CN104451621A - Preparation method of silver-coated silicon dioxide composite powder - Google Patents

Preparation method of silver-coated silicon dioxide composite powder Download PDF

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Publication number
CN104451621A
CN104451621A CN201410735024.1A CN201410735024A CN104451621A CN 104451621 A CN104451621 A CN 104451621A CN 201410735024 A CN201410735024 A CN 201410735024A CN 104451621 A CN104451621 A CN 104451621A
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China
Prior art keywords
silver
sio
powder
preparation
formaldehyde
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Pending
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CN201410735024.1A
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Chinese (zh)
Inventor
汪理文
李庆贵
翁永华
丁贤麟
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SUZHOU RUNJIA ENGINEER PLASTIC CO Ltd
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SUZHOU RUNJIA ENGINEER PLASTIC CO Ltd
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Priority to CN201410735024.1A priority Critical patent/CN104451621A/en
Publication of CN104451621A publication Critical patent/CN104451621A/en
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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
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents
    • 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

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention belongs to the field of chemical silver coating of powder, and particularly relates to a preparation method of silver-coated silicon dioxide composite powder. The preparation method comprises the following steps: (1) weighing SiO2 powder, heating the SiO2 powder until the SiO2 powder is melted, dropwise adding polyvinyl alcohol and blending to prepare a SiO2 gelatineous solution; (2) centrifugally treating the SiO2 gelatineous solution to prepare SiO2 particles; (3) chemically coating silver on the SiO2 particles by the effect of ultrasonic wave by using a formaldehyde-silver-ammonia solution, wherein the PH of the formaldehyde-silver-ammonia solution is 10-10.5. According to the preparation method disclosed by the invention, polyvinyl alcohol is added dropwise so that a system is dispersed more uniformly; the PH of the silver coating solution is 10 to 10.5, especially when the PH is 10.5, the silver coating efficiency and the stability of the silver coating solution can be guaranteed as far as possible so as to prevent agglomeration of the particles; formaldehyde and a silver-ammonia solution are prepared separately, so that improvement of the stability of the silver coating solution is facilitated.

