CN109355686A - A kind of alkali copper electrolyte using HEDP as main complexing agent and preparation method thereof and electroplating technology - Google Patents
A kind of alkali copper electrolyte using HEDP as main complexing agent and preparation method thereof and electroplating technology Download PDFInfo
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- CN109355686A CN109355686A CN201811514330.7A CN201811514330A CN109355686A CN 109355686 A CN109355686 A CN 109355686A CN 201811514330 A CN201811514330 A CN 201811514330A CN 109355686 A CN109355686 A CN 109355686A
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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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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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
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- Electroplating And Plating Baths Therefor (AREA)
Abstract
Alkali copper electrolyte that the invention discloses a kind of using HEDP as main complexing agent and preparation method thereof and electroplating technology, each component content is as follows in plating solution: content of copper ion 5-12g/L, HEDP content is 84-140g/L, auxiliary complex-former content is 13-30g/L, carbonic acid potassium content is 16-40g/L, ammonium salt class walks agent content as 0.4-4g/L, and anode dissolution agent content is 0.5-2g/L.Plating solution of the invention has good covering power and covering power, and binding force is good, under cooling thermal impact and the crossed grid skill in using a kitchen knife in cookery, shows excellent；Current density range is wider, up to 1-4A/dm2；Bath stability, each component keep balancing in the plating process；Each component chemical property is more stable, and during continuous electroplating, anti-oxidant anti-electrolysis performance is strong, consumes low；Current efficiency is high, reaches as high as 90%, can keep 60% or more substantially；Technology controlling and process is simple, and failure rate is low.
Description
Technical field
The present invention relates to electroplating technology technical fields, and in particular to a kind of electrolytic copper plating solution and preparation method thereof and galvanizer
Skill.
Background technique
Copper standard electrode potential calibration (compared to iron, aluminium, zinc electrode potential for), the copper facing on iron-based or Zinc Matrix
Layer belongs to cathodic coating, therefore, only just has mechanical protective effect to matrix when plated layer compact is non-porous.It was verified that some gold
Category is easy to deposit on copper, and binding force is good, therefore copper coating can be used as the bottom of pre-plating layer or multi-layer plating.Production at present
Upper common copper-plating technique has cyanide electroplating, acid copper-plating, pyrophosphate copper plating, also meets the non-cyanide alkali plating of clean manufacturing
Copper etc..The covering power and leveling ability of cyanide electroplating plating solution are good, and it is careful, good with the binding force of matrix that coating crystallizes, by compared with
Prolonged development, technology is quite mature, has been widely used for the bottoming coating of various metal matrix materials.But
The toxicity of cyanide is very big, and lethal dose is only 50mg, and China has put into effect related decree policy and has been forbidden to use cyanide plating.
Therefore, cyanide-free copper electroplating becomes imperative trend.In existing cyanide-free copper electroplating, especially using iron, aluminium, zinc class as matrix
In copper-plating technique, the plating solution situation bad in the prevalence of some defects and performance seriously restricts substitution cyanide electroplating
Process.
Summary of the invention
The technical problem to be solved by the present invention is in view of the shortcomings of the prior art, provide a kind of covering power and covering power
It is good, binding force is good, stable chemical performance, current efficiency are high using HEDP as the alkali copper electrolyte of main complexing agent and its preparation side
Method and electroplating technology.
In order to solve the above technical problems, the present invention adopts the following technical scheme: one kind is with HEDP(1-hydroxy ethylidene-1,1-diphosphonic acid)
Alkali copper electrolyte as main complexing agent, it is characterised in that: each component content is as follows in plating solution: copper ion Cu2+Content is 5-12g/
L, HEDP content are 84-140g/L, and auxiliary complex-former content is 13-30g/L, and carbonic acid potassium content is 16-40g/L, and ammonium salt class is walked
Position agent content is 0.4-4g/L, and anode dissolution agent content is 0.5-2g/L, and anode chaotropic agent is amino-containing compound.
