CN113583495A - Low-air-out-rate antistatic optical absorption coating and preparation method thereof - Google Patents

Low-air-out-rate antistatic optical absorption coating and preparation method thereof Download PDF

Info

Publication number
CN113583495A
CN113583495A CN202110997957.8A CN202110997957A CN113583495A CN 113583495 A CN113583495 A CN 113583495A CN 202110997957 A CN202110997957 A CN 202110997957A CN 113583495 A CN113583495 A CN 113583495A
Authority
CN
China
Prior art keywords
coating
optical absorption
silsesquioxane
preparing
absorption coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110997957.8A
Other languages
Chinese (zh)
Other versions
CN113583495B (en
Inventor
俞兵
王啸
袁林光
郭朝龙
范纪红
史浩飞
李燕
朴明星
秦艳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian institute of Applied Optics
Original Assignee
Xian institute of Applied Optics
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian institute of Applied Optics filed Critical Xian institute of Applied Optics
Priority to CN202110997957.8A priority Critical patent/CN113583495B/en
Publication of CN113583495A publication Critical patent/CN113583495A/en
Application granted granted Critical
Publication of CN113583495B publication Critical patent/CN113583495B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/017—Additives being an antistatic agent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

The invention belongs to the technical field of optical absorption coatings, and discloses a preparation method of an antistatic optical absorption coating with low air-out rate, which comprises the following steps: preparing a primary coating dispersion liquid, preparing a primary coating, preparing a top coating suspension, preparing a top coating and carrying out coating heat treatment. The invention adopts a non-polymer reaction system which mainly adopts carbon materials, has the characteristics of no decomposition products, no free small molecules and the like, and eliminates the gas pollution from coating material components; hydrophilic functional groups in the high-hydrophobicity siloxane closed carbon material are adopted, so that the adsorption capacity of the coating to environmental gases such as water vapor is greatly reduced; meanwhile, the coating has better antistatic performance and can meet the application requirement of a specific space environment.

