CN101643930A - Compound plating bath for producing high-hardness wear-reduction wear-resistance nanometer compound claddings and electroplating method - Google Patents
Compound plating bath for producing high-hardness wear-reduction wear-resistance nanometer compound claddings and electroplating method Download PDFInfo
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- CN101643930A CN101643930A CN200910066070A CN200910066070A CN101643930A CN 101643930 A CN101643930 A CN 101643930A CN 200910066070 A CN200910066070 A CN 200910066070A CN 200910066070 A CN200910066070 A CN 200910066070A CN 101643930 A CN101643930 A CN 101643930A
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Abstract
The invention discloses a compound plating bath for producing high-hardness wear-reduction wear-resistance nanometer compound cladding and an electroplating method. Nanometer yttria (Y2O3) particles and nanometer zirconia (ZrO2) particles are added to the plating bath to produce the compound plating bath, and the compound plating bath and substrate metal deposit together to produce the compound cladding. The nanometer Y2O3 particles are rare-earth nanometer particles and have the advantages of favorable corrosion resistance as well as high temperature stability and light transmittance. The nanometer ZrO2 particles are hard ceramic nanometer particles and have the advantages of high hardness, favorable thermal stability and oxidation resistance. The compound plating bath combines the advantages of the nanometer yttria (Y2O3) particles and the nanometer zirconia (ZrO2) particles so as to prepare the compound cladding with favorable performance. The compound cladding has the advantages ofhigh microhardness as well as favorable wear reduction performance and wear resistance. The preparation method has the advantages of simple technique, low cost and convenient popularization and application.
Description
Technical field
The present invention relates to the protecting metallic surface technical field, be specifically related to a kind of composite plating bath and electro-plating method that obtains high rigidity, anti-friction wear-resistant nano-composite plate.
Background technology
Composite plating claims again to disperse to electroplate, be that solia particle is dispersed in the electroplate liquid, make suspension and electroplate, make solia particle and electroplate the matrix metal codeposition, thereby obtain to have wear-resisting, self-lubricating, corrosion-resistant, the composite deposite of function such as decorating, electrically contact.In recent years, the composite plating technology development is very rapid, has become part the most active in the modern electroplating technology.
Nano compound electroplating is on the basis of common composite plating, make insoluble solid particulate and the metal ion of nanoscale between 1～100nm realize codeposition, have a kind of NEW TYPE OF COMPOSITE electroplating technology of the composite deposite of specific function with acquisition at cathode surface.Because nanoparticle has special propertys such as surface effects, volume effect, quantum size effect, macro quanta tunnel effect, make and adopt the composite deposite of nano compound electroplating technology preparation to have many special performances.At present, domestic and international many scholars have been matrix metal or alloy with Ni, Cr, Co, Ni-Fe, Ni-Co, Ni-P, Ni-B etc., add Al
2O
3, SiC, WC, TiC, ZrO
2, MoS
2, TiO
2, SiO
2With nano particles such as diamonds, prepared have high microhardness, the composite deposite of excellent property such as corrosion-resistant, resistance to high temperature oxidation and anti-friction wear-resistant.For example, add Al with high chemical stability
2O
3The Zn-Ni-Al that nano particle obtains
2O
3Composite deposite has good corrosion resistance; Add the ZrO of high rigidity
2The Ni-ZrO that nano particle obtains
2Composite deposite has the microhardness more much higher than pure-nickel-layer; Add La
2O
3The Ni-La of preparation of nanoparticles
2O
3The abrasion resistance properties of composite deposite is good.Therefore, the nano compound electroplating technology has wide future in engineering applications.Nano compound electroplating technology great majority are that employing a kind of nano particle of interpolation in electroplate liquid prepares composite deposite at present.
Summary of the invention
One of purpose of the present invention provides a kind of composite plating bath that obtains high rigidity, anti-friction wear-resistant nano-composite plate.
Two of purpose of the present invention provides a kind of electro-plating method that is prepared composite deposite by this composite plating bath.
