CN111205501A - Method for improving surface activity of organic polymer material or composite material - Google Patents
Method for improving surface activity of organic polymer material or composite material Download PDFInfo
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- CN111205501A CN111205501A CN201811394554.9A CN201811394554A CN111205501A CN 111205501 A CN111205501 A CN 111205501A CN 201811394554 A CN201811394554 A CN 201811394554A CN 111205501 A CN111205501 A CN 111205501A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/123—Treatment by wave energy or particle radiation
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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Abstract
The invention belongs to the technical field of materials, and particularly relates to a method for improving the surface activity of an organic polymer material or a composite material. The surface inertness of the organic polymer material and the composite material is improved by using asymmetric bipolar pulse bias. The surface activity of the modified organic polymer material and the modified composite material is obviously improved, and the material body is not influenced.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a method for improving surface activity of a material.
Background
The organic polymer material not only has excellent performances of high specific strength, corrosion resistance, electric insulation and the like, but also has the characteristics of good plasticity, easy processing and forming, low price and the like, is widely applied to the fields of aerospace, military, automobiles, manufacturing, electronics and electricity and the like, and particularly shows more and more important functions in the fields of structural materials of aerospace and the like. However, for organic polymer materials, due to low surface energy, lack of active groups on the surface, weak boundary layers and the like, the surface of the organic polymer material is inert and hydrophobic, so that the interfacial adhesion between the organic polymer material and other materials is poor, which limits the application of the material to a certain extent. Therefore, in order to improve the surface performance of the organic polymer material, the surface of the organic polymer material is functionalized by an effective surface modification method, and the application range of the organic polymer material is further expanded, which is a problem to be solved urgently at present.
In the prior art, the traditional method for surface modification of organic polymer materials mainly comprises surface grafting: through a plurality of different initiation modes, active centers are generated on the surface of the high molecular material, and the grafting polymerization of monomers is initiated, or the active groups on the surface of the polymer are utilized to graft through chemical reaction. Furthermore, chemical modifications may also be used: the organic polymer material is impregnated with a chemical agent to cause chemical and physical changes on the surface, such as sodium ammonia or sodium naphthalene treatment. In the above method, the surface grafting and chemical modification have a very limited industrial application due to the complicated process and difficult control.
Disclosure of Invention
The invention aims to provide a method for improving the surface activity of an organic polymer material or a composite material, which can effectively improve the surface inertness of the organic polymer material and the composite material.
The technical scheme of the invention is as follows:
a method for improving the surface activity of an organic polymer material or a composite material, which comprises the following steps:
step 1), pretreatment of a base material;
step 2) positioning and mounting of base material
Installing and positioning the base material by using a clamp, exposing a region to be activated, and loading the base material into a vacuum chamber, so that the material can revolve and rotate in the vacuum chamber;
step 3) activation treatment
Pumping the vacuum chamber to the background with the vacuum degree superior to 6 x 10-3Pa；
Introducing working gas, performing cleaning and activating treatment on the base material by using an asymmetric bipolar pulse bias voltage source, adjusting related parameters and improving the surface activity of the material;
the parameters include
The working air pressure is 0.1Pa to 5 Pa;
the output frequency of the power supply is 20 kHz-60 kHz;
the duty ratio of the negative pulse is 30-80%, the voltage is 500-1000V, and the current is 0.2-2A;
the positive pulse duty ratio is 5% -30%, the voltage is 0V-100V, and the current is 0.2A-2A;
the activation treatment time is 5 to 30 minutes.
The working gas comprises Ar and O2、N2、H2、NH3One of them.
The pretreatment comprises the following steps:
degreasing agent scrubbing → deionized water washing → alcohol ultrasonic cleaning → deionized water ultrasonic cleaning → compressed air drying.
And ultrasonically cleaning the glass substrate with deionized water for 10-30 minutes.
And ultrasonically cleaning the glass substrate with alcohol for 10-30 minutes.
When the substrate is a glass fiber reinforced plastic composite material, introducing working gas Ar to adjust the flow until the working pressure is 3.0Pa, starting an asymmetric bipolar pulse bias power supply, adjusting the negative pulse duty ratio of the power supply to 70%, adjusting the voltage to 1000V and adjusting the output current to 0.3A; the duty ratio of the positive pulse is 10%, the voltage is 50V, the output current is 0.2A, and the processing time is 20 minutes.
When the base material is PTFE, the working gas O is introduced2Adjusting the flow to the working air pressure of 2.0Pa, starting the asymmetric bipolar pulse bias power supply, adjusting the negative pulse duty ratio of the power supply to 70%, adjusting the voltage to 900V and adjusting the output current to 0.3A; the duty ratio of the positive pulse is 10%, the voltage is 100V, the output current is 0.2A, and the processing time is 20 minutes.
The invention has the following remarkable effects: the method utilizes asymmetric bipolar pulse bias to improve the surface inertness of organic polymer materials and composite materials. The surface activity of the modified organic polymer material and the modified composite material is obviously improved, and the material body is not influenced. The method has the advantages of simple operation, low cost, no environmental pollution and convenient industrial application.
