CN100567587C - Zn-Ni-Al 2O 3Nano-composite plate and preparation method thereof - Google Patents
Zn-Ni-Al 2O 3Nano-composite plate and preparation method thereof Download PDFInfo
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- CN100567587C CN100567587C CNB2006100098151A CN200610009815A CN100567587C CN 100567587 C CN100567587 C CN 100567587C CN B2006100098151 A CNB2006100098151 A CN B2006100098151A CN 200610009815 A CN200610009815 A CN 200610009815A CN 100567587 C CN100567587 C CN 100567587C
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Abstract
Zn-Ni-Al
2O
3The preparation method of nano-composite plate relates to a kind of Zn-Ni-Al
2O
3Nano-composite plate and preparation technology thereof.In plating bath, disperse problem inhomogeneous, easy reunion, Zn-Ni-Al of the present invention at nano particle in the prior art plating process
2O
3In the nano-composite plate, nano aluminium oxide accounts for 1%～30% of coating cumulative volume, and Ni accounts for 10%～20% of Zn-Ni alloy total mass.Its preparation method is: a, nano alumina particles is joined in the Zn-Ni alloy plating bath magnetic agitation, ultra-sonic oscillation; B, composite plating bath poured in the electrolyzer electroplate, the limit disperses the plating bath limit to carry out compound plating with physical method.The present invention has obtained that nano aluminium oxide is uniformly dispersed, coating light, hardness and all good than the Zn-Ni alloy coating Zn-Ni-Al of solidity to corrosion
2O
3Nano-composite plate.
Description
Technical field
The present invention relates to a kind of Zn-Ni-Al
2O
3The preparation technology of nano-composite plate.
Background technology
Development along with defense and commercial industry, people require more and more higher to the solidity to corrosion of ferrous materials and various component, nickel content is that 10%～15% Zn-Ni alloy coating is owing to its good solidity to corrosion is widely used in industries such as automotive industry, aerospace, light industry, household electrical appliances, improve the corrosion resisting property of product greatly, and saved starting material.
Compound plating is that the method with galvanic deposit or electroless plating makes metal and solia particle codeposition and obtains the technological process of composite layer.Its coating is when keeping original matrix metal coating character, strengthened the character of original metal plating, and former coating carried out modification, this has suitable degree of freedom with regard to the function that makes composite deposite, can obtain wear-resisting, self-lubricating, anti-corrosion, functional coating such as decorate, electrically contact.Therefore, compound coating technology for a change provides great possibility with physics, machinery, the chemical property of adjusting coating, and has become the Zhi Xin army in the metal-base composites, has obtained widespread use in engineering.
The second phase particle that traditional composite plating is selected for use is micron-sized mostly, (patent No.: the alumina particle particle diameter that uses JP61235600) is 50 μ m as Japanese Patent " the compound plating of the Zn-Ni alloy on the steel matrix ", because grain graininess is bigger, suspending power in plating bath is poor, make coating surface coarse, outward appearance is bad.Therefore, fail to obtain excellent popularization uses always.
The appearance of nanoparticle is for the compound coating technology of galvanic deposit has brought new opportunity.If with the micron particle in the nano particle replacement composite plating bath, because character such as surface effects, volume effect, quantum size effect, macro quanta tunnel effect that nano particle has and the light that some are unusual, electricity, magnetic, can make the performance of composite deposite excellent more, market outlook will be more wide.
Be suspended in nanoparticle in the solution because its surfactivity height is easy to reunite together, this has brought very big difficulty to nano compound electroplating.In order to prevent the reunion of nano particle, take chemical dispersion method or physics dispersing method usually.Chemical process is as selecting suitable ionogen as dispersion agent, can make nanoparticle surface attract different electron ion to form electrostatic double layer like this, by the repulsive interaction between the electrostatic double layer gravitation that takes place between the particle to reunite is reduced greatly, realize nanoparticle dispersive purpose, or nanoparticle carried out finishing, as add tensio-active agent parcel particulate.No matter be to add dispersion agent or nano-particle surface is modified, when solving nanoparticle agglomerates, tend to reduce the performance of composite deposite on the contrary because of the composition introduced produces negative effect to the performance of coating.The useful mechanical stirring of physics dispersing method, circulation stirring or ultra-sonic oscillation etc.Use ultrasonic wave dispersing nanometer particle effectively, but generally be before plating, to use ultrasonic wave that nano particle is separated reunion at present, when electroplating, then do not use ultrasonic wave, but, make compound plating process be difficult to carry out in case ultrasonic or mechanical agitation stops that nano particle can be reunited again again, sedimentation.Galvanized use simultaneously blade stirring or ultrasonic agitation or mechanical pump circulation stirring have been proposed in " a kind of raising metallic surface is high temperature resistant and anti abrasive galvanic deposit composite plating method " (CN 1552952A), but the rotating speed that blade stirs is not described, the flow velocity that ultransonic power and frequency, circulation are stirred, and these factors will directly have influence on the effect and the compounding quantity of nano particle in composite deposite of nanoparticulate dispersed.
