CN104073848A - Cyanide-free copper-plating preplating-free rapid presoak and preparation and use method thereof - Google Patents
Cyanide-free copper-plating preplating-free rapid presoak and preparation and use method thereof Download PDFInfo
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- CN104073848A CN104073848A CN201410185243.7A CN201410185243A CN104073848A CN 104073848 A CN104073848 A CN 104073848A CN 201410185243 A CN201410185243 A CN 201410185243A CN 104073848 A CN104073848 A CN 104073848A
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Abstract
The invention provides a cyanide-free copper-plating preplating-free rapid presoak and preparation and an use method thereof, wherein each liter of cyanide-free copper-plating preplating-free rapid presoak comprises 400-800g of potassium pyrophosphate trihydrate, 10-20g of dipotassium phosphate and water. The cyanide-free copper-plating preplating-free rapid presoak provided by the invention can guarantee the good binding force between an electroplated workpiece and a plated copper layer, the operation is fast and simple, the processes of nickel preplating, cyanide copper preplating and chemical preplating are avoided, the presoak is non-toxic and environmentally friendly, the presoak is stable, and can be stably used for a long time without adjusting components before use.
Description
Technical field
The present invention relates to cyanide-free copper electroplating technical field, relate in particular to a kind of cyanide-free copper electroplating and exempt from the quick presoak of preplating and preparation and application thereof.
Background technology
Cyanide copper plating technique is to apply the earliest and copper-plating technique the most widely.Plating solution is mainly made up of copper cyano complex and a certain amount of free cyanide, is strong basicity.Because cyanide ion has very strong activation capacity and complex ability, so being exactly solution, a feature of this copper electroplating method there is certain deoiling and activation capacity.In addition, because used plating solution comprises the prussiate that complex ability is very strong, complex ion is difficult for electric discharge, so plating solution has good covering power and covering power.
But cyanide copper plating technique serious environment pollution, can produce severe toxicity, harmful to health.For a long time, people are substitute copper-plating technique, have carried out unremitting effort, the each tool relative merits of various copper-plating techniques of research and development so far, but mostly still owe ripe and stable, be all defeated by poisonous cyanide copper plating technique.
Have only without cyanogen pyrophosphate copper plating technique and can desirablely substitute or surmount cyanide copper plating technique, formula without cyanogen pyrophosphate copper plating technique is simple, bath stability, crystallization is careful, current efficiency is high, covering power and covering power are good, and barrel plating or rack plating all can plate gets light or half bright looking, and can obtain and add thickness coating.Without cyanogen pyrophosphate copper plating technique have pollute little, non-stimulated smell, without real-time monitoring device, the advantage such as etching apparatus is not better than other cyanide-free copper electroplatings and cyanide copper plating technique comprehensively.
But, the same with other cyanide-free copper electroplating techniques without cyanogen pyrophosphate copper plating technique, there is the weak problem of bonding force between coating and workpiece, that is: can not be as cyanide copper plating technique, workpiece can directly be plated, but need to carry out Pre-treatment before plating, otherwise there will be the phenomenon of the bubble of peeling.
Pre-treatment before plating comprises: electrolysis nickel preplating, the pre-copper facing of prussiate or the pre-copper facing of chemical method.These Pre-treatment before platings exist and repeat second time electroplating, operation very complicated, the problem of generation toxic cyanide.The main salt that the pre-copper facing of chemical method is used is CuSO
4, this main salt have change large, consume fast feature, agent propenyl thiocarbamide very easily decomposes, cost is high in organic inhibition (slow resistance) of use; Winter, situation was slightly good, but in spring, autumn, especially must monitor and frequently add organic inhibition (slow resistance) agent in every day in summer, need 1 to N (N is greater than 1 natural number) inferior adjustment, adjust frequent, and dosage all will be strictly controlled in each adjustment, operation must be careful, many interpolations can make reaction stagnate, there is loose copper layer in few interpolation, even and strictly monitor the content of organic inhibition (slow resistance) agent, also still can often occur that binding force of cladding material is poor, cause the low-quality phenomenon of doing over again, the quality guaranteed period is short.