In the surface activation process of the organic polymer material and the composite material, the surface energy and the surface activity of the organic polymer material and the composite material are improved by using an asymmetric bipolar pulse bias technology, so that the application range of the materials is widened. The technology can solve the problem that the unipolar pulse bias lights the fire in the surface activation process of the organic polymer material and the composite material, and can replace a radio frequency source or a Hall ion source, thereby not only saving the space and the cost, but also having simple operation, no pollution to the environment and being more beneficial to industrialization; on the other hand, the asymmetric bipolar pulse bias can also be used for subsequent surface modification of organic polymer materials and composite materials, such as surface metallization and the like.
Detailed Description
The present invention is further illustrated by the following specific embodiments.
Step one, pretreatment of base material
The substrate refers to an organic polymer material or a composite material, and the pretreatment refers to conventional oil removal and decontamination, so as to clean the surface of the substrate.
In this embodiment, the following steps are adopted for pretreatment:
scrubbing with a degreasing agent → washing with deionized water → ultrasonically cleaning with alcohol for 15 minutes → ultrasonically cleaning with deionized water for 10 minutes → drying with compressed air;
the organic polymer material can be PTFE, PI, PEEK, LCP, PPS, PET, PA, PAI, POM, PVC, but is not limited thereto;
the composite material can be carbon fiber composite material, glass fiber composite material, carbon fiber composite material, boron fiber composite material, aramid fiber composite material, silicon carbide fiber composite material, asbestos fiber composite material and whisker composite material, but is not limited to the above;
step two, positioning and mounting the base material
Installing and positioning the base material by using a clamp, exposing a region to be activated, and loading the base material into a vacuum chamber, so that the material can revolve and rotate in the vacuum chamber;
step three, activation treatment
Pumping the vacuum chamber to the background with the vacuum degree superior to 6 x 10-3Pa; introducing working gas, performing cleaning and activating treatment on the base material by using an asymmetric bipolar pulse bias voltage source, adjusting related parameters and improving the surface activity of the material;
the working gas comprises Ar and O2、N2、H2、NH3One of them;
the working air pressure is 0.1Pa to 5 Pa;
the output frequency of the power supply is 20 kHz-60 kHz;
the duty ratio of the negative pulse is 30-80%, the voltage is 500-1000V, and the current is 0.2-2A;
the positive pulse duty ratio is 5% -30%, the voltage is 0V-100V, and the current is 0.2A-2A;
the activation treatment time is 5 to 30 minutes;
example 1
The embodiment provides a method for improving the surface activity of an organic polymer material and a composite material, wherein a glass fiber reinforced plastic composite material is selected as a base material, and the method for activating the surface of the material comprises the following steps:
the method comprises the following steps: pretreatment of substrates
Performing pretreatment, scrubbing the degreasing agent → washing with deionized water → ultrasonically cleaning with alcohol for 15 minutes → ultrasonically cleaning with deionized water for 10 minutes → drying with compressed air.
Step two: preparation of the experiment
And (3) loading the glass fiber reinforced plastic composite material pretreated in the first step into a special tool clamp according to requirements, and exposing the area needing to be activated. Loading the pretreated substrate into a vacuum chamber to make the glass fiber reinforced plastic composite material to be treated realize revolution and autorotation in the vacuum chamber, and then pumping the vacuum chamber to a background vacuum of 5 x 10-3Pa, introducing working gas Ar to adjust the flow until the working gas pressure is 3.0Pa, starting an asymmetric bipolar pulse bias power supply, adjusting the negative pulse duty ratio of the power supply to 70%, adjusting the voltage to 1000V, and adjusting the output current to 0.3A; the duty ratio of the positive pulse is 10%, the voltage is 50V, the output current is 0.2A, and the processing time is 20 minutes.
Example 2
The embodiment provides a method for improving the surface activity of an organic polymer material and a composite material, wherein a base material is selected from PTFE, and the method for activating the surface of the material comprises the following steps:
the method comprises the following steps: pretreatment of substrates
Performing pretreatment on PTFE, and scrubbing a degreasing agent → washing with deionized water → ultrasonically cleaning with alcohol for 15 minutes → ultrasonically cleaning with deionized water for 10 minutes → drying with compressed air.
Step two: preparation of the experiment
And (4) loading the PTFE pretreated in the step one into a special tool clamp according to requirements, and exposing the area needing to be activated. Loading the pretreated substrate into a vacuum chamber to make the PTFE to be treated realize revolution and autorotation in the vacuum chamber, and then pumping the vacuum chamber to a background vacuum of 5 x 10-3Pa, introducing working gas O2 to adjust the flow to 2.0Pa, starting the asymmetric bipolar pulse bias power supply, adjusting the duty ratio of the negative pulse of the power supply to 70%, adjusting the voltage to 900V, and adjusting the output current to 0.3A; the duty ratio of the positive pulse is 10%, the voltage is 100V, the output current is 0.2A, and the processing time is 20 minutes.