Description

Low-air-out-rate antistatic optical absorption coating and preparation method thereof
Technical Field
The invention belongs to the technical field of optical absorption coatings, and relates to an antistatic optical absorption coating with low air-out rate and a preparation method thereof.
Background
The optical absorption coating is a functional coating widely used in a space load system, and plays an important role in the fields of stray light inhibition, thermal radiation control, black body calibration and the like. When the coating is in a space vacuum environment, due to the fact that external air pressure is reduced, concentration balance inside and outside the coating is broken, certain substances inside and on the surface of the coating can be diffused, evaporated and sublimated to be separated from the surface, a gas outlet phenomenon is generated, the escaped small molecules are further condensed or deposited on the surfaces of sensitive devices such as an optical lens, a heat radiation material and a heat control material in a space load system, a pollution effect is generated, and the function of the system is reduced or even the system fails. The indexes of the coating such as Total Mass Loss (TML), condensable volatile matters (CVCM) and water vapor resorption amount (WVR) in a space vacuum environment are main indexes for judging the air pollution. Coating materials for space loading of spacecraft and the like generally require TML < 1% and CVCM < 0.1%. The requirements of a space optical load system and a low-temperature infrared system on coating gas outlet pollution control are more strict, the signal intensity of the optical system is reduced by pollutants, the signal-to-noise ratio is reduced, the surface of the low-temperature optical load is easy to condense the pollutants, the reliability of the system is seriously reduced, and the service life of the system is seriously shortened, so that the CVCM of the coating is generally required to be less than 0.01%. The existing commercial coatings represented by Z306, E51 and the like are difficult to realize good condensable volatile pollution control, and the performance of the optical system is reduced by more than 10 percent, and some coatings even exceed 30 percent. At the present stage, along with the continuous development of the applied satellite technology, stricter requirements are put forward on the control of the outgassing pollution source, and the preparation of the optical coating with low outgassing rate needs to be further explored by the design and development departments of the space vehicle.
Research shows that under a space vacuum environment, small molecule sources escaping from the interior and the surface of the coating mainly comprise three types: the coating absorbs gases such as water vapor, oxygen, nitrogen, carbon dioxide and the like; some components in the coating material are slowly decomposed to generate small molecules; free small molecules in the coating composition that have not polymerized to completion. Therefore, inhibiting the generation of these escaping small molecules becomes a key problem to solve the coating outgassing pollution.
Disclosure of Invention
Objects of the invention
In order to solve the problem of inhibiting three types of gas outlet sources proposed in the prior art, the invention provides an antistatic optical absorption coating with low gas outlet rate and a preparation method thereof, the method adopts a non-polymer reaction system which mainly adopts carbon materials, has the characteristics of no decomposition products, no free small molecules and the like, and eliminates the gas outlet pollution from coating material components; hydrophilic functional groups in the high-hydrophobicity siloxane closed carbon material are adopted, so that the adsorption capacity of the coating to environmental gases such as water vapor is greatly reduced; meanwhile, the coating has better antistatic performance and can meet the application requirement of a specific space environment.
(II) technical scheme
In order to solve the technical problems, the invention provides a preparation method of an antistatic optical absorption coating with low air-out rate, which is characterized in that the optical absorption coating with low air-out rate and antistatic function is prepared by depositing a graphene oxide/silsesquioxane primer coating and a carbon nanotube/silsesquioxane topcoat step by step. The preparation process of the coating comprises the following steps:
s1: preparation of the basecoat Dispersion
Uniformly dispersing graphene oxide micro-sheets in an organic solvent for ultrasonic treatment, adding silsesquioxane, and mixing and stirring at room temperature to obtain a graphene oxide/silsesquioxane dispersion liquid.
Wherein, according to mass fraction, the graphene oxide is 50-99 parts, and the silsesquioxane is 1-50 parts.
S2: preparation of the base coat
And (3) uniformly depositing the primer dispersion prepared in the step S1 on the clean substrate surface, and volatilizing at a proper amount at room temperature to obtain the primer.
S3: preparation of the topcoat suspension
And (2) carrying out ultrasonic treatment on the carbon nano tube in an organic solvent, adding silsesquioxane, mixing and stirring at room temperature to obtain a carbon nano tube/silsesquioxane suspension.
Wherein, according to the mass fraction, the carbon nano tube is 75-95 parts, and the silsesquioxane is 5-25 parts.
S4: preparing a top coat:
the top-coat suspension prepared in step S3 was uniformly deposited on the undercoated surface prepared in step S2, and then transferred to a fume hood and the solvent was evaporated at room temperature to obtain a top-coat.
S5: heat treatment of coatings
And (4) placing the coating prepared in the step S4 in a vacuum oven for heat treatment, and naturally cooling to room temperature along with the furnace.
Wherein the heat treatment conditions are as follows: keeping the temperature at 50-80 ℃ for 6-48 hours, then heating to 180-220 ℃ and keeping the temperature for 5-60 minutes.
Preferably, in step S1, the organic solvent is tetrahydrofuran, n-hexane, chloroform, acetone, toluene or dichloromethane; the diameter of the graphene oxide microchip is 0.05-50 μm; the silsesquioxane structure is irregular, trapezoidal, cage-shaped or semi-cage-shaped; the side group R is epoxy group, hydroxyl or amino; the concentration of the priming paint dispersion liquid is 0.1-10 mg/ml.
