CN103290458B - The preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite - Google Patents
The preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite Download PDFInfo
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- CN103290458B CN103290458B CN201310211302.9A CN201310211302A CN103290458B CN 103290458 B CN103290458 B CN 103290458B CN 201310211302 A CN201310211302 A CN 201310211302A CN 103290458 B CN103290458 B CN 103290458B
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Abstract
The invention discloses a kind of preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite, comprise the following steps: A) basic nickel plating solution preparation: by NiSO
46H
2o, H
3bO
3and NiCl
26H
2o mixes and is mixed with plating solution, obtains basic nickel plating solution; B) nano particle pre-treatment: by attapulgite clay nano particle before plating through ultrasonic oscillation 30min, and then mechanical stirring 0.5-1h; C) composite plating solution preparation: by step B) in be added in basic nickel plating solution through the attapulgite clay nano particle of ultrasonic oscillation process, ultrasonic oscillation 30min, mechanical stirring 0.5-1h, obtain composite plating solution; D) prepare composite deposite: energising, when coating reaches required thickness, stop energising, take out sample, plating terminates, and obtains composite deposite.Adopt technical scheme of the present invention, nano particle can be impelled to disperse well in the plating solution, make the crystal grain more refinement of composite deposite, improve microhardness and the wear resisting property of composite deposite.
Description
Technical field
The invention belongs to composite deposite preparing technical field, particularly relate to the preparation field of nanometer insoluble solid Particles dispersed coating, be specifically related to a kind of preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite.
Background technology
As everyone knows, general material corrosion and wearing and tearing mostly occur in surface.Adopt effective preventive means, at least can reduce corrosion loss 15% ~ 35%, reduce wear loss about 1/3.Surface coating technique is high-quality, the efficient and effective means of increasing economic efficiency.As the composite plating technology of one of surface coating technique, because its equipment is simple, easy to operate, speed is fast, temperature is low, cheap, be easy to the advantages such as control, can improve that metallic surface is corrosion-resistant, wear-resisting, antioxidant property, and give finishing property outward appearance, be used widely in fields such as aviation, electronics, machinery, chemical industry, metallurgy and nuclear energy.
Nickel coating, owing to having good corrosion resistance nature and mechanical property, has purposes widely at protection finishing property coating and functional coating.Along with the change of structural parts working conditions and the variation of function, single nickel coating can not meet service requirements.With nickel metal for matrix metal, add micron particle in plating solution and prepare composite deposite, especially, after the difficult problem that nano particle is produced solves, substitute composite deposite prepared by micron particle with nano particle, the nano-composite plate more more excellent than micron composite deposite properties can be prepared.The mechanical property performance of composite deposite depends on the grain-size of the endocorpuscular deposition of coating and matrix metal.The grain-size of matrix metal crystallization is less, and the mechanical property of composite deposite is better, also improves the performance such as anti-oxidant of coating simultaneously.
At present, the main method of refinement matrix metal grain-size has: the refinement realizing coating grain-size by improving the measures such as the compound (as Palladous chloride) of cathode current density and interpolation rare precious metals.By increasing the cathode current density in electroplating process, matrix metal sedimentation velocity increases, and coating crystal grain obtains refinement, but the deposition of nano particle reduces on the contrary; Add scarce metallic compound refinement coating crystal grain in plating solution, obviously increase the cost of preparation of coatings.
Attapulgite is a kind of crystalloid hydrous magnesium aluminium silicate mineral, has unique chain stratiform constitutional features, in its structure, there is crystal lattice, the Na containing non-quantitative in crystal
+, Ca
2+, Fe
3+, Al
3+, crystal is needle-like, threadiness or fiber collection shape.Because attapulgite clay has special fibrous texture, unique good colloidal property and the higher adsorption bleaching ability such as dispersion, heatproof, Salt And Alkali Tolerance, being widely used in the industries such as food, agricultural, light industry.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of method preparing the attapulgite modified nickel base nanometer ceramic particle composite deposite that Ni-based matter metal grain size is little, composite deposite mechanical property is high.
In order to solve the problem, the technical solution adopted in the present invention is as follows: the preparation method of this attapulgite modified nickel base nanometer ceramic particle composite deposite, comprises the following steps:
A) basic nickel plating solution preparation: by NiSO
46H
2o, H
3bO
3and NiCl
26H
2o mixes and is mixed with plating solution, obtains basic nickel plating solution;
B) nano particle pre-treatment: by attapulgite clay nano particle before plating through ultrasonic oscillation 30min, and then mechanical stirring 1h;
C) composite plating solution preparation: will through step B) pretreated attapulgite clay nano particle is added in basic nickel plating solution, and ultrasonic oscillation 30min, mechanical stirring 0.5-1h, obtain composite plating solution;
D) prepare composite deposite: energising, when coating reaches required thickness, stop energising, take out sample, plating terminates, and obtains composite deposite.
Further improvement is, NiSO
46H
2o250g/L, H
3bO
340g/L, NiCl
26H
2o50g/L.
Further improvement is, described step B) in also include nano-ceramic particle, described nano-ceramic particle is through ultrasonic oscillation 30min, and then mechanical stirring 0.5-1h;
Described step C) be: will through step B) pretreated nano-ceramic particle is added to steps A) basic nickel plating solution in, churned mechanicallyly carry out ultrasonic oscillation process 0.5-1h simultaneously; Simultaneously will through step B) pretreated attapulgite clay nano particle is added in basic nickel plating solution, and ultrasonic oscillation 30min, mechanical stirring 0.5-1h, obtain composite plating bath.
Further improvement is, described step C) in nano-ceramic particle, attapulgite clay nano particle in electroplate liquid, be in dispersion, suspended state.
Further improvement is, described nano-ceramic particle is Al
2o
3nano-ceramic particle or TiC nano-ceramic particle.
Further improvement is, the step B described) in, the particle diameter of described attapulgite clay nano particle is 40nm, concentration 0.5 ~ 3.0g/L in the plating solution.
Further improvement is, described step D) in, when current density is 2A/dm
2time, rotating speed is 200r/min, and electroplating time is 10h, and thickness of multiple plating is 210 ~ 220 μm.
Compared to prior art, beneficial effect of the present invention is:
(1) the present invention has very large difference owing to preparing plating solution with existing nano-composite plate on plating solution composition, be mainly manifested in nano-composite plate preparation process, attapulgite is added in plating solution, play heterogeneous nuclei and suspension effect, the grain-size of composite deposite mesostroma metal significantly reduces, and hardness, wear resisting property and antioxidant property improve;
(2) another obvious advantage of the present invention is, additive attapulgite wide material sources, and cheap, environmental protection;
(3) the nano ceramics composite deposite prepared of the present invention, has the advantage that compactness is good.
Accompanying drawing explanation
Fig. 1 is the Ni/Al of no concave-convex rod soil preparation in plating solution
2o
3nano-composite plate surface microscopic topographic;
Fig. 2 adds Ni/Al prepared by 0.5g/L attapulgite in plating solution
2o
3nano-composite plate surface microscopic topographic;
Fig. 3 is the Ni/TiC nano-composite plate surface microscopic topographic of no concave-convex rod soil preparation in plating solution;
Fig. 4 is the Ni/TiC nano-composite plate surface microscopic topographic prepared after adding 0.5g/L attapulgite in plating solution;
Fig. 5 is the Ni coating surface microscopic appearance of no concave-convex rod soil preparation in plating solution;
Fig. 6 adds Ni coating surface microscopic appearance prepared by 0.5g/L attapulgite in plating solution.
Embodiment
Below in conjunction with specific embodiment, explanation is further explained to the present invention:
Embodiment 1:
The preparation method of this attapulgite modified nickel base nanometer ceramic particle composite deposite, comprises the following steps:
A) basic nickel plating solution preparation: by NiSO
46H
2o, H
3bO
3and NiCl
26H
2o mixes and is mixed with 2L plating solution, obtains basic nickel plating solution;
B) nano particle pre-treatment: Al
2o
3nano-ceramic particle ultrasonic oscillation 30min, and then mechanical stirring 1h, by attapulgite clay nano particle before plating through ultrasonic oscillation 30min, and then mechanical stirring 1h;
C) composite plating solution preparation: by step B) in through pretreated Al
2o
3nano-ceramic particle is added to steps A) in basic nickel plating solution in, Al
2o
3nano-ceramic particle concentration is 6g/L; Churned mechanicallyly carry out ultrasonic oscillation process 0.5h simultaneously, simultaneously by step B) in be added in basic nickel plating solution through the attapulgite clay nano particle of ultrasonic oscillation process, ultrasonic oscillation 30min, mechanical stirring 1h, obtain composite plating bath, it is 0.5g/L that attapulgite clay nano particle adds concentration;
D) composite deposite is prepared: energising, when current density is 2A/dm
2time, rotating speed is 200r/min, and electroplating time is 10h, and thickness of multiple plating is 210 μm, stops energising, takes out sample, and plating terminates, and obtains composite deposite.
Utilize attapulgite in composite plating process, to Al
2o
3nanoparticle suspension effect, plays heterogeneous nuclei during matrix nickel metallic crystal simultaneously.Finally obtain the Ni/Al that crystal grain is tiny, surface compact, antioxidant property are good
2o
3nano-composite plate.
Be illustrated in figure 2 in plating solution the Ni/Al adding 0.5g/L attapulgite clay nano particle and prepare
2o
3nano-composite plate surface microscopic topographic.
Embodiment 2:
Embodiment 2 is the comparative examples as embodiment 1, is not both, and does not add attapulgite clay nano particle, as shown in Figure 1, is the Ni/Al of no concave-convex rod soil preparation in plating solution
2o
3nano-composite plate surface microscopic topographic.
Embodiment 3:
Concrete steps are with embodiment 1, and difference adds TiC nano-ceramic particle in plating solution, is not Al
2o
3nano-ceramic particle, base material is Q235, and the composition of electroplate liquid is NiSO
4.6H
2o250g/L, H
3bO
340g/L, NiCl
26H
2o50g/L, it is 0.5g/L that attapulgite clay nano particle adds interpolation concentration, the size of TiC nano-ceramic particle is 40nm, add-on is 9g/L, thickness of coating reaches 210 μm, and plating terminates, and finally obtains surface compact, hardness is high, Ni/TiC nano-composite plate that wear resisting property is good, as shown in Figure 4, the Ni/TiC nano-composite plate surface microscopic topographic for preparing after adding 0.5g/L attapulgite clay nano particle in plating solution.
Embodiment 4:
Concrete steps are with embodiment 3, and difference does not add attapulgite clay nano particle in plating solution, as shown in Figure 3, are Ni/TiC nano-composite plate surface microscopic topographic prepared by the native nano particle of no concave-convex rod in plating solution.
Embodiment 5:
Concrete steps are with embodiment 1, and difference does not add nano-ceramic particle in plating solution, and base material is Q235, and the composition of electroplate liquid is NiSO
46H
2o250g/L, H
3bO
340g/L, NiCl
26H
2o50g/L, it is 0.5g/L that attapulgite clay nano particle adds interpolation concentration, after ultrasonic oscillation 30min, mechanical stirring 1h process, prepare composite deposite.Plating solution rotating speed is 200r/min, and current density is 2A/dm
2, plating 600min, thickness of coating reaches 200 μm, and plating terminates.Last to having the pure Ni coating that crystal grain is tiny, wear resisting property is good.
As shown in Figure 6, for adding Ni coating surface microscopic appearance prepared by 0.5g/L attapulgite clay nano particle in plating solution.
Embodiment 6:
Concrete steps are with embodiment 5, and difference does not add attapulgite clay nano particle in plating solution, as shown in Figure 5, are Ni coating surface microscopic appearance prepared by the native nano particle of no concave-convex rod in plating solution.
Adopt technical scheme of the present invention, nano particle can be impelled to disperse well in the plating solution, make the crystal grain more refinement of composite deposite, improve microhardness and the wear resisting property of composite deposite, equally distributed nano particle is while the grain refining of accelerating oxidation film, improve the growth mechanism of oxide film, thus improve the high temperature oxidation resistance of composite deposite.Electro-plating method technique of the present invention is simple, and attapulgite wide material sources are with low cost, conveniently apply.
Claims (1)
1. a preparation method for attapulgite modified nickel base nanometer ceramic particle composite deposite, comprises the following steps:
A) basic nickel plating solution preparation: by NiSO
46H
2o, H
3bO
3and NiCl
26H
2o mixes and is mixed with plating solution, obtains basic nickel plating solution;
B) nano particle pre-treatment: by attapulgite clay nano particle before plating through ultrasonic oscillation 30min, and then mechanical stirring 0.5-1h;
C) composite plating solution preparation: will through step B) pretreated attapulgite clay nano particle is added in basic nickel plating solution, and ultrasonic oscillation 30min, mechanical stirring 0.5-1h, obtain composite plating solution;
D) prepare composite deposite: energising, when coating reaches required thickness, stop energising, take out sample, plating terminates, and obtains composite deposite; In steps A) in, NiSO
46H
2o250g/L, H
3bO
340g/L, NiCl
26H
2o50g/L; Described step B) in also include nano-ceramic particle, described nano-ceramic particle is through ultrasonic oscillation 30min, and then mechanical stirring 0.5-1h;
Described step C) be: will through step B) pretreated nano-ceramic particle is added to steps A) basic nickel plating solution in, churned mechanicallyly carry out ultrasonic oscillation process 0.5-1h simultaneously; Simultaneously will through step B) pretreated attapulgite clay nano particle is added in basic nickel plating solution, and ultrasonic oscillation 30min, mechanical stirring 0.5-1h, obtain composite plating bath;
Described step C) in nano-ceramic particle, attapulgite clay nano particle in electroplate liquid, be in dispersion, suspended state; Described nano-ceramic particle is Al
2o
3nano-ceramic particle or TiC nano-ceramic particle; Step B described) in, the particle diameter of described attapulgite clay nano particle is 40nm, concentration 0.5 ~ 3.0g/L in the plating solution; Described step D) in, when current density is 2A/dm
2time, rotating speed is 200r/min, and electroplating time is 10h, and thickness of multiple plating is 210 ~ 220 μm.
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| CN201310211302.9A CN103290458B (en) | 2013-07-11 | 2013-07-11 | The preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite |
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| CN103290458A CN103290458A (en) | 2013-09-11 |
| CN103290458B true CN103290458B (en) | 2015-12-09 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556253A (en) * | 2004-01-06 | 2004-12-22 | 上海维安热电材料股份有限公司 | Preparation method of composite cladding material and equipment |
| CN1807702A (en) * | 2005-12-19 | 2006-07-26 | 吉林大学 | Process for preparing gradient nano compound coating on powder metallurgy part surface |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55161090A (en) * | 1979-06-04 | 1980-12-15 | Hitachi Ltd | Dispersion plating solution of nickel-tungsten alloy |
| EP0441636B1 (en) * | 1990-02-09 | 1994-06-22 | Nihon Parkerizing Co., Ltd. | Process for surface treating titanium-containing metallic material |
| KR100709290B1 (en) * | 2005-11-15 | 2007-04-19 | 한국과학기술연구원 | Composite layer including metal and inorganic powders and method for manufacturing the same |
-
2013
- 2013-07-11 CN CN201310211302.9A patent/CN103290458B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556253A (en) * | 2004-01-06 | 2004-12-22 | 上海维安热电材料股份有限公司 | Preparation method of composite cladding material and equipment |
| CN1807702A (en) * | 2005-12-19 | 2006-07-26 | 吉林大学 | Process for preparing gradient nano compound coating on powder metallurgy part surface |
Non-Patent Citations (1)
| Title |
|---|
| "凹凸棒土研究与应用进展";马玉恒等，;《材料导报》;20060915;第20卷(第9期);第43-46页 * |
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