Summary of the invention
The invention provides a kind of cyanide-free copper electroplating and exempt from the quick presoak of preplating, for carrying out Pre-treatment before plating without cyanogen pyrophosphate copper plating technique, solve and existingly need repeat second time electroplating without cyanogen pyrophosphate copper plating technique, operation very complicated, batching consumes large, the weak problem of bonding force between coating and workpiece.
Wherein, every liter of cyanide-free copper electroplating provided by the invention is exempted from the quick presoak of preplating and is comprised that three water potassium pyrophosphates 400 are to 800g, dipotassium hydrogen phosphate 10 to 20g and water.
In preferred scheme, the pH value that described cyanide-free copper electroplating is exempted from the quick presoak of preplating is 8 to 10.
The preparation method that the present invention also provides above-mentioned cyanide-free copper electroplating to exempt from the quick presoak of preplating, comprises and carries out in order following steps:
Step 1: add water in non-metallic container;
Step 2: add three water potassium pyrophosphates, and by stirring, described three water potassium pyrophosphates are dissolved;
Step 3: add dipotassium hydrogen phosphate and water;
Wherein, make the final cyanide-free copper electroplating obtaining exempt to contain three water potassium pyrophosphates 400 to 800g in every liter of the quick presoak of preplating by described preparation method, dipotassium hydrogen phosphate 10 is to 20g.
In preferred scheme, the volume of the water adding in step 1 is 1/2 to 2/3 of the final cyanide-free copper electroplating the obtaining volume of exempting from the quick presoak of preplating.
In preferred scheme, after step 3, also comprise step 4: add three water potassium pyrophosphate and dipotassium hydrogen phosphates according to the weight ratio of 40:1 to 80:1, exempt from the density of the quick presoak of preplating to adjust cyanide-free copper electroplating.
In preferred scheme, the temperature while carrying out described preparation method is 5 to 35 DEG C.
The invention provides above-mentioned cyanide-free copper electroplating and exempt from the using method of the quick presoak of preplating, comprise and carry out in order following steps:
Step 11: workpiece is carried out to degreasing, pickling, then workpiece is washed;
Step 12: the described workpiece after washing is immersed to described cyanide-free copper electroplating and exempt from the quick presoak of preplating, and stop 30-60 second;
Step 13: exempt to take out described workpiece the quick presoak of preplating from described cyanide-free copper electroplating, then exempt from washing and directly by copper plating groove, described workpiece is carried out to copper electroplating.
In preferred scheme, exempt from before the quick presoak of preplating at the described cyanide-free copper electroplating of use, measuring described cyanide-free copper electroplating exempts from the quick presoak of preplating and whether meets specification of quality, be whether degree Beaume is more than or equal to 18 Baumes and is less than or equal to 28 Baumes, or whether density is more than or equal to 1.15g/ml and is less than or equal to 1.25g/ml; If do not meet specification of quality, add three water potassium pyrophosphates and dipotassium hydrogen phosphate to meet specification of quality until described cyanide-free copper electroplating is exempted from the quick presoak of preplating according to the weight ratio of 40:1 to 80:1.
Beneficial effect of the present invention is as follows:
One, cyanide-free copper electroplating is exempted from the quick presoak of preplating, feature is to have changed traditional technology in the past with brand-new technical concept, substitute Pre-treatment before plating operation in cyanide-free copper electroplating technique, in the density value limiting and pH value, form special effect, solved cyanide-free copper electroplating technique and formed copper layer in conjunction with not firm common fault.
1, in the time electroplating, the bare metallic surface of holding workpiece is plated under activated state, but not is plated under passivation state;
2, make workpiece not produce the replacement(metathesis)reaction film (responding layer) of harmful (affecting bonding force) in plating moment, thereby ensured the bonding force between institute's copper plate and workpiece.