Summary of the invention
In plating bath, disperse problem inhomogeneous, easy reunion at nano particle in the prior art plating process, the invention provides a kind of Zn-Ni-Al
2O
3The preparation method of nano-composite plate.
Zn-Ni-Al of the present invention
2O
3In the nano-composite plate, nano aluminium oxide accounts for 1%～30% of coating cumulative volume, Ni accounts for 10%～20% of Zn-Ni alloy total mass, and its preparation method is: a, nano alumina particles is joined in the Zn-Ni alloy plating bath, control nano aluminium oxide consumption is 1～50gL
-1, magnetic agitation 6～24h, ultra-sonic oscillation 0.1～1h; B, scattered composite plating bath poured in the electrolyzer electroplate, with nickel plate or zine plate is anode, with workpiece to be plated is negative electrode, the limit disperses the plating bath limit to carry out compound plating with physical method, and magnetic agitation is that intermittent type stirs during plating, stirs 10～30s, static 1～3min, rotating speed is 100～1000 rev/mins, and ultrasonic frequency is 25～100kHz, and ultrasound intensity is 10～100Wdm
-2, the nano aluminium oxide that contains in the nano-composite plate that galvanic deposit obtains accounts for the 1vol.%～30vol.% of coating cumulative volume.The nano-composite plate that above-mentioned galvanic deposit obtains can carry out aftertreatments such as passivation.
The present invention selects the composite particles of the α phase nano alumina particles of wide material sources, cheap, excellent corrosion-proof performance as Zn-Ni alloy coating for use, adopt the nano alumina particles in the built-in ultrasonic generator dispersion composite plating bath, and apply sonic oscillation and magnetic agitation simultaneously, thereby obtained that nano aluminium oxide is uniformly dispersed, coating light, hardness and all good Zn-Ni-Al of solidity to corrosion than Zn-Ni alloy coating galvanized
2O
3Nano-composite plate.
Description of drawings
Fig. 1 is the structural representation of the used compound plating appts of the present invention, wherein 1: magnetic stirring apparatus, 2: ultrasonic generator, 3: ultrasonic generator probe, 4: temperature sensor, 5: anode, 6: negative electrode, 7: the magnetic agitation rotor.
Embodiment
Embodiment one: the Zn-Ni-Al in the present embodiment
2O
3In the nano-composite plate, nano aluminium oxide accounts for 1%～30% of coating cumulative volume, and Ni accounts for 10%～20% of Zn-Ni alloy total mass.
Embodiment two: present embodiment is prepared as follows Zn-Ni-Al
2O
3Nano-composite plate: a, nano alumina particles is joined in the Zn-Ni alloy plating bath, control nano aluminium oxide consumption is 1～50gL
-1, magnetic agitation 6～24h, ultra-sonic oscillation 0.1～1h; B, scattered composite plating bath poured in the electrolyzer electroplate, with nickel plate or zine plate is anode, with workpiece to be plated is negative electrode, the limit disperses the plating bath limit to carry out compound plating with physical method, and magnetic agitation is that intermittent type stirs during plating, stirs 10～30s, static 1～3min, rotating speed is 100～1000 rev/mins, and ultrasonic frequency is 25～100kHz, and ultrasound intensity is 10～100Wdm
-2
The Zn-Ni alloy plating bath also can use other acid system or basic plating Zn-Ni alloy system in the present embodiment except acid chlorization potassium system Zn-Ni alloy plating bath.Wherein acid chlorization potassium system Zn-Ni alloy plating bath composition and processing condition are as follows: nickelous chloride: 100～120gL
-1, zinc chloride: 60～80gL
-1, Repone K: 120～140gL
-1, ammonium chloride: 100～120gL
-1, additive: 2～3mlL
-1, regulate pH value=4.5～5.0, temperature is 30～40 ℃; Cathode current density is 2～12Adm
-2Described additive is YZ additive (Shanghai immortality auxiliary reagent factory).
