CN108588768B - Steel and iron parts alkalinity deep hole nickel-plating additive, pre-plating solution and pre-plating process - Google Patents
Steel and iron parts alkalinity deep hole nickel-plating additive, pre-plating solution and pre-plating process Download PDFInfo
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- CN108588768B CN108588768B CN201810529343.5A CN201810529343A CN108588768B CN 108588768 B CN108588768 B CN 108588768B CN 201810529343 A CN201810529343 A CN 201810529343A CN 108588768 B CN108588768 B CN 108588768B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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Abstract
The present invention relates to a kind of steel and iron parts alkalinity deep hole nickel-plating additive, pre-plating solution and pre-plating process.Steel and iron parts alkalinity deep hole nickel-plating additive includes open cylinder agent and deep hole agent, and the open cylinder agent is by following material composition: alkalescent complexing agent, alcohol compound, additive A, anionic surfactant, chloride, fluoride, aldehyde compound, alkaloid compound, phosphate compounds, boric acid and/or borate compound；The deep hole agent is by following material composition: phosphate compounds, alkaloid compound, chloride, aldehyde compound, additive B.Pre-plating solution includes seven water nickel sulfates and above-mentioned nickel-plating additive, wherein contains seven water nickel sulfate 15-35g/L, open cylinder agent 200-250g/L, deep hole agent 15-30g/L, the pH value of steel and iron parts alkalinity deep hole nickel plating pre-plating solution is 8.5-10.0.The present invention can inner wall disposably completes preplating at article surface and product tube wall, deep hole simultaneously, and solves the problems of dissolution of nickel anode simultaneously, and the present invention is free of the alkaline deep hole nickel plating technology of ammonia, reduces secondary pollution.
Description
Technical field
The present invention relates to the electroplating technologies of electro-deposition, more particularly, to steel and iron parts alkalinity deep hole nickel-plating additive, in advance
Plating solution and pre-plating process.
Background technique
The Protective-deeorative plating of current steel and iron parts, when steel and iron parts are directly electroplated in acid copper sulfate solution, due to copper
It is differed farther out with the normal potential of iron, before steel and iron parts immersion solution and electric current are not yet connected, meeting fast exchange is heavy on matrix
Product goes out the very poor loose layers of copper of binding force.Therefore, necessary before steel member acidic copper facing in order to obtain the good electroplated layer of binding force
Carry out preplating.Other than the product high to quality requirements is using MULTI-LAYER NICKEL, chromium plating, most products are first plated on steel substrate
After upper one layer 0.2-0.5 microns thick of pre-plating layers, then carry out acid bright copper plating then nickel plating, chromium or other coating again.
Now common pre- electroplating method have faintly acid nickel plating, organic phosphonate cyanide-free alkaline copper plating, acidic nickel plating, neutrality or
Alkalescent nickel plating and cyanide electroplating etc..It is current since cyanide copper plating process has the advantages that performance is good, at low cost, management is easy
Most widely used pre-plating process in production, but since cyanide copper plating process is because containing hypertoxic cyanide, country has prohibited or limited
System uses.Several pre- electroplating methods above-mentioned, can solve the better simply steel and iron parts preplating of shape, but for tubulose or complex-shaped
Deep hole part, because coating is very thin inside pipe wall after preplating and deep hole or at all can not plate coating, when subsequent production, will appear plating
The bad defect that copper powder is generated with steel inside pipe wall and deep hole position of layer binding force.Therefore, seek that a kind of production cost is low, quality
Stablize, without hypertoxic cyanide and be suitble to the pre- electroplating method of all steel and iron parts (including tube-like piece and deep hole part), is always the country
The hot subject that foreign-plated worker competitively studies.
