CN109468620A - A kind of process of flaky metallic material surface silanization processing - Google Patents
A kind of process of flaky metallic material surface silanization processing Download PDFInfo
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- CN109468620A CN109468620A CN201811329181.7A CN201811329181A CN109468620A CN 109468620 A CN109468620 A CN 109468620A CN 201811329181 A CN201811329181 A CN 201811329181A CN 109468620 A CN109468620 A CN 109468620A
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- silane
- metallic material
- flaky metallic
- material surface
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
-
- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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Abstract
The present invention provides a kind of processes of flaky metallic material surface silanization processing, and it includes following steps: S1, providing the metal plate material after cleaning；And S2, the flaky metallic material after cleaning is immersed in solution of silane, the solution of silane is the water-soluble solution composition for including silane coupling agent and hydrolysising solvent, the silane coupling agent be selected from vinyl silanes, amino silane, methacryloxypropyl silane, phenyl silane, esters of silicon acis, epoxy silane it is one or more.This method is more environmentally-friendly compared to conventional method, endangers operator small；It is surface-treated more uniform；Possess better performance feature, such as wetting, anti-settling, bonding etc.；It can effectively reduce surface treatment cost；Handled obtained flake metal powder, can be not only used for the traditional fields such as ink, coating, improve the performance of its product various aspects, and simultaneously for the novel field such as electromagnetic shielding material, unique process for treating surface can also play good effect.
Description
Technical field
The present invention relates to technical field of metal material surface treatment, more particularly to a kind of more environmentally friendly, acquisition properties of product
More preferably, the process of the lower flaky metallic material surface silanization processing of processing cost.
Background technique
Flaky metallic material is made of metal-powder through techniques such as ball millings, since it is with good adhesive force, significant
The characteristics such as screen effect, the ability of stronger reflection light and other excellent physical properties, so by difference should be arrived extensively
The fields such as field, such as coating, ink and electromagnetic shielding.Usual flaky metallic material surface needs to perform corresponding processing, from
And to meet requirement of the different product for performances such as amphipathic property, wetability, dispersibility, corrosion resistances.At present for gold
The processing method of metal surface has: cathode protection method, anodic protection method, corrosion inhibiter facture and metal surface coating method etc..Its
Middle metal surface coating method is a kind of common method in industrial production, spray in metal surface, serve as a contrast, seeping, plating, coat one layer it is resistance to
The preferable metal of corrosivity or nonmetallic substance and metal is subjected to phosphatization, oxidation processes, make to be protected metal surface and is situated between
Matter mechanical isolation and reduce metal erosion.
In the field of Treatment of Metal Surface, although traditional phosphate conversion and chromating process for treating surface can be with
Contain heavy metal ion and the nitrous such as zinc, manganese, nickel, chromium in the waste liquid that certain effect can be played, but be discharged in treatment process
The carcinogens such as hydrochlorate, environmental pollution are very serious.If the process for treating surface is applied directly to flaky metallic material
Surface treatment procedure in, it may appear that the problems such as processing is not exclusively, uneven, treatment effect is undesirable.Silane is containing there are two types of not
Same chemical functional group, one end can be reacted with inorganic material surfaces amount hydroxyls such as metals, and the other end can be generated with organic material
Covalent bond can improve flaky metallic material in different mixed systems while providing protection to inorganic metal surface
The performances such as dispersibility, adhesiveness and cohesive strength.Specifically, the prior art has the disadvantages that and reason:
1, the use of phosphate and heavy metal salt, environmental pollution is serious, will also result in very big influence to human body；
2, traditional metal surface processing method, because of flaky metallic material large bulk density, spatial gaps are small, and draw ratio is big, right
It is bad in such material surface treatment effect；
3, it is not able to satisfy different application field for the performance requirement of flaky metallic material, application range of products is limited；
4, the use of a large amount of industrial reagents can improve Treatment of Metal Surface cost.
Summary of the invention
In order to solve the above problem, the present invention provides a kind of replacements or part to replace at the surface of traditional heavy metal phosphatization
Reason technology reduces the process of the flaky metallic material surface silanization processing influenced on human body and environment.
The present invention provides a kind of processes of flaky metallic material surface silanization processing, and it includes following steps:
S1, the metal plate material after cleaning is provided；And
S2, the flaky metallic material after cleaning is immersed in solution of silane, the solution of silane be include silane coupling agent
With the water-soluble solution composition of hydrolysising solvent, the silane coupling agent is selected from vinyl silanes, amino silane, metering system
Acyloxy silane, phenyl silane, esters of silicon acis, epoxy silane it is one or more.
