CN103290458A - Preparation method of attapulgite modified nickel-based nano ceramic particle composite coating - Google Patents
Preparation method of attapulgite modified nickel-based nano ceramic particle composite coating Download PDFInfo
- Publication number
- CN103290458A CN103290458A CN2013102113029A CN201310211302A CN103290458A CN 103290458 A CN103290458 A CN 103290458A CN 2013102113029 A CN2013102113029 A CN 2013102113029A CN 201310211302 A CN201310211302 A CN 201310211302A CN 103290458 A CN103290458 A CN 103290458A
- Authority
- CN
- China
- Prior art keywords
- preparation
- nano
- ceramic particle
- attapulgite
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses a preparation method of an attapulgite modified nickel-based nano ceramic particle composite coating. The preparation method comprises the following steps of: (A) preparation of a basic electro nickeling solution preparation: uniformly mixing NiSO4.6H2O, H3BO3 and NiCl2.6H2O to prepare a plating solution which is the basic electro nickeling solution; (B) pretreatment of nano-particles: performing ultrasonic oscillation on attapulgite nano-particles for 30 minutes before plating and then mechanically stirring for 0.5-1 hour; (C) preparation of a composite electroplating solution preparation: adding the attapulgite nano-particles subjected to the ultrasonic oscillation in the step (B) into the basic electro nickeling solution, performing ultrasonic oscillation for 30 minutes, and mechanically stirring for 0.5-1 hour to obtain the composite electroplating solution; and (D) preparation of a composite coating: electrifying, stopping electrifying when the coating reaches a required thickness, taking a test sample out, and ending electroplating to obtain the composite coating. By adopting the technical scheme of the invention, the nano particles can be promoted to be well dispersed in the electroplating solution to ensure that the grains of the composite coating are finer, and the micro-hardness and wear resistance of the composite coating are improved.
Description
Technical field
The invention belongs to the composite deposite preparing technical field, relate in particular to the preparation field of nanometer insoluble solid particle composite deposite, be specifically related to a kind of preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite.
Background technology
As everyone knows, the corrosion of general material and wearing and tearing mostly occur in the surface.Adopt effective preventive means, can reduce corrosion loss 15% ~ 35% at least, loss about 1/3 reduces wear.Surface coating technique is high-quality, the efficient and effective means of increasing economic efficiency.Composite plating technology as one of surface coating technique, because its equipment is simple, easy to operate, speed is fast, temperature is low, cheap, be easy to advantage such as control, can improve that the 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 has purposes widely owing to have excellent corrosion resisting performance and mechanical property at protection finishing property coating and functional coating.Along with the variation of structural parts working conditions and the variation of function, single nickel coating can not satisfy service requirements.Be matrix metal with the nickel metal, add micron particle in the plating bath and prepare composite deposite, especially after the difficult problem solution that nano particle is produced, substitute the composite deposite that micron particle prepares with nano particle, can prepare than the more excellent nano-composite plate of the every performance of micron composite deposite.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 more little, and the mechanical property of composite deposite is more good, also improves simultaneously the performance such as anti-oxidant of coating.
At present, the main method of refinement matrix metal grain-size has: by improving cathode current density and adding the refinement of compound measures such as (as Palladous chlorides) the realization coating grain-size of rare precious metals.By increasing the cathode current density in the electroplating process, the 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 the plating bath, obviously increase the cost of coating preparation.
Attapulgite is a kind of crystalloid hydrous magnesium aluminium silicate mineral, has unique chain laminate structure feature, has the lattice displacement in its structure, contains the Na of non-quantitative in the crystal
+, Ca
2+, Fe
3+, Al
3+, crystal is needle-like, fibrous or fiber collection shape.Because attapulgite clay has good colloidal property such as special fibrous texture, unique dispersion, heatproof, salt tolerant alkali and higher adsorption bleaching ability, being widely used in industries such as food, agricultural, light industry.
Summary of the invention
The technical problem to be solved in the present invention is that a kind of method for preparing the attapulgite modified nickel base nanometer ceramic particle composite deposite that Ni-based matter metal grain size is little, the composite deposite mechanical property is high is provided.
In order to address the above 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 may further comprise the steps:
A) basic electronickelling solution preparation: with NiSO
46H
2O, H
3BO
3And NiCl
26H
2O mixes and is mixed with plating bath, obtains basic electronickelling solution;
B) nano particle pre-treatment: with the attapulgite clay nano particle before plating through ultrasonic oscillation 30min, and then mechanical stirring 1h;
C) composite plating solution preparation: will be through step B) pretreated attapulgite clay nano particle is added in the basic electronickelling solution, ultrasonic oscillation 30min, and mechanical stirring 0.5-1h obtains composite plating solution;
D) preparation composite deposite: energising, when coating reaches required thickness, stop energising, take out sample, electroplate and finish, obtain composite deposite.
