CN108950525A - A kind of compound colloid palladium composition and preparation method thereof - Google Patents
A kind of compound colloid palladium composition and preparation method thereof Download PDFInfo
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- CN108950525A CN108950525A CN201810858657.XA CN201810858657A CN108950525A CN 108950525 A CN108950525 A CN 108950525A CN 201810858657 A CN201810858657 A CN 201810858657A CN 108950525 A CN108950525 A CN 108950525A
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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
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1875—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment only one step pretreatment
- C23C18/1879—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 present invention relates to colloid chemistry technical fields, and in particular to a kind of compound colloid palladium composition and preparation method thereof.The compound colloid palladium composition, it includes the following raw material components: deionized water, palladium chloride, cobalt chloride, silica solution, hydrazine and surfactant；Wherein, the palladium chloride containing 10 ~ 20g in 1L deionized water, 5 ~ 10g cobalt chloride, 60 ~ 100g silica solution, 40 ~ 100g hydrazine, 1 ~ 5g surfactant.The composition is using palladium chloride and cobalt chloride as raw material, then silica solution is added, restore to obtain the compound colloid palladium composition containing colloid type Metal Palladium and metallic cobalt particle through the method for the present invention again, the compound colloid palladium composition carries out electroless copper plating as activating solution, the adhesive ability of colloidal particles and substrate surface can be promoted, and then promotes substrate after being conducive to electroless copper plating and plates the binding force of interlayer.
Description
Technical field
The present invention relates to colloid chemistry technical fields, and in particular to a kind of compound colloid palladium composition and its preparation side
Method.
Background technique
Electroless copper is one of circuit board fabrication technique, is generally also heavy copper or hole (PTH) is a kind of itself urge
The property changed redox reaction.(usually using the activating solution containing colloid palladium) is handled with activating solution first, makes insulating substrate table
Upper one layer of active particle is adsorbed in face, and logical the most commonly used is Metal Palladium particles, and copper ion is first in these active Metal Palladium particles
On be reduced, and metallic copper nucleus that these are reduced itself become copper ion Catalytic Layer, continue the reduction reaction of copper
It is carried out on these new copper nucleating surfaces.
Although existing activating solution can satisfy general electroless copper requirement, in activation, colloidal particles exist
Adhesive force on substrate surface is ideal not enough, causes to carry out electroless copper rear substrate using existing activating solution and plates interlayer
It still needs further improvement for binding force, can meet the electroless copper of requirements at the higher level.
Summary of the invention
The technical problem to be solved by the present invention is in order to overcome existing activating solution colloidal particles on substrate surface attached
Put forth effort technical deficiency ideal not enough, a kind of compound colloid palladium composition and preparation method thereof is provided, it is compound using this
Colloid palladium composition can promote the adhesive ability of colloidal particles and substrate surface as activating solution, and then be conducive to electroless copper plating
It promotes substrate afterwards and plates the binding force of interlayer.
Above-mentioned technical problem to be solved by this invention, is achieved by the following technical programs:
A kind of compound colloid palladium composition, it includes the following raw material components: deionized water, palladium chloride, cobalt chloride, silica solution,
Hydrazine and surfactant；
Wherein, the palladium chloride containing 10 ~ 20g in 1L deionized water, 5 ~ 10g cobalt chloride, 60 ~ 100g silica solution, 40 ~ 100g hydrazine, 1 ~ 5g
Surfactant.
Preferably, the palladium chloride containing 15 ~ 20g in 1L deionized water, 8 ~ 10g cobalt chloride, 80 ~ 100g silica solution, 60 ~ 80g hydrazine,
1 ~ 3g surfactant.
Most preferably, palladium chloride containing 15g in 1L deionized water, 8g cobalt chloride, 80g silica solution, 60g hydrazine, 2g surface-active
Agent.
Preferably, the silica solution is alkaline silica sol, and silica weight percentage is in the alkaline silica sol
30 ~ 35%, average grain diameter is 5 ~ 15nm.
Preferably, the silica solution is modified silicasol；The modified silicasol is prepared via a method which to obtain:
S11. alkaline silica sol is exchanged into obtain acidic silicasol through cation exchange resin (PC003 type)；
S12. acidic silicasol is heated to 80 ~ 100 DEG C, palladium chloride solution is added under agitation, reacted 1 ~ 3h, must change
Property silica solution；
Silica weight percentage is 30 ~ 35% in alkaline silica sol described in step S11, and average grain diameter is 5 ~ 15nm；
1 ~ 5g palladium chloride is added in step 12 in every 100g acidic silicasol；The concentration of palladium chloride solution is 0.1 ~ 0.5g/mL.