Preferably, in step S2, the substrate is made of metal, glass, ceramic or polymer; the volatilization time of the solvent is 0.5 to 12 hours.
Preferably, in step S3, the outer wall of the carbon nanotube contains functional groups such as hydroxyl and/or carboxyl; the organic solvent is the same as the organic solvent used in step S1; the silsesquioxane is the same as the silsesquioxane used in step S1; the concentration of the top coating suspension is 0.1-10 mg/ml.
Preferably, in step S4, the solvent volatilization time is 6 to 24 hours.
The invention also provides an optical absorption coating prepared by the preparation method based on the low-air-out-rate antistatic optical absorption coating.
(III) advantageous effects
The antistatic optical absorption coating with low air yield and the preparation method thereof provided by the technical scheme have the following beneficial effects:
(1) according to the invention, non-polymer systems such as carbon nanotubes and graphene with high optical absorption capacity are used as components of the coating, no decomposition products and free small molecules are generated in a space vacuum environment, and the total mass loss and the detection value of the condensable volatile matter of the coating reach extremely low levels.
(2) The invention utilizes the silsesquioxane to carry out hydrophilic and hydrophobic modification on a coating material system, converts the original hydrophilic coating into a high-hydrophobic coating, reduces the adsorption of the coating on water vapor and the like in the environment, reduces the escape of the environmental gases in a space vacuum environment, and greatly reduces the water vapor resorption amount of the coating.
(3) The coating prepared by the invention has good antistatic performance, can be applied to specific space environment, and expands the use scene of the coating.
In conclusion, the invention effectively inhibits the generation of three types of common escaping molecular sources of the coating in a space vacuum environment, solves the problem of pollution of the outgassing of the optical absorption coating to a system sensitive device, and provides a support for the development of space load with long service life and high stability.
Drawings
FIG. 1 is a schematic structural view of the low outgassing antistatic optical absorption coating of the present invention.
Detailed Description
In order to make the objects, contents and advantages of the present invention clearer, the following detailed description of the embodiments of the present invention will be made in conjunction with the accompanying drawings and examples.
Example 1:
the preparation process of the antistatic optical absorption coating with low air-out rate comprises the following steps:
s1: preparation of the undercoating dispersion:
uniformly dispersing graphene oxide micro-sheets with the average diameter of 10 mu m in organic solvent tetrahydrofuran for ultrasonic treatment, adding a certain amount of cage type silsesquioxane with amino side groups, and mixing and stirring at room temperature to obtain graphene oxide/silsesquioxane dispersion liquid, wherein the weight ratio of graphene oxide to silsesquioxane is 70: 30. The concentration of the dispersion was 1 mg/ml.
S2: preparation of the base coat:
and (4) uniformly depositing the dispersion liquid prepared in the step S1 on a clean aluminum-based surface, and volatilizing at room temperature for 6 hours to obtain a base coat.
S3: preparation of topcoat suspensions:
the method comprises the following steps of carrying out ultrasonic treatment on a hydroxylated carbon nano tube in organic solvent tetrahydrofuran, adding a certain amount of cage type silsesquioxane with amino as a side group, mixing and stirring at room temperature to obtain a carbon nano tube/silsesquioxane suspension, wherein the weight ratio of the carbon nano tube to the silsesquioxane is 75: 25. The suspension concentration was 1 mg/ml.
S4: preparing a top coat:
the suspension prepared in step S3 was uniformly deposited on the undercoated surface prepared in step S2, and then transferred to a fume hood and the solvent was evaporated at room temperature for 12 hours to obtain a topcoat.
S5: coating heat treatment:
and (4) placing the coating prepared in the step S4 in a vacuum oven for heat treatment, and naturally cooling to room temperature along with the furnace. Wherein the heat treatment conditions are as follows: the incubation was carried out at 60 ℃ for 48 hours, then at 200 ℃ and for 5 minutes.
For the determination of TML, CVCM and WVR values in vacuum environment of coating space, the test sample is heated to 125 ℃ + -1 deg.C, the collection temperature of condensable volatile is 25 ℃ + -1 deg.C, and the vacuum degree is better than 1x10-3Pa, test time 24 hours. Three samples are taken for testing, and the test result is the average value of the three samples. Coating TML as 0.08% as prepared in this example; CVCM ═ c0.005％；WVR＝0.09％。
The coating prepared in this example had a conductivity of 0.03S/cm.
Example 2:
the antistatic optical absorption coating with low air-out rate is prepared by the following steps:
s1: preparation of the undercoating dispersion:
uniformly dispersing graphene oxide micro-sheets with the average diameter of 10 mu m in an organic solvent tetrahydrofuran for ultrasonic treatment, adding a certain amount of cage type silsesquioxane with amino side groups, and mixing and stirring at room temperature to obtain a graphene oxide/silsesquioxane dispersion liquid, wherein the weight ratio of the graphene oxide to the silsesquioxane is 95: 5. The concentration of the dispersion was 1 mg/ml.
S2: preparation of the base coat:
and (4) uniformly depositing the dispersion liquid prepared in the step S1 on a clean aluminum-based surface, and volatilizing at room temperature for 6 hours to obtain a base coat.
S3: preparation of topcoat suspensions:
carrying out ultrasonic treatment on a hydroxylated carbon nano tube in an organic solvent tetrahydrofuran, adding a certain amount of cage type silsesquioxane with amino as a side group, mixing and stirring at room temperature to obtain a carbon nano tube/silsesquioxane suspension, wherein the weight ratio of the carbon nano tube to the silsesquioxane is 95: 5. The suspension concentration was 1 mg/ml.