Nano aluminium oxide described in the present embodiment is a α phase nano aluminium oxide, is commonly called as corundum.The nano alumina particles mean diameter is 10～200nm, and the nano aluminium oxide consumption is 1～50gL in the composite plating bath
-1
Workpiece to be plated described in the present embodiment can be steel, also can be not with any metal of plating bath generation chemical reaction.
Employed electroplanting device and ultrasonic generator are as shown in Figure 1 in the present embodiment.In the present embodiment ultrasonic generator probe is directly inserted plating bath, make the ultra-sonic dispersion nano particle more abundant.
Magnetic agitation or blade stir to continous way stirs before electroplating described in the present embodiment, and rotating speed is 1000～3000 rev/mins.
The ultrasonic frequency of the nano aluminium oxide before electroplating described in the present embodiment in the ultrasonic dispersing plating bath is 25～100khz, and ultrasound intensity is 10～100WL
-1
Galvanized magnetic agitation and the ultra-sonic oscillation of adopting simultaneously described in the present embodiment.
The nano aluminium oxide that contains in the nano-composite plate that galvanic deposit described in the present embodiment obtains accounts for the 1vol.%～30vol.% of coating cumulative volume, and Ni accounts for 10%～20% of Zn-Ni alloy total mass.
The nano-composite plate that galvanic deposit described in the present embodiment obtains can carry out aftertreatments such as passivation.
Embodiment three: what present embodiment and embodiment two were different is that the composition and the processing condition of acid chlorization potassium system Zn-Ni alloy plating bath are: nickelous chloride: 110gL
-1, zinc chloride: 70gL
-1, Repone K: 130gL
-1, ammonium chloride: 110gL
-1, additive: 3mlL
-1, regulate pH value=4.5, temperature is 35 ℃; Cathode current density is 6Adm
-2
Embodiment four: present embodiment is according to being prepared as follows Zn-Ni-Al
2O
3Nano-composite plate:
(1) the preparation plating bath consists of nickelous chloride: 110gL
-1, zinc chloride: 70gL
-1, Repone K: 130gL
-1, ammonium chloride: 110gL
-1, additive: 2mlL
-11 liter of Zn-Ni alloy plating bath, regulating the pH value with hydrochloric acid or potassium hydroxide is 4.5.
(2) adding consumption in the Zn-Ni alloy plating bath is 1gL
-1, particle diameter is the alumina particle of 30nm, magnetic agitation 6h, 2500 rev/mins of rotating speeds.Nano aluminium oxide in the ultrasonic dispersing plating bath then, ultrasonic frequency is 28khz, ultrasound intensity is 30WL
-1, sonic oscillation 10min.
(3) scattered composite plating bath is poured in the electrolyzer electroplated.Ultrasonic frequency is 28khz during plating, and ultrasound intensity is 30Wdm
-2Magnetic force intermittently stirs during plating, magnetic agitation 10s, and static 3min, rotating speed are 100 rev/mins.Wherein: control composite plating bath temperature is 35 ℃; Anode: 5cm * 10cm nickel plate; Negative electrode: 5cm * 3cm mild steel plate, steel plate is through polishing, alkali cleaning, cleanup acid treatment; Cathode current density 6Adm
-2, electroplating time 20min.
The Zn-Ni-Al that obtains according to the method described above
2O
3The careful light in nano-composite plate surface contains 4.2vol.%Al in the nano aluminium oxide content measuring overlay coating
2O
3Nano particle.Hardness test shows: Zn-Ni-Al
2O
3The hardness of nano-composite plate is 471HV, and the hardness of Zn-Ni alloy coating is 186HV under the identical plating condition.Tafel curve test shows: Zn-Ni-Al
2O
3The corrosion current of nano-composite plate is 2.3 * 10
-5Acm
-2, corrosion potential is-0.78V.The corrosion current of Zn-Ni alloy coating is 3.2 * 10 under the identical plating condition
-5Acm
-2, corrosion potential is-0.86V.As seen Zn-Ni-Al
2O
3The hardness of nano-composite plate is significantly increased with comparing all of Zn-Ni alloy coating with solidity to corrosion.
Embodiment five: present embodiment is prepared as follows Zn-Ni-Al
2O
3Nano-composite plate:
(1) the preparation plating bath consists of nickelous chloride: 110gL
-1, zinc chloride: 70gL
-1, Repone K: 130gL
-1, ammonium chloride: 110gL
-1, additive: 2.5mlL
-11 liter of Zn-Ni alloy plating bath, regulating the pH value with hydrochloric acid or potassium hydroxide is 4.5.
