and preparation method thereof |
| CN114952073A (en) * | 2022-05-09 | 2022-08-30 | 广西大学 | Preparation method of nickel-plated graphene reinforced tin-based soldering paste |
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| CN106637158A (en) * | 2016-12-27 | 2017-05-10 | 上海应用技术大学 | Nd-Ni-Mo-P/Go chemical composite deposition layer and preparation method thereof |
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