Two, cyanide-free copper electroplating is exempted from the quick presoak of preplating and is had, and reaction fast, simple to operation, simple, immersion liquid is stable, permanently effective, processing range extra wide, bonding force is good, daily administration convenient (only needing a Beaumé scale), save time, economize material, exempt from washing, without discharging of waste liquid, the advantage of energy-conserving and environment-protective.
In the time using cyanide-free copper electroplating of the present invention to exempt from the quick presoak of preplating, adjust without the composition of cyanide-free copper electroplating being exempted to the quick presoak of preplating, two kinds of main components (three water potassium pyrophosphate and dipotassium hydrogen phosphate) that cyanide-free copper electroplating is exempted from the quick presoak of preplating form biofilm as thin as a wafer at workpiece surface, these two kinds of main components are taken out of presoak with fixed proportion, consumption equilibrium, micro-consumption, can not consume unbalance.In addition, use separately three water potassium pyrophosphates also can reach the similar effect with the present invention, but suppress the generation of orthophosphoric acid salt owing to lacking dipotassium hydrogen phosphate, so the presoak quality guaranteed period that uses separately three water potassium pyrophosphates to prepare is short.Cyanide-free copper electroplating of the present invention is exempted from the quick presoak of preplating due to the proportional consumption of main component, so can not lose efficacy along with use, can exempt the process of carrying out composition adjustment before use, can steady in a long-termly use.
Embodiment
To the technical scheme in the embodiment of the present invention be clearly and completely described below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of cyanide-free copper electroplating to exempt from the quick presoak of preplating, and every liter of cyanide-free copper electroplating is exempted from the quick presoak of preplating and comprised three water potassium pyrophosphate 400g, dipotassium hydrogen phosphate 10g, and all the other are water; The density that this cyanide-free copper electroplating is exempted from the quick presoak of preplating is 1.15g/ml, and pH value is 8.
The preparation method that above-mentioned cyanide-free copper electroplating is exempted from the quick presoak of preplating comprises and carries out in order following steps:
Step 1: add water in non-metallic container;
Step 2: add three water potassium pyrophosphate 400g, and by stirring, three water potassium pyrophosphates are dissolved;
Step 3: add dipotassium hydrogen phosphate 10g and water to 1 to be only upgraded to;
Wherein, the density of exempting from the quick presoak of preplating by the final cyanide-free copper electroplating obtaining of described preparation method is 1.15g/ml; Temperature while carrying out this preparation method is 20 DEG C.
Embodiment 2
The present embodiment provides a kind of cyanide-free copper electroplating to exempt from the quick presoak of preplating, and every liter of cyanide-free copper electroplating is exempted from the quick presoak of preplating and comprised three water potassium pyrophosphate 800g, dipotassium hydrogen phosphate 20g, and all the other are water; The density that this cyanide-free copper electroplating is exempted from the quick presoak of preplating is 1.25g/ml, and pH value is 10.
The preparation method that above-mentioned cyanide-free copper electroplating is exempted from the quick presoak of preplating comprises and carries out in order following steps:
Step 1: add water in non-metallic container;
Step 2: add three water potassium pyrophosphate 800g, and by stirring, three water potassium pyrophosphates are dissolved;
Step 3: add dipotassium hydrogen phosphate 20g and water to 1 to be only upgraded to;
Wherein, the density of exempting from the quick presoak of preplating by the final cyanide-free copper electroplating obtaining of described preparation method is 1.25g/ml; Temperature while carrying out this preparation method is 24 DEG C.
Embodiment 3
The present embodiment provides a kind of cyanide-free copper electroplating to exempt from the quick presoak of preplating, and every liter of cyanide-free copper electroplating is exempted from the quick presoak of preplating and comprised three water potassium pyrophosphate 500g, dipotassium hydrogen phosphate 13g, and all the other are water; The density that this cyanide-free copper electroplating is exempted from the quick presoak of preplating is 1.17g/ml, and pH value is 8.5.
