CN104878422B - A kind of activation method of palladium activating solution and preparation method thereof and plastics - Google Patents
A kind of activation method of palladium activating solution and preparation method thereof and plastics Download PDFInfo
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- CN104878422B CN104878422B CN201410071763.5A CN201410071763A CN104878422B CN 104878422 B CN104878422 B CN 104878422B CN 201410071763 A CN201410071763 A CN 201410071763A CN 104878422 B CN104878422 B CN 104878422B
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Abstract
The invention provides a kind of palladium activating solution, soluble palladium salt, acid and ATS (Ammonium thiosulphate) are contained in the palladium activating solution.Present invention also offers the preparation method of the palladium activating solution and frosting activation method.Do not overflow and plate in the frosting chemical plating activated with the palladium activating solution of the present invention.
Description
Technical field
The invention belongs to plastic electroplating field, more particularly to the activation side of a kind of palladium activating solution and preparation method thereof and plastics
Method.
Background technology
Existing non-metallic metal chemical industry skill generally requires after the metals such as copper facing, nickel plating, rather than metal copper facing that nickel plating is most again
One of common plastics metalizing technique.Plastics partially plating gold category is the most frequently used plastics metalizing technique.Plastics will carry out electricity
Plating, generally requires to carry out corresponding pre-treatment, including removing oil-removing wax, is roughened, and neutralizes, and activates, reduction, the handling process such as dispergation.
Electroless copper is not because layers of copper has catalytic action to chemical nickel, so needing in layers of copper surface replacement palladium atom ability catalytic chemistry
Nickel plating.This formula in layers of copper exactly by displacing palladium atom so that the plastics after copper facing being capable of chemical nickel plating.Existing plastics
It is immersed in palladium activating solution, non-ization plating region easily remains the palladium activating solution taken out of, has part palladium ion to become hydrogen after washing
Palladium oxide is adsorbed on surface, is caused non-ization plating region nickel to overflow and is plated so that product yield reduces.
Publication No. CN102330132A Chinese patent discloses a kind of stable plastic plating colloid palladium activating solution
Preparation method, it is characterised in that this method comprises the following steps that：
（1）0.5-0.6g palladium bichlorides are added in the hydrochloric acid that 50-55g concentration is 80%, then add 50-55g distillations
Water, stirring is until be completely dissolved；
（2）Then 1.5-5g stannous chlorides are added, solution A is obtained after stirring and dissolving；
（3）Separately take 75-80g sodium chloride to be dissolved in 300-350g distilled water, add 3.5-4g sodium stannates and 25-30g chlorinations
Stannous, B solution is obtained after stirring；
（4）Solution A and B solution are mixed, 2-20g urea and 2-20g resorcinols are then added under stirring,
It is that can obtain colloidal pd activation solution that 2-4 hours are incubated at 45-60 DEG C.
The activating solution is although more stable, but it has plating of overflowing.
The content of the invention
The present invention is to solve the technical problem that existing palladium activating solution has plating of overflowing, there is provided a kind of palladium without excessive plating activates
The activation method of liquid and preparation method thereof and plastics.
The invention provides a kind of palladium activating solution, soluble palladium salt, acid and ATS (Ammonium thiosulphate) are contained in the palladium activating solution.
Present invention also offers a kind of preparation method of palladium activating solution, this method is that acid is dissolved in into water, and then adding can
Dissolubility palladium salt, ATS (Ammonium thiosulphate) dissolving is added after dissolving and obtains palladium activating solution.
Present invention also offers a kind of frosting activation method, including by the plastic basis material and activating solution Jing Guo pre-treatment
Contact, obtains the plastic basis material at the active center in surface；Wherein, the activating solution is palladium activating solution of the present invention.
Contain ATS (Ammonium thiosulphate) in the palladium activating solution of the present invention, ATS (Ammonium thiosulphate) can combine to form one kind with palladium ion
Soluble complex compound so that remaining in the palladium ion of substrate surface can easily be washed away, so as to solve well
Excessive plating phenomenon during follow-up plating.
Embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only explaining
The present invention, it is not intended to limit the present invention.
The invention provides a kind of palladium activating solution, soluble palladium salt, acid and ATS (Ammonium thiosulphate) are contained in the palladium activating solution.
According to palladium activating solution provided by the present invention, overflow to further improve the activity function of palladium activating solution and reduce
Plating, it is preferable that the content of the soluble palladium salt is 0.01-1g/L, and the sour content is 10-100g/L, the thio sulphur
The content of sour ammonium is 1-20g/L.
According to palladium activating solution provided by the present invention, the soluble palladium salt has no particular limits, and can be this area
Conventional various soluble palladium salts, such as palladium bichloride and/or palladium sulfate；The acid has no particular limits, as long as palladium can be complexed
Ion, such as hydrochloric acid and/or sulfuric acid.
According to palladium activating solution provided by the present invention, it is preferable that also include complexing agent in the palladium activating solution.The complexing
Agent can be complexed the copper ion in the palladium activating solution, other metal impurities such as calcium, magnesium in water, avoid excessive impurity from causing palladium
Ion precipitation makes palladium activating solution fail, and improves the life-span of palladium activating solution.
According to palladium activating solution provided by the present invention, palladium activating solution is not influenceed for more preferable complex copper ion but again
Performance, it is preferable that the content of the complexing agent is 1-10g/L.
According to palladium activating solution provided by the present invention, the complexing agent has no particular limits, as long as can be complexed well
Copper ion, such as sodium citrate, potassium citrate, citric acid, at least one of sulfamic acid and sulfamic acid sodium.In order to carry
The stability of macroion palladium activating solution, it is preferable that the complexing agent is sodium citrate and/or potassium citrate.
Present invention also offers a kind of preparation method of palladium activating solution, this method is that acid is dissolved in into water, and then adding can
Dissolubility palladium salt, ATS (Ammonium thiosulphate) dissolving is added after dissolving and obtains palladium activating solution.
According to preparation method provided by the present invention, it is preferable that the content of the soluble palladium salt is 0.01-1g/L, institute
The content for stating acid is 10-100g/L, and the content of the ATS (Ammonium thiosulphate) is 1-20g/L.
According to preparation method provided by the present invention, it is preferable that the soluble palladium salt is palladium bichloride and/or palladium sulfate；
The acid is hydrochloric acid and/or sulfuric acid.
According to preparation method provided by the present invention, it is preferable that add after ATS (Ammonium thiosulphate) is added or simultaneously complexing
Agent.
According to preparation method provided by the present invention, it is preferable that the content of the complexing agent is 1-10g/L；The complexing
Agent is at least one of sodium citrate, potassium citrate, citric acid, sulfamic acid and sulfamic acid sodium.
Present invention also offers a kind of frosting activation method, including by the plastic basis material and activating solution Jing Guo pre-treatment
Contact, obtains the plastic basis material at the active center in surface；Wherein, the activating solution is palladium activating solution of the present invention.
The present invention is described in further detail with reference to specific embodiment.
Embodiment 1
1st, palladium activating solution is prepared
Dissolving with hydrochloric acid in water, palladium bichloride is added, stirring, ATS (Ammonium thiosulphate), citric acid are added after palladium dissolving to be chlorinated
Sodium is to be mixed to obtain activating solution A1 to after being completely dissolved.Wherein, palladium bichloride 0.5g/L, hydrochloric acid 50g/L, ATS (Ammonium thiosulphate) 10g/
L, sodium citrate 5g/L.
2nd, frosting activates
（1）Pretreatment of base material（3 dual-color plastics（PC and ABS, chemical plating region are molded with ABS, and non-chemical plating region is used
PC is molded））：Dual-color plastic is put into degreasing fluid（NaOH 1mol/L、Na2CO31mol/L, dodecyl sodium sulfate 0.1mol/
L）, embathe 8 minutes at 50 DEG C, cleaned after taking-up with running water.
（2）Dual-color plastic after cleaning is subjected to roughening treatment（Chromium oxide：300g/L, 98% sulfuric acid:100g/L）In, it is molten
Liquid temperature degree is 70 DEG C, soak time 10-30 minutes.Cleaned after taking-up with running water.
