CN107400881A - A kind of nano composite colloid palladium composition and preparation method thereof - Google Patents
A kind of nano composite colloid palladium composition and preparation method thereof Download PDFInfo
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- CN107400881A CN107400881A CN201710684547.1A CN201710684547A CN107400881A CN 107400881 A CN107400881 A CN 107400881A CN 201710684547 A CN201710684547 A CN 201710684547A CN 107400881 A CN107400881 A CN 107400881A
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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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1831—Use of metal, e.g. activation, sensitisation with noble metals
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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
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Abstract
The invention provides a kind of nano composite colloid palladium composition and preparation method thereof, including titanium dioxide nanoparticle and the palladium nano-particles for being deposited on the titanium dioxide nanoparticle surface, deionized water, hydrochloric acid.Further add surfactant and other additives.The present invention improves activity, and lift the quality of electroless copper by the way that palladium particle in nano-titanium oxide colloid surface photocatalysis in-situ deposition palladium particle, can be made to control the diameter within 3 nanometers, and extremely dispersion；The dosage of palladium can be greatly decreased with nano titanium oxide composite construction form for palladium, reduce cost；Due to particle fine uniform, and there is hydroxyl on nano-titanium oxide surface, is easily attached electric charge, thus need to only mix a small amount of hydrochloric acid achieve that it is colloid-stabilised, be also beneficial to improve with the adhesive force of PCB substrate, lift the reliability of copper plate.
Description
Technical field
The invention belongs to field of material technology, more particularly to a kind of nano composite colloid palladium composition and its preparation side
Method.
Background technology
Printed circuit board (PCB) (PCB) is the important component for realizing electronic component allomeric function, is widely used in electronics industry, and
Colloid palladium is the important catalyst of PCB electroless coppers.
Such as：CN103422132A discloses a kind of colloidal pd activation solution, it is characterised in that in the colloidal pd activation solution
Palladium acid potassium and auxiliary agent are closed containing palladium bichloride, hydrochloric acid, stannous chloride, four cyanogen.The average grain diameter of gained colloid palladium is 50-150nm.
In addition, Su Liangfei etc., the 5th the youth of the nation printed circuit science nd Annual Meeting collection, stannous chloride are made molten
Liquid, it is 2 according to Sn/Pd ratios:L, measure SnC12Solution, it is slowly stirred under 35 DEG C or so with frequency control agitator, this is molten
Liquid is added in the solution containing PdC12, and remaining SnC1 has been added after solution switchs to brownish black2Solution, lasting stirring are certain
Colloid palladium is obtained after time, by this colloid palladium be dispersed in sodium chloride-containing, appropriate additive solution in, be warming up to 50 DEG C, curing
4h, you can obtain Salt-Based Colloid Palladium.Palladium micelle size is 95nm or so.
A kind of Ou Sheng etc., there is provided Pd colloids catalyst of ultralow tank liquor concentration.The main composition of the Pd colloids catalyst
For：Pd：7.0-10.0g/l、SnCl2：500—600g/l、HCI：500-600g/l.Preparation method and foregoing paper method are basic
Identical, palladium micelle size is also close.
Ding Yu, 2012, Institutes Of Technology Of Changsha's Master's thesis, printed wiring board electroless copper activator-colloid palladium was ground
Study carefully, the Salt-Based Colloid Palladium provided prepares more excellent condition and is：PdCl2For 2.5g/L, Sn/Pd 50:1st, NaCl 175g/L, tin
Sour na concn is 5g/L, and reaction time 8min, reaction temperature are 25~35 DEG C, curing temperature is 55 DEG C or so.Performance is with before
It is essentially identical to state scheme.
Subject matter existing for prior art and shortcoming are：
(1), the palladium particle size that existing colloid palladium technology of preparing is formed is generally all more than 80 nanometers, it is difficult to obtains thinner
Small and stable colloid；
(2), the dosage of palladium is larger, it is difficult to reduces, cost is high；
(3), need to mix substantial amounts of stannic chloride and sodium stannate, hydrochloric acid and sodium chloride etc. to remain colloid-stabilised, after causing
It is continuous to increase solution adhesive process.