S4: preparing a top coat:
the suspension prepared in step S3 was uniformly deposited on the undercoated surface prepared in step S2, and then transferred to a fume hood and the solvent was evaporated at room temperature for 12 hours to obtain a topcoat.
S5: coating heat treatment:
step S4: the coating prepared in the step (1) is placed in a vacuum oven for heat treatment, and then is naturally cooled to room temperature along with the furnace. Wherein the heat treatment conditions are as follows: the incubation was carried out at 60 ℃ for 48 hours, then at 200 ℃ and for 5 minutes.
To determine the TML, CVCM and WVR values in a vacuum environment in the coating space, the test specimens were tested for heat exposureThe temperature is 125 +/-1 ℃, the collection temperature of the condensable volatile is 25 +/-1 ℃, and the vacuum degree is better than 1x10-3Pa, test time 24 hours. Three samples are taken for testing, and the test result is the average value of the three samples. The coating prepared in this example had TML of 0.10%; CVCM is 0.006%; WVR is 0.11%.
The coating prepared in this example had a conductivity of 7.2S/cm.
Example 3:
the antistatic optical absorption coating with low air-out rate is prepared by the following steps:
s1: preparation of the undercoating dispersion:
uniformly dispersing graphene oxide micro-sheets with the average diameter of 10 mu m in organic solvent tetrahydrofuran for ultrasonic treatment, adding a certain amount of cage type silsesquioxane with amino side groups, and mixing and stirring at room temperature to obtain graphene oxide/silsesquioxane dispersion liquid, wherein the weight ratio of graphene oxide to silsesquioxane is 90: 10. The concentration of the dispersion was 1 mg/ml.
S2 preparation of the base coat:
and (4) uniformly depositing the dispersion liquid prepared in the step S1 on a clean aluminum-based surface, and volatilizing at room temperature for 6 hours to obtain a base coat.
S3 preparation of topcoat suspensions:
the method comprises the following steps of carrying out ultrasonic treatment on a hydroxylated carbon nano tube in organic solvent tetrahydrofuran, adding a certain amount of cage type silsesquioxane with amino as a side group, mixing and stirring at room temperature to obtain a carbon nano tube/silsesquioxane suspension, wherein the weight ratio of the carbon nano tube to the silsesquioxane is 80: 20. The suspension concentration was 1 mg/ml.
S4 preparation of the top coating:
the suspension prepared in step S3 was uniformly deposited on the undercoated surface prepared in step S2, and then transferred to a fume hood and the solvent was evaporated at room temperature for 12 hours to obtain a topcoat.
S5, coating heat treatment:
and (4) placing the coating prepared in the step S4 in a vacuum oven for heat treatment, and naturally cooling to room temperature along with the furnace. Wherein the heat treatment conditions are as follows: the incubation was carried out at 60 ℃ for 48 hours, then at 200 ℃ and for 5 minutes.
For the determination of TML, CVCM and WVR values in vacuum environment of coating space, the test sample is heated to 125 ℃ + -1 deg.C, the collection temperature of condensable volatile is 25 ℃ + -1 deg.C, and the vacuum degree is better than 1x10-3Pa, test time 24 hours. Three samples are taken for testing, and the test result is the average value of the three samples. Coating TML prepared in this example was 0.09%; CVCM is 0.006%; WVR is 0.10%.
The coating prepared in this example had a conductivity of 0.8S/cm.
Example 4:
the antistatic optical absorption coating with low air-out rate is prepared by the following steps:
s1 preparation of priming dispersion:
uniformly dispersing graphene oxide micro-sheets with the average diameter of 10 mu m in an organic solvent tetrahydrofuran for ultrasonic treatment, adding a certain amount of cage type silsesquioxane with amino side groups, and mixing and stirring at room temperature to obtain a graphene oxide/silsesquioxane dispersion liquid, wherein the weight ratio of the graphene oxide to the silsesquioxane is 70: 30. The concentration of the dispersion was 1 mg/ml.
S2 preparation of the base coat:
and (4) uniformly depositing the dispersion liquid prepared in the step S1 on a clean aluminum-based surface, and volatilizing at room temperature for 6 hours to obtain a base coat.
S3 preparation of topcoat suspensions:
the method comprises the following steps of carrying out ultrasonic treatment on a hydroxylated carbon nano tube in organic solvent tetrahydrofuran, adding a certain amount of cage type silsesquioxane with amino as a side group, mixing and stirring at room temperature to obtain a carbon nano tube/silsesquioxane suspension, wherein the weight ratio of the carbon nano tube to the silsesquioxane is 75: 25. The suspension concentration was 1 mg/ml.
S4 preparation of the top coating:
the suspension prepared in step S3 was uniformly deposited on the undercoated surface prepared in step S2, and then transferred to a fume hood and the solvent was evaporated at room temperature for 12 hours to obtain a topcoat.
S5, coating heat treatment:
and (4) placing the coating prepared in the step S4 in a vacuum oven for heat treatment, and naturally cooling to room temperature along with the furnace. Wherein the heat treatment conditions are as follows: the incubation was carried out at 60 ℃ for 48 hours, then at 200 ℃ and for 10 minutes.
For the determination of TML, CVCM and WVR values in vacuum environment of coating space, the test sample is heated to 125 ℃ + -1 deg.C, the collection temperature of condensable volatile is 25 ℃ + -1 deg.C, and the vacuum degree is better than 1x10-3Pa, test time 24 hours. Three samples are taken for testing, and the test result is the average value of the three samples. The coating prepared in this example had a TML of 0.07%; CVCM ═ 0.004%; WVR is 0.08%.
The coating prepared in this example had a conductivity of 0.02S/cm.
Example 5:
the antistatic optical absorption coating with low air-out rate is prepared by the following steps:
s1 preparation of priming dispersion:
uniformly dispersing graphene oxide micro-sheets with the average diameter of 10 mu m in an organic solvent tetrahydrofuran for ultrasonic treatment, then adding a certain amount of cage type silsesquioxane with a carboxyl side group, mixing and stirring at room temperature to obtain a graphene oxide/silsesquioxane dispersion liquid, wherein the weight ratio of the graphene oxide to the silsesquioxane is 70: 30. The concentration of the dispersion was 1 mg/ml.
S2 preparation of the base coat:
and (4) uniformly depositing the dispersion liquid prepared in the step S1 on a clean aluminum-based surface, and volatilizing at room temperature for 6 hours to obtain a base coat.
S3 preparation of topcoat suspensions:
the method comprises the following steps of carrying out ultrasonic treatment on a hydroxylated carbon nano tube in organic solvent tetrahydrofuran, adding a certain amount of cage type silsesquioxane with amino as a side group, mixing and stirring at room temperature to obtain a carbon nano tube/silsesquioxane suspension, wherein the weight ratio of the carbon nano tube to the silsesquioxane is 75: 25. The suspension concentration was 1 mg/ml.
S4 preparation of the top coating:
the suspension prepared in step S3 was uniformly deposited on the undercoated surface prepared in step S2, and then transferred to a fume hood and the solvent was evaporated at room temperature for 12 hours to obtain a topcoat.
S5, coating heat treatment:
and (4) placing the coating prepared in the step S4 in a vacuum oven for heat treatment, and naturally cooling to room temperature along with the furnace. Wherein the heat treatment conditions are as follows: the incubation was carried out at 60 ℃ for 48 hours, then heated to 220 ℃ and incubated for 10 minutes.
For the determination of TML, CVCM and WVR values in vacuum environment of coating space, the test sample is heated to 125 ℃ + -1 deg.C, the collection temperature of condensable volatile is 25 ℃ + -1 deg.C, and the vacuum degree is better than 1x10-3Pa, test time 24 hours. Three samples are taken for testing, and the test result is the average value of the three samples. Coating TML prepared in this example was 0.11%; CVCM is 0.007%; WVR is 0.12%.
The coating prepared in this example had a conductivity of 0.01S/cm.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of an antistatic optical absorption coating with low air-out rate is characterized by comprising the following steps:
s1: preparation of the basecoat Dispersion
Uniformly dispersing graphene oxide micro-sheets in an organic solvent for ultrasonic treatment, adding silsesquioxane, and mixing and stirring at room temperature to obtain a graphene oxide/silsesquioxane dispersion liquid;
s2: preparation of the base coat
Uniformly depositing the primer dispersion liquid prepared in the step S1 on the surface of a clean substrate, and volatilizing at a proper amount at room temperature to obtain a primer;
s3: preparation of the topcoat suspension
Carrying out ultrasonic treatment on the carbon nano tube in an organic solvent, adding silsesquioxane, and mixing and stirring at room temperature to obtain a carbon nano tube/silsesquioxane suspension;
s4: preparation of the topcoat
Uniformly depositing the topcoat suspension prepared in step S3 on the undercoated surface prepared in step S2, and then transferring to a fume hood and volatilizing the solvent at room temperature to obtain a topcoat;
s5: heat treatment of coatings
And (4) placing the coating prepared in the step S4 in a vacuum oven for heat treatment, and naturally cooling to room temperature along with the furnace.
2. The method for preparing the low-outgassing antistatic optical absorption coating of claim 1, wherein in step S1, the graphene oxide is 50-99 parts and the silsesquioxane is 1-50 parts by mass.
3. The method for preparing the low outgassing rate antistatic optical absorption coating of claim 2, wherein in step S1, the organic solvent is tetrahydrofuran, n-hexane, chloroform, acetone, toluene or dichloromethane.
4. The method for preparing the low outgassing rate, antistatic optical absorption coating of claim 3, wherein the graphene oxide nanoplatelets have a diameter of 0.05-50 μm; the silsesquioxane structure is irregular, trapezoidal, cage-shaped or semi-cage-shaped; the side group R is epoxy group, hydroxyl or amino; the concentration of the priming paint dispersion liquid is 0.1-10 mg/ml.
5. The method for preparing the low outgassing rate antistatic optical absorption coating of claim 4, wherein in step S2, the substrate is metal, glass, ceramic or polymer material; the volatilization time of the solvent is 0.5 to 12 hours.
6. The method for preparing the antistatic optical absorption coating with low air permeability as claimed in claim 5, wherein in the step S3, the carbon nanotubes comprise 75 to 95 parts by mass and the silsesquioxane comprises 5 to 25 parts by mass.
7. The method for preparing the antistatic optical absorption coating with low outgassing rate as claimed in claim 6, wherein in step S3, the outer wall of the carbon nanotube contains functional groups such as hydroxyl and/or carboxyl; the organic solvent is the same as the organic solvent used in step S1; the silsesquioxane is the same as the silsesquioxane used in step S1; the concentration of the top coating suspension is 0.1-10 mg/ml.
8. The method for preparing the antistatic optical absorption coating with low outgassing rate of claim 7, wherein in step S4, the solvent volatilization time is 6 to 24 hours.
9. The method for preparing the antistatic optical absorption coating with low outgassing rate of claim 8, wherein in step S5, the heat treatment conditions are: keeping the temperature at 50-80 ℃ for 6-48 hours, then heating to 180-220 ℃ and keeping the temperature for 5-60 minutes.
10. A low outgassing rate antistatic optical absorption coating prepared by the method for preparing the low outgassing rate antistatic optical absorption coating according to any one of claims 1 to 9.
CN202110997957.8A 2021-08-27 2021-08-27 Low-air-out-rate antistatic optical absorption coating and preparation method thereof Active CN113583495B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110997957.8A CN113583495B (en) 2021-08-27 2021-08-27 Low-air-out-rate antistatic optical absorption coating and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110997957.8A CN113583495B (en) 2021-08-27 2021-08-27 Low-air-out-rate antistatic optical absorption coating and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113583495A true CN113583495A (en) 2021-11-02
CN113583495B CN113583495B (en) 2022-08-09

