CN110318043A - A kind of high stability, the colloid palladium manufacture craft of high activity - Google Patents
A kind of high stability, the colloid palladium manufacture craft of high activity Download PDFInfo
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- CN110318043A CN110318043A CN201810264608.3A CN201810264608A CN110318043A CN 110318043 A CN110318043 A CN 110318043A CN 201810264608 A CN201810264608 A CN 201810264608A CN 110318043 A CN110318043 A CN 110318043A
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- palladium
- sulfonic acid
- weight percent
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to printed wiring board processing technique field, a kind of high stability, the colloid palladium manufacture craft of high activity are specifically disclosed, specifically comprises the following steps: that (1) first cleans up reaction kettle with tap water；It is cleaned 30 minutes with deionized water again；(2) deionized water, methane sulfonic acid and stannous chloride is added and is heated up to 100 DEG C；(3) in addition palladium chloride is added in hydrochloric acid, it adds methane sulfonic acid, resorcinol, ascorbic acid and is heated up to 50 DEG C of dissolutions, (4) slowly (3) solution is added under stiring to solution (2) in, be heated up to 100 DEG C and keep the temperature 100 DEG C, 21 minutes；(5) methane sulfonic acid in addition is added in deionized water and stannous chloride is stirred to dissolution, under stiring (5) solution is added to solution (4) in, supplement deionized water to liquid level stirs evenly, the present invention improves the stability and activity of colloid palladium, so as to improve generation quality and reduce production cost, production process is pollution-free, is suitble to industrialized production.
Description
Technical field
The invention belongs to printed wiring board processing technique fields, specifically, being related to the glue of a kind of high stability, high activity
Body palladium manufacture craft.Invention and created name: a kind of high stability, the colloid palladium manufacture craft of high activity
Background technique
With the continuous development of printed wiring plate technique, the aperture of via hole is smaller and smaller, by original minimum aperture aperture
0.3mm development is 0.075mm, and the density in hole is increasing, is a sheet 15-35 ten thousand by ten thousand hole development of original sheet 2-3
Hole, in addition to this, a large amount of blind hole, buried via hole printed wiring board (blind hole aperture is less to 0.050mm) batch production, for tradition
Hole metallization vertical production method, much can not meet quality requirements, therefore the production method of horizontal hole metallization is only
The Production trend of the high-grade plate of one production, however the catalysis before horizontal chemical copper facing, the technique for mostly using ionic palladium greatly all the time,
But since the contamination resistance of ionic palladium is particularly poor, change it is the cylinder period two months or so especially short, not only influence production more make
At the substantial increase of cost, but horizontal chemical copper facing takes colloid palladium used in vertical electroless copper there is also as follows not
Foot:
1, horizontal mode electroless copper makes liquid medicine that violent impact occur, and easily decomposes colloid palladium cohesion；
2, horizontal production method due to electroless copper unit volume liquid medicine production plate surface area very little, to colloid palladium
Activity more stringent requirements are proposed is otherwise unable to ensure the quality of mesoporous metal, to cause via hole conduction defect, influence electricity
Sub-information transmission.
Therefore, the manufacture craft of the colloid palladium of high stability, high activity used in horizontal mode electroless copper has been compeled
In the eyebrows and eyelashes.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide a kind of high stability, the colloid palladium manufacture craft of high activity,
It is poor to solve ionic palladium contamination resistance, the problem that the cylinder period is short, at high cost is changed, while providing high stability, high activity colloid
Palladium is to ensure hole metallization quality, to guarantee that electronic signal transmission is unobstructed.
To achieve the goals above, the present invention is the technical solution for solving its technical problem and providing are as follows:
A kind of high stability, the colloid palladium manufacture craft of high activity, high stability, the colloid palladium manufacture craft of high activity
Include the following steps:
(1) first reaction kettle is cleaned up with tap water, then is cleaned 30 minutes with deionized water；
(2) deionized water, methane sulfonic acid and stannous chloride is added to reaction kettle and is heated up to 100 DEG C, stirring and dissolving；
(3) palladium chloride is in addition added to stirring and dissolving in hydrochloric acid, adds methane sulfonic acid, resorcinol, Vitamin C
Acid is simultaneously heated up to 50 DEG C of stirring and dissolvings；
(4) slowly step (3) solution is added into step (2) solution under stiring and is heated to 100 DEG C and keep the temperature 21 points
Clock；
(5) methane sulfonic acid and stannous chloride are in addition added in deionized water and stirs to dissolution；
(6) under stiring (5) solution is added to solution (4) in, and add deionized water to liquid level and stir evenly, that is, be made
Colloid palladium before high stability, high activity horizontal chemical copper facing.