Problem above and shortcoming are as caused by colloid palladium chemical composition in itself and synthesis technique, it is difficult to overcome reconciliation
Certainly.
The content of the invention
In view of the problem of prior art is present, primary and foremost purpose of the invention there is provided a kind of nano composite colloid palladium group
Compound, including titania nanoparticles and it is deposited on the palladium nano-particles on titania nanoparticles surface group together
Into composite nanoparticle, deionized water, hydrochloric acid.It is preferred that add or do not add more than one surfactant and other additions
Agent.
The composite nanoparticle is by 1 titania nanoparticles and the palladium nanometer for being deposited on titanium dioxide granule surface
Multiple particles form composite nanostructure, and wherein titania nanoparticles particle diameter is 3-20 nanometers, and palladium nano-particles particle diameter is
1-10 nanometers.
It is preferred that the percentage by weight of titanium dioxide is 90-99% in the composite nanoparticle, the percentage by weight of palladium is
1-10%.The composite nanometer particle so formed is excellent to base material adhesive force, and chemism is high, and the use of palladium can be greatly decreased
Amount.
Foregoing preferred scheme is that the percentage by weight of each component is：Composite nanoparticle 0.1-10%；Deionization
Water 85-99.5%；Hydrochloric acid 0.01-1%；Surfactant 0-3%；Other additive 0-2%, each component percentage by weight sum
For 100%.
In the present compositions, composite nanoparticle is the activating agent of electroless copper plating, and it is firmly attached on hole wall, induction
Copper uniform deposition in chemical plating fluid further forms copper coating to particle surface.Hydrochloric acid can be in nano grain surface shape
Into the electric charge to repel each other, keep colloid-stabilised.Surfactant further prevents particle agglomeration, makes solution more stable.Thickener and
The addition of anti-settling agent makes particle not free settling, solution is maintained a long-term stability during using and storing.
More specifically optimal technical scheme is：The composite nanoparticle content is preferably 1-3%；Deionized water content
Preferably 97-99%；Content of hydrochloric acid is preferably 0.05-0.1%；Surface-active contents are preferably 0.5-1%；Other additives
Content is preferably 0.5-1%, and each component percentage by weight sum is 100%.
Such ratio combination both can guarantee that the efficiency of heavy copper, and but also with good economy, and acidity is fitted to technique
Answering property is good, the excellent in stability of solution.
The surfactant is nonionic surface active agent OMA, acid amides based surfactants TMA-1, surface-active
The combination of one or both of agent NOS, oreodaphene diglycollic amide, solution can be improved in the present compositions using process
In stability, and protect copper plate not oxidizable.
Other additives are one in thickener polyethylene glycol stearate diester, thickener CTF, hydroxypropyl methyl cellulose
Kind or two kinds of combination, can improve the viscosity of solution, solution is possessed more preferable bearing capacity to particle, together in the present compositions
When possess more preferable processing performance.
The preferred aerosil of anti-settling agent, effectively can prevent particle from settling in the present compositions.
Another object of the present invention is to provide a kind of a kind of preparation side of foregoing nano composite colloid palladium composition
Method, processing step are：
Nanometer titanium dioxide colloid solution containing hydrochloric acid is held into stirring or sonic oscillation in a reservoir, uses ultraviolet light
Irradiation colloidal sol makes titanium dioxide nanoparticle surface active；
Palladium bichloride or palladium nitrate solution are instilled, in the presence of UV-activated, palladium will be gradually in nano titanium oxide
Particle surface is nucleated and grows greatly nano level palladium particle, forms the structure of composite nanometer particle.
The processing step is simple, be able to can be completed in conventional instrument, and production efficiency is high, and product is good into rate.
Thickener is further preferably added after the completion of the structural response of composite nanometer particle is formed and anti-settling agent stirring is equal
It is even, form stable composition.