Last decade reduces environmental pollution to replace the cyanide of severe toxicity, the research of the domestic and international pre- coating technology of steel and iron parts
Achievement more successfully has the copper facing of alkaline phosphonate type multicomponent complex, acid direct copper pre-plating, also has using alkaline nickel preplating
Report.Acid nickel preplating is because nickel high price is expensive, and sulfur acid nickel 150-200g/L in solution, heavy metal nickel concentration is higher, raw
Produce and environmental protection treatment expense it is larger, chemical nickel plating pre-plating process will be regularly updated because plating solution life cycle is short, production cost compared with
Height, only producer can just use under particular/special requirement；Organic phosphonate multicomponent complex alkaline copper plating technique, is presently preferred
Environment-friendly type preplating new process, but it fails to solve steel tube-like piece in preplating and the binding force and copper powder of deep hole part inner wall are asked
Topic；The alkaline nickel plating technology reported or produced and used at present, uses the higher ammonium hydroxide of concentration or ammonium-containing compound, production site
Ammonia taste is dense, generates secondary pollution.In addition, there is the dissolution supplement that not can effectively solve nickel anode in existing alkalinity nickel plating technology
Problem, the nickel glue compounds that can generate a large amount of greens when production on anode make Bath mudding, and blocking filtering stamen hole simultaneously generates big
Measure foam.The anodic solution problem of alkaline deep hole nickel plating technology, which normally produces nickel plating, to be had a major impact, and is showed themselves in that
(1) anode surface when production is made to produce green glue object, it is suppressed that anodic solution, nickel ion in plating solution when making to produce
Concentration constantly declines and affects preplating quality；
(2) the green glue object generated on anode, which can float in the plating solution, makes plating solution generate muddiness；
(3) the green object generated on anode can also generate colloid (such as NiOHCl) other than being nickel hydroxide and block
Stamen filter opening to be filtered, filtration difficult is made, the sediment and colloid in plating solution can also cause to generate a large amount of foams when inflating production,
Even overflow outside slot.
Currently, having no the research report to the production anodic control dissolution of alkali nickel in the prior art；Both alkaline deep hole had been can solve
Effective problems of dissolution of nickel anode and can disposably complete steel and iron parts (including tube-like piece and deep hole part) preplating technology more
There is not yet report.
Summary of the invention
Based on this, the object of the present invention is to provide a kind of steel and iron parts alkalinity deep hole nickel-plating additive, pre-plating solution and preplating
Technique solves steel substrate in electroplating bright acid under the premise of meeting plating user to production cost and environmental protection requirement
The binding force problem of pre-plating layer and matrix before copper；Can simultaneously at article surface and product tube wall, deep hole inner wall it is disposable
Preplating is completed, and fine and close nickel coating on the pipe fitting and deep hole part inner wall that electric current cannot reach also chemical plating, the present invention adopt
With the alkaline deep hole nickel plating technology for being free of ammonia, reduces secondary pollution, improve production environment, while solving the molten of nickel anode
Solution problem, make plating solution nickel ion concentration keep stablize, also overcoming makes Bath mudding because anodic solution is bad, it is difficult to filtering and
Occurs the problem of a large amount of foams in air stirring.
The present invention is achieved by the following technical solutions:
A kind of steel and iron parts alkalinity deep hole nickel-plating additive, characterized by comprising: open cylinder agent and deep hole agent, the open cylinder agent
By following material composition: (1) the alkalescent complexing agent of complex compound can be formed with nickel ion；(2) alcohol compound；(3) additive
A, one in propinyl sodium sulfonate, butynediols ethyoxyl ether, propine alcohol ethoxy ether, pyridine hydroxypropyl sulfobetaines
Kind is to three kinds；(4) anionic surfactant；(5) chloride；(6) fluoride；(7) aldehyde compound；(8) alkaloid compound；
(9) phosphate compounds；(10) boric acid and/or borate compound；The deep hole agent is by following material composition: (1) phosphate
Compound；(2) alkaloid compound；(3) chloride；(4) aldehyde compound；(5) additive B is selected from pyridine hydroxypropyl sulfo group sweet tea
Dish alkali, propine alcohol ethoxy ether, in propinyl sodium sulfonate one kind to two kinds.