Description

The preparation method of the silver-plated composite granule of silicon-dioxide
Technical field
The invention belongs to Electroless Silver Plating of Powders field, be specifically related to the preparation method of the silver-plated composite granule of a kind of silicon-dioxide.
Background technology
Powder is compared with the chemical plating technology of block large size material, and powder body material has larger specific surface area relative to bulk material, and therefore electroless plating reaction is general fiercer, and in reaction, various processing parameter is wayward, as concentration, PH etc.
At present, the silver-plated technology of powder has obtained certain progress, but also exist that the less stable of silver plating liquid, electroless plating efficiency are not high, the bonding force of higher, the silvered film of reunion degree and matrix is not strong between particle shortcoming.
Summary of the invention
The object of the invention is to overcome the problems referred to above, provide that a kind of yield is higher, the preparation method of the better silicon dioxide composite powder of uniform surface degree.
To achieve these goals, the technical solution used in the present invention is: the preparation method of the silver-plated composite granule of silicon-dioxide, is characterized in that, comprise the steps:
(1) SiO is taken 2powder, heating SiO 2powder is to melting, and mixing, makes SiO 2colloidal fluid;
(2) to SiO 2colloidal fluid carries out centrifugal treating, makes SiO 2particulate;
(3) with formaldehyde-silver ammino solution, more dropwise polyvinyl alcohol is added, then to SiO under ul-trasonic irradiation 2particulate carries out chemical silvering; Wherein the PH of formaldehyde-silver ammino solution is 10-10.5.Preferably, PH is 10.5.
Further, described SiO 2the mol ratio of powder and polyvinyl alcohol is 5:1-10:1; A speed of polyvinyl alcohol is 2ml/min.
Preferably, described SiO 2the diameter of particulate is 7-12nm.
Preferably, silver ions and SiO in described formaldehyde-silver ammino solution 2the mol ratio of powder is 1:1-2:1.
Preferably, the formaldehyde in described formaldehyde-silver ammino solution and SiO 2the mol ratio of powder is 0.5:1; Ammonia in described formaldehyde-silver ammino solution and and SiO 2the mol ratio of powder is 1:1-2:1.
Further, also pyridine is added in described step (3).Described pyridine and SiO 2powder mol ratio is 1:5-1:10.
Further, in step (2), centrifugal rotational speed is 3000rpm/min, and centrifugation time is 3min.
In step (3), the step of supersound process is: supersound process 3s, stops 3s, repeats above operation.
Preparation method of the present invention selects dropwise to add polyvinyl alcohol, makes system more even dispersedly, and the PH of silver plating liquid selects 10-10.5, when especially PH selects 10.5, farthest can take into account silver-plated efficiency and silver plating liquid stability, prevent particle from producing reunion; Formaldehyde and silver ammino solution separate configuration, contribute to the stability improving silver plating liquid.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail:
Embodiment 1
(1) SiO is got 2powder 0.1mol, heating SiO 2powder mixes to melting, makes SiO 2colloidal fluid;
(2) to SiO 2colloidal fluid carries out centrifugal treating, makes SiO 2particulate; Centrifugal rotational speed is 3000rpm/min, and centrifugation time is 3min; SiO 2the diameter of particulate is 8nm;
(3) with formaldehyde-silver ammino solution, polyvinyl alcohol 0.02mol is dropwise added, under pyridine exists, to SiO under ul-trasonic irradiation 2particulate carries out chemical silvering; Wherein the PH of formaldehyde-silver ammino solution is 10.Formaldehyde solution and silver ammino solution configure respectively, silver ions and SiO 2the mol ratio of powder is 1:1; Formaldehyde and SiO 2the mol ratio of powder is 0.5:1; Ammonia and and SiO 2the mol ratio of powder is 1:1.Pyridine and SiO 2powder mol ratio is 1:5.The step of supersound process is: supersound process 3s, stops 3s, repeats above operation.A speed of polyvinyl alcohol is 2ml/min.
Embodiment 2
(1) SiO is got 2powder 0.1mol, heating SiO 2powder is to melting, and mixing, makes SiO 2colloidal fluid;
(2) to SiO 2colloidal fluid carries out centrifugal treating, makes SiO 2particulate; Centrifugal rotational speed is 3000rpm/min, and centrifugation time is 3min; SiO 2the diameter of particulate is 10nm;
(3) with formaldehyde-silver ammino solution, then polyvinyl alcohol 0.01mol is dropwise added, under pyridine exists, to SiO under ul-trasonic irradiation 2particulate carries out chemical silvering; Wherein the PH of formaldehyde-silver ammino solution is 10.5.Formaldehyde solution and silver ammino solution configure respectively, silver ions and SiO 2the mol ratio of powder is 2:1; Formaldehyde and SiO 2the mol ratio of powder is 0.5:1; Ammonia and and SiO 2the mol ratio of powder is 2:1.Pyridine and SiO 2powder mol ratio is 1:10.The step of supersound process is: supersound process 3s, stops 3s, repeats above operation.A speed of polyvinyl alcohol is 2ml/min.
Embodiment 3
(1) SiO is got 2powder 0.1mol, heating SiO 2powder is to melting, and mixing, makes SiO 2colloidal fluid;
(2) to SiO 2colloidal fluid carries out centrifugal treating, makes SiO 2particulate; Centrifugal rotational speed is 3000rpm/min, and centrifugation time is 3min; SiO 2the diameter of particulate is 12nm;
(3) with formaldehyde-silver ammino solution, then polyvinyl alcohol 0.015mol is dropwise added under pyridine exists, to SiO under ul-trasonic irradiation 2particulate carries out chemical silvering; Wherein the PH of formaldehyde-silver ammino solution is 10.5.Formaldehyde solution and silver ammino solution configure respectively, silver ions and SiO 2the mol ratio of powder is 2:1; Formaldehyde and SiO 2the mol ratio of powder is 0.5:1; Ammonia and and SiO 2the mol ratio of powder is 1:1.Pyridine and SiO 2powder mol ratio is 1:7.The step of supersound process is: supersound process 3s, stops 3s, repeats above operation.A speed of polyvinyl alcohol is 2ml/min.
Comparative example 1
(1) SiO is got 2powder 0.1mol, heating SiO 2powder is to melting, and mixing, makes SiO 2colloidal fluid;
(2) to SiO 2colloidal fluid carries out centrifugal treating, makes SiO 2particulate; Centrifugal rotational speed is 3000rpm/min, and centrifugation time is 3min; SiO 2the diameter of particulate is 9nm;
(3) with formaldehyde-silver ammino solution, then polyvinyl alcohol 0.015mol is dropwise added, under pyridine exists, to SiO under ul-trasonic irradiation 2particulate carries out chemical silvering; Wherein the PH of formaldehyde-silver ammino solution is 9.8.Formaldehyde solution and silver ammino solution configure respectively, silver ions and SiO 2the mol ratio of powder is 1:1; Formaldehyde and SiO 2the mol ratio of powder is 0.5:1; Ammonia and and SiO 2the mol ratio of powder is 1:1.Pyridine and SiO 2powder mol ratio is 1:8.The step of supersound process is: supersound process 3s, stops 3s, repeats above operation.A speed of polyvinyl alcohol is 2ml/min.
Comparative example 2
(1) SiO is got 2powder 0.1mol, heating SiO 2powder is to melting, and mixing, makes SiO 2colloidal fluid;
(2) to SiO 2colloidal fluid carries out centrifugal treating, makes SiO 2particulate; Centrifugal rotational speed is 3000rpm/min, and centrifugation time is 3min; SiO 2the diameter of particulate is 8nm;
(3) with formaldehyde-silver ammino solution, then polyvinyl alcohol 0.01mol is dropwise added, under pyridine exists, to SiO under ul-trasonic irradiation 2particulate carries out chemical silvering; Wherein the PH of formaldehyde-silver ammino solution is 10.8.Formaldehyde solution and silver ammino solution configure respectively, silver ions and SiO 2the mol ratio of powder is 1:1; Formaldehyde and SiO 2the mol ratio of powder is 0.5:1; Ammonia and and SiO 2the mol ratio of powder is 1:1.Pyridine and SiO 2powder mol ratio is 1:8.The step of supersound process is: supersound process 3s, stops 3s, repeats above operation.A speed of polyvinyl alcohol is 2ml/min.
Performance evaluation mode and the standard of implementation:
Reclaim the silicon dioxide composite powder of each embodiment and comparative example, verify the uniformity on yield and surface respectively.Wherein uniform surface degree is artificial definition, and be defined as I level, II level and III level according to the degree of roughness on surface, wherein I level is the most smooth.
The performance test results of 5 embodiments is shown in lower each table (table 1):
Table 1: the performance test results table
As can be seen from the above table, the preparation method of the silver-plated composite granule of silicon-dioxide of the present invention, the yield of its obtained silicon dioxide composite powder is higher, and uniform surface degree is better, illustrates that it effectively prevent intergranular reunion.
More than show and describe ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.