The preparation method that above-mentioned cyanide-free copper electroplating is exempted from the quick presoak of preplating comprises and carries out in order following steps:
Step 1: add water in non-metallic container;
Step 2: add three water potassium pyrophosphate 500g, and by stirring, three water potassium pyrophosphates are dissolved;
Step 3: add dipotassium hydrogen phosphate 13g and water to 1 to be only upgraded to;
Wherein, the density of exempting from the quick presoak of preplating by the final cyanide-free copper electroplating obtaining of described preparation method is 1.17g/ml; Temperature while carrying out this preparation method is 5 DEG C.
Embodiment 4
The present embodiment provides a kind of cyanide-free copper electroplating to exempt from the quick presoak of preplating, and every liter of cyanide-free copper electroplating is exempted from the quick presoak of preplating and comprised three water potassium pyrophosphate 600g, dipotassium hydrogen phosphate 16g, and all the other are water; The density that this cyanide-free copper electroplating is exempted from the quick presoak of preplating is 1.21g/ml, and pH value is 9.1.
The preparation method that above-mentioned cyanide-free copper electroplating is exempted from the quick presoak of preplating comprises and carries out in order following steps:
Step 1: add water in non-metallic container;
Step 2: add three water potassium pyrophosphate 600g, and by stirring, three water potassium pyrophosphates are dissolved;
Step 3: add dipotassium hydrogen phosphate 16g and water to 1 to be only upgraded to;
Wherein, the density of exempting from the quick presoak of preplating by the final cyanide-free copper electroplating obtaining of described preparation method is 1.21g/ml; Temperature while carrying out this preparation method is 30 DEG C.
Embodiment 5
The present embodiment provides a kind of cyanide-free copper electroplating to exempt from the quick presoak of preplating, and every liter of cyanide-free copper electroplating is exempted from the quick presoak of preplating and comprised three water potassium pyrophosphate 700g, dipotassium hydrogen phosphate 18g, and all the other are water; The density that this cyanide-free copper electroplating is exempted from the quick presoak of preplating is 1.23g/ml, and pH value is 9.6.
The preparation method that above-mentioned cyanide-free copper electroplating is exempted from the quick presoak of preplating comprises and carries out in order following steps:
Step 1: add water in non-metallic container;
Step 2: add three water potassium pyrophosphate 700g, and by stirring, three water potassium pyrophosphates are dissolved;
Step 3: add dipotassium hydrogen phosphate 18g and water to 1 to be only upgraded to;
Wherein, the density of exempting from the quick presoak of preplating by the final cyanide-free copper electroplating obtaining of described preparation method is 1.23g/ml; Temperature while carrying out this preparation method is 35 DEG C.
In above-described embodiment 1 to 5, the water adding is tap water or deionized water etc., can use Beaumé scale measure solution density and ensure that density is in 1.15 to 1.25g/ml scope, if need to adjust density, add three water potassium pyrophosphate and dipotassium hydrogen phosphates according to the weight ratio of 40:1 to 80:1.For example, exempting from the quick presoak of preplating through step 1 to the cyanide-free copper electroplating obtaining after step 3 when not meeting density or degree Beaume and requiring, also need to be in the rear execution step 4 of step 3: add three water potassium pyrophosphate and dipotassium hydrogen phosphates according to the weight ratio of 40:1 to 80:1, so that the density that the final cyanide-free copper electroplating obtaining is exempted from the quick presoak of preplating meets the demands.
The density requirements that above-mentioned cyanide-free copper electroplating is exempted from the quick presoak of preplating also can be replaced by degree Beaume requirement, that is: the degree Beaume that cyanide-free copper electroplating is exempted from the quick presoak of preplating, for being more than or equal to 18 Baumes, is less than or equal to 28 Baumes.