Further, in the open cylinder agent, (1) can form the alkalescent complexing agent of complex compound with nickel ion, selected from burnt phosphorus
One of hydrochlorate, tartrate, citrate, edetate, nitrilotriacetic acid salt, triethanolamine are to four kinds；(2) alcohol
Class compound, selected from one of ethyl alcohol, methanol, glycerine to two kinds；(4) anionic surfactant is selected from isethionic acid
One of sodium, succinic acid dihexyl sodium sulfonate, lauryl sodium sulfate are to two kinds；(5) chloride is selected from sodium chloride, potassium chloride
One of to two kinds；(6) fluoride is selected from one of potassium fluoride, sodium fluoride, potassium hydrogen fluoride to two kinds；(7) aldehydes chemical combination
Object is selected from one of formaldehyde, acetaldehyde, chloraldurate to two kinds；(8) alkaloid compound is in sodium hydroxide, potassium hydroxide
One kind is to two kinds；(9) phosphate compounds is selected from one of disodium hydrogen phosphate, tertiary sodium phosphate to two kinds；(10) boric acid
And/or borate compound is selected from one of boric acid, borax to two kinds.
Further, in the deep hole agent, (1) phosphate compounds is selected from sodium hypophosphite, disodium hydrogen phosphate, tertiary sodium phosphate
One of to two kinds；(2) alkaloid compound is selected from one of sodium hydroxide, potassium hydroxide to two kinds；(3) chloride is selected from
One of sodium chloride, potassium chloride are to two kinds；(4) aldehyde compound is selected from one of formaldehyde, acetaldehyde, chloraldurate to two
Kind.
The each component weight in every liter of open cylinder agent aqueous solution as a preferred method, are as follows: alkalescent complexing agent 265-540
Gram, 1-15 grams of alcohol compound, 0.03-0.55 grams of additive A, 0.05-2.01 grams of anionic surfactant, chloride 2-
21 grams, 2-15 grams of fluoride, 0.3-1.5 grams of aldehyde compound, 50-80 grams of alkaloid compound, 10-40 grams of phosphate compounds,
Boric acid and/or 7-22 grams of borate compound.
Further, each component weight in every liter of open cylinder agent aqueous solution are as follows: 100-150 grams of potassium pyrophosphate, potassium tartrate
150-200 grams of sodium, 10-30 grams of sodium citrate, 8-20 grams of disodium ethylene diamine tetraacetate, 10-30 grams of sodium ammonium triacetate, triethanolamine
5-15 grams, 1-5 grams of ethyl alcohol, 0.03-0.1 grams of ether of propine alcohol ethoxy, 0.1-1.0 grams of sulfobetaines of pyridine hydroxypropyl, hydroxyl second
0.5-1.0 grams of base sodium sulfonate, 0.005-0.01 grams of lauryl sodium sulfate, 3-20 grams of potassium chloride, 2-15 grams of potassium fluoride, formaldehyde
0.5-1.0 grams, 50-80 grams of potassium hydroxide, 20-40 grams of disodium hydrogen phosphate, 10-20 grams of boric acid.
As an implementation, each component weight in every liter of deep hole agent aqueous solution are as follows: phosphate compounds 270-480
Gram, 7-25 grams of alkaloid compound, 6-15 grams of chloride, 0.1-1 grams of aldehyde compound, 0.03-3.2 grams of additive B.
Further, each component weight in every liter of deep hole agent aqueous solution are as follows: 250-400 grams of sodium hypophosphite, phosphoric acid hydrogen two
20-50 grams of sodium, 5-15 grams of potassium hydroxide, 8-15 grams of potassium chloride, 0.5-1 grams of formaldehyde, pyridine hydroxypropyl sulfobetaines 0.3-3
Gram, 0.03-0.2 grams of ether of propine alcohol ethoxy, surplus is water.