The present invention includes relative to the beneficial effect of prior art：
(1), by the nano-titanium oxide colloid surface photocatalysis in-situ deposition palladium particle in maturation, palladium particle control can be made
The diameter within 3 nanometers, and extremely dispersion are made, improves activity, and lift the quality of electroless copper；
(2), the dosage of palladium can be greatly decreased in palladium and nano titanium oxide composite construction form, reduce cost；
(3), due to particle fine uniform, and there is hydroxyl on nano-titanium oxide surface, is easily attached electric charge, therefore only needs to mix
A small amount of hydrochloric acid achieves that colloid-stabilised；
(4), due to particle fine uniform, and there is hydroxyl on nano-titanium oxide surface, is also beneficial to improve attached with PCB substrate
Put forth effort, lift the reliability of copper plate.
Brief description of the drawings
Fig. 1, palladium of the present invention and nano titanium oxide composite particles schematic diagram
Embodiment
The present invention is described in further detail with reference to specific embodiments and the drawings, but the present invention is not limited to
This.
Embodiment 1
A kind of nano composite colloid palladium composition, including titania nanoparticles and it is deposited on the titanium dioxide
The composite nanoparticle that the palladium nano-particles of nano grain surface form together, deionized water, hydrochloric acid.
The composite nanoparticle is by 1 titania nanoparticles and the palladium nanometer for being deposited on titanium dioxide granule surface
Multiple particles form composite nanostructure as shown in Figure 1, and wherein titania nanoparticles particle diameter is 14 nanometers, palladium nanometer
Grain diameter is 2 nanometers.
The percentage by weight of titanium dioxide is 95% in the composite nanoparticle, and the percentage by weight of palladium is 5%.
The percentage by weight of each component is：Composite nanoparticle 6%；Deionized water 94.5%；Hydrochloric acid 0.5%.
Preparation method is：1000 milliliters of the nano titanium oxide colloid of 6% concentration is taken, the palladium bichloride for adding 10% concentration is molten
30 milliliters of liquid, sonic oscillation, while irradiated 30 minutes with the ultraviolet lamp tube of 40W, 365 nano wave lengths, resulting solution test contains admittedly
Appropriate deionized water is added after amount and adjusts concentration to solid content 6%.
Note：Foregoing solid content is emulsion or coating dry under prescribed conditions after remainder account for the quality percentage of total amount
Number.
Embodiment 2
A kind of nano composite colloid palladium composition, including titania nanoparticles and it is deposited on the titanium dioxide
The composite nanoparticle that the palladium nano-particles of nano grain surface form together, deionized water, hydrochloric acid.
The composite nanoparticle is by 1 titania nanoparticles and the palladium nanometer for being deposited on titanium dioxide granule surface
Multiple particles form composite nanostructure as shown in Figure 1, and wherein titania nanoparticles particle diameter is 10 nanometers, palladium nanometer
Grain diameter is 1 nanometer.
The percentage by weight of titanium dioxide is 98% in the composite nanoparticle, and the percentage by weight of palladium is 2%.
The composite nanoparticle content is preferably 2%；Deionized water content is preferably 97.4%；Content of hydrochloric acid is preferably
0.1%；Surface-active contents are preferably 0.4%；Other additive levels are preferably 0.1%.
Preparation method is：500 milliliters of the nano titanium oxide colloid of 2% concentration is taken, adds the palladium chloride solution of 5% concentration
5 milliliters, sonic oscillation, while irradiated 60 minutes with the ultraviolet lamp tube of 30W, 365 nano wave lengths, add 20 grams of hydroxypropyl methyl fibres
Dimension element stirring 10 minutes, adds 5 grams of aerosils and stirs 10 minutes.Added in right amount after resulting solution test solid content
Deionized water adjusts concentration to solid content 3%.
Note：Foregoing solid content is emulsion or coating dry under prescribed conditions after remainder account for the quality percentage of total amount
Number.
The effect assessment of embodiment 3
Contrasted, found in prior art by the scheme of previous embodiment 1 and 2：The present invention solves following prior art and asked
Topic：
(1), the palladium particle size that existing colloid palladium technology of preparing is formed is generally all more than 80 nanometers, it is difficult to obtains thinner
Small and stable colloid；And palladium particle of the present invention controls the diameter within 3 nanometers, and extremely dispersion, activity is improved, and lifted
The quality of electroless copper；
(2), the dosage of prior art palladium is larger, it is difficult to reduces, cost is high；And the dosage of palladium of the present invention is significantly reduced；
(3), prior art needs to mix substantial amounts of stannic chloride and sodium stannate, hydrochloric acid and sodium chloride etc. to maintain colloid steady
It is fixed, cause subsequently increase solution adhesive process.And the composition stability of the present invention is high, can directly use.