Generally, the volume of the water adding in the step 1 of each embodiment is 1/2 to 2/3 of the final cyanide-free copper electroplating the obtaining volume of exempting from the quick presoak of preplating, for example, need to prepare 1L cyanide-free copper electroplating and exempt from the quick presoak of preplating, can in step 1, add the water of 0.5L to 0.67L, water has lacked that three water potassium pyrophosphates are not soluble, and water is many, and solution is thinning, is not easy to meet density requirements.
The using method that above-mentioned cyanide-free copper electroplating is exempted from the quick presoak of preplating comprises carries out following steps in order:
Step 11: workpiece is carried out to degreasing, pickling, then workpiece is washed; Degreasing, pickling are grease and the iron rust in order to remove workpiece surface, to carry out copper facing;
Step 12: the workpiece after washing is immersed to cyanide-free copper electroplating and exempt from the quick presoak of preplating, and stop 30-60 second; Cyanide-free copper electroplating is exempted from the quick presoak of preplating and is formed layer protective layer at workpiece surface, the Pre-treatment before plating operation of the similar traditional cyanide-free copper electroplating technique of this step;
Step 13: exempt to take out described workpiece the quick presoak of preplating from described cyanide-free copper electroplating, then exempt from washing and directly by copper plating groove, described workpiece is carried out to copper electroplating; Copper plating bath in copper plating groove can adopt existing copper plating bath, and workpiece surface forms the replacement(metathesis)reaction that protective layer can prevent workpiece oxidation and copper and iron occur, and ensures institute's copper plate stable performance.
In execution step 12 rear general needs execution step 13 fast, to obtain better copper facing effect.
Exempt from before the quick presoak of preplating at use cyanide-free copper electroplating, can also exempt from the quick presoak of preplating by survey instrument measurement cyanide-free copper electroplatings such as Beaumé scale and whether meet specification of quality, be whether degree Beaume is more than or equal to 18 Baumes and is less than or equal to 28 Baumes, or whether density is more than or equal to 1.15g/ml and is less than or equal to 1.25g/ml; If do not meet specification of quality, add three water potassium pyrophosphates and dipotassium hydrogen phosphate to meet specification of quality until described cyanide-free copper electroplating is exempted from the quick presoak of preplating according to the weight ratio of 40:1 to 80:1.
It is as follows that above-mentioned cyanide-free copper electroplating is exempted from the effect of each composition in the quick presoak of preplating:
Three water potassium pyrophosphates: promote activation, prevent workpiece passivation, suppress moment replacement(metathesis)reaction generation simultaneously; Dipotassium hydrogen phosphate: the generation that suppresses, delays resistance orthophosphoric acid salt; Three water potassium pyrophosphates and dipotassium hydrogen phosphate form protective layer at workpiece surface, and three water potassium pyrophosphates and dipotassium hydrogen phosphate equal proportion consume, and can not make cyanide-free copper electroplating exempt from the quick presoak of preplating and lose efficacy because a kind of composition exhausts in use for some time.
Ensure that pH value is in order to keep appropriate acid-basicity in 8 to 10 scope, the collaborative generation that stops copper and iron replacement(metathesis)reaction;
Ensure density or degree Beaume be for: guarantee that main salt (three water potassium pyrophosphate and dipotassium hydrogen phosphate) has enough concentration.
After execution step 12, mustn't wash, directly drop in copper plating groove and electroplate as early as possible, can obtain the good workpiece of bonding force.
Bonding force test (caloric test)
Use the inventive method to carry out after copper facing workpiece, get workpiece that thickness of coating is respectively 5 μ m, 10 μ m, 15 μ m, 20 μ m as workpiece 1 to workpiece 4, these four workpiece are heated to 200 DEG C and keep 2 hours in baking oven, and then extremely cold in cold water, test-results is in table 1.