(2) adding consumption in above-mentioned plating bath is 10gL
-1, particle diameter is the alumina particle of 100nm, magnetic agitation 12h, 2500 rev/mins of rotating speeds.Nano aluminium oxide in the ultrasonic dispersing plating bath then, ultrasonic frequency is 45khz, ultrasound intensity is 50WL
-1, sonic oscillation 30min.
(3) scattered composite plating bath is poured in the electrolyzer electroplated.Ultrasonic frequency is 45khz during plating, and ultrasound intensity is 50Wdm
-2Magnetic force intermittently stirs during plating, magnetic agitation 20s, and static 2min, rotating speed are 500 rev/mins.Wherein: control composite plating bath temperature is 35 ℃; Anode: 5cm * 10cm nickel plate; Negative electrode: 5cm * 3cm mild steel plate, steel plate is through polishing, alkali cleaning, cleanup acid treatment; Cathode current density is 6Adm
-2, electroplating time is 20min.
The Zn-Ni-Al that obtains according to the method described above
2O
3The careful light in nano-composite plate surface contains 16.3vol.%Al in the nano aluminium oxide content measuring overlay coating
2O
3Nano particle.Hardness test shows: Zn-Ni-Al
2O
3The hardness of nano-composite plate is 532HV; The hardness of Zn-Ni alloy coating is 206HV under the identical plating condition.Tafel curve test shows: Zn-Ni-Al
2O
3The corrosion current of nano-composite plate is 1.8 * 10
-5Acm
-2, corrosion potential is-0.71V; The corrosion current of Zn-Ni alloy coating is 3.8 * 10 under the identical plating condition
-5Acm
-2, corrosion potential is-0.82V.As seen Zn-Ni-Al
2O
3The hardness of nano-composite plate is significantly increased with comparing all of Zn-Ni alloy coating with solidity to corrosion.
Embodiment six: present embodiment is prepared as follows Zn-Ni-Al
2O
3Nano-composite plate:
(1) the preparation plating bath consists of nickelous chloride: 120gL
-1, zinc chloride: 80gL
-1, Repone K: 140gL
-1, ammonium chloride: 120gL
-1, additive: 3mlL
-11 liter of Zn-Ni alloy plating bath, regulating the pH value with hydrochloric acid or potassium hydroxide is 5.
(2) adding consumption in above-mentioned plating bath is 100gL
-1, particle diameter is the alumina particle of 200nm, magnetic agitation 24h, 2500 rev/mins of rotating speeds.Nano aluminium oxide in the ultrasonic dispersing plating bath then, ultrasonic frequency is 100khz, ultrasound intensity is 100WL
-1, sonic oscillation 1h.
(3) scattered composite plating bath is poured in the electrolyzer electroplated.Ultrasonic frequency is 45khz during plating, and ultrasound intensity is 100Wdm
-2Magnetic force intermittently stirs during plating, magnetic agitation 30s, and static 1min, rotating speed are 1000 rev/mins.Wherein: control composite plating bath temperature is 35 ℃; Anode: 5cm * 10cm nickel plate; Negative electrode: 5cm * 3cm mild steel plate, steel plate is through polishing, alkali cleaning, cleanup acid treatment; Cathode current density is 12Adm
-2, electroplating time is 20min.
The Zn-Ni-Al that obtains according to the method described above
2O
3The careful light in nano-composite plate surface contains 25.8vol.%Al in the nano aluminium oxide content measuring overlay coating
2O
3Nano particle.Hardness test shows: Zn-Ni-Al
2O
3The hardness of nano-composite plate is 787HV, and the hardness of Zn-Ni alloy coating is 219HV under the identical plating condition.Tafel curve test shows: Zn-Ni-Al
2O
3The corrosion current of nano-composite plate is 2.4 * 10
-5Acm
-2, corrosion potential is-0.68V; The corrosion current of Zn-Ni alloy coating is 3.7 * 10 under the identical plating condition
-5Acm
-2, corrosion potential is-0.83V.As seen Zn-Ni-Al
2O
3The hardness of nano-composite plate is significantly increased with comparing all of Zn-Ni alloy coating with solidity to corrosion.
