CN109457238A - Stable chemical bronze plating liquid and preparation method thereof at a high speed - Google Patents
Stable chemical bronze plating liquid and preparation method thereof at a high speed Download PDFInfo
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- CN109457238A CN109457238A CN201811592325.8A CN201811592325A CN109457238A CN 109457238 A CN109457238 A CN 109457238A CN 201811592325 A CN201811592325 A CN 201811592325A CN 109457238 A CN109457238 A CN 109457238A
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- high speed
- plating liquid
- bronze plating
- chemical bronze
- stable
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
Abstract
The invention discloses a kind of chemical bronze plating liquids and preparation method thereof that high speed is stable, the stable chemical bronze plating liquid of the high speed includes following components by volumetric concentration: Salzburg vitriol 8g/L~25g/L, 15~40g/L of sodium potassium tartrate tetrahydrate, 5~20ml/L of formaldehyde, 5~20g/L of sodium hydroxide, 10~500mg/L of stabilizer, surplus are water.The stable chemical bronze plating liquid of the high speed further includes combined additive, and ammonia carboxylic compound of the combined additive by thiourea derivative and containing hydroxyalkyl forms.Salzburg vitriol is miscible with water, after being stirred well to solution clarification, sodium potassium tartrate tetrahydrate, stabilizer, combined additive, sodium hydroxide, formaldehyde are sequentially added, solution clarification is stirred well to, with water constant volume, the stable chemical bronze plating liquid of high speed can be obtained.The stable chemical bronze plating liquid of high speed in the present invention, deposition velocity meet functional chemical copper facing requirement in 10 μm/h or more, bath stability, copper plate even uniform.
Description
Technical field
The present invention relates to nonmetallic surface electroless plating technology field more particularly to a kind of chemical bronze plating liquid that high speed is stable and
Preparation method.
Background technique
Chemical plating is also known as autocatalytic plating, refers under conditions of no impressed current, metal ion and reduction in solution
Agent with catalytic activity matrix surface occur autocatalyzed oxidation reduction reaction, matrix surface chemical deposition formed metal or
A kind of process for treating surface of alloy layer.Electroless copper is important one of electroless plating technology, and chemical plating copper layer is due to having
Good ductility, thermal conductivity and electric conductivity have been widely used in the conducting of printed wiring board through-hole, Electronic Packaging connection, electricity
Each industry such as magnetic wave shielding, decorative electroplating and civil field.
Chemical copper plating solution is mainly by mantoquita, complexing agent, reducing agent, stabilizer, pH adjuster and other additive groups
At.Overwhelming majority commercial chemistry copper plating bath is used as reducing agent using formaldehyde (molecular formula HCHO) at present, in chemical copper plating solution,
HCHO and hydroxide ion reaction generate hydrogen gas and water and Carboxylic Acid Ions, while bivalent cupric ion is reduced into metal copper simple substance, sink
Product is in the matrix surface with catalytic activity.Total chemical equation of electroless copper are as follows: Cu2++2HCHO+4OH-→Cu+H2+2H2O
+2HCOO-.This reaction equation only indicates the relationship of reactant and final reacting product, and real reaction process is more complex, exists
Many side reactions, and there is unstable cuprous ion to generate, it may cause chemical plating fluid decomposition, chemical plating copper layer is coarse, therefore needs
Want the addition of stabilizer.
It needs to carry out under alkaline condition when it is found that formaldehyde is as reducing agent by above-mentioned electroless copper reaction mechanism, generally
Plating solution is adjusted to pH between 11~12, with this condition, to prevent copper ion from forming hydrogen in alkali plating solution with pH regulator
Copper oxide precipitating, need to be added complexing agent and copper ion forms complex compound, to guarantee being normally carried out for reaction.Ethylenediamine tetrem at present
Sour (EDTA) is the common complexing agent of chemical bronze plating liquid, but EDTA influences the neutralization and precipitating of heavy metal, useless to electroless copper
The processing of liquid increases difficulty.Increasingly raising with manufacturing industry to environmental requirement, chemical bronze plating liquid is more towards using tartaric acid
Complexing agent of the salt as copper ion.Tartrate is also known as Rochelle salt, is easy to carry out liquid waste processing, but as chemical bronze plating liquid
Complexing agent when, deposition velocity is generally lower, is only applicable to low speed chemical-copper-plating process.Such as Publication No. CN104372315A
Using tartrate as the chemical plating fluid of complexing agent disclosed in Chinese patent, deposition velocity is about in 1.2~2.5 μm/h, coating
About 0.5 μm of thickness, it is suitable for the thin copper of chemical plating.For functional chemical copper facing, chemical bronze plating liquid deposition velocity will at least reach
To 4~6 μm/h, it just can guarantee that the thickness of final coating meets the Functional Requirement of material.In Publication No. CN106086836
A kind of high Speed Electroless Copper Plating Solution of state's patent disclosure can guarantee high copper facing rate, and deposition velocity reaches 5~10 μm/h, but adopts
It also added the complexing agents such as EDTA, the application of this mixing complexing agent is again to chemistry in addition to tartrate with mixing complexing agent
The processing of copper waste liquid increases difficulty.