Preferably, a kind of high stability provided by the invention, in the colloid palladium manufacture craft of high activity, the weight of methane sulfonic acid
Amount percentage is 15-35wt%, and SnCI22H2O weight percent is 25-45wt%, and the weight percent of PdCl2 is 0.2-
The weight percent of 0.4wt%, HCI are 0.4-0.8wt%, the weight percent of resorcinol is 0.1-0.8wt%, anti-bad
The weight percent of hematic acid is 0.01-0.07wt%.
Preferably, a kind of high stability provided by the invention, in the colloid palladium manufacture craft of high activity, the pH of colloid palladium <
1, specific gravity 1.14-1.18g/cm3.
Preferably, a kind of high stability provided by the invention, in the colloid palladium manufacture craft of high activity, step is matched in (2)
The solution set is made of following weight percent: methane sulfonic acid: 10-30wt%, stannous chloride: 10-30wt%.
Preferably, a kind of high stability provided by the invention, in the colloid palladium manufacture craft of high activity, step is matched in (3)
The solution set is made of following weight percent: palladium chloride: 0.2-0.4wt%, hydrochloric acid: 0.4-0.8wt%, methane sulfonic acid:
1-4wt%, resorcinol: 0.1-0.8wt%, ascorbic acid: 0.01-0.07wt%.
Preferably, a kind of high stability provided by the invention, in the colloid palladium manufacture craft of high activity, step is matched in (5)
The solution set is made of following weight percent: methane sulfonic acid: 1.5-3.5wt%, stannous chloride: 3.5-9.5wt%.
The present invention beneficial technical effect compared with prior art:
(1) colloid palladium is in horizontal chemical copper facing, contamination resistance to be strong, changes the slot period and by two months was extended down to half a year, raw
Producing cost reduces by 30% or more；
(2) the copper-plated quality of horizontal chemical is improved, the backlight series of electroless copper is promoted to 9.5 grades by 8.5 grades；
(3) the quality fraction defective of via hole is promoted to 0.1 ‰ by 3 ‰；
(4) it reduces and causes the wastes of human resources because colloid palladium cylinder frequently changes cylinder；
(5) continuity and production production capacity of horizontal chemical copper facing production are ensured；
(6) consumption of precious metal palladium has been saved；
(7) at low cost, production process is pollution-free, therefore is with a wide range of applications in printed wiring board field.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right below in conjunction with specification embodiment
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention,
It is not intended to limit the present invention.
There is following mass percent in a kind of high stability disclosed by the invention, the colloid palladium manufacture craft of high activity
Composition:
The weight percent of methane sulfonic acid is 15-35wt%, and SnCI22H2O weight percent is 25-45wt%,
The weight percent of PdCl2 be the weight percent of 0.2-0.4wt%, HCI be 0.4-0.8wt%, the weight hundred of resorcinol
Divide than being 0.1-0.8wt%, the weight percent of ascorbic acid is 0.01-0.07wt%.
One mass percentage composition of preferred embodiment are as follows:
Methane sulfonic acid: 15wt%, stannous chloride: 25wt%, palladium chloride: 0.2wt%, hydrochloric acid: 0.4wt%, isophthalic two
Phenol: 0.1wt%, ascorbic acid: 0.01wt%.
Two mass percentage composition of preferred embodiment are as follows:
Methane sulfonic acid: 35wt%, stannous chloride: 45wt%, palladium chloride: 0.4wt%, hydrochloric acid: 0.8wt%, isophthalic two
Phenol: 0.8wt%, ascorbic acid: 0.07wt%.
By taking preferred embodiment one as an example, various components are configured according to following processing step and carry out copper facing colloid by the present invention
Palladium manufacture craft, the specific steps are as follows:
Embodiment 1
(1) first reaction kettle is cleaned up with tap water, then is cleaned 30 minutes with deionized water；
(2) weight percent disclosed in one forms to reaction kettle and deionized water, 15wt% is added according to the preferred embodiment
Methane sulfonic acid and 25wt% stannous chloride and be heated up to 100 DEG C, dissolution is mixed, is configured to weight percent composition
Are as follows: methane sulfonic acid: 10wt%, stannous chloride: the solution of 10wt%；
(3) palladium chloride is in addition added to stirring and dissolving in hydrochloric acid, adds methane sulfonic acid, resorcinol, Vitamin C
Acid is simultaneously heated up to 50 DEG C of stirring and dissolvings, is configured to weight percent composition are as follows: palladium chloride: 0.2wt%, hydrochloric acid: 0.4wt%,
Methane sulfonic acid: 1wt%, resorcinol: 0.1wt%, ascorbic acid: 0.01wt%；
(4) slowly the step (3) solution is added into the step (2) solution under stiring and is heated to 100 DEG C of guarantors
Temperature 21 minutes；
(5) methane sulfonic acid and stannous chloride are in addition added in deionized water and stirs to dissolving, is configured to weight percent
Than are as follows: the concentration of methane sulfonic acid are as follows: 1.5wt%, stannous chloride concentration are as follows: 3.5wt%；
(6) under stiring (5) solution is added to solution (4) in, and add deionized water to liquid level and stir evenly, that is, be made
Colloid palladium before high stability, high activity horizontal chemical copper facing.