Further, the temperature of the plating solution be 40-50 DEG C, current density 1-4A/dm2, slot coefficient be 13.026, roller
Revolving speed linear velocity is 0.8-1.2m/S, anode and cathode area ratio is 1:1.5-2, Anode-cathode Distance 50-80mm, preheating time 5-
10S, thickness of coating 1-1.5um.
Further, copper ion needed for providing plating solution using the raw material of copper sulphate, basic copper carbonate, Kocide SD.
Further, auxiliary complex-former is potassium citrate sodium, in sodium potassium tartrate tetrahydrate, ethylenediamine, biuret, triethanolamine
A kind of or several mixing compounding.
Further, ammonium salt class walks agent as one of ammonium carbonate, ammonium citrate, ammonium nitrate or several compounding.
Further, anode chaotropic agent is one of sulfamic acid, amion acetic acid, aminoglucose acid or several multiple
Match.
A kind of preparation method of the alkali copper electrolyte based on aforementioned using HEDP as main complexing agent, it is characterised in that: by following
Step carries out,
1) pure water is injected in stirring container first, main complexing agent HEDP is then weighed and is added in stirring container, stir to complete
Dissolution；
2) copper raw material is weighed, is added in stirring container by the expense that Molecular weights calculate copper ion, stirring is to being completely dissolved；
3) it weighs potassium hydroxide to be slowly added in stirring container, until plating solution PH is about 8, stirring is to being completely dissolved；
4) it weighs potassium carbonate to be added in stirring container, stirring is to being completely dissolved；
5) it weighs auxiliary complex-former to be added in stirring container, stirring is to being completely dissolved；
6) it weighs the agent that walks to be added in stirring container, stirring is to being completely dissolved；
7) it weighs anode chaotropic agent to be added in stirring container, stirring is to being completely dissolved；
8) stir 20 minutes or more, supplement pure water to setting value, stirring 60 minutes or more, filtering packing.
Preferably, a kind of preparation method of the alkali copper electrolyte based on aforementioned using HEDP as main complexing agent, it is characterised in that:
It carries out according to the following steps, the plating solution of every production 1000L:
1) pure water is injected in stirring container first, then weighing main complexing agent HEDP is 84-140kg, it is added in stirring container,
Stirring is to being completely dissolved；
2) copper raw material is weighed, expense of the copper ion in 8-12g/L is calculated by Molecular weights and is added in stirring container, stirring is extremely
It is completely dissolved；
3) it weighs potassium hydroxide to be slowly added in stirring container, controls temperature in container in order to avoid boiling, until plating solution PH is on 8 left sides
The right side, stirring is to being completely dissolved；
4) it weighs potassium carbonate 16-40kg to be added in stirring container, stirring is to being completely dissolved；
5) it weighs auxiliary complex-former 13-30kg to be added in stirring container, stirring is to being completely dissolved；
6) it weighs the agent 0.4-4kg that walks to be added in stirring container, stirring is to being completely dissolved；
7) it weighs anode chaotropic agent 0.5-2kg to be added in stirring container, stirring is to being completely dissolved；
8) stir 20 minutes or more, supplement pure water to 1000kg, stirring 60 minutes or more, filtering packing.
A kind of electroplating technology of the alkali copper electrolyte based on aforementioned using HEDP as main complexing agent, it is characterised in that: by following
Step carries out,
1) polishing oil removing: copper material surface to be plated is polished, and oil removing；
2) it washes: by the copper material to be plated after oil removing until being washed to clean surface no-sundries；
3) it sprays: preparing 5% dilute potassium carbonate solution, the dilute potassium carbonate solution of one layer 5% of spray after copper material to be plated washing；
4) its electroplating parameter direct copper plating copper facing: is pressed with the plating solution.