Table 1:
Conclusion: the performance of four workpiece after bonding force test is good, does not all occur peeling or bubble phenomenon, compared with the product obtaining by cyanide copper plating technique, has equally even better properties, and asepsis environment-protecting; The workpiece obtaining by method of the present invention aspect such as bonding force between copper plate and workpiece is better than the product obtaining by cyanide-free copper electroplating technique.Visible product provided by the invention and method will replace traditional cyanide copper plating technique and solve the cyanide-free copper electroplating technique that other comprise electrolysis nickel preplating, the pre-copper facing of prussiate or the pre-copper facing step of chemical method; offer convenience for producing; save production cost; increase work efficiency, protection of the environment.
These are only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. cyanide-free copper electroplating is exempted from the quick presoak of preplating, it is characterized in that: every liter of cyanide-free copper electroplating is exempted from the quick presoak of preplating and comprised that three water potassium pyrophosphates 400 are to 800g, dipotassium hydrogen phosphate 10 to 20g and water.
2. a kind of cyanide-free copper electroplating according to claim 1 is exempted from the quick presoak of preplating, it is characterized in that: the pH value that described cyanide-free copper electroplating is exempted from the quick presoak of preplating is 8 to 10.
3. a kind of cyanide-free copper electroplating as claimed in claim 1 or 2 is exempted from a preparation method for the quick presoak of preplating, it is characterized in that: comprise and carry out in order following steps:
Step 1: add water in non-metallic container;
Step 2: add three water potassium pyrophosphates, and by stirring, described three water potassium pyrophosphates are dissolved;
Step 3: add dipotassium hydrogen phosphate and water;
Wherein, make the final cyanide-free copper electroplating obtaining exempt to contain three water potassium pyrophosphates 400 to 800g in every liter of the quick presoak of preplating by described preparation method, dipotassium hydrogen phosphate 10 is to 20g.
4. a kind of cyanide-free copper electroplating according to claim 3 is exempted from the preparation method of the quick presoak of preplating, it is characterized in that: the volume of the water adding in step 1 is 1/2 to 2/3 of the final cyanide-free copper electroplating the obtaining volume of exempting from the quick presoak of preplating.
5. a kind of cyanide-free copper electroplating according to claim 3 is exempted from the preparation method of the quick presoak of preplating, it is characterized in that: after step 3, also comprise step 4: add three water potassium pyrophosphate and dipotassium hydrogen phosphates according to the weight ratio of 40:1 to 80:1, exempt from the density of the quick presoak of preplating to adjust cyanide-free copper electroplating.
6. a kind of cyanide-free copper electroplating according to claim 3 is exempted from the preparation method of the quick presoak of preplating, it is characterized in that: the temperature while carrying out described preparation method is 5 to 35 DEG C.
7. a kind of cyanide-free copper electroplating as claimed in claim 1 or 2 is exempted from a using method for the quick presoak of preplating, it is characterized in that: comprise and carry out in order following steps:
Step 11: workpiece is carried out to degreasing, pickling, then workpiece is washed;
Step 12: the described workpiece after washing is immersed to described cyanide-free copper electroplating and exempt from the quick presoak of preplating, and stop 30-60 second;
Step 13: exempt to take out described workpiece the quick presoak of preplating from described cyanide-free copper electroplating, then exempt from washing and directly by copper plating groove, described workpiece is carried out to copper electroplating.
8. using method according to claim 7, it is characterized in that, exempt from before the quick presoak of preplating at the described cyanide-free copper electroplating of use, also comprise that measuring described cyanide-free copper electroplating exempts from the quick presoak of preplating and whether meet specification of quality, be whether degree Beaume is more than or equal to 18 Baumes and is less than or equal to 28 Baumes, or whether density is more than or equal to 1.15g/ml and is less than or equal to 1.25g/ml; If do not meet specification of quality, add three water potassium pyrophosphates and dipotassium hydrogen phosphate to meet specification of quality until described cyanide-free copper electroplating is exempted from the quick presoak of preplating according to the weight ratio of 40:1 to 80:1.
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