It is further preferred that the amount ratio of step S11 neutral and alkali silica solution and cation exchange tree is 1:1 ~ 3.
It is further preferred that 3 ~ 5g palladium chloride is added in step 12 in every 100g acidic silicasol；Palladium chloride solution it is dense
Degree is 0.3 ~ 0.5g/mL.
It is further preferred that acidic silicasol is heated to 100 DEG C in step 12, it is molten that palladium chloride is added under agitation
Liquid reacts 2h, obtains modified silicasol.
Preferably, the surfactant is Surfactant OP -10.
The present invention also provides the preparation methods of above-mentioned compound colloid palladium composition, and it includes following steps:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, solution 1 is then added after surfactant stirring and dissolving to obtain；
S22. solution 1 is stirred, silica solution is added while stirring or modified silicasol, silica solution or modified silicasol add
After entering, continue 20 ~ 60min of stirring, obtains solution 2；
S23. solution 2 is stirred, hydrazine is added while stirring and continues 2 ~ 6h of stirring after hydrazine is added to get described
Compound colloid palladium composition.
The utility model has the advantages that the compound colloid palladium composition that (1) is completely new the present invention provides one kind, the composition
Using palladium chloride and cobalt chloride as raw material, silica solution is then added, then restore to obtain containing colloid type gold through the method for the present invention
Belong to the compound colloid palladium composition of palladium and metallic cobalt particle, the compound colloid palladium composition is as activating solution
Heavy copper is learned, the adhesive ability of colloidal particles and substrate surface can be promoted, and then promotes substrate and plating after being conducive to electroless copper plating
The binding force of interlayer；(2) further, using palladium chloride and cobalt chloride as raw material, it is molten that modified silicon of the present invention is then added
The compound colloid palladium composition being prepared after glue, can further be substantially improved the energy of attachment of colloidal particles and substrate surface
Power, and then promote substrate after electroless copper plating can be substantially improved and plate the binding force of interlayer.
Specific embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not do any type of limit to the present invention
It is fixed.
The preparation of the compound colloid palladium composition of embodiment 1
Raw material composition: deionized water, palladium chloride, cobalt chloride, the alkaline silica sol (alkali purchased from favour and WELL board model S-830
Property silica solution), hydrazine and Surfactant OP -10；Wherein, palladium chloride containing 15g in 1L deionized water, 8g cobalt chloride, 80g silicon are molten
Glue, 60g hydrazine, 2g Surfactant OP -10.
Preparation method:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, are then added after -10 stirring and dissolving of Surfactant OP molten
Liquid 1；
S22. solution 1 is stirred, the alkaline silica sol (alkali purchased from favour and WELL board model S-830 is added while stirring
Property silica solution), alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) be added after, continue to stir
40min is mixed, solution 2 is obtained；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of the compound colloid palladium composition of embodiment 2
Raw material composition: deionized water, palladium chloride, cobalt chloride, the alkaline silica sol (alkali purchased from favour and WELL board model S-830
Property silica solution), hydrazine and Surfactant OP -10；Wherein, palladium chloride containing 10g in 1L deionized water, 10g cobalt chloride, 60g silicon
Colloidal sol, 40g hydrazine, 1g Surfactant OP -10.
Preparation method:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, are then added after -10 stirring and dissolving of Surfactant OP molten
Liquid 1；
S22. solution 1 is stirred, the alkaline silica sol (alkali purchased from favour and WELL board model S-830 is added while stirring
Property silica solution), alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) be added after, continue to stir
40min is mixed, solution 2 is obtained；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of the compound colloid palladium composition of embodiment 3
Raw material composition: deionized water, palladium chloride, cobalt chloride, the alkaline silica sol (alkali purchased from favour and WELL board model S-830
Property silica solution), hydrazine and Surfactant OP -10；Wherein, palladium chloride containing 20g in 1L deionized water, 5g cobalt chloride, 100g silicon
Colloidal sol, 100g hydrazine, 5g Surfactant OP -10.