In order to realize above purpose, the technical solution adopted in the present invention is:
The main ingredient of composite plating bath is:
Nano yttrium oxide 5～60g/L
Nano zircite 10～70g/L
Ni(NH
2SO
3)
2·4H
2O????200～500g/L
NH
4Cl????????????????5～30g/L
H
3BO
3????????????????10～80g/L
C
12H
25SO
4Na??????????0.05～5g/L。
Wherein nano yttrium oxide particle grain size scope is 40～70nm, and nano zircite particle grain size scope is 45～75nm.
Prepare the method for composite deposite by this composite plating bath, comprise the following steps:
A. prepare composite plating bath;
B. select cathode base and anode substrate;
C. determine the composite plating process parameter;
D. opening power is carried out composite plating.
Composite plating bath main ingredient described in the step a is:
Nano yttrium oxide 5～60g/L
Nano zircite 10～70g/L
Ni(NH
2SO
3)
2·4H
2O???????200～500g/L
NH
4Cl???????????????????5～30g/L
H
3BO
3???????????????????10～80g/L
C
12H
25SO
4Na?????????????0.05～5g/L。
Wherein cathode base is stainless steel substrates or copper sheet, and anode substrate is a sheet nickel.
Before the plating, anticathode to carry out physics rust cleaning and electrochemical deoiling processing.
The processing parameter of composite plating is:
PH value 3～5
30～50 ℃ of temperature
Cathode current density 2～8A/dm
2
The yttrium oxide nano particle that the present invention adopts is a rare earth nanometer particle, has excellent erosion resistance, high-temperature stability and high light transmittance, and Zirconium oxide nano grain is the hard ceramic nano particle, has high rigidity, good thermostability and antioxidant property.Rare earth nanometer particle integrates the characteristic of rare earth characteristic and nano particle; be applied in the composite plating, can obtain the coating of excellent performance, hard ceramic nano particle chemical property is stable; the present invention combines the advantage of two kinds of nano particles, has prepared a kind of NEW TYPE OF COMPOSITE coating.
The present invention promotes the codeposition of two kinds of nano particles and matrix metal by the rational proportion of yttrium oxide and two kinds of nano particles of zirconium white, a large amount of nano particles enters and has served as new nucleation site in the composite deposite, not only interrupted the crystal growth of matrix metal itself, and increased nucleation rate, cause the crystal grain of matrix metal constantly to be interrupted and regrow at new nucleus growth point, thus refinement the weave construction of composite deposite.In addition, the embedding of a large amount of nano particles, make nano particle in the composite deposite hinder the expansion of moving of the inner dislocation of composite deposite and tiny crack effectively, the slippage between the electrocrystallization crystal boundary has been produced inhibition, improved composite deposite microhardness and wear resistance.
Advantage of the present invention is:
(1) this preparation method's technology is simple, with low cost, conveniently applies;
(2) the composite deposite microhardness height that makes of the present invention, anti-friction wear-resistant is good.
Embodiment
Below by embodiment, technical scheme of the present invention is described further.
The nano yttrium oxide particle grain size scope of wherein choosing is 40～70nm, and nano zircite particle grain size scope is 45～75nm.
Embodiment 1
Take by weighing Ni (NH by calculating good amount
2SO
3)
24H
2O, NH
4Cl, H
3BO
3And C
12H
25SO
4Na adds a certain amount of water, is mixed with Ni (NH
2SO
3)
24H
2O 200g/L, NH
4Cl 15g/L, H
3BO
325g/L, C
12H
25SO
4The basic plating bath of Na 0.1g/L; With load weighted nano yttrium oxide and nano zircite uniform mixing, add in the basic plating bath again, fully stir, be mixed with and contain nano yttrium oxide 25g/L, nano zircite 30g/L, Ni (NH
2SO
3)
24H
2O 200g/L, NH
4Cl 15g/L, H
3BO
325g/L, C
12H
25SO
4The composite plating solution of Na 0.1g/L.