Therefore how to improve using tartrate as the deposition velocity of the chemical bronze plating liquid of complexing agent, reach high-speed chemical
The requirement of copper-plating technique, the problem of becoming urgent need to resolve in the industry.For electroless copper, fast higher, the stability of plating solution is plated
It is more difficult to control；And the stability of plating solution is better, plating speed is just difficult to improve.Therefore chemical bronze plating liquid is coordinated (especially with wine
Stone hydrochlorate is the chemical bronze plating liquid of complexing agent) stability and plating speed relationship, obtain the stable chemical plating fluid of high speed, be always
The research direction in electroless copper field.
Summary of the invention
The purpose of the present invention is to the deficiencies in the prior art, a kind of chemical bronze plating liquid that high speed is stable and its system are proposed
Preparation Method, deposition velocity meet functional chemical copper facing requirement in 10 μm/h or more, bath stability, copper plate even uniform.
To achieve the goals above, the present invention adopts the following technical scheme:
The first aspect of the present invention provides a kind of chemical bronze plating liquid that high speed is stable, the stable electroless copper of the high speed
Liquid includes following components by volumetric concentration:
Salzburg vitriol 8g/L~25g/L,
15~40g/L of sodium potassium tartrate tetrahydrate,
5~20ml/L of formaldehyde,
5~20g/L of sodium hydroxide,
10~500mg/L of stabilizer,
Its surplus is water.
Further, the mass concentration of the formaldehyde is 37%.
Further, the stabilizer is the derivative of glycolylurea, and the derivative of the glycolylurea is nontoxic, biological degradability is good,
Chemical plating fluid stablizing effect is poor when lower than 10mg/L, and be greater than 500mg/L when chemical plating fluid deposition rate reduce.
Preferably, the stabilizer is glycolylurea, 5,5 Dimethyl Hydan and 5, one of 5 diethyl glycolylureas.
Further, the stable chemical bronze plating liquid of the high speed further includes combined additive, and the combined additive is by sulphur
Urea derivative and containing hydroxyalkyl ammonia carboxylic compound composition.Wherein, the combined additive can be complexing agent in sodium potassium tartrate tetrahydrate
Chemical plating fluid in, not only improved deposition rate but stablize plating solution.
Preferably, the thiourea derivative is one of thiosemicarbazides and allylthiourea, the ammonia containing hydroxyalkyl
Carboxylic compound is a kind of in N-hydroxyethyl-ethylenediamine triacetic acid (HEDTA) and tetrahydroxypropyl ethylenediamine (EDTP).
Preferably, the volumetric concentration of thiourea derivative described in the stable chemical bronze plating liquid of the high speed is 0.1~50mg/
L, the volumetric concentration of the ammonia carboxylic compound described in the stable chemical bronze plating liquid of the high speed containing hydroxyalkyl are 0.1~5g/L.
The second aspect of the present invention provides the preparation method of the stable chemical bronze plating liquid of above-mentioned high speed, and its step are as follows: will
Salzburg vitriol is miscible with water, after being stirred well to solution clarification, sequentially adds sodium potassium tartrate tetrahydrate, stabilizer, combination addition
Agent, sodium hydroxide, formaldehyde are stirred well to solution clarification, with water constant volume, can obtain the stable chemical bronze plating liquid of high speed.
Compared with prior art, the present invention realize the utility model has the advantages that the stable chemical bronze plating liquid of high speed in the present invention, sinks
Product speed meets functional chemical copper facing requirement in 10 μm/h or more, bath stability, copper plate even uniform.
Specific embodiment
In the following, further illustrating the content of present invention with embodiment, but protection scope of the present invention is not limited in implementing
Example.The others that those skilled in the art makes without departing substantially from spirit of that invention and protection scope are changed and repaired
Change, is included within the scope of the present invention.