Preparation method:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, are then added after -10 stirring and dissolving of Surfactant OP molten
Liquid 1；
S22. solution 1 is stirred, the alkaline silica sol (alkali purchased from favour and WELL board model S-830 is added while stirring
Property silica solution), alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) be added after, continue to stir
40min is mixed, solution 2 is obtained；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of the compound colloid palladium composition of embodiment 4
Raw material composition: deionized water, palladium chloride, cobalt chloride, modified silicasol, hydrazine and Surfactant OP -10；Wherein, 1L
Palladium chloride containing 15g in deionized water, 8g cobalt chloride, 80g silica solution, 60g hydrazine, 2g Surfactant OP -10；
The modified silicasol is prepared via a method which to obtain:
S11. by alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) through cation exchange resin
(PC003 type) exchanges to obtain acidic silicasol；
S12. acidic silicasol is heated to 80 ~ 100 DEG C, palladium chloride solution is added under agitation, reacted 1 ~ 3h, must change
Property silica solution；
The amount ratio of step S11 neutral and alkali silica solution and cation exchange tree is 1:1；
3g palladium chloride is added in step 12 in every 100g acidic silicasol；The concentration of palladium chloride solution is 0.3g/mL；In step 12
Acidic silicasol is heated to 100 DEG C, palladium chloride solution is added under agitation, 2h is reacted, obtains modified silicasol.
The preparation method of compound colloid palladium composition:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, are then added after -10 stirring and dissolving of Surfactant OP molten
Liquid 1；
S22. solution 1 is stirred, modified silicasol is added while stirring and continues to stir after modified silicasol is added
40min obtains solution 2；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of the compound colloid palladium composition of embodiment 5
Raw material composition: deionized water, palladium chloride, cobalt chloride, modified silicasol, hydrazine and Surfactant OP -10；Wherein, 1L
Palladium chloride containing 10g in deionized water, 10g cobalt chloride, 60g silica solution, 40g hydrazine, 1g Surfactant OP -10；
The modified silicasol is prepared via a method which to obtain:
S11. by alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) through cation exchange resin
(PC003 type) exchanges to obtain acidic silicasol；
S12. acidic silicasol is heated to 80 ~ 100 DEG C, palladium chloride solution is added under agitation, reacted 1 ~ 3h, must change
Property silica solution；
The amount ratio of step S11 neutral and alkali silica solution and cation exchange tree is 1:1；
3g palladium chloride is added in step 12 in every 100g acidic silicasol；The concentration of palladium chloride solution is 0.3g/mL；In step 12
Acidic silicasol is heated to 100 DEG C, palladium chloride solution is added under agitation, 2h is reacted, obtains modified silicasol.
The preparation method of compound colloid palladium composition:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, are then added after -10 stirring and dissolving of Surfactant OP molten
Liquid 1；
S22. solution 1 is stirred, modified silicasol is added while stirring and continues to stir after modified silicasol is added
40min obtains solution 2；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of the compound colloid palladium composition of embodiment 6
Raw material composition: deionized water, palladium chloride, cobalt chloride, modified silicasol, hydrazine and Surfactant OP -10；Wherein, 1L
Palladium chloride containing 20g in deionized water, 5g cobalt chloride, 100g silica solution, 100g hydrazine, 5g Surfactant OP -10.
The modified silicasol is prepared via a method which to obtain:
S11. by alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) through cation exchange resin
(PC003 type) exchanges to obtain acidic silicasol；
S12. acidic silicasol is heated to 80 ~ 100 DEG C, palladium chloride solution is added under agitation, reacted 1 ~ 3h, must change
Property silica solution；
The amount ratio of step S11 neutral and alkali silica solution and cation exchange tree is 1:1；
3g palladium chloride is added in step 12 in every 100g acidic silicasol；The concentration of palladium chloride solution is 0.3g/mL；In step 12
Acidic silicasol is heated to 100 DEG C, palladium chloride solution is added under agitation, 2h is reacted, obtains modified silicasol.
The preparation method of compound colloid palladium composition:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, are then added after -10 stirring and dissolving of Surfactant OP molten
Liquid 1；
S22. solution 1 is stirred, modified silicasol is added while stirring and continues to stir after modified silicasol is added
40min obtains solution 2；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of 1 colloid palladium composition of comparative example
Raw material composition: (the alkaline silicon purchased from favour and WELL board model S-830 is molten for deionized water, palladium chloride, alkaline silica sol
Glue), hydrazine and Surfactant OP -10；Wherein, palladium chloride containing 15g in 1L deionized water, 80g silica solution, 60g hydrazine, 2g table
Face activating agent OP-10.
