CN106146873B - A method of titanium dioxide nano-film is prepared on expanded PTFE surface - Google Patents
A method of titanium dioxide nano-film is prepared on expanded PTFE surface Download PDFInfo
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- CN106146873B CN106146873B CN201610491060.7A CN201610491060A CN106146873B CN 106146873 B CN106146873 B CN 106146873B CN 201610491060 A CN201610491060 A CN 201610491060A CN 106146873 B CN106146873 B CN 106146873B
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- expanded ptfe
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- 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
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- 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 discloses a kind of methods for preparing titanium dioxide nano-film on expanded PTFE surface, step includes: to handle the expanded PTFE substrate after cleaning in plasma reactor, then the spin coating solution of tetrabutyl titanate on expanded PTFE substrate；Hydro-thermal method processing is carried out again.Preparation method simple process of the invention, it is easy to operate, it is easy to accomplish.TiO in film obtained2Nano particle even compact, and it is very secured with the binding force of expanded PTFE substrate, there is stronger optical Response, have huge potential application in the fields such as photocatalysis and organizational project.
Description
Technical field
The present invention relates to a kind of methods for preparing titanium dioxide nano-film on organic polymer surface, and in particular to a kind of
On expanded PTFE surface, preparation has the method for the titanium dioxide nano-film of optical Response.
Background technique
TiO2It is a kind of nontoxic inorganic material, there is fabulous chemical stability, stronger photocatalytic activity and good
Good biocompatibility.After passing through ultraviolet lighting for a period of time, TiO2Surface can become super hydrophilic state.Have and grinds
Study carefully discovery, TiO2Material has relatively broad application [Yoshiaki in fields such as photocatalytic self-cleaning, bioengineered tissues
Taguchi. et al. Photo-induced properties of non-annealed anatase TiO2
mesoporous film prepared by anodizing in the hot phosphate/glycerol
electrolyte. Chem. Applied Surface Science 258 (2012) 9810-9815]、[K. Cheng,
H. P. Wan. et al. A facile approach to improve light induced cell sheet
harvesting through nanostructure optimization. RSC Adv., 2015, 5, 88965-
88972]。
Expanded PTFE be it is a kind of it is nontoxic, without new medical macromolecule material carcinogenic and with multiple microcellular structure
Material, not only resistance to biological aging had good biocompatibility again, and it is medical to be widely used in manufacture cardiac patch, artificial blood vessel etc.
Arts.
TiO2Inorganic material and expanded PTFE have the advantages that many practical, and the two, which combines, can more promote it at oneself
The application of cleaning and organizational project and other field.But on expanded PTFE surface, preparation has firm connection power at present
TiO2There are larger difficulty in terms of nanometer particle film.Due to expanded PTFE be a kind of high degree of symmetry nonpolarity it is linear
Structure, internal carbon are surrounded by fluorine atom, therefore show stronger hydrophobic performance.It would generally be first to the high molecular material table
Face carries out chemical modification, then prepares TiO again2Nanometer particle film, but such method operating process is more complicated, cost compared with
Height, and TiO2Nano particle is insecure in conjunction with expanded PTFE substrate, significantly limits its application.
Summary of the invention
The purpose of the present invention is to provide one kind expanded PTFE surface preparation have good biocompatibility and
The titanium dioxide nano-film method of optical Response.
The method for preparing titanium dioxide nano-film on expanded PTFE surface of the invention, includes the following steps:
1) expanded PTFE substrate is cleaned, substrate surface adsorbate is removed, is spontaneously dried；
2) oxygen is passed through in plasma reactor, will cleaning, it is dry after expanded PTFE substrate be placed in away from
From the plasma discharge region position 10 ~ 30cm, 10 ~ 60s is handled；
3) by butyl titanate and dehydrated alcohol, 1:1 ~ 1:6 is mixed and stirred for uniformly, obtaining solution A by volume；
4) 20 ul ~ 30ul A solution is added dropwise on step 2 treated expanded PTFE substrate, with
30 ~ 40s of revolving speed spin coating of 7000r/min, 60 DEG C of dryings obtain butyl titanate film；
5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermals
2 ~ 4h is handled, obtains titanium dioxide nano-film in expanded PTFE substrate surface.
Cleaning expanded PTFE substrate described in step 1) of the