The deposition velocity measuring method of the stable chemical bronze plating liquid of the high speed of following embodiment preparation is as follows: (1) taking ruler
Very little is 69mm × 69mm without the full epoxy resin base plate of copper, and the temperature for being put into baking oven at 120 DEG C is toasted 1 hour；Place into drier
Middle cooling 10-15 minutes；(2) taking-up weighing is accurate to 0.0001 gram and obtains starting weight G1；(3) specimen surface is cleaned,
Roughening and activation processing；(4) it is deposited 1 hour in 1 liter of beaker with chemical bronze plating liquid prepared by embodiment, depositing temperature control exists
40℃；(5) it takes out template and is put into baking oven at temperature baking 1 hour of 120 DEG C, further take out and be put into drier cooling 10-15 points
Clock；(6) taking-up weighing is accurate to 0.0001 gram and obtains weight G2 after electroless copper；(7) calculation formula: chemical plating fluid deposition velocity (μ
M/h)=(G2-G1)/0.08.Observation chemical bronze plating liquid clarifies situation during the reaction, observes electroless copper after the reaction was completed
Layer surface situation.
Embodiment 1
A kind of chemical bronze plating liquid that high speed is stable, each component content are as follows: Salzburg vitriol 15g/L, sodium potassium tartrate tetrahydrate
25g/L, formaldehyde (37%) 20ml/L, sodium hydroxide 10g/L, glycolylurea 30mg/L, thiosemicarbazides 1.5mg/L, four hydroxypropyl second two
Amine 0.75g/L, surplus are water.
The stable chemical bronze plating liquid of above-mentioned high speed the preparation method comprises the following steps: Salzburg vitriol is miscible with water, be sufficiently stirred
It is clarified to solution, sequentially adds sodium potassium tartrate tetrahydrate, glycolylurea, thiosemicarbazides, tetrahydroxypropyl ethylenediamine, sodium hydroxide and formaldehyde are abundant
Stirring to solution is clarified, and is finally settled to 1 liter with water.
The stable chemical bronze plating liquid of above-mentioned high speed measures deposition velocity as 12 μm/h, and in chemical deposition process, working solution is steady
Determine without decomposition, beaker inner wall is generated without copper particle, chemical plating copper layer even uniform, without coarse defect.
Embodiment 2
A kind of chemical bronze plating liquid that high speed is stable, each component content are as follows: Salzburg vitriol 25g/L, sodium potassium tartrate tetrahydrate
40g/L, formaldehyde (37%) 10ml/L, sodium hydroxide 15g/L, 5,5 Dimethyl Hydan 60mg/L, allylthiourea 5mg/L, N- hydroxyl
Ethyl-3-acetic acid ethylenediamine 1.5g/L, surplus are water.
The stable chemical bronze plating liquid of above-mentioned high speed the preparation method comprises the following steps: first that Salzburg vitriol is miscible with water, sufficiently
Stirring to solution is clarified, and sodium potassium tartrate tetrahydrate, 5,5 Dimethyl Hydan, allylthiourea, three second of N-hydroxyethyl-ethylenediamine are sequentially added
Acid, sodium hydroxide and formaldehyde are stirred well to solution clarification, are finally settled to 1 liter with water.
The stable chemical bronze plating liquid of above-mentioned high speed measures deposition velocity as 15 μm/h, and in chemical deposition process, working solution is steady
Determine without decomposition, beaker inner wall is generated without copper particle, chemical plating copper layer even uniform, without coarse defect.
Embodiment 3
A kind of chemical bronze plating liquid that high speed is stable, each component content are as follows: Salzburg vitriol 20g/L, sodium potassium tartrate tetrahydrate
30g/L, formaldehyde (37%) 5ml/L, sodium hydroxide 10g/L, 5,5 diethyl glycolylurea 40mg/L, thiosemicarbazides 10mg/L, N- hydroxyl second
Base ethylenediamine triacetic acid 5g/L, surplus are water.
The stable chemical bronze plating liquid of above-mentioned high speed the preparation method comprises the following steps: first that Salzburg vitriol is miscible with water, sufficiently
Stirring to solution is clarified, and sodium potassium tartrate tetrahydrate, 5,5 diethyl glycolylureas, thiosemicarbazides, three second of N-hydroxyethyl-ethylenediamine are sequentially added
Acid, sodium hydroxide and formaldehyde are stirred well to solution clarification, are finally settled to 1 liter with water.
The stable chemical bronze plating liquid of above-mentioned high speed measures deposition velocity as 18 μm/h, and in chemical deposition process, working solution is steady
Determine without decomposition, beaker inner wall is generated without copper particle, chemical plating copper layer even uniform, without coarse defect.
Embodiment 4
A kind of chemical bronze plating liquid that high speed is stable, each component content are as follows: Salzburg vitriol 25g/L, sodium potassium tartrate tetrahydrate
30g/L, formaldehyde (37%) 15ml/L, sodium hydroxide 5g/L, 5,5 diethyl glycolylurea 50mg/L, allylthiourea 20mg/L, four hydroxyls
Propyl ethylenediamine 4g/L, surplus are water.