Prepare the method for composite deposite by this composite plating bath, comprise the following steps:
A. prepare composite plating bath;
B. select cathode base and anode substrate;
Cathode base selection stainless steel substrates (150mm * 20mm * 2mm), wherein the plating area is 50mm * 20mm, rest part is done insulation and is handled, anode substrate is a sheet nickel, nickel plate purity is greater than 99.9%, and the ratio of the area of negative and positive two-stage is 2: 3, and two interpole gaps are 30mm, before the plating, anticathode carries out the physics rust cleaning and electrochemical deoiling is handled;
C. determine the composite plating process parameter;
Processing parameter is: the pH value is 3, and temperature is 40 ℃, and cathode current density is 2A/dm
2
D. opening power is carried out composite plating.
Embodiment 2
Take by weighing Ni (NH by calculating good amount
2SO
3)
24H
2O, NH
4Cl, H
3BO
3And C
12H
25SO
4Na adds a certain amount of water, is mixed with Ni (NH
2SO
3)
24H
2O 300g/L, NH
4Cl 5g/L, H
3BO
310g/L, C
12H
25SO
4The basic plating bath of Na 0.5g/L; With load weighted nano yttrium oxide and nano zircite uniform mixing, add in the basic plating bath again, fully stir, be mixed with and contain nano yttrium oxide 40g/L, nano zircite 10g/L, Ni (NH
2SO
3)
24H
2O 300g/L, NH
4Cl 5g/L, H
3BO
310g/L, C
12H
25SO
4The composite plating solution of Na 0.5g/L.
Prepare the method for composite deposite by this composite plating bath, comprise the following steps:
A. prepare composite plating bath;
B. select cathode base and anode substrate;
Cathode base selection copper sheet (150mm * 20mm * 2mm), wherein the plating area is 50mm * 20mm, rest part is done insulation and is handled, anode substrate is a sheet nickel, nickel plate purity is greater than 99.9%, and the ratio of the area of negative and positive two-stage is 2: 3, and two interpole gaps are 30mm, before the plating, anticathode carries out the physics rust cleaning and electrochemical deoiling is handled;
C. determine the composite plating process parameter;
Processing parameter is: the pH value is 3, and temperature is 30 ℃, and cathode current density is 4A/dm
2
D. opening power is carried out composite plating.
Embodiment 3
Take by weighing Ni (NH by calculating good amount
2SO
3)
24H
2O, NH
4Cl, H
3BO
3And C
12H
25SO
4Na adds a certain amount of water, is mixed with Ni (NH
2SO
3)
24H
2O 400g/L, NH
4Cl 25g/L, H
3BO
365g/L, C
12H
25SO
4The basic plating bath of Na 0.05g/L; With load weighted nano yttrium oxide and nano zircite uniform mixing, add in the basic plating bath again, fully stir, be mixed with and contain nano yttrium oxide 10g/L, nano zircite 45g/L, Ni (NH
2SO
3)
24H
2O 400g/L, NH
4Cl 25g/L, H
3BO
365g/L, C
12H
25SO
4The composite plating solution of Na 0.05g/L.
Prepare the method for composite deposite by this composite plating bath, comprise the following steps:
A. prepare composite plating bath;
B. select cathode base and anode substrate;
Cathode base selection stainless steel substrates (150mm * 20mm * 2mm), wherein the plating area is 50mm * 20mm, rest part is done insulation and is handled, anode substrate is a sheet nickel, nickel plate purity is greater than 99.9%, and the ratio of the area of negative and positive two-stage is 2: 3, and two interpole gaps are 30mm, before the plating, anticathode carries out the physics rust cleaning and electrochemical deoiling is handled;
C. determine the composite plating process parameter;
Processing parameter is: the pH value is 4, and temperature is 50 ℃, and cathode current density is 6A/dm