Please refer to table 1, listed in table 1 by select in embodiment 1 pH after the completion of step (1) to (6) manufacture craft configuration <
1, the colloid palladium of specific gravity 1.14g/cm3 carries out stability, activity and the related ginseng of backlight (electroless copper) detection to common colloid
Number, may know that, the colloid palladium obtained according to high stability provided by the invention, the colloid palladium manufacture craft of high activity from table 1
Active high, stability is good, and the backlight series of electroless copper is good.
Table 1 is the colloid palladium that manufacture craft obtains in the preferred embodiment of the present invention 1 and common colloid palladium to stability, work
Property and backlight influence relevant parameter
Embodiment 2
By taking preferred embodiment two as an example, various components are configured according to following processing step and carry out copper facing colloid by the present invention
Palladium manufacture craft, the specific steps are as follows:
(1) first reaction kettle is cleaned up with tap water, then is cleaned 30 minutes with deionized water；
(2) weight percent disclosed in one forms to reaction kettle and deionized water, 35wt% is added according to the preferred embodiment
Methane sulfonic acid and 45wt% stannous chloride and be heated up to 100 DEG C, dissolution is mixed, is configured to weight percent composition
Are as follows: methane sulfonic acid: 30wt%, stannous chloride: the solution of 30wt%；
(3) palladium chloride is in addition added to stirring and dissolving in hydrochloric acid, adds methane sulfonic acid, resorcinol, Vitamin C
Acid is simultaneously heated up to 50 DEG C of stirring and dissolvings, is configured to weight percent composition are as follows: palladium chloride: 0.4wt%, hydrochloric acid: 0.8wt%,
Methane sulfonic acid: 4wt%, resorcinol: 0.8wt%, ascorbic acid: 0.07wt%；
(4) slowly the step (3) solution is added into the step (2) solution under stiring and is heated to 100 DEG C of guarantors
Temperature 21 minutes；
(5) methane sulfonic acid and stannous chloride are in addition added in deionized water and stirs to dissolving, is configured to weight percent
Than are as follows: the concentration of methane sulfonic acid are as follows: 3.5wt%, stannous chloride concentration are as follows: 9.5wt%；
(6) under stiring (5) solution is added to solution (4) in, and add deionized water to liquid level and stir evenly, that is, be made
Colloid palladium before high stability, high activity horizontal chemical copper facing.
Please refer to table 2, listed in table 2 by select in embodiment 2 pH after the completion of step (1) to (6) manufacture craft configuration <
1, the colloid palladium of specific gravity 1.18g/cm3 carries out stability, activity and the related ginseng of backlight (electroless copper) detection to common colloid
Number, may know that, the colloid palladium obtained according to high stability provided by the invention, the colloid palladium manufacture craft of high activity from table 1
Active high, stability is good, and the backlight series of electroless copper is good.
Table 2 is the colloid palladium that manufacture craft obtains in the preferred embodiment of the present invention 2 and common colloid palladium to stability, work
Property and backlight influence relevant parameter
Specification table 1 and table 2 is combined to elaborate the preferred embodiment of the present invention above, it should illustrate
, protection scope of the present invention includes but is not limited to above-described embodiment；Specific structure disclosed in specification is also this hair
Bright preferred embodiment, the technical staff in the field can also develop other embodiments on this basis, any not depart from
The simple deformation or equivalent replacement of innovative idea of the present invention, are covered by the present invention, belong to the scope of protection of the present invention.
Claims (6)
1. the colloid palladium manufacture craft of a kind of high stability, high activity, which is characterized in that the glue of the high stability, high activity
Body palladium manufacture craft includes the following steps:
(1) first reaction kettle is cleaned up with tap water, then is cleaned 30 minutes with deionized water；
(2) deionized water, methane sulfonic acid and stannous chloride is added to reaction kettle and is heated up to 100 DEG C, stirring and dissolving；
(3) palladium chloride is in addition added to stirring and dissolving in hydrochloric acid, adds methane sulfonic acid, resorcinol, ascorbic acid simultaneously
It is heated up to 50 DEG C of stirring and dissolvings；
(4) slowly the step (3) solution is added into the step (2) solution under stiring and is heated to 100 DEG C of heat preservations 21
Minute；
(5) methane sulfonic acid and stannous chloride are in addition added in deionized water and stirs to dissolution；
(6) under stiring (5) solution is added to solution (4) in, and add deionized water to liquid level and stir evenly, that is, be made high steady
Colloid palladium qualitative, before high activity horizontal chemical copper facing.