Family

ID=78239964

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110997957.8A Active CN113583495B (en) 2021-08-27 2021-08-27 Low-air-out-rate antistatic optical absorption coating and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113583495B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102912626A (en) * 2012-11-06 2013-02-06 沈阳航空航天大学 Preparation method of fiber surface sizing agent based on carbon nanotube/graphene oxide/POSS (Polysilsesquioxane) monomer
CN104591164A (en) * 2014-12-30 2015-05-06 常州碳星科技有限公司 Method for preparing graphene microspheres
CN106047077A (en) * 2016-07-20 2016-10-26 太原理工大学 Carbon nanomaterial composite conductive mica/epoxy-group static conducting anticorrosive coating material and preparation method
CN108276576A (en) * 2018-02-02 2018-07-13 天津工业大学 Carbon nanotube and graphene are covalently attached collaboration enhancing composite polyimide material and preparation method thereof
CN108676346A (en) * 2018-04-13 2018-10-19 太仓运通新材料科技有限公司 graphene modified aqueous polyurethane and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102912626A (en) * 2012-11-06 2013-02-06 沈阳航空航天大学 Preparation method of fiber surface sizing agent based on carbon nanotube/graphene oxide/POSS (Polysilsesquioxane) monomer
CN104591164A (en) * 2014-12-30 2015-05-06 常州碳星科技有限公司 Method for preparing graphene microspheres
CN106047077A (en) * 2016-07-20 2016-10-26 太原理工大学 Carbon nanomaterial composite conductive mica/epoxy-group static conducting anticorrosive coating material and preparation method
CN108276576A (en) * 2018-02-02 2018-07-13 天津工业大学 Carbon nanotube and graphene are covalently attached collaboration enhancing composite polyimide material and preparation method thereof
CN108676346A (en) * 2018-04-13 2018-10-19 太仓运通新材料科技有限公司 graphene modified aqueous polyurethane and preparation method thereof