Claims (9)

1. the preparation method of the silver-plated composite granule of silicon-dioxide, is characterized in that, comprise the steps:
(1) SiO is taken 2powder, heating SiO 2powder dropwise adds polyvinyl alcohol again to melting, and mixing, makes SiO 2colloidal fluid;
(2) to SiO 2colloidal fluid carries out centrifugal treating, makes SiO 2particulate;
(3) with formaldehyde-silver ammino solution, to SiO under ul-trasonic irradiation 2particulate carries out chemical silvering; Wherein the PH of formaldehyde-silver ammino solution is 10-10.5.
2. the preparation method of the silver-plated composite granule of silicon-dioxide according to claim 1, is characterized in that: in step (1), described SiO 2the mol ratio of powder and polyvinyl alcohol is 5:1-10:1; A speed of polyvinyl alcohol is 2ml/min.
3. the preparation method of the silver-plated composite granule of silicon-dioxide according to claim 1, is characterized in that: described SiO 2the diameter of particulate is 7-12nm.
4. the preparation method of the silver-plated composite granule of the silicon-dioxide according to claim 1-3 any one, is characterized in that: silver ions and SiO in described formaldehyde-silver ammino solution 2the mol ratio of powder is 1:1-2:1.
5. the preparation method of the silver-plated composite granule of silicon-dioxide according to claim 4, is characterized in that, the formaldehyde in described formaldehyde-silver ammino solution and SiO 2the mol ratio of powder is 0.5:1; Ammonia in described formaldehyde-silver ammino solution and and SiO 2the mol ratio of powder is 1:1-2:1.
6. the preparation method of the silver-plated composite granule of silicon-dioxide according to claim 4, is characterized in that, also adds pyridine in described step (3).
7. the preparation method of the silver-plated composite granule of silicon-dioxide according to claim 6, is characterized in that, described pyridine and SiO 2powder mol ratio is 1:5-1:10.
8. the preparation method of the silver-plated composite granule of silicon-dioxide according to claim 1, is characterized in that, in step (2), centrifugal rotational speed is 3000rpm/min, and centrifugation time is 3min.
9. the preparation method of the silver-plated composite granule of silicon-dioxide according to claim 1, is characterized in that, in step (3), the step of supersound process is: supersound process 3s, stops 3s, repeats above operation.
CN201410735024.1A 2014-12-04 2014-12-04 Preparation method of silver-coated silicon dioxide composite powder Pending CN104451621A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109273657A (en) * 2018-08-21 2019-01-25 厦门纬达科技有限公司 A kind of silver-plated tab of positive aluminium and its manufacture craft of flexible package lithium cell

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CN101767769A (en) * 2009-12-31 2010-07-07 浙江大学 Method for preparing silica/silver nuclear shell structure granules by using polyvinyl pyrrolidone (PVP) in an assistant way
CN102656117A (en) * 2010-01-07 2012-09-05 三菱综合材料株式会社 Synthetic amorphous silica powder and method for producing same
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109273657A (en) * 2018-08-21 2019-01-25 厦门纬达科技有限公司 A kind of silver-plated tab of positive aluminium and its manufacture craft of flexible package lithium cell

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Application publication date: 20150325