In a preferred embodiment of the invention, the quality of the silane coupling agent and hydrolysising solvent is 0.05- than ratio ranges
0.3。
In a preferred embodiment of the invention, the silane coupling agent is the water containing vinyl silanes and amino silane
Soluble solution composition.
Wherein, the concentration of the vinyl silanes and the concentration of amino silane are 1-5 than ratio ranges.
The hydrolysising solvent is selected from one of ionized water, methanol, deionized water, ethyl alcohol or a variety of.Different water
Solution solvent will lead to solution stability and hydrolysis degree it is different, according to the water solubility and hydrolysis-condensation reaction of silane coupling agent
Equilibrium system is classified as hydrophobic silane and selects methanol/ethanol+deionized water as hydrolysising solvent, hydrophilic silane selection go from
Sub- water is hydrolysising solvent.
The metal sheet is selected from flake aluminum, flake copper powder, zinc flake, flake silver powder and sheet Fe based alloy
Micro mist is one such.
Specific to step S1 is comprised the steps of:
S11, flaky metallic material is added to prepared alkaline solution in 50-80 DEG C of ultrasonic cleaning 5-10min；The alkali
Property solution be alkaline system solution made of selecting any alkaline matter proportion, pH value can adjust accordingly as required.
S12, the flaky metallic material after first time alkali cleaning is filtered and is rinsed well with deionized water；
S13, the flaky metallic material rinsed well is put into alkaline solution it is cleaned by ultrasonic 1- under the conditions of 50-80 DEG C of temperature
5min。
Preferably, also include step S14: the metal sheet after secondary alkali cleaning being rinsed well with deionized water, indifferent gas
It is dried under the conditions of 80-120 DEG C of temperature under body atmosphere.
Preferably, the process also packet step S3 of flaky metallic material surface silanization processing:
Flaky metallic material in solution of silane is filtered and is taken out, and hot setting obtains target production under inert gas atmosphere
Product.
A kind of process of flaky metallic material surface silanization processing provided by the invention, the preparation work such as ball milling annealing
The flaky metallic material obtained after sequence is impregnated by solution of silane again after alkali cleaning, under inert gas atmosphere after high temperature drying i.e.
Flaky metallic material of the surface through silanization treatment can be obtained.Compared to traditional metal surface treatment technology, have following excellent
Point:
1, more environmentally-friendly, operator is endangered small；
2, surface treatment is more uniform, and effect is good；
3, silanization treatment can make flaky metallic material possess the performance characteristics more preferably soak, is anti-settling, bonding etc.；
4, the cost of surface treatment can be effectively reduced；
5, handled obtained flake metal powder, can be not only used for the traditional fields such as ink, coating, improve its product each side
The performance in face, simultaneously for the novel field such as electromagnetic shielding material, unique process for treating surface can also be played well
Effect.
Detailed description of the invention
With reference to the accompanying drawing, by the way that detailed description of specific embodiments of the present invention, technical solution of the present invention will be made
And other beneficial effects are apparent.
Fig. 1 is through surface silanization treated flaky metallic material chemical structure schematic diagram.
Specific embodiment
Further to illustrate technological means and its effect adopted by the present invention, below in conjunction with preferred implementation of the invention
Example and its attached drawing are described in detail.
The present invention provides a kind of processes of flaky metallic material surface silanization processing, to replace or part generation
For the process for treating surface of traditional heavy metal phosphatization.The flaky metallic material obtained after the preparation sections such as ball milling annealing, through alkali
It is impregnated again by solution of silane after washing, sheet of the surface through silanization treatment can be obtained after high temperature drying under inert gas atmosphere
Metal material, its chemical structure schematic diagram is as shown in Figure 1 after processing.
Embodiment 1:
S1, sheet Fe based alloy micro mist is selected as raw material and to be cleaned；
S11,30g sheet Fe based alloy micro mist is added into prepared 100g alkaline solution, it is ultrasonic under the conditions of 50 DEG C of temperature
Clean 5min；
S12, the sheet Fe based alloy micro mist after first time alkali cleaning is filtered and is rinsed well with deionized water；
It is cleaned by ultrasonic 1min again for 50 DEG C in S13, alkaline solution
It after the completion of S14, operation, is rinsed well with deionized water, is dried under the conditions of the lower 80 DEG C of temperature of inert gas atmosphere；
S2, by treated, sheet Fe based alloy micro mist is added in prepared solution of silane, and silane coupling agent selects 9g ethylene
Base silane and 3g amino silane are added to the medicinal alcohol that 100g concentration is 75% and are formulated, and impregnate 5min；
S3, the sheet Fe based alloy micro mist in solution of silane is filtered and is taken out, and in a nitrogen atmosphere, 160 DEG C of hot settings
Sheet Fe based alloy micro mist of the surface through silanization treatment can be obtained in 120min.