The present invention also provides a kind of steel and iron parts alkalinity deep hole nickel plating pre-plating solutions, it is characterised in that: including seven water nickel sulfates and
Steel and iron parts alkalinity deep hole nickel-plating additive as claimed in claim 1 to 7, wherein contain seven water nickel sulfate 15-35g/L, open cylinder
Agent 200-250g/L, deep hole agent 15-30g/L, the pH value of steel and iron parts alkalinity deep hole nickel plating pre-plating solution are 8.5-10.0.
Nickel-plating additive open cylinder agent and deep hole of the invention is added in the solution that alkaline medium and nickel salt form in the present invention
Agent, using nickel-plating additive to the stable bond of nickel ion, polarization and selective absorption effect on cathode and anode make to plate
Layer energy uniform and delicate is deposited on product simultaneously and nickel anode is enable normally to dissolve, final to obtain the good pre-plating layer of binding force.
Heavy metal nickel concentration only has 4-7 grams per liter in electroplate liquid of the invention, belongs to low metal concentration process, in plating solution both
It is free of the cyanide and irritation ammoniate of severe toxicity again without lead, cadmium, mercury and Cr VI, is easy to after electroplating wastewater acidification contact break
Precipitation process, production cost is close with cyanide electroplating, has reached requirement of the user to preplating cost and environmental protection.
The present invention also provides a kind of preparation methods of steel and iron parts alkalinity deep hole nickel plating pre-plating solution, it is characterised in that including following
Step:
(1) add water toward coating bath, additional amount is 2/3rds of predetermined volume, 50-55 DEG C is heated to, by required open cylinder agent
It is added in slot with deep hole agent, then the sodium hydroxide of 0.3g/L, stirring and dissolving is added by predetermined volume；
(2) after dissolving seven required water nickel sulfates with water, coating bath is added portionwise under stirring, solution is adjusted into pH to 8.5-
10.0, it adds water to predetermined volume and obtains steel and iron parts alkalinity deep hole nickel plating pre-plating solution.
The present invention also provides a kind of steel and iron parts alkalinity deep hole nickel plating pre-plating process, it is characterised in that the following steps are included:
(1) pre-plating solution is prepared according to the above method, continuously filters 4-6 hours, while coating bath with the filter with active carbon
In be linked into steel and iron parts 0.5-2.0A/dm to be plated2Current cathode, which is powered, to be electrolysed 1-2 hours, and the steel and iron parts to be plated are being linked into plating
By following processing before slot: steel and iron parts → electrochemical deoiling → washing → acid pickling and rust removing → washing → alkaline electrolysis oil removing to be plated →
Washing → weak sulfuric acid activated → washing；
(2) pre-plating solution is adjusted to starting preplating after 30-45 DEG C.
Steel and iron parts alkalinity deep hole nickel-plating additive, pre-plating solution and pre-plating process of the invention, has the advantages that
(1) present invention is acted on by nickel ion and multicomponent complex, generates stable polynary nickel complex ion.When plating, one
Aspect, since cathodic polarization increases, the discharge potential of nickel complex ion is increased, and reaches optimal discharge performance, and it is careful to obtain crystallization
Nickel coating, on the other hand, due to the reducing agent composition in additive containing chemical nickel plating, in the pipe fitting that electric current cannot reach and
Deep hole part inner wall also disposably fine and close nickel coating in chemical plating.Cyanide electroplating/acidic nickel plating/alkali that the prior art uses
Property cyanide-free copper electroplating/alkalinity deep hole nickel plating not in preplating simultaneously at article surface and product tube wall, deep hole inner wall it is primary
Property complete preplating property.
(2) conventional alkaline deep hole nickel plating, contains the higher ammonium salt of concentration and ammonium hydroxide, and ammonia is seriously polluted when production, and
The present invention reduces secondary pollution using the alkaline deep hole nickel plating technology for being free of ammonia by the compound action of additive, improves
Production environment.