（3）Reduction：Step will be passed through（2）Dual-color plastic after cleaning carries out reduction treatment（10% oxalic acid solution）, solution temperature
Spend for 30 DEG C, soak time 3 minutes.Cleaned after taking-up with running water.
（4）Salt pickling：Step will be passed through（3）Dual-color plastic after cleaning carries out salt pickling（Concentration is 30% hydrochloric acid）, it is molten
Liquid temperature degree is 20-30 DEG C, soak time 1 minute.Cleaned after taking-up with running water.
（5）Activation：Colloidal pd activation solution prepared by dual-color plastic immersion embodiment 1（It is limited that Sheng letter conjunction science and technology is risen in Tianjin
Company, model colloid palladium activator TS-3316）, the temperature of activating solution is 25 DEG C, and soak time is 3 minutes.With originally after taking-up
Water cleans.（6）Dispergation：Step will be passed through（5）Dual-color plastic after cleaning carries out dispergation（Concentration is 10% hydrochloric acid）, solution temperature
Spend for 45 DEG C, soak time 3 minutes.Cleaned after taking-up with running water.
（7）Chemical plating：It will be put into by the dual-color plastic of dispergation in 200mL chemical plating baths, electroless plating time is 20 points
Clock；In chemical plating fluid, the concentration of copper sulphate is 0.040mol/L, EDTA 0.107mol/L, potassium ferrocyanide
0.0000237mol/L, neopelex 0.00230mol/L, 2,2 ,-bipyridyl 0.000192mol/L, glyoxalic acid
0.0304mol/ L。
（8）Dual-color plastic after chemical plating is washed, then soaks activating solution A1 3 minutes, is then changed again through washing
Learn nickel plating, the plating solution of chemical nickel plating is phosphorus high temeperature chemistry nickel in Le Si companies, time 10min.After the completion of chemical nickel plating, spend
Ionized water washing surface, obtains plating piece, is designated as Y1.
Embodiment 2
Method according to embodiment 1 prepares palladium activating solution A2.Difference is that ionic palladium activating solution contains：Palladium bichloride 0.3g/
L, hydrochloric acid 30g/L, ATS (Ammonium thiosulphate) 6g/L, citric acid 3g/L.
Method according to embodiment 1 activates to plastics, obtains plating piece Y2.
Embodiment 3
Method according to embodiment 1 prepares palladium activating solution A3.Difference is that palladium activating solution contains：Palladium bichloride 0.1g/L, salt
Sour 10g/L, ATS (Ammonium thiosulphate) 1g/L, sulfamic acid 1g/L.
Method according to embodiment 1 activates to plastics, obtains plating piece Y3.
Embodiment 4
Method according to embodiment 1 prepares palladium activating solution A4.Difference is that palladium activating solution contains：Palladium sulfate 1g/L, sulfuric acid
100g/L, ATS (Ammonium thiosulphate) 20g/L, potassium citrate 10g/L.
Method according to embodiment 1 activates to plastics, obtains plating piece Y4.
Embodiment 5
Method according to embodiment 1 prepares palladium activating solution A5.Difference is that palladium activating solution contains：Palladium bichloride 0.5g/L, salt
Sour 50g/L, ATS (Ammonium thiosulphate) 10g/L.
Method according to embodiment 1 activates to plastics, obtains plating piece Y5.
Comparative example 1
Method according to embodiment 1 prepares palladium activating solution CA1.Difference is that palladium activating solution contains：Palladium bichloride 0.5g/L,
Hydrochloric acid 50g/L, sodium citrate 5g/L.
Method according to embodiment 1 activates to plastics, obtains plating piece CY1.
Comparative example 2
Dissolving with hydrochloric acid in water, palladium bichloride is added, palladium activating solution CA2 is obtained after stirring.Wherein, palladium activating solution contains
Have：Palladium bichloride 0.5g/L, hydrochloric acid 50g/L.
Method according to embodiment 1 activates to plastics, obtains plating piece CY2.