Preparation method:
S21. it is water-soluble palladium chloride to be dissolved in deionization, solution 1 is then added after -10 stirring and dissolving of Surfactant OP to obtain；
S22. solution 1 is stirred, the alkaline silica sol (alkali purchased from favour and WELL board model S-830 is added while stirring
Property silica solution), alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) be added after, continue to stir
40min is mixed, solution 2 is obtained；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of 2 colloid palladium composition of comparative example
Raw material composition: (the alkaline silicon purchased from favour and WELL board model S-830 is molten for deionized water, palladium chloride, alkaline silica sol
Glue), hydrazine and Surfactant OP -10；Wherein, palladium chloride containing 10g in 1L deionized water, 60g silica solution, 40g hydrazine, 1g table
Face activating agent OP-10.
Preparation method:
S21. it is water-soluble palladium chloride to be dissolved in deionization, solution 1 is then added after -10 stirring and dissolving of Surfactant OP to obtain；
S22. solution 1 is stirred, the alkaline silica sol (alkali purchased from favour and WELL board model S-830 is added while stirring
Property silica solution), alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) be added after, continue to stir
40min is mixed, solution 2 is obtained；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
The preparation of 3 colloid palladium composition of comparative example
Raw material composition: (the alkaline silicon purchased from favour and WELL board model S-830 is molten for deionized water, palladium chloride, alkaline silica sol
Glue), hydrazine and Surfactant OP -10；Wherein, palladium chloride containing 20g in 1L deionized water, 100g silica solution, 100g hydrazine, 5g
Surfactant OP -10.
Preparation method:
S21. it is water-soluble palladium chloride to be dissolved in deionization, solution 1 is then added after -10 stirring and dissolving of Surfactant OP to obtain；
S22. solution 1 is stirred, the alkaline silica sol (alkali purchased from favour and WELL board model S-830 is added while stirring
Property silica solution), alkaline silica sol (alkaline silica sol purchased from favour and WELL board model S-830) be added after, continue to stir
40min is mixed, solution 2 is obtained；
S23. solution 2 is stirred, hydrazine is added while stirring, after hydrazine is added, continued stirring 3h and answered to get described
Mould assembly colloid palladium composition.
Test example
By the compound colloid palladium composition that embodiment 1 ~ 6 is prepared and the colloid palladium that comparative example 1 ~ 3 is prepared combination
Object, to pcb board substrate, carries out surface active using conventional method and carries out electroless copper plating, in electroless copper plating process as activating solution
It is middle to use sodium hypophosphite for reducing agent.The binding force of pcb board coating is examined after electroless copper plating with the following method: using and draws
Lattice device draws 100 1 millimeter × 1 millimeter of square lattice on coating surface.With Minnesota Mining and Manufacturing Company produce model 600 it is saturating
Gelatin band is smooth to be bonded on grid, does not stay a gap, is then uncovered with most fast 60 degree of angles of speed, is observed at scratching edge
Whether depainting is had, and according to depainting areal calculation depainting amount, wherein the smaller binding force of depainting amount is stronger,.Such as without any depainting
For 5B, it is 3B between 5~15% that depainting amount, which is 4B between 0~5%, is 2B between 15~35%, is between 35~65%
1B, 65% the above are 0B.Test result is shown in Table 1.
1. binding force of cladding material test result of table
| Sample | Depainting amount |
| The compound colloid palladium composition that embodiment 1 is prepared | 9% |
| The compound colloid palladium composition that embodiment 2 is prepared | 11% |
| The compound colloid palladium composition that embodiment 3 is prepared | 11% |
| The compound colloid palladium composition that embodiment 4 is prepared | 0%(is without depainting phenomenon) |
| The compound colloid palladium composition that embodiment 5 is prepared | 0%(is without depainting phenomenon) |
| The compound colloid palladium composition that embodiment 6 is prepared | 0%(is without depainting phenomenon) |
| The colloid palladium composition that comparative example 1 is prepared | 22% |
| The colloid palladium composition that comparative example 2 is prepared | 25% |
| The colloid palladium composition that comparative example 3 is prepared | 23% |
From 1 test data of table as can be seen that using compound colloid palladium composition described in embodiment 1 ~ 3, as activating solution
Coating its depainting amount obtain after electroless copper plating is 10% or so, and the depainting amount of comparative example 1 ~ 3 is 20% or more.This says
It is bright, implement that silica solution is then added 1 ~ 3 using palladium chloride and cobalt chloride as raw material, then be prepared through the method for the present invention compound
Type colloid palladium composition is combined than comparative example 1 ~ 3 using the colloid palladium that palladium chloride is prepared as raw material (being added without cobalt chloride)
Object can significantly deduct a percentage the binding force of coating in application.