(3) alkaline deep hole nickel plating electroplating additive of the invention, is to study to obtain by many years of applicant, by this hair
The application of bright alkalinity deep hole nickel plating electroplating additive makes best section of nickel anode when producing in passivation with activation, solves
The problem of number of drawbacks caused by nickel anode solubilizing poorly, makes plating solution nickel ion concentration keep stablizing, also overcomes because of anode
Solubilizing poorly and make Bath mudding, it is difficult to filtering and occur the problem of a large amount of foams in air stirring.
In order to better understand and implement, the present invention will be described in detail With reference to embodiment.
Specific embodiment
The unit of each raw material is g/L in following example 1~12.
Embodiment 1
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 2
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 3
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 4
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 5
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 6
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 7
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 8
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 9
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 10
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 10-1
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 10-2
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 10-3
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 10-4
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 11
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 11-1
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 11-2
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 11-3
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 11-4
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 12
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 12-1
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 12-2
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 12-3
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 12-4
The steel and iron parts alkalinity deep hole nickel-plating additive of the present embodiment, including open cylinder agent and deep hole agent, surplus are water.Wherein open
The formula of cylinder agent is as follows:
The formula of deep hole agent is as follows:
Embodiment 13
Steel and iron parts alkalinity deep hole nickel plating pre-plating solution, including seven water nickel sulfates and steel and iron parts alkalinity deep hole nickel-plating additive, steel
Ironware alkalinity deep hole nickel-plating additive includes open cylinder agent and deep hole agent again.Wherein, seven water nickel sulfate contents are 15-35g/L, open cylinder
Agent 200-250g/L, deep hole agent 15-30g/L, the pH value of steel and iron parts alkalinity deep hole nickel plating pre-plating solution are 8.5-10.0.
Pre-plating solution the preparation method is as follows:
(1) add water toward coating bath, additional amount is 2/3rds of predetermined volume, is heated to 50-55 DEG C, needed for being calculated
Open cylinder agent and deep hole agent be added slot in, then by predetermined volume be added 0.3g/L sodium hydroxide, stirring and dissolving；
(2) after dissolving seven required water nickel sulfates with water, coating bath is added portionwise under stirring, solution is adjusted into pH to 8.5-
10.0, it adds water to predetermined volume and obtains steel and iron parts alkalinity deep hole nickel plating pre-plating solution.
Respectively to above embodiments 1-9, embodiment 10.1~10.4, embodiment 11.1~11.4, embodiment 12.1~
12.4 steel and iron parts alkalinity deep hole nickel-plating additive (totally 21 formulas) is configured to steel by following three kinds of modes with seven water nickel sulfates
Ironware alkalinity deep hole nickel plating pre-plating solution, 63 kinds of pre-plating solutions available in this way (number is 1~No. 63 respectively).
Plating solution cost of the invention be only 6-8 member/liter, it is suitable with the existing cyanide electroplating plating solution cost largely used, with
Cyanide-free alkaline copper plating is compared, and plating solution cost is only its half to a quarter.
Alkali nickel plating bath of the invention is free of ammonium hydroxide, the secondary pollution without ammonia in the existing conventional alkali nickel plating bath of appearance,
This invention also solves the normal problems of dissolution of nickel anode, keep plating solution more stable, can be used for a long time.
Bath element of the present invention is simple, and operation is easy, and performance is stablized, and meets the technical requirements of national clean manufacturing.
Embodiment 14
The steel and iron parts alkalinity deep hole nickel plating pre-plating process of the present embodiment, step include:
(1) pre-plating solution is continuously filtered 4-6 hours with the filter with active carbon, while steel and iron parts to be plated are linked into coating bath
Use 0.5-2.0A/dm2Current cathode be powered electrolysis 1-2 hours, in coating bath the ratio between cathode area and annode area be 1:(1.5~
2.5), the steel and iron parts to be plated pass through following processing: steel and iron parts → electrochemical deoiling → washing → acid to be plated before being linked into coating bath
Remove rust → washing → alkaline electrolysis oil removing → washing → weak sulfuric acid activated → washing；
(2) pre-plating solution is adjusted to starting preplating after 30-45 DEG C.