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 (9)
1. a kind of nano composite colloid palladium composition, it is characterised in that including titania nanoparticles and be deposited on institute
State the composite nanoparticle that the palladium nano-particles on titania nanoparticles surface form together, deionized water, hydrochloric acid.
2. a kind of nano composite colloid palladium composition as claimed in claim 1, it is characterised in that composite nanoparticle is by 1
Individual titania nanoparticles and the multiple particles formation composite nanostructures of palladium nanometer for being deposited on titanium dioxide granule surface, its
Middle titania nanoparticles particle diameter is 3-20 nanometers, and palladium nano-particles particle diameter is 1-10 nanometers.
A kind of 3. nano composite colloid palladium composition as claimed in claim 1 or 2, it is characterised in that the composite Nano
The percentage by weight of titanium dioxide is 90-99% in particle, and the percentage by weight of palladium is 1-10%.
4. a kind of nano composite colloid palladium composition as claimed in claim 1 or 2, it is characterised in that the composition adds
Add or do not add more than one surfactant and other additives, the percentage by weight of each component is：Composite Nano
Particle 0.1-10%；Deionized water 85-99.5%；Hydrochloric acid 0.01-1%；Surfactant 0-3%；Other additive 0-2%,
Each component percentage by weight sum is 100%.
A kind of 5. nano composite colloid palladium composition as claimed in claim 4, it is characterised in that the composite nanoparticle
Content is preferably 1-3%；Deionized water content is preferably 97-99%；Content of hydrochloric acid is preferably 0.05-0.1%；Surfactant
Content is preferably 0.5-1%；Other additive levels are preferably 0.5-1%, and each component percentage by weight sum is 100%.
6. a kind of nano composite colloid palladium composition as claimed in claim 4, it is characterised in that the surfactant is
Nonionic surface active agent；Other additives are thickener and anti-settling agent.
7. a kind of nano composite colloid palladium composition as claimed in claim 6, it is characterised in that the surfactant is
Nonionic surface active agent is selected from OMA, acid amides based surfactants TMA-1, surfactant NOS, oreodaphene diethanol acyl
The combination of one or both of amine；Other additives are thickener and anti-settling agent, and thickener is selected from the double stearic acid of polyethylene glycol
The combination of one or both of ester, thickener CTF, hydroxypropyl methyl cellulose；Anti-settling agent is selected from aerosil.
8. a kind of preparation method for preparing a kind of nano composite colloid palladium composition as described in claim any one of 1-7,
Characterized in that, processing step is：
Nanometer titanium dioxide colloid solution containing hydrochloric acid is held into stirring or sonic oscillation in a reservoir, uses ultraviolet light
Colloidal sol makes titanium dioxide nanoparticle surface active；
Palladium bichloride or palladium nitrate solution are instilled, in the presence of UV-activated, palladium will be gradually in titanium dioxide nanoparticle
Surface nucleation and long greatly nano level palladium particle, form the structure of composite nanometer particle.
9. the preparation method of a kind of nano composite colloid palladium composition according to claim 8, it is characterised in that formed
Thickener is added after the completion of the reaction of the structure of composite nanometer particle and anti-settling agent stirs, and forms stable composition.
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Cited By (3)
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| CN108866516A (en) * | 2018-08-27 | 2018-11-23 | 合肥学院 | A method of selective chemical plating polymeric substrate is prepared using base metal |
| CN108950525A (en) * | 2018-07-31 | 2018-12-07 | 广东利尔化学有限公司 | A kind of compound colloid palladium composition and preparation method thereof |
| CN109468617A (en) * | 2018-11-30 | 2019-03-15 | 浙江长兴电子厂有限公司 | A kind of local electroplating nickel gold process |
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