Claims (9)
1, a kind of Zn-Ni-Al
2O
3The preparation method of nano-composite plate is characterized in that described Zn-Ni-Al
2O
3Nano-composite plate is prepared according to following steps: a, nano alumina particles is joined in the Zn-Ni alloy plating bath, control nano aluminium oxide consumption is 1～50gL
-1, magnetic agitation 6～24h, ultra-sonic oscillation 0.1～1h; B, scattered composite plating bath poured in the electrolyzer electroplate, with nickel plate or zine plate is anode, with workpiece to be plated is negative electrode, the limit disperses the plating bath limit to carry out compound plating, and magnetic agitation is that intermittent type stirs during plating, stirs 10～30s, static 1～3min, rotating speed is 100～1000 rev/mins, and ultrasonic frequency is 25～100kHz, and ultrasound intensity is 10～100Wdm
-2
2, Zn-Ni-Al according to claim 1
2O
3The preparation method of nano-composite plate is characterized in that described nano alumina particles mean diameter is 10～200nm.
3, Zn-Ni-Al according to claim 1
2O
3The preparation method of nano-composite plate is characterized in that described nano aluminium oxide is a α phase nano aluminium oxide.
4, Zn-Ni-Al according to claim 1
2O
3The preparation method of nano-composite plate is characterized in that described workpiece to be plated is steel, or not with any metal of plating bath generation chemical reaction.
5, Zn-Ni-Al according to claim 1
2O
3The preparation method of nano-composite plate is characterized in that the alr mode in the described a step is that continous way stirs, and rotating speed is 1000～3000 rev/mins.
6, Zn-Ni-Al according to claim 1
2O
3The preparation method of nano-composite plate, the ultrasonic frequency that it is characterized in that the nano aluminium oxide in the ultrasonic dispersing plating bath in the described a step is 25～100kHz, ultrasound intensity is 10～100WL
-1
7, Zn-Ni-Al according to claim 1
2O
3The preparation method of nano-composite plate is characterized in that described Zn-Ni alloy plating bath is an acid chlorization potassium system Zn-Ni alloy plating bath.
8, Zn-Ni-Al according to claim 7
2O
3The preparation method of nano-composite plate is characterized in that the composition and the processing condition of described acid chlorization potassium system Zn-Ni alloy plating bath are: nickelous chloride: 100～120gL
-1, zinc chloride: 60～80gL
-1, Repone K: 120～140gL
-1, ammonium chloride: 100～120gL
-1, additive: 2～3mlL
-1, regulate pH value=4.5～5.0, temperature is 30～40 ℃; Cathode current density is 2～12Adm
-2
9, Zn-Ni-Al according to claim 8
2O
3The preparation method of nano-composite plate is characterized in that the composition and the processing condition of described acid chlorization potassium system Zn-Ni alloy plating bath are: nickelous chloride: 110gL
-1, zinc chloride: 70gL
-1, Repone K: 130gL
-1, ammonium chloride: 110gL
-1, additive: 3mlL
-1, regulate pH value=4.5, temperature is 35 ℃; Cathode current density is 6Adm
-2
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| CN103243373A (en) * | 2012-02-13 | 2013-08-14 | 南车戚墅堰机车车辆工艺研究所有限公司 | Brush plating solution for Zn-Ni-Al2O3 composite coating and preparation method thereof |
| CN103243361B (en) * | 2012-02-13 | 2016-09-14 | 南车戚墅堰机车车辆工艺研究所有限公司 | Composite deposite and the brush plating method of composite deposite |
| CN102703936B (en) * | 2012-06-28 | 2015-06-03 | 华南理工大学 | Carbon nano tube/cobalt composite coating and preparation method thereof |
| CN103388166A (en) * | 2013-08-07 | 2013-11-13 | 苏州扬清芯片科技有限公司 | Electrolytic tank for rapidly preparing anodic aluminum oxide template |
| CN105112961A (en) * | 2015-09-22 | 2015-12-02 | 太仓市金鹿电镀有限公司 | Zinc-nickel alloy electroplating process |
| CN105239137A (en) * | 2015-10-29 | 2016-01-13 | 无锡桥阳机械制造有限公司 | Electroplating technology |
| JP7417888B2 (en) | 2019-02-28 | 2024-01-19 | 奥野製薬工業株式会社 | Zinc-based composite plating solution, method for forming zinc-based composite plating film, and method for forming composite oxide film |
| CN111962110A (en) * | 2020-08-03 | 2020-11-20 | 顺科新能源技术股份有限公司 | Zn-Ni alloy electroplating solution and electroplating method |
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