2
D. opening power is carried out composite plating.
Embodiment 4
Take by weighing Ni (NH by calculating good amount
2SO
3)
24H
2O, NH
4Cl, H
3BO
3And C
12H
25SO
4Na adds a certain amount of water, is mixed with Ni (NH
2SO
3)
24H
2O 500g/L, NH
4Cl 30g/L, H
3BO
380g/L, C
12H
25SO
4The basic plating bath of Na 2g/L; With load weighted nano yttrium oxide and nano zircite uniform mixing, add in the basic plating bath again, fully stir, be mixed with and contain nano yttrium oxide 60g/L, nano zircite 60g/L, Ni (NH
2SO
3)
24H
2O 500g/L, NH
4Cl 30g/L, H
3BO
380g/L, C
12H
25SO
4The composite plating solution of Na 2g/L.
Prepare the method for composite deposite by this composite plating bath, comprise the following steps:
A. prepare composite plating bath;
B. select cathode base and anode substrate;
Cathode base selection copper sheet (150mm * 20mm * 2mm), wherein the plating area is 50mm * 20mm, rest part is done insulation and is handled, anode substrate is a sheet nickel, nickel plate purity is greater than 99.9%, and the ratio of the area of negative and positive two-stage is 2: 3, and two interpole gaps are 30mm, before the plating, anticathode carries out the physics rust cleaning and electrochemical deoiling is handled;
C. determine the composite plating process parameter;
Processing parameter is: the pH value is 5, and temperature is 30 ℃, and cathode current density is 2A/dm
2
D. opening power is carried out composite plating.
Embodiment 5
Take by weighing Ni (NH by calculating good amount
2SO
3)
24H
2O, NH
4Cl, H
3BO
3And C
12H
25SO
4Na adds a certain amount of water, is mixed with Ni (NH
2SO
3)
24H
2O 300g/L, NH
4Cl 15g/L, H
3BO
340g/L, C
12H
25SO
4The basic plating bath of Na 1g/L; With load weighted nano yttrium oxide and nano zircite uniform mixing, add in the basic plating bath again, fully stir, be mixed with and contain nano yttrium oxide 50g/L, nano zircite 30g/L, Ni (NH
2SO
3)
24H
2O 300g/L, NH
4Cl 15g/L, H
3BO
340g/L, C
12H
25SO
4The composite plating solution of Na 1g/L.
Prepare the method for composite deposite by this composite plating bath, comprise the following steps:
A. prepare composite plating bath;
B. select cathode base and anode substrate;
Cathode base selection stainless steel substrates (150mm * 20mm * 2mm), wherein the plating area is 50mm * 20mm, rest part is done insulation and is handled, anode substrate is a sheet nickel, nickel plate purity is greater than 99.9%, and the ratio of the area of negative and positive two-stage is 2: 3, and two interpole gaps are 30mm, before the plating, anticathode carries out the physics rust cleaning and electrochemical deoiling is handled;
C. determine the composite plating process parameter;
Processing parameter is: the pH value is 4, and temperature is 50 ℃, and cathode current density is 8A/dm
2
D. opening power is carried out composite plating.
Embodiment 6
Take by weighing Ni (NH by calculating good amount
2SO
3)
24H
2O, NH
4Cl, H
3BO
3And C
12H
25SO
4Na adds a certain amount of water, is mixed with Ni (NH
2SO
3)
24H
2O 300g/L, NH
4Cl 25g/L, H
3BO
325g/L, C
12H
25SO
4The basic plating bath of Na 5g/L; With load weighted nano yttrium oxide and nano zircite uniform mixing, add in the basic plating bath again, fully stir, be mixed with and contain nano yttrium oxide 5g/L, nano zircite 70g/L, Ni (NH
2SO
3)
24H
2O 300g/L, NH
4Cl 25g/L, H
3BO
325g/L, C
12H
25SO
4The composite plating solution of Na 5g/L.