Also Published As

Publication number Publication date
CN113583495B (en) 2022-08-09

Similar Documents

Publication Publication Date Title
Kavale et al. Optically transparent, superhydrophobic methyltrimethoxysilane based silica coatings without silylating reagent
Zhang et al. Waterborne nonfluorinated superhydrophobic coatings with exceptional mechanical durability based on natural nanorods
CN103339154B (en) Method for producing flake graphite-polymer composite material
Rao et al. Water repellent porous silica films by sol–gel dip coating method
Dhere et al. Transparent water repellent silica films by sol–gel process
RU2539694C2 (en) Application of coating on metal and electronic device to be applied in sea conditions and other media
CN113583495B (en) Low-air-out-rate antistatic optical absorption coating and preparation method thereof
CN111908480A (en) Super-amphiphobic material, preparation method thereof and preparation method of super-amphiphobic surface coating
Li et al. Vapor lubrication for reducing water and ice adhesion on poly (dimethylsiloxane) brushes
Delozier et al. Preparation and characterization of space durable polymer nanocomposite films
Kim et al. Synthesis of superhydrophobic SiO2 layers via combination of surface roughness and fluorination
Shu et al. Surface modification of poly (4, 4′-oxydiphenylene pyromellitimide)(Kapton) by alkali solution and its applications to atomic oxygen protective coating
CN114855142B (en) Low surface energy parylene material and its preparation method
Baker et al. The use of perfluoroalkyl polyether fluids in vacuum pumps
Castaneda-Montes et al. Atomised spray plasma deposition of hierarchical superhydrophobic nanocomposite surfaces
Chen et al. Grafting of poly (ethylene-block-ethylene oxide) onto a vapor grown carbon fiber surface by γ-ray radiation grafting
Qin et al. Fast pyrolysis of silicones at low temperatures catalyzed by anatase titanium dioxide
CN110387191A (en) A kind of hydrophobic coating and preparation method thereof, hydrophobic coating solution
Shi et al. Preparation of poly (ɛ-caprolactone) grafted titanate nanotubes
Kumar et al. Biocatalytic synthesis of highly flame retardant inorganic–organic hybrid polymers
Kavale et al. Enrichment in hydrophobicity and scratch resistant properties of silica films on glass by grafted microporosity of the network
Oya et al. Characterization of organic polymer thin films deposited by rf magnetron sputtering
Ashmead et al. Adsorption of polydimethylsiloxanes from solution on glass
Jeong et al. Preparation of super-hydrophilic amorphous titanium dioxide thin film via PECVD process and its application to dehumidifying heat exchangers
Eltekova et al. Adsorption of aromatic compounds from solutions on titanium dioxide and silica

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB03 Change of inventor or designer information

Inventor after: Yu Bing

Inventor after: Wang Xiao

Inventor after: Yuan Linguang

Inventor after: Li Chaolong

Inventor after: Fan Jihong

Inventor after: Shi Haofei

Inventor after: Li Yan

Inventor after: Park Mingxing

Inventor after: Qin Yan

Inventor before: Yu Bing

Inventor before: Wang Xiao

Inventor before: Yuan Linguang

Inventor before: Guo Chaolong

Inventor before: Fan Jihong

Inventor before: Shi Haofei

Inventor before: Li Yan

Inventor before: Park Mingxing

Inventor before: Qin Yan

CB03 Change of inventor or designer information
GR01 Patent grant
GR01 Patent grant