The foregoing is only a preferred embodiment of the invention. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
Claims (7)
1. A method for improving the surface activity of an organic polymer material or a composite material is characterized by comprising the following steps:
step 1), pretreatment of a base material;
step 2) positioning and mounting of base material
Installing and positioning the base material by using a clamp, exposing a region to be activated, and loading the base material into a vacuum chamber, so that the material can revolve and rotate in the vacuum chamber;
step 3) activation treatment
Pumping the vacuum chamber to the background with the vacuum degree superior to 6 x 10-3Pa；
Introducing working gas, performing cleaning and activating treatment on the base material by using an asymmetric bipolar pulse bias voltage source, adjusting related parameters and improving the surface activity of the material;
the parameters include
The working air pressure is 0.1Pa to 5 Pa;
the output frequency of the power supply is 20 kHz-60 kHz;
the duty ratio of the negative pulse is 30-80%, the voltage is 500-1000V, and the current is 0.2-2A;
the positive pulse duty ratio is 5% -30%, the voltage is 0V-100V, and the current is 0.2A-2A;
the activation treatment time is 5 to 30 minutes.
2. The method according to claim 1, wherein the surface activity of the organic polymer material or the composite material is improved by: the working gas comprises Ar and O2、N2、H2、NH3One of themAnd (4) seed preparation.
3. The method for improving the surface activity of the organic polymer material or the composite material according to claim 1, wherein the pretreatment comprises the following steps:
degreasing agent scrubbing → deionized water washing → alcohol ultrasonic cleaning → deionized water ultrasonic cleaning → compressed air drying.
4. A method according to claim 3, wherein the surface activity of the organic polymer material or the composite material is improved by: and ultrasonically cleaning the glass substrate with deionized water for 10-30 minutes.
5. A method according to claim 3, wherein the surface activity of the organic polymer material or the composite material is improved by: and ultrasonically cleaning the glass substrate with alcohol for 10-30 minutes.
6. The method according to claim 1, wherein the surface activity of the organic polymer material or the composite material is improved by: when the substrate is a glass fiber reinforced plastic composite material, introducing working gas Ar to adjust the flow until the working pressure is 3.0Pa, starting an asymmetric bipolar pulse bias power supply, adjusting the negative pulse duty ratio of the power supply to 70%, adjusting the voltage to 1000V and adjusting the output current to 0.3A; the duty ratio of the positive pulse is 10%, the voltage is 50V, the output current is 0.2A, and the processing time is 20 minutes.
7. The method according to claim 1, wherein the surface activity of the organic polymer material or the composite material is improved by: when the base material is PTFE, the working gas O is introduced2Adjusting the flow to the working air pressure of 2.0Pa, starting the asymmetric bipolar pulse bias power supply, adjusting the negative pulse duty ratio of the power supply to 70%, adjusting the voltage to 900V and adjusting the output current to 0.3A; the duty ratio of the positive pulse is 10%, the voltage is 100V, the output current is 0.2A, and the processing time is 20 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811394554.9A CN111205501A (en) | 2018-11-22 | 2018-11-22 | Method for improving surface activity of organic polymer material or composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811394554.9A CN111205501A (en) | 2018-11-22 | 2018-11-22 | Method for improving surface activity of organic polymer material or composite material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5895558A (en) * | 1995-06-19 | 1999-04-20 | The University Of Tennessee Research Corporation | Discharge methods and electrodes for generating plasmas at one atmosphere of pressure, and materials treated therewith |
| JP2001214269A (en) * | 2000-01-31 | 2001-08-07 | Shinko Seiki Co Ltd | Hard carbon laminated film and deposition method therefor |
| CN101790596A (en) * | 2007-08-13 | 2010-07-28 | 英科特有限责任公司 | Method for producing a metal-oxide-coated workpiece surface with predeterminable hydrophobic behaviour |
| CN101897240A (en) * | 2007-12-10 | 2010-11-24 | 建筑研究和技术有限公司 | Method and device for the treatment of surfaces |
-
2018
- 2018-11-22 CN CN201811394554.9A patent/CN111205501A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5895558A (en) * | 1995-06-19 | 1999-04-20 | The University Of Tennessee Research Corporation | Discharge methods and electrodes for generating plasmas at one atmosphere of pressure, and materials treated therewith |
| JP2001214269A (en) * | 2000-01-31 | 2001-08-07 | Shinko Seiki Co Ltd | Hard carbon laminated film and deposition method therefor |
| CN101790596A (en) * | 2007-08-13 | 2010-07-28 | 英科特有限责任公司 | Method for producing a metal-oxide-coated workpiece surface with predeterminable hydrophobic behaviour |
| CN101897240A (en) * | 2007-12-10 | 2010-11-24 | 建筑研究和技术有限公司 | Method and device for the treatment of surfaces |
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