In addition, from the depainting amount data of compound colloid palladium composition described in embodiment 4 ~ 5 can be seen that embodiment 4 ~
Compound colloid palladium composition described in 5 carries out the coating obtained after electroless copper plating without depainting phenomenon as activating solution, and comparison is real
For applying example 1 ~ 3, binding force substantially enhances, and effect is very significant.This is because compound colloid palladium group described in embodiment 4 ~ 5
It closes object and uses effect brought by modified silicasol of the present invention during the preparation process.
Claims (10)
1. a kind of compound colloid palladium composition, which is characterized in that include the following raw material component: deionized water,
Palladium chloride, cobalt chloride, silica solution, hydrazine and surfactant；
Wherein, the palladium chloride containing 10 ~ 20g in 1L deionized water, 5 ~ 10g cobalt chloride, 60 ~ 100g silica solution, 40 ~ 100g hydrazine, 1 ~ 5g
Surfactant.
2. compound colloid palladium composition according to claim 1, which is characterized in that the chlorine containing 15 ~ 20g in 1L deionized water
Change palladium, 8 ~ 10g cobalt chloride, 80 ~ 100g silica solution, 60 ~ 80g hydrazine, 1 ~ 3g surfactant.
3. compound colloid palladium composition according to claim 2, which is characterized in that chlorination containing 15g in 1L deionized water
Palladium, 8g cobalt chloride, 80g silica solution, 60g hydrazine, 2g surfactant.
4. compound colloid palladium composition according to claim 1, which is characterized in that the silica solution is that alkaline silicon is molten
Glue (S-830), silica weight percentage is 30 ~ 35% in the alkaline silica sol, and average grain diameter is 5 ~ 15nm.
5. compound colloid palladium composition according to claim 1, which is characterized in that the silica solution is that modified silicon is molten
Glue；The modified silicasol is prepared via a method which to obtain:
S11. alkaline silica sol is exchanged into obtain acidic silicasol through cation exchange resin (PC003 type)；
S12. acidic silicasol is heated to 80 ~ 100 DEG C, palladium chloride solution is added under agitation, reacted 1 ~ 3h, must change
Property silica solution；
Silica weight percentage is 30 ~ 35% in alkaline silica sol described in step S11, and average grain diameter is 5 ~ 15nm；
1 ~ 5g palladium chloride is added in step 12 in every 100g acidic silicasol；The concentration of palladium chloride solution is 0.1 ~ 0.5g/mL.
6. compound colloid palladium composition according to claim 5, which is characterized in that step S11 neutral and alkali silica solution and
The amount ratio of cation exchange tree is 1:1 ~ 3.
7. compound colloid palladium composition according to claim 5, which is characterized in that every 100g acidity silicon is molten in step 12
3 ~ 5g palladium chloride is added in glue；The concentration of palladium chloride solution is 0.3 ~ 0.5g/mL.
8. compound colloid palladium composition according to claim 5, which is characterized in that add acidic silicasol in step 12
Palladium chloride solution is added to 100 DEG C in heat under agitation, reacts 2h, obtains modified silicasol.
9. compound colloid palladium composition according to claim 1, which is characterized in that the surfactant is surface
Activating agent OP-10.
10. the preparation method of the described in any item compound colloid palladium compositions of claim 1 ~ 9, which is characterized in that comprising such as
Lower step:
S21. it is water-soluble palladium chloride and cobalt chloride to be dissolved in deionization, surfactant is then added, after stirring and dissolving solution 1；
S22. solution 1 is stirred, silica solution is added while stirring or modified silicasol, silica solution or modified silicasol add
After entering, continue 20 ~ 60min of stirring, obtains solution 2；
S23. solution 2 is stirred, hydrazine is added while stirring and continues 2 ~ 6h of stirring after hydrazine is added to get described
Compound colloid palladium composition.
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