Preplating test is carried out using the 0.2mm thick cold rolled steel sheet of 63 5 × 5cm of test piece, number 1-63, respectively corresponds reality
The 1-63 pre-plating solution for applying the preparation of example 13 is handled, table specific as follows by above-mentioned pre-plating process:
It can be further continued for plating acid copper after the above alkalinity nickel preplating, its step are as follows: recycling → washing → faintly acid activation
→ washing → plating Technology Bright Acidic copper to finished product.
The test of 15 coating of embodiment
(1) binding force of cladding material is tested
To the plating piece handled through steel and iron parts alkalinity deep hole nickel plating pre-plating process of the present invention in embodiment 14, nickel preplating is chosen
With a thickness of plated again after 0.15 μm, 0.22 μm, 0.51 μm of plating piece and nickel preplating acid copper overall thickness be 6.1 μm, 8.2 μm,
10.5 μm, 15.2 μm of plating piece press " GB235-82 reverse bend test of metal method " respectively, take alternating bending to fractureing and
Plating piece is heated to taking out two kinds of test methods of chilling in room temperature water immediately after 300 ± 25 DEG C, coating is not blistering, no after test
Decortication is considered as that binding force is good, and test result is as follows:
(2) cathode deposition velocity is tested
It selects different test pieces (the 0.2mm thick cold rolled steel sheet of 5 × 5cm), the pre-plating solution that embodiment 13 is prepared, with embodiment
14 pre-plating process is electroplated 10 minutes under different current densities, and the method for being converted into average thickness with coating weighing, measurement is not
With the deposition velocity of coating under cathode-current density.
| Cathode-current density (A/dm2) | Alkali nickel coating deposition velocity (micro- m/min) |
| 0.5 | 0.12 |
| 1.0 | 0.22 |
| 1.5 | 0.28 |
| 2.0 | 0.31 |
(3) covering power is tested
Diameter 2mm, 4mm, 6mm, hole depth 50mm are taken respectively, and one end is three kinds of iron pipes of blind hole, immerses embodiment 13 respectively
63 kinds of pre-plating solutions, be electroplated 6 minutes, aperture is upward, complete to immerse in pre-plating solution when plating, and test obtains the upper plating rate result of iron pipe
It is as follows:
| Deep hole iron pipe diameter (mm) | Blind hole depth (mm) | Plating rate (%) on inner hole |
| 2 | 50 | 100 |
| 4 | 50 | 100 |
| 6 | 50 | 100 |
As it can be seen that being 100% to plating rate on the inner hole of iron pipe using nickel-plating additive and pre-plating solution of the invention.
Using additive of the invention, preplating, alkalinity can be carried out to steel and iron parts and its deep hole part in weakly alkaline solution
The pre- matrix of pre-nickel plating and subsequent acid bright copper plating binding force are good, to really effectively solve steel and iron parts and its deep hole part
Galvanization coating binding force problem.
The test of 16 nickel anode solubility property of embodiment
Steps are as follows for test method:
(1) it is tested with 250 milliliters of Hull slots, 3 kinds of different preplating formula of liquid: prior art A are respectively adopted in test
Any one in the 1-63 pre-plating solution of company's pre-plating solution, prior art B company's pre-plating solution and the embodiment of the present invention 13；
(2) select nickel anode surface area for 0.25dm2, total current 0.5A adds air stirring；
(3) according to different electroplating times, the area for occurring green insoluble matter on anode is calculated, to account for the total face of anode surface
Long-pending percentage calculates, and test result is as follows:
Embodiment 17
The present embodiment is carried out to through steel and iron parts alkalinity deep hole nickel plating technology and other electroplating technologies of the prior art of the invention
Contrast on effect is as follows:
Preferable embodiment of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but
It cannot be understood as the limitations to patent of invention range.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.