2. a kind of high stability according to claim 1, the colloid palladium manufacture craft of high activity, which is characterized in that methyl
The weight percent of sulfonic acid is 15-35wt%, and SnCI22H2O weight percent is 25-45wt%, the weight percent of PdCl2
Than the weight percent for 0.2-0.4wt%, HCI be 0.4-0.8wt%, the weight percent of resorcinol is 0.1-
0.8wt%, the weight percent of ascorbic acid are 0.01-0.07wt%.
3. a kind of high stability according to claim 1, the colloid palladium manufacture craft of high activity, which is characterized in that described
PH < 1 of colloid palladium, specific gravity 1.14-1.18g/cm3.
4. a kind of high stability according to claim 1, the colloid palladium manufacture craft of high activity, which is characterized in that described
The solution configured in step (2) is made of following weight percent: methane sulfonic acid: 10-30wt%, stannous chloride: 10-
30wt%.
5. a kind of high stability according to claim 1, the colloid palladium manufacture craft of high activity, which is characterized in that described
The solution configured in step (3) is made of following weight percent: palladium chloride: 0.2-0.4wt%, hydrochloric acid: 0.4-
0.8wt%, methane sulfonic acid: 1-4wt%, resorcinol: 0.1-0.8wt%, ascorbic acid: 0.01-0.07wt%.
6. a kind of high stability according to claim 1, the colloid palladium manufacture craft of high activity, which is characterized in that described
The solution configured in step (5) is made of following weight percent: methane sulfonic acid: 1.5-3.5wt%, stannous chloride: 3.5-
9.5wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810264608.3A CN110318043A (en) | 2018-03-28 | 2018-03-28 | A kind of high stability, the colloid palladium manufacture craft of high activity |
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| CN201810264608.3A CN110318043A (en) | 2018-03-28 | 2018-03-28 | A kind of high stability, the colloid palladium manufacture craft of high activity |
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| CN201810264608.3A Pending CN110318043A (en) | 2018-03-28 | 2018-03-28 | A kind of high stability, the colloid palladium manufacture craft of high activity |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112626502A (en) * | 2020-11-30 | 2021-04-09 | 南通麦特隆新材料科技有限公司 | Chemical copper plating activator for PCB and preparation method thereof |
| CN113355661A (en) * | 2021-05-31 | 2021-09-07 | 江苏软讯科技有限公司 | High-activity high-stability colloidal palladium catalyst and preparation process thereof |
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| CN102909078A (en) * | 2012-10-25 | 2013-02-06 | 南京大地冷冻食品有限公司 | Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof |
| CN104005008A (en) * | 2013-02-24 | 2014-08-27 | 罗门哈斯电子材料有限公司 | Plating catalyst and method |
| CN106591809A (en) * | 2016-12-26 | 2017-04-26 | 长沙理工大学 | Low-concentration colloid palladium activation solution for printed circuit board electroless copper |
| CN107034453A (en) * | 2016-02-04 | 2017-08-11 | 中国科学院金属研究所 | A kind of preparation method of palladium colloidal activation solution |
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2018
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Patent Citations (4)
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| CN102909078A (en) * | 2012-10-25 | 2013-02-06 | 南京大地冷冻食品有限公司 | Non-metallic material chemical plating high-activity palladium catalyst concentrated solution and preparation method thereof |
| CN104005008A (en) * | 2013-02-24 | 2014-08-27 | 罗门哈斯电子材料有限公司 | Plating catalyst and method |
| CN107034453A (en) * | 2016-02-04 | 2017-08-11 | 中国科学院金属研究所 | A kind of preparation method of palladium colloidal activation solution |
| CN106591809A (en) * | 2016-12-26 | 2017-04-26 | 长沙理工大学 | Low-concentration colloid palladium activation solution for printed circuit board electroless copper |
Non-Patent Citations (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112626502A (en) * | 2020-11-30 | 2021-04-09 | 南通麦特隆新材料科技有限公司 | Chemical copper plating activator for PCB and preparation method thereof |
| CN113355661A (en) * | 2021-05-31 | 2021-09-07 | 江苏软讯科技有限公司 | High-activity high-stability colloidal palladium catalyst and preparation process thereof |
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Application publication date: 20191011 |