Prepare the method for composite deposite by this composite plating bath, comprise the following steps:
A. prepare composite plating bath;
B. select cathode base and anode substrate;
Cathode base selection copper sheet (150mm * 20mm * 2mm), wherein the plating area is 50mm * 20mm, rest part is done insulation and is handled, anode substrate is a sheet nickel, nickel plate purity is greater than 99.9%, and the ratio of the area of negative and positive two-stage is 2: 3, and two interpole gaps are 30mm, before the plating, anticathode carries out the physics rust cleaning and electrochemical deoiling is handled;
C. determine the composite plating process parameter;
Processing parameter is: the pH value is 3, and temperature is 40 ℃, and cathode current density is 4A/dm
2
D. opening power is carried out composite plating.
The composite deposite for preparing among each embodiment is carried out ultrasonic cleaning, test its microhardness, load 50g, hold-time 10s; Adopt pin disc type friction wear testing machine that composite deposite is carried out friction-wear test, measure its frictional coefficient and wear rate.
The measurement result of the nickel coating that makes when not adding nanometer yttrium oxide and nano zircite in the measurement result of composite deposite, the basic plating bath among each embodiment, in basic plating bath, only add nanometer Y
2O
3The time Ni-Y that makes
2O
3The measurement result of coating and in basic plating bath, only add nanometer ZrO
2The time Ni-ZrO that makes
2The measurement result of coating sees Table 1.Measurement result shows that the composite deposite microhardness that the present invention obtains improves greatly, and properties of antifriction and wear resistance is good.
Table 1 measurement result
| Sample to be determined | Microhardness (HV) | Frictional coefficient | Wear rate (mg/min) |
| The composite deposite of embodiment 1 preparation | ??565 | ??0.35 | ??12.9 |
| The nickel coating for preparing down with embodiment 1 the same terms (does not add Y 2O 3And ZrO 2) | ??272 | ??0.79 | ??23.1 |
| Ni-Y with preparation under embodiment 1 the same terms 2O 3Coating | ??508 | ??0.40 | ??16.8 |
| Ni-ZrO with preparation under embodiment 1 the same terms 2Coating | ??512 | ??0.68 | ??16.2 |
| The composite deposite of embodiment 2 preparations | ??542 | ??0.36 | ??13.2 |
| The nickel coating for preparing down with embodiment 2 the same terms (does not add Y 2O 3And ZrO 2) | ??265 | ??0.82 | ??23.3 |
| Ni-Y with preparation under embodiment 2 the same terms 2O 3Coating | ??456 | ??0.39 | ??17.6 |
| Ni-ZrO with preparation under embodiment 2 the same terms 2Coating | ??490 | ??0.69 | ??17.8 |
| The composite deposite of embodiment 3 preparations | ??502 | ??0.38 | ??14.3 |
| The nickel coating for preparing down with embodiment 3 the same terms (does not add Y 2O 3And ZrO 2) | ??248 | ??0.83 | ??23.9 |
| Ni-Y with preparation under embodiment 3 the same terms 2O 3Coating | ??463 | ??0.43 | ??18.3 |
| Ni-ZrO with preparation under embodiment 3 the same terms 2Coating | ??489 | ??0.65 | ??17.9 |
| The composite deposite of embodiment 4 preparations | ??475 | ??0.40 | ??15.4 |
| The nickel coating for preparing down with embodiment 4 the same terms (does not add Y 2O 3And ZrO 2) | ??260 | ??0.82 | ??23.5 |
| Ni-Y with preparation under embodiment 4 the same terms 2O 3Coating | ??430 | ??0.43 | ??18.8 |
| Ni-ZrO with preparation under embodiment 4 the same terms 2Coating | ??465 | ??0.69 | ??17.5 |
| The composite deposite of embodiment 5 preparations | ??460 | ??0.43 | ??16.1 |
| The nickel coating for preparing down with embodiment 5 the same terms (does not add Y 2O 3And ZrO 2) | ??230 | ??0.79 | ??24.2 |
| Ni-Y with preparation under embodiment 5 the same terms 2O 3Coating | ??411 | ??0.45 | ??19.6 |