The stable chemical bronze plating liquid of above-mentioned high speed the preparation method comprises the following steps: first that Salzburg vitriol is miscible with water, sufficiently
Stirring to solution is clarified, and sodium potassium tartrate tetrahydrate, 5,5 diethyl glycolylureas, allylthiourea, tetrahydroxypropyl ethylenediamine, hydrogen are sequentially added
Sodium oxide molybdena and formaldehyde are stirred well to solution clarification, are finally settled to 1 liter with water.
The stable chemical bronze plating liquid of above-mentioned high speed measures deposition velocity as 14 μm/h, and in chemical deposition process, working solution is steady
Determine without decomposition, beaker inner wall is generated without copper particle, chemical plating copper layer even uniform, without coarse defect.
Embodiment 5
A kind of chemical bronze plating liquid that high speed is stable, each component content are as follows: Salzburg vitriol 20g/L, sodium potassium tartrate tetrahydrate
40g/L, formaldehyde (37%) 15ml/L, sodium hydroxide 20g/L, 5,5 diethyl glycolylurea 20mg/L, thiosemicarbazides 10mg/L, four hydroxyls
Propyl ethylenediamine 2g/L, surplus are water.
The stable chemical bronze plating liquid of above-mentioned high speed the preparation method comprises the following steps: first that Salzburg vitriol is miscible with water, sufficiently
Stirring to solution is clarified, and sodium potassium tartrate tetrahydrate, 5,5 diethyl glycolylureas, thiosemicarbazides, tetrahydroxypropyl ethylenediamine, hydrogen-oxygen are sequentially added
Change sodium and formaldehyde is stirred well to solution clarification, is finally settled to 1 liter with water.
The stable chemical bronze plating liquid of above-mentioned high speed measures deposition velocity as 18 μm/h, and in chemical deposition process, working solution is steady
Determine without decomposition, beaker inner wall is generated without copper particle, chemical plating copper layer even uniform, without coarse defect.
The above specific embodiments are only exemplary, is to preferably make skilled artisans appreciate that originally
Patent, be not to be construed as include to this patent range limitation；As long as appointing made by the spirit according to disclosed in this patent
How with change or modification, the range that this patent includes is each fallen within.
Claims (8)
1. a kind of chemical bronze plating liquid that high speed is stable, which is characterized in that the stable chemical bronze plating liquid of the high speed presses volumetric concentration
Including following components:
Salzburg vitriol 8g/L~25g/L,
15~40g/L of sodium potassium tartrate tetrahydrate,
5~20ml/L of formaldehyde,
5~20g/L of sodium hydroxide,
10~500mg/L of stabilizer,
Its surplus is water.
2. the stable chemical bronze plating liquid of high speed as described in claim 1, which is characterized in that the mass concentration of the formaldehyde is
37%.
3. the stable chemical bronze plating liquid of high speed as described in claim 1, which is characterized in that the stabilizer is the derivative of glycolylurea
Object.
4. the stable chemical bronze plating liquid of high speed as claimed in claim 3, which is characterized in that the stabilizer be glycolylurea, 5,5 two
One of methyl hydantoin and 5,5 diethyl glycolylureas.
5. the stable chemical bronze plating liquid of high speed as described in claim 1, which is characterized in that the stable electroless copper of the high speed
Liquid further includes combined additive, and ammonia carboxylic compound of the combined additive by thiourea derivative and containing hydroxyalkyl forms.
6. the stable chemical bronze plating liquid of high speed as claimed in claim 5, which is characterized in that the thiourea derivative is amino sulphur
One of urea and allylthiourea, the ammonia carboxylic compound containing hydroxyalkyl is N-hydroxyethyl-ethylenediamine triacetic acid (HEDTA)
With one kind in tetrahydroxypropyl ethylenediamine (EDTP).
7. the stable chemical bronze plating liquid of high speed as claimed in claim 5, which is characterized in that the stable electroless copper of the high speed
The volumetric concentration of thiourea derivative described in liquid is 0.1~50mg/L, and hydroxyl is contained described in the stable chemical bronze plating liquid of the high speed
The volumetric concentration of the ammonia carboxylic compound of alkyl is 0.1~5g/L.
8. a kind of method for preparing the stable chemical bronze plating liquid of the described in any item high speeds of claim 1-7, which is characterized in that packet
Include following steps: Salzburg vitriol is miscible with water, after being stirred well to solution clarification, sequentially add sodium potassium tartrate tetrahydrate, steady
Determine agent, combined additive, sodium hydroxide, formaldehyde, is stirred well to solution clarification, with water constant volume, the stable change of high speed can be obtained
Learn copper plating bath.
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| CN2018110001244 | 2018-08-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115418632A (en) * | 2022-07-27 | 2022-12-02 | 深圳市富利特科技有限公司 | High-speed high-ductility chemical copper suitable for horizontal line equipment and preparation method thereof |
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