Embodiment 2:
S1, flake aluminum is selected as raw material and to be cleaned,
S11,30 flake aluminums are entered to prepared 100g alkaline solution, 60 DEG C of ultrasonic cleaning 8min；
S12, the flake aluminum after first time alkali cleaning is filtered and is rinsed well with deionized water；
S13, the flake aluminum rinsed well is cleaned by ultrasonic 2min under the conditions of 70 DEG C of temperature in alkaline solution again；
S14, the flake aluminum after second of alkali cleaning is rinsed well with deionized water, 100 DEG C of temperature in inert gas atmosphere
It is dried under the conditions of degree；
S2, treated flake aluminum is added in prepared solution of silane, silane coupling agent select 9g vinyl silanes and
4.5g amino silane is added to the methanol that 100g concentration is 75% and is formulated, and impregnates 3min；
S3, the flake aluminum in solution of silane is filtered and is taken out, and in a nitrogen atmosphere, 160 DEG C of hot setting 120min
Obtain flake aluminum of the surface through silanization treatment.
Embodiment 3:
S1, flake copper powder is selected as raw material and to be cleaned,
S11,30 flake copper powders are entered into prepared 100g alkaline solution, 60 DEG C of ultrasonic cleaning 6min.
S12, the flake copper powder after first time alkali cleaning is filtered and is rinsed well with deionized water；
S13, the flake copper powder rinsed well is cleaned by ultrasonic 3min for 60 DEG C in alkaline solution again；
S14, the flake copper powder after second of alkali cleaning is rinsed well with deionized water, 110 DEG C of temperature in inert gas atmosphere
The carefully lower drying of degree condition；
S2, treated flake copper powder is added in prepared solution of silane, silane coupling agent select 5g vinyl silanes and
1g amino silane is added to the medicinal alcohol that 100g concentration is 75% and is formulated, and impregnates 4min；
S3, the sheet Fe based alloy micro mist in solution of silane is filtered and is taken out, and in a nitrogen atmosphere, 160 DEG C of hot settings
Flake copper powder of the surface through silanization treatment can be obtained in 120min.
Embodiment 4:
S1, zinc flake is selected as raw material and to be cleaned,
S11,30 zinc flakes are entered to prepared 100g alkaline solution, 80 DEG C of ultrasonic cleaning 10min.
S12, the zinc flake after first time alkali cleaning is filtered and is rinsed well with deionized water；
S13, the zinc flake rinsed well is cleaned by ultrasonic 4min for 70 DEG C in alkaline solution again；
S14, the zinc flake after second of alkali cleaning is rinsed well with deionized water, 110 DEG C of temperature in inert gas atmosphere
It is dried under the conditions of degree；
S2, by treated, zinc flake is added in prepared solution of silane, and silane coupling agent selects 9g phenyl silane and 3g
Epoxy silane is added to the methanol that 100g concentration is 75% and is formulated, and impregnates 5min；
S3, the zinc flake in solution of silane is filtered and is taken out, and in a nitrogen atmosphere, 160 DEG C of hot setting 120min
Obtain zinc flake of the surface through silanization treatment.
Embodiment 5:
S1, flake silver powder is selected as raw material and to be cleaned,
S11,30g flake silver powder is entered to prepared 100g alkaline solution, 50 DEG C of ultrasound 5min.
S12, the flake silver powder after first time alkali cleaning is filtered and is rinsed well with deionized water；
S13, the flake silver powder rinsed well is cleaned by ultrasonic 5min for 80 DEG C in alkaline solution again；
S14, the flake silver powder after second of alkali cleaning is rinsed well with deionized water, 120 DEG C in inert gas atmosphere
It is dried under the conditions of temperature.
S2, by treated, flake silver powder is added in prepared solution of silane, and silane coupling agent selects 6g metering system
The medicinal alcohol that acyloxy silane and 3g phenyl silane are 75% with addition to 100g concentration is formulated, and impregnates 5min；
S3, the flake silver powder in solution of silane is filtered and is taken out, and in a nitrogen atmosphere, 160 DEG C of hot setting 120min
Obtain flake silver powder of the surface through silanization treatment.