Plating solution of the invention has good covering power and covering power (uniformity COV≤10%) and covering power (right
In aperture 0.25mm, hole depth 1.5mm, depth capability T/P >=90%), binding force is good, under cooling thermal impact and the crossed grid skill in using a kitchen knife in cookery,
Show it is excellent (wherein cooling thermal impact mode are as follows: Hull cell sample is heated to 300-400 DEG C, is directly placed into cold water, coating without
Bubbling phenomenon；The crossed grid skill in using a kitchen knife in cookery: the scratch and scratch infall of coating are without skin effect phenomenon)；Current density range is wider, reachable
1-4A/dm2；Bath stability, each component keep balancing in the plating process；Each component chemical property is more stable, in continuous electroplating
In the process, anti-oxidant anti-electrolysis performance is strong, and consumption is low, and (1L plating solution continuous electroplating 40AH, plating solution performance is unchanged, plating solution principal component
Variation is little, it is only necessary to add the agent that walks within 0.1g)；Current efficiency is high, reaches as high as 90%, can keep 60% or more substantially；
Technology controlling and process is simple, and failure rate is low.
Specific embodiment
It is described further With reference to embodiment:
One, prepared by plating solution
Embodiment 1
The plating solution of every production 1000L:
1) pure water is injected in stirring container first, then weighing main complexing agent HEDP is 84kg, is added in stirring container, stirring
To being completely dissolved；
2) copper raw material is weighed, expense of the copper ion in 8g/L is calculated by Molecular weights and is added in stirring container, stir to complete
Fully dissolved；
3) it weighs potassium hydroxide to be slowly added in stirring container, controls temperature in container in order to avoid boiling, until plating solution PH 8, is stirred
It mixes to being completely dissolved；
4) it weighs potassium carbonate 16kg to be added in stirring container, stirring is to being completely dissolved；
5) it weighs potassium citrate sodium 13kg to be added in stirring container, stirring is to being completely dissolved；
6) it weighs ammonium carbonate 0.4kg to be added in stirring container, stirring is to being completely dissolved；
7) it weighs sulfamic acid 0.5kg to be added in stirring container, stirring is to being completely dissolved；
8) stir 20 minutes or more, supplement pure water to 1000kg, stirring 60 minutes or more, filtering packing.
Embodiment 2
The plating solution of every production 1000L:
1) pure water is injected in stirring container first, then weighing main complexing agent HEDP is 110kg, is added in stirring container, stirs
It mixes to being completely dissolved；
2) copper raw material is weighed, expense of the copper ion in 10g/L is calculated by Molecular weights and is added in stirring container, stir to complete
Fully dissolved；
3) it weighs potassium hydroxide to be slowly added in stirring container, controls temperature in container in order to avoid boiling, until plating solution PH 8, is stirred
It mixes to being completely dissolved；
4) it weighs potassium carbonate 28kg to be added in stirring container, stirring is to being completely dissolved；
5) it weighs sodium potassium tartrate tetrahydrate and ethylenediamine compounding (ratio 1:1) 22kg is added in stirring container, stirring is to being completely dissolved；
6) it weighs ammonium citrate 2.5kg to be added in stirring container, stirring is to being completely dissolved；
7) it weighs amion acetic acid 1.3kg to be added in stirring container, stirring is to being completely dissolved；
8) stir 20 minutes or more, supplement pure water to 1000kg, stirring 60 minutes or more, filtering packing.
Embodiment 3
The plating solution of every production 1000L:
1) pure water is injected in stirring container first, then weighing main complexing agent HEDP is 140kg, is added in stirring container, stirs
It mixes to being completely dissolved；
2) copper raw material is weighed, expense of the copper ion in 12g/L is calculated by Molecular weights and is added in stirring container, stir to complete
Fully dissolved；
3) it weighs potassium hydroxide to be slowly added in stirring container, controls temperature in container in order to avoid boiling, until plating solution PH 8, is stirred
It mixes to being completely dissolved；
4) it weighs potassium carbonate 40kg to be added in stirring container, stirring is to being completely dissolved；
5) it weighs biuret and triethanolamine compounding (ratio 2:1) 30kg is added in stirring container, stirring is to being completely dissolved；
6) it weighs ammonium citrate and ammonium nitrate compounding (ratio 3:1) 4kg is added in stirring container, stirring is to being completely dissolved；
7) it weighs amion acetic acid and aminoglucose acid compounding (ratio 1:1) 2kg is added in stirring container, stir to completely molten
Solution；
8) stir 20 minutes or more, supplement pure water to 1000kg, stirring 60 minutes or more, filtering packing.