Claims (10)
1. a kind of steel and iron parts alkalinity deep hole nickel-plating additive, characterized by comprising: open cylinder agent and deep hole agent,
The open cylinder agent is by following material composition:
(1) the alkalescent complexing agent of complex compound can be formed with nickel ion；
(2) alcohol compound, selected from one of ethyl alcohol, methanol, glycerine to two kinds；
(3) additive A is selected from propinyl sodium sulfonate, butynediols ethyoxyl ether, propine alcohol ethoxy ether, pyridine hydroxypropyl sulphur
One of base glycine betaine is to three kinds；
(4) anionic surfactant；
(5) chloride；
(6) fluoride；
(7) aldehyde compound, selected from one of formaldehyde, acetaldehyde, chloraldurate to two kinds；
(8) alkaloid compound, selected from one of sodium hydroxide, potassium hydroxide to two kinds；
(9) phosphate compounds；
(10) boric acid and/or borate compound；
The deep hole agent is by following material composition:
(1) phosphate compounds；
(2) alkaloid compound, selected from one of sodium hydroxide, potassium hydroxide to two kinds；
(3) chloride；
(4) aldehyde compound, selected from one of formaldehyde, acetaldehyde, chloraldurate to two kinds；
(5) additive B, one kind is to two in pyridine hydroxypropyl sulfobetaines, propine alcohol ethoxy ether, propinyl sodium sulfonate
Kind.
2. steel and iron parts alkalinity deep hole nickel-plating additive according to claim 1, it is characterised in that: in the open cylinder agent,
(1) the alkalescent complexing agent that complex compound can be formed with nickel ion, is selected from pyrophosphate, tartrate, citrate, second two
One of amine tetraacetate, nitrilotriacetic acid salt, triethanolamine are to four kinds；
(4) anionic surfactant is in sodium isethionate, succinic acid dihexyl sodium sulfonate, lauryl sodium sulfate
One kind is to two kinds；
(5) chloride is selected from one of sodium chloride, potassium chloride to two kinds；
(6) fluoride is selected from one of potassium fluoride, sodium fluoride, potassium hydrogen fluoride to two kinds；
(9) phosphate compounds is selected from one of disodium hydrogen phosphate, tertiary sodium phosphate to two kinds；
(10) boric acid and/or borate compound are selected from one of boric acid, borax to two kinds.
3. steel and iron parts alkalinity deep hole nickel-plating additive according to claim 2, it is characterised in that: in the deep hole agent,
(1) phosphate compounds is selected from one of sodium hypophosphite, disodium hydrogen phosphate, tertiary sodium phosphate to two kinds；
(3) chloride is selected from one of sodium chloride, potassium chloride to two kinds.
4. steel and iron parts alkalinity deep hole nickel-plating additive according to claim 1, it is characterised in that: water-soluble in every liter of open cylinder agent
Each component weight in liquid are as follows: 265-540 grams of alkalescent complexing agent, 1-15 grams of alcohol compound, 0.03-0.55 grams of additive A, yin
0.05-2.01 grams of ionic surface active agent, 2-21 grams of chloride, 2-15 grams of fluoride, 0.3-1.5 grams of aldehyde compound, bases
50-80 grams of compound, 10-40 grams of phosphate compounds, boric acid and/or 7-22 grams of borate compound.
5. steel and iron parts alkalinity deep hole nickel-plating additive according to claim 4, it is characterised in that: water-soluble in every liter of open cylinder agent
Each component weight in liquid are as follows: 100-150 grams of potassium pyrophosphate, 150-200 grams of sodium potassium tartrate tetrahydrate, 10-30 grams of sodium citrate, ethylenediamine
8-20 grams of tetraacethyl disodium, 10-30 grams of sodium ammonium triacetate, 5-15 grams of triethanolamine, 1-5 grams of ethyl alcohol, propine alcohol ethoxy ether
0.03-0.1 grams, 0.1-1.0 grams of sulfobetaines of pyridine hydroxypropyl, 0.5-1.0 grams of sodium isethionate, lauryl sodium sulfate
0.005-0.01 grams, 3-20 grams of potassium chloride, 2-15 grams of potassium fluoride, 0.5-1.0 grams of formaldehyde, 50-80 grams of potassium hydroxide, phosphoric acid hydrogen two
20-40 grams of sodium, 10-20 grams of boric acid.