| Ni-ZrO with preparation under embodiment 5 the same terms 2Coating | ??446 | ??0.68 | ??18.9 |
| The composite deposite of embodiment 6 preparations | ??507 | ??0.35 | ??14.6 |
| The nickel coating for preparing down with embodiment 6 the same terms (does not add Y 2O 3And ZrO 2) | ??250 | ??0.80 | ??23.6 |
| Ni-Y with preparation under embodiment 6 the same terms 2O 3Coating | ??446 | ??0.42 | ??17.4 |
| Ni-ZrO with preparation under embodiment 6 the same terms 2Coating | ??472 | ??0.69 | ??18.6 |
Annotate: with the Ni-Y of preparation under embodiment 1 the same terms
2O
3Coating is meant and only adds nanometer Y in basic plating bath
2O
3, and nanometer Y among add-on and the embodiment 1
2O
3The coating that makes when identical of add-on; Ni-ZrO with preparation under embodiment 1 the same terms
2Coating is meant and only adds nanometer ZrO in basic plating bath
2, and nanometer ZrO among add-on and the embodiment 1
2The coating that makes when identical of add-on.Other can in like manner be known by inference.
The present invention is to be that example describes with nickel plating, but is not limited in nickel plating, also can be used for copper facing, zinc-plated and alloy plating etc.Variation, modification, interpolation or replacement that those skilled in the art are done in essential scope of the present invention also should belong to the scope of protection of the invention.
Claims (8)
1, a kind of composite plating bath that obtains high rigidity, anti-friction wear-resistant nano-composite plate is characterized in that main ingredient is:
Nano yttrium oxide 5～60g/L
Nano zircite 10～70g/L
Ni(NH
2SO
3)
2·4H
2O?????????200～500g/L
NH
4Cl????????????????????????5～30g/L
H
3BO
3???????????????????????10～80g/L
C
12H
25SO
4Na????????????????0.05～5g/L。
2, the composite plating bath of acquisition high rigidity according to claim 1, anti-friction wear-resistant nano-composite plate is characterized in that, wherein nano yttrium oxide particle grain size scope is 40～70nm.
3, the composite plating bath of acquisition high rigidity according to claim 1, anti-friction wear-resistant nano-composite plate is characterized in that, wherein nano zircite particle grain size scope is 45～75nm.
4, a kind ofly prepare the electro-plating method of composite deposite, it is characterized in that, comprise the following steps: by the described composite plating bath of claim 1
A. prepare composite plating bath;
B. select cathode base and anode substrate;
C. determine the composite plating process parameter;
D. opening power is carried out composite plating.
5, electro-plating method according to claim 4 is characterized in that, the composite plating bath main ingredient described in the step a is:
Nano yttrium oxide 5～60g/L
Nano zircite 10～70g/L
Ni(NH
2SO
3)
2·4H
2O?????200～500g/L
NH
4Cl????????????????????5～30g/L
H
3BO
3???????????????????10～80g/L
C
12H
25SO
4Na????????????0.05～5g/L。
6, electro-plating method according to claim 4 is characterized in that, wherein cathode base is stainless steel substrates or copper sheet, and anode substrate is a sheet nickel.
7, electro-plating method according to claim 4 is characterized in that, before the plating, anticathode carries out the physics rust cleaning and electrochemical deoiling is handled.
8, electro-plating method according to claim 4 is characterized in that, wherein the processing parameter of composite plating is:
PH value 3～5
30～50 ℃ of temperature
Cathode current density 2～8A/dm
2
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| US5266181A (en) * | 1991-11-27 | 1993-11-30 | C. Uyemura & Co., Ltd. | Controlled composite deposition method |
| CN1114720C (en) * | 1999-07-14 | 2003-07-16 | 昆明理工大学 | Process for electrically depositing multifunctional metal-base composite |
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