Two, electroplating technology
1) polishing oil removing: copper material surface to be plated is polished, and oil removing；
2) it washes: by the copper material to be plated after oil removing until being washed to clean surface no-sundries；
3) it sprays: preparing 5% dilute potassium carbonate solution, the dilute potassium carbonate solution of one layer 5% of spray after copper material to be plated washing；
4) its electroplating parameter direct copper plating copper facing: is pressed with the plating solution.
The above has been described in detail, described above, is only a preferred embodiment of the present invention, when cannot
Limit practical range of the invention, i.e., it is all according to the made equivalent changes and modifications of the application range, it should still belong to the present invention and cover model
In enclosing.
Claims (9)
1. a kind of alkali copper electrolyte using HEDP as main complexing agent, it is characterised in that: each component content is as follows in plating solution: copper ion
Content is 5-12g/L, and HEDP content is 84-140g/L, and auxiliary complex-former content is 13-30g/L, and carbonic acid potassium content is 16-
40g/L, ammonium salt class walk agent content as 0.4-4g/L, and anode dissolution agent content is 0.5-2g/L, and anode chaotropic agent is containing amino
Compound.
2. the alkali copper electrolyte according to claim 1 using HEDP as main complexing agent, it is characterised in that: the temperature of the plating solution
For 40-50 DEG C, current density 1-4A/dm2, slot coefficient be 13.026, roller revolving speed linear velocity is 0.8-1.2m/S, anode and cathode
Area ratio is 1:1.5-2, Anode-cathode Distance 50-80mm, preheating time 5-10S, thickness of coating 1-1.5um.
3. the alkali copper electrolyte according to claim 1 using HEDP as main complexing agent, it is characterised in that: using copper sulphate,
Basic copper carbonate, Kocide SD raw material provide plating solution needed for copper ion.
4. the alkali copper electrolyte according to claim 1 using HEDP as main complexing agent, it is characterised in that: auxiliary complex-former is
One of potassium citrate sodium, sodium potassium tartrate tetrahydrate, ethylenediamine, biuret, triethanolamine or several mixing compounding.
5. the alkali copper electrolyte according to claim 1 using HEDP as main complexing agent, it is characterised in that: ammonium salt class walks agent
For one of ammonium carbonate, ammonium citrate, ammonium nitrate or several compounding.
6. the alkali copper electrolyte according to claim 1 using HEDP as main complexing agent, it is characterised in that: anode chaotropic agent is
One of sulfamic acid, amion acetic acid, aminoglucose acid or several compounding.
7. a kind of preparation method of the alkali copper electrolyte described in claim 1 using HEDP as main complexing agent, it is characterised in that: press
Following steps carry out,
1) pure water is injected in stirring container first, main complexing agent HEDP is then weighed and is added in stirring container, stir to complete
Dissolution；
2) copper raw material is weighed, is added in stirring container by the expense that Molecular weights calculate copper ion, stirring is to being completely dissolved；
3) it weighs potassium hydroxide to be slowly added in stirring container, until plating solution PH is about 8, stirring is to being completely dissolved；
4) it weighs potassium carbonate to be added in stirring container, stirring is to being completely dissolved；
5) it weighs auxiliary complex-former to be added in stirring container, stirring is to being completely dissolved；
6) it weighs the agent that walks to be added in stirring container, stirring is to being completely dissolved；
7) it weighs anode chaotropic agent to be added in stirring container, stirring is to being completely dissolved；
8) stir 20 minutes or more, supplement pure water to setting value, stirring 60 minutes or more, filtering packing.