Further improve and be NiSO
46H
2O 250g/L, H
3BO
340g/L, NiCl
26H
2O 50g/L.
Further improve and be 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 be through step B) pretreated nano-ceramic particle is added to steps A) basic electronickelling solution in, the churned mechanically ultrasonic oscillation that carries out is simultaneously handled 0.5-1h; Simultaneously will be through step B) pretreated attapulgite clay nano particle is added in the basic electronickelling solution, ultrasonic oscillation 30min, mechanical stirring 0.5-1h obtains composite plating bath.
Further improve and be described step C) in nano-ceramic particle, attapulgite clay nano particle in electroplate liquid, be in dispersion, suspended state.
Further improve and be that described nano-ceramic particle is Al
2O
3Nano-ceramic particle or TiC nano-ceramic particle.
Further improve being, at described step B) in, described attapulgite clay nano particle grain size is 40nm, concentration 0.5 ~ 3.0 g/L in plating bath.
Further improve and be described step D) in, when current density is 2A/dm
2The time, rotating speed is 200 r/min, and electroplating time is 10h, and thickness of multiple plating is 210 ~ 220 μ m.
Than prior art, beneficial effect of the present invention is:
(1) the present invention has very big difference owing to prepare plating bath with existing nano-composite plate on plating bath is formed, mainly show in the nano-composite plate preparation process, add attapulgite in the plating bath, play heterogeneous core 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 also cheap, environmental protection;
(3) the nano ceramics composite deposite of the present invention's preparation has the good advantage of compactness.
Description of drawings
Fig. 1 is the Ni/ Al of no concave-convex rod soil preparation in the plating bath
2O
3The nano-composite plate surface microscopic topographic;
Fig. 2 is the Ni/ Al that adds the preparation of 0.5g/L attapulgite in the plating bath
2O
3The nano-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 the plating bath;
Fig. 4 is for adding the Ni/TiC nano-composite plate surface microscopic topographic for preparing behind the 0.5g/L attapulgite in the plating bath;
Fig. 5 is the Ni coating surface microscopic appearance of no concave-convex rod soil preparation in the plating bath;
Fig. 6 is the Ni coating surface microscopic appearance that adds the preparation of 0.5g/L attapulgite in the plating bath.
Embodiment
Come the present invention is further explained below in conjunction with specific embodiment:
Embodiment 1:
The preparation method of this attapulgite modified nickel base nanometer ceramic particle composite deposite may further comprise the steps:
A) basic electronickelling solution preparation: with NiSO
46H
2O, H
3BO
3And NiCl
26H
2O mixes and is mixed with the 2L plating bath, obtains basic electronickelling solution;
B) nano particle pre-treatment: Al
2O
3Nano-ceramic particle ultrasonic oscillation 30min, and then mechanical stirring 1h, with the attapulgite clay nano particle before plating through ultrasonic oscillation 30min, and then mechanical stirring 1h;
C) the pretreated Al of process composite plating solution preparation: with step B)
2O
3Nano-ceramic particle is added to steps A) in basic electronickelling solution in, Al
2O
3Nano-ceramic particle concentration is 6g/L; The churned mechanically ultrasonic oscillation that carries out is simultaneously handled 0.5h, simultaneously with step B) in the attapulgite clay nano particle handled through ultrasonic oscillation be added in the basic electronickelling solution, ultrasonic oscillation 30min, mechanical stirring 1h, obtain composite plating bath, it is 0.5g/L that the attapulgite clay nano particle adds concentration;
D) preparation composite deposite: energising, when current density is 2A/dm
2The time, rotating speed is 200 r/min, and electroplating time is 10h, and thickness of multiple plating is 210 μ m, stops energising, takes out sample, electroplates and finishes, and obtains composite deposite.
Utilize attapulgite in the composite plating process, to Al
2O
3The nanoparticle suspension effect plays simultaneously heterogeneous core during matrix nickel metallic crystal.Obtain at last that crystal grain is tiny, surface compact, Ni/Al that antioxidant property is good
2O
3Nano-composite plate.
Be illustrated in figure 2 as the Ni/ Al that adds 0.5g/L attapulgite clay nano granules preparation in the plating bath
2O
3The nano-composite plate surface microscopic topographic.
Embodiment 2:
Embodiment 2 is as the comparative example of embodiment 1, is not both, and does not add the attapulgite clay nano particle, as shown in Figure 1, is the Ni/ Al of no concave-convex rod soil preparation in the plating bath
2O
3The nano-composite plate surface microscopic topographic.