Take 10g through above-mentioned steps surface silanization treated sheet Fe base alloy powder, flake aluminum, flake copper powder,
Zinc flake and flake silver powder carry out thermal expansion coefficient and corrosion resistance salt spray test, and thermal expansion coefficient is 10.6 × 10-6 K-11、20.2×10-6 K-1、15.4×10-6 K-1、32.3×10-6 K-1With 16.8 × 10-6 K-1, relative to the sheet material before processing
Material, thermal expansion coefficient is to reduce, and by each test sample after 35 DEG C × 15 days salt spray tests, test specimens quality is unchanged.
Illustrate that surface has been provided with excellent corrosion resistance through the sheet Fe base alloy powder of silanization treatment, meets quality requirement.
The above for those of ordinary skill in the art can according to the technique and scheme of the present invention and technology
Other various corresponding changes and modifications are made in design, and all these change and modification all should belong to the claims in the present invention
Protection scope.
Claims (9)
1. a kind of process of flaky metallic material surface silanization processing, which is characterized in that comprise the steps of:
S1, the metal plate material after cleaning is provided；And
S2, the flaky metallic material after cleaning is immersed in solution of silane, the solution of silane be include silane coupling agent
With the water-soluble solution composition of hydrolysising solvent, the silane coupling agent is selected from vinyl silanes, amino silane, metering system
Acyloxy silane, phenyl silane, esters of silicon acis, epoxy silane it is one or more.
2. the process of flaky metallic material surface silanization processing according to claim 1, which is characterized in that described
The quality of silane coupling agent and hydrolysising solvent is 0.05-0.3 than ratio ranges.
3. the process of flaky metallic material surface silanization processing according to claim 1, which is characterized in that described
Silane coupling agent is the water-soluble solution composition containing vinyl silanes and amino silane.
4. the process of flaky metallic material surface silanization processing according to claim 3, which is characterized in that described
The concentration of vinyl silanes and the concentration of amino silane are 1-5 than ratio ranges.
5. the process of flaky metallic material surface silanization processing according to claim 1, which is characterized in that described
Hydrolysising solvent is selected from one of ionized water, methanol, deionized water, ethyl alcohol or a variety of.
6. the process of flaky metallic material surface silanization processing according to claim 1, which is characterized in that described
Metal sheet is selected from flake aluminum, flake copper powder, zinc flake, flake silver powder and sheet Fe based alloy micro mist therein one
Kind.
7. the process of flaky metallic material surface silanization processing according to claim 1, which is characterized in that step
S1 is comprised the steps of:
S11, flaky metallic material is added to prepared alkaline solution in 50-80 DEG C of ultrasonic cleaning 5-10min；
S12, the flaky metallic material after first time alkali cleaning is filtered and is rinsed well with deionized water；
S13, the flaky metallic material rinsed well is put into alkaline solution it is cleaned by ultrasonic 1- under the conditions of 50-80 DEG C of temperature
5min。
8. the process of flaky metallic material surface silanization processing according to claim 7, which is characterized in that also wrap
S14 containing step: the metal sheet after secondary alkali cleaning is rinsed well with deionized water, at 80-120 DEG C under inert gas atmosphere
It is dried under the conditions of temperature.
9. the process of flaky metallic material surface silanization processing according to claim 1 or 8, which is characterized in that
Also packet step S3:
Flaky metallic material in solution of silane is filtered and is taken out, and hot setting obtains target production under inert gas atmosphere
Product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111073507A (en) * | 2019-10-12 | 2020-04-28 | 广东省测试分析研究所（中国广州分析测试中心） | Water-based chromium-free zinc-aluminum anticorrosive paint and preparation method thereof |
| CN113770348A (en) * | 2021-09-09 | 2021-12-10 | 清华大学 | Preparation method and application of ultrahigh-conductivity material |
| CN115874186A (en) * | 2022-12-05 | 2023-03-31 | 诺泰生物科技(合肥)有限公司 | Preparation method and application of water-based siloxane aluminum copper corrosion inhibitor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111073507A (en) * | 2019-10-12 | 2020-04-28 | 广东省测试分析研究所（中国广州分析测试中心） | Water-based chromium-free zinc-aluminum anticorrosive paint and preparation method thereof |
| CN111073507B (en) * | 2019-10-12 | 2022-03-25 | 广东省测试分析研究所（中国广州分析测试中心） | Water-based chromium-free zinc-aluminum anticorrosive paint and preparation method thereof |
| CN113770348A (en) * | 2021-09-09 | 2021-12-10 | 清华大学 | Preparation method and application of ultrahigh-conductivity material |
| CN115874186A (en) * | 2022-12-05 | 2023-03-31 | 诺泰生物科技(合肥)有限公司 | Preparation method and application of water-based siloxane aluminum copper corrosion inhibitor |
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