8. a kind of preparation method of the alkali copper electrolyte as claimed in claim 7 using HEDP as main complexing agent, it is characterised in that: press
Following steps carry out, the plating solution of every production 1000L:
1) pure water is injected in stirring container first, then weighing main complexing agent HEDP is 84-140kg, it is added in stirring container,
Stirring is to being completely dissolved；
2) copper raw material is weighed, expense of the copper ion in 8-12g/L is calculated by Molecular weights and is added in stirring container, stirring is extremely
It is completely dissolved；
3) it weighs potassium hydroxide to be slowly added in stirring container, controls temperature in container in order to avoid boiling, until plating solution PH is on 8 left sides
The right side, stirring is to being completely dissolved；
4) it weighs potassium carbonate 16-40kg to be added in stirring container, stirring is to being completely dissolved；
5) it weighs auxiliary complex-former 13-30kg to be added in stirring container, stirring is to being completely dissolved；
6) it weighs the agent 0.4-4kg that walks to be added in stirring container, stirring is to being completely dissolved；
7) it weighs anode chaotropic agent 0.5-2kg to be added in stirring container, stirring is to being completely dissolved；
8) stir 20 minutes or more, supplement pure water to 1000kg, stirring 60 minutes or more, filtering packing.
9. a kind of electroplating technology of the alkali copper electrolyte based on as claimed in claim 2 using HEDP as main complexing agent, feature exist
In: it carries out according to the following steps,
1) polishing oil removing: copper material surface to be plated is polished, and oil removing；
2) it washes: by the copper material to be plated after oil removing until being washed to clean surface no-sundries；
3) it sprays: preparing 5% dilute potassium carbonate solution, the dilute potassium carbonate solution of one layer 5% of spray after copper material to be plated washing；
4) its electroplating parameter direct copper plating copper facing: is pressed with the plating solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811514330.7A CN109355686A (en) | 2018-12-12 | 2018-12-12 | A kind of alkali copper electrolyte using HEDP as main complexing agent and preparation method thereof and electroplating technology |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811514330.7A CN109355686A (en) | 2018-12-12 | 2018-12-12 | A kind of alkali copper electrolyte using HEDP as main complexing agent and preparation method thereof and electroplating technology |
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| CN109355686A true CN109355686A (en) | 2019-02-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110184631A (en) * | 2019-06-04 | 2019-08-30 | 广东达志环保科技股份有限公司 | A kind of cyanogen-less gold plating solution and preparation method thereof and electroplating technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550569A (en) * | 2009-04-13 | 2009-10-07 | 昆明理工大学 | Non-cyanide alkaline copper plating bath, preparation and use method thereof |
| CN104630847A (en) * | 2013-11-08 | 2015-05-20 | 无锡市雪江环境工程设备有限公司 | Electroplating solution for HEDP cyanide-free copper plating and electroplating method |
| CN107829116A (en) * | 2017-12-14 | 2018-03-23 | 广州三孚新材料科技股份有限公司 | Cyanide-free alkaline copper plating electroplate liquid |
-
2018
- 2018-12-12 CN CN201811514330.7A patent/CN109355686A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550569A (en) * | 2009-04-13 | 2009-10-07 | 昆明理工大学 | Non-cyanide alkaline copper plating bath, preparation and use method thereof |
| CN104630847A (en) * | 2013-11-08 | 2015-05-20 | 无锡市雪江环境工程设备有限公司 | Electroplating solution for HEDP cyanide-free copper plating and electroplating method |
| CN107829116A (en) * | 2017-12-14 | 2018-03-23 | 广州三孚新材料科技股份有限公司 | Cyanide-free alkaline copper plating electroplate liquid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110184631A (en) * | 2019-06-04 | 2019-08-30 | 广东达志环保科技股份有限公司 | A kind of cyanogen-less gold plating solution and preparation method thereof and electroplating technology |
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Application publication date: 20190219 |