Embodiment 3:
Concrete steps are with embodiment 1, and difference is to add the TiC nano-ceramic particle in the plating bath, is not Al
2O
3Nano-ceramic particle, base material are Q235, and the composition of electroplate liquid is NiSO
4. 6H
2O 250g/L, H
3BO
340g/L, NiCl
26H
2O 50g/L, it is 0.5g/L that the 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 μ m, electroplate to finish, and obtains surface compact, hardness height, Ni/TiC nano-composite plate that wear resisting property is good at last, as shown in Figure 4, for adding the Ni/TiC nano-composite plate surface microscopic topographic for preparing behind the 0.5g/L attapulgite clay nano particle in the plating bath.
Embodiment 4:
Concrete steps are with embodiment 3, and difference is not add the attapulgite clay nano particle in the plating bath, as shown in Figure 3, are the Ni/TiC nano-composite plate surface microscopic topographic of the native preparation of nanoparticles of no concave-convex rod in the plating bath.
Embodiment 5:
Concrete steps are with embodiment 1, and difference is not add nano-ceramic particle in the plating bath, and base material is Q235, and the composition of electroplate liquid is NiSO
46H
2O 250g/L, H
3BO
340g/L, NiCl
26H
2It is 0.5g/L that O 50g/L, attapulgite clay nano particle add interpolation concentration, and through ultrasonic oscillation 30min, mechanical stirring 1h handles back preparation composite deposite.The plating bath rotating speed is 200r/min, and current density is 2A/dm
2, electroplate 600min, thickness of coating reaches 200 μ m, electroplates and finishes.Last to having the pure Ni coating that crystal grain is tiny, wear resisting property is good.
As shown in Figure 6, for adding the Ni coating surface microscopic appearance of 0.5g/L attapulgite clay nano granules preparation in the plating bath.
Embodiment 6:
Concrete steps are with embodiment 5, and difference is not add the attapulgite clay nano particle in the plating bath, as shown in Figure 5, are the Ni coating surface microscopic appearance of the native preparation of nanoparticles of no concave-convex rod in the plating bath.
Adopt technical scheme of the present invention, can impel nano particle to be dispersed in the plating bath well, make the more refinement of crystal grain of composite deposite, microhardness and the wear resisting property of composite deposite have been improved, equally distributed nano particle is in the grain refining of promotes oxidn film, improve the growth mechanism of oxide film, thereby improved the high temperature oxidation resistance of composite deposite.Electro-plating method technology of the present invention is simple, and the attapulgite wide material sources are with low cost, conveniently apply.
Claims (7)
1. the preparation method of an attapulgite modified nickel base nanometer ceramic particle composite deposite may further comprise the steps:
A) basic electronickelling solution preparation: with NiSO
46H
2O, H
3BO
3And NiCl
26H
2O mixes and is mixed with plating bath, obtains basic electronickelling solution;
B) nano particle pre-treatment: with the attapulgite clay nano particle before plating through ultrasonic oscillation 30min, and then mechanical stirring 0.5-1h;
C) composite plating solution preparation: will be through step B) pretreated attapulgite clay nano particle is added in the basic electronickelling solution, ultrasonic oscillation 30min, and mechanical stirring 0.5-1h obtains composite plating solution;
D) preparation composite deposite: energising, when coating reaches required thickness, stop energising, take out sample, electroplate and finish, obtain composite deposite.
2. the preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite according to claim 1 is characterized in that, in steps A) in, NiSO
46H
2O 250g/L, H
3BO
340g/L, NiCl
26H
2O 50g/L.
3. the preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite according to claim 2, it is characterized in that, described step B) also include nano-ceramic particle in, described nano-ceramic particle is through ultrasonic oscillation 30min, and then mechanical stirring 0.5-1h;
Described step C) be: will be through step B) pretreated nano-ceramic particle is added to steps A) basic electronickelling solution in, the churned mechanically ultrasonic oscillation that carries out is simultaneously handled 0.5-1h; Simultaneously will be through step B) pretreated attapulgite clay nano particle is added in the basic electronickelling solution, ultrasonic oscillation 30min, mechanical stirring 0.5-1h obtains composite plating bath.
4. the preparation method of a kind of attapulgite modified nickel base nanometer ceramic particle composite deposite according to claim 3, it is characterized in that described step C) in nano-ceramic particle, attapulgite clay nano particle in electroplate liquid, be in dispersion, suspended state.
5. the preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite according to claim 4 is characterized in that, described nano-ceramic particle is Al
2O
3Nano-ceramic particle or TiC nano-ceramic particle.
6. according to the preparation method of each described attapulgite modified nickel base nanometer ceramic particle composite deposite of claim 1 ~ 5, it is characterized in that, at described step B) in, described attapulgite clay nano particle grain size is 40nm, concentration 0.5 ~ 3.0 g/L in plating bath.