6. steel and iron parts alkalinity deep hole nickel-plating additive according to claim 4, it is characterised in that: water-soluble in every liter of deep hole agent
Each component weight in liquid are as follows: 270-480 grams of phosphate compounds, 7-25 grams of alkaloid compound, 6-15 grams of chloride, aldehydes chemical combination
0.1-1 grams of object, 0.03-3.2 grams of additive B.
7. steel and iron parts alkalinity deep hole nickel-plating additive according to claim 6, it is characterised in that: water-soluble in every liter of deep hole agent
Each component weight in liquid are as follows: 250-400 grams of sodium hypophosphite, 20-50 grams of disodium hydrogen phosphate, 5-15 grams of potassium hydroxide, potassium chloride 8-
15 grams, 0.5-1 grams of formaldehyde, 0.3-3 grams of sulfobetaines of pyridine hydroxypropyl, 0.03-0.2 grams of ether of propine alcohol ethoxy, surplus is
Water.
8. a kind of steel and iron parts alkalinity deep hole nickel plating pre-plating solution, it is characterised in that: any including seven water nickel sulfates and claim 1-7
The steel and iron parts alkalinity deep hole nickel-plating additive, wherein contain seven water nickel sulfate 15-35g/L, open cylinder agent 200-250g/L, it is deep
Hole agent 15-30g/L, the pH value of steel and iron parts alkalinity deep hole nickel plating pre-plating solution are 8.5-10.0.
9. the preparation method of steel and iron parts alkalinity deep hole nickel plating pre-plating solution according to claim 8, it is characterised in that including with
Lower step:
(1) add water toward coating bath, additional amount is 2/3rds of predetermined volume, 50-55 DEG C is heated to, by required open cylinder agent and depth
Hole agent is added in slot, then the sodium hydroxide of 0.3g/L, stirring and dissolving are added by predetermined volume；
(2) after dissolving seven required water nickel sulfates with water, coating bath is added portionwise under stirring, solution is adjusted into pH to 8.5-
10.0, it adds water to predetermined volume and obtains steel and iron parts alkalinity deep hole nickel plating pre-plating solution.
10. a kind of steel and iron parts alkalinity deep hole nickel plating pre-plating process, it is characterised in that the following steps are included:
(1) pre-plating solution is prepared by claim 9, is continuously filtered 4-6 hours with the filter with active carbon, while being hung in coating bath
Enter steel and iron parts 0.5-2.0A/dm to be plated2Current cathode be powered electrolysis 1-2 hours, the steel and iron parts to be plated be linked into coating bath it
It is preceding to pass through following processing: steel and iron parts → electrochemical deoiling → washing → acid pickling and rust removing → washing → alkaline electrolysis oil removing → washing to be plated
It is → weak sulfuric acid activated → to wash；
(2) pre-plating solution is adjusted to starting preplating after 30-45 DEG C.
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| CN110344088B (en) * | 2019-08-26 | 2021-05-07 | 钢铁研究总院 | Deep hole nickel electroplating solution and preparation method thereof |
| CN113151869A (en) * | 2021-04-13 | 2021-07-23 | 苏州磊屹光电科技有限公司 | Nickel pretreatment method for improving appearance of stainless steel/foreign copper material nickel layer |
| CN114059053B (en) * | 2021-11-09 | 2023-10-10 | 苏州汉宜纳米新材料有限公司 | Electroless Ni-W-P plating solution and preparation method thereof, ni-W-P plating layer and preparation method thereof |
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