Comparative example 3
The palladium activating solution CA3 referred in Publication No. CN102330132A patent.
Method according to embodiment 1 activates to plastics, obtains plating piece CY3.
Method of testing and result
1st, overflow and plate
Range estimation, it is plating of overflowing to have coating or copper point in non-ABS area.It the results are shown in Table 1.
2nd, service life
Activating solution after embodiment 6-10 and comparative example 4-6 is used is placed, logger produces the time of precipitation.As a result
It is shown in Table 1.
Table 1
。
Plated from table 1 it follows that not overflow in the frosting chemical plating activated with the palladium activating solution of the present invention,
And the frosting that the palladium activating solution of Comparison study example is activated carries out chemical plating, there is plating phenomenon of overflowing.So with the present invention
Palladium activating solution can suppress frosting chemical plating occur overflow plating.After adding complexing agent in the palladium activating solution of the present invention simultaneously,
Its service life is grown.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (12)
1. a kind of palladium activating solution, it is characterised in that contain soluble palladium salt, acid and ATS (Ammonium thiosulphate) in the palladium activating solution.
2. palladium activating solution according to claim 1, it is characterised in that the content of the soluble palladium salt is 0.01-1g/L,
The sour content is 10-100g/L, and the content of the ATS (Ammonium thiosulphate) is 1-20g/L.
3. palladium activating solution according to claim 1 or 2, it is characterised in that the soluble palladium salt is palladium bichloride and/or sulphur
Sour palladium；The acid is hydrochloric acid and/or sulfuric acid.
4. palladium activating solution according to claim 3, it is characterised in that also include complexing agent in the palladium activating solution.
5. palladium activating solution according to claim 4, it is characterised in that the content of the complexing agent is 1-10g/L.
6. palladium activating solution according to claim 5, it is characterised in that the complexing agent is sodium citrate, potassium citrate, lemon
At least one of lemon acid, sulfamic acid and sulfamic acid sodium.
7. a kind of preparation method of palladium activating solution, it is characterised in that this method is that acid is dissolved in into water, then adds soluble palladium
Salt, ATS (Ammonium thiosulphate) dissolving is added after dissolving and obtains palladium activating solution.
8. preparation method according to claim 7, it is characterised in that the content of the soluble palladium salt is 0.01-1g/L,
The sour content is 10-100g/L, and the content of the ATS (Ammonium thiosulphate) is 1-20g/L.
9. the preparation method according to claim 7 or 8, it is characterised in that the soluble palladium salt is palladium bichloride and/or sulphur
Sour palladium；The acid is hydrochloric acid and/or sulfuric acid.
10. preparation method according to claim 7, it is characterised in that add after ATS (Ammonium thiosulphate) is added or simultaneously
Complexing agent.
11. preparation method according to claim 7, it is characterised in that the content of the complexing agent is 1-10g/L；It is described
Complexing agent is at least one of sodium citrate, potassium citrate, citric acid, sulfamic acid and sulfamic acid sodium.
12. a kind of frosting activation method, including the plastic basis material Jing Guo pre-treatment is contacted with activating solution, obtain surface tool
The plastic basis material at active center；Characterized in that, the activating solution is the palladium activating solution described in claim any one of 1-7.
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| CN105112968A (en) * | 2015-09-22 | 2015-12-02 | 太仓市金鹿电镀有限公司 | Electroplating process for plastic on surface of automobile gear rod |
| CN112742606B (en) * | 2020-12-24 | 2022-10-28 | 辽宁省地质矿产研究院有限责任公司 | Novel pyrrhotite composite activation agent and application thereof |
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| US6296897B1 (en) * | 1998-08-12 | 2001-10-02 | International Business Machines Corporation | Process for reducing extraneous metal plating |
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| US5518760A (en) * | 1994-10-14 | 1996-05-21 | Macdermid, Incorporated | Composition and method for selective plating |
| CN1247577A (en) * | 1997-12-18 | 2000-03-15 | 株式会社日本能源 | Pretreatment solution and pretreatment process of chemical nickle plating |
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