7. the preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite according to claim 6 is characterized in that: described step D), when current density is 2A/dm
2The time, rotating speed is 200 r/min, and electroplating time is 10h, and thickness of multiple plating is 210 ~ 220 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310211302.9A CN103290458B (en) | 2013-07-11 | 2013-07-11 | The preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310211302.9A CN103290458B (en) | 2013-07-11 | 2013-07-11 | The preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103290458A true CN103290458A (en) | 2013-09-11 |
| CN103290458B CN103290458B (en) | 2015-12-09 |
Family
ID=49091964
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310211302.9A Expired - Fee Related CN103290458B (en) | 2013-07-11 | 2013-07-11 | The preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103290458B (en) |
Citations (5)
| 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 |
| EP0441636A1 (en) * | 1990-02-09 | 1991-08-14 | Nihon Parkerizing Co., Ltd. | Process for surface treating titanium-containing metallic material |
| 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 |
| US20070108059A1 (en) * | 2005-11-15 | 2007-05-17 | Ji-Young Byun | 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 (5)
| 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 |
| EP0441636A1 (en) * | 1990-02-09 | 1991-08-14 | Nihon Parkerizing Co., Ltd. | Process for surface treating titanium-containing metallic material |
| 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 |
| US20070108059A1 (en) * | 2005-11-15 | 2007-05-17 | Ji-Young Byun | Composite layer including metal and inorganic powders and method for manufacturing the same |
| 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 |
|---|
| 马玉恒等，: ""凹凸棒土研究与应用进展"", 《材料导报》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103290458B (en) | 2015-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gül et al. | Effect of particle concentration on the structure and tribological properties of submicron particle SiC reinforced Ni metal matrix composite (MMC) coatings produced by electrodeposition | |
| CN101205623B (en) | Nano compound electroplating new method for preservation of neodymium iron boron ferrite | |
| Gül et al. | Effect of PC electrodeposition on the structure and tribological behavior of Ni–Al2O3 nanocomposite coatings | |
| CN101210305A (en) | Tungsten alloy composite plating coat material and manufacturing method thereof | |
| CN102773434A (en) | Nanocomposite electroplating layer copper plate of continuous casting crystallizer and preparation process of nanocomposite electroplating layer copper plate | |
| CN101532151B (en) | Electric deposition nickel pottery plating solution and preparing method thereof | |
| CN102002748A (en) | Method for preparing ferromagnetic nano composite material with pulse-ultrasound electrodeposition | |
| Pushpanathan et al. | On the microstructure and tribological properties of pulse electrodeposited Ni-B4C-TiC nano composite coating on AZ80 magnesium alloy | |
| CN107737892B (en) | Nickel cobalt manganese alloy coating and its preparation process is electroplated in continuous casting crystallizer copper plate | |
| Li et al. | Pulse electrodepsoited Ni-Cu/TiN-ZrO2 nanocomposite coating: microstructural and electrochemical properties | |
| CN105568348A (en) | Method for assisting composite plating with magnetic field | |
| CN104313656A (en) | Nickel-tungsten-silicon carbide-aluminum oxide composite electroplate liquid as well as preparation method and application thereof | |
| Nguyen et al. | Nickel composite plating with fly ash as inert particle | |
| Fahami et al. | Influence of surfactants on the characteristics of nickel matrix nanocomposite coatings | |
| CN106011955A (en) | Corrosion-resistant and wear-resistant Ni-W/Al2O3 CMMA protective layer for maritime work machinery, and preparation method thereof | |
| CN101122044A (en) | Nickel-base composite coat containing nano diamond and ultrasound wave auxiliary preparation method thereof | |
| CN103290458B (en) | The preparation method of attapulgite modified nickel base nanometer ceramic particle composite deposite | |
| Borkar | Electrodeposition of nickel composite coatings | |
| CN109487261B (en) | Method for quickly electrodepositing coating on surface of magnesium alloy | |
| CN103806075A (en) | Surface electroplating process of thin cutting tool | |
| CN1308496C (en) | Electrodeposition composite plating method for improving metal surface high temperature and abrasion resistant performance | |
| CN102383118B (en) | Preparation method of aluminum alloy and rare earth nickel base electromagnetic shielding layer | |
| CN100464010C (en) | Ni-P-W alpha aluminium oxide composite electroplating formula and its technology | |
| Wang et al. | Effect of attapulgite added in plating bath on the properties of Ni/TiC nano-composite coatings | |
| CN1265029C (en) | Nano composite plating paste material and its preparation and electroplating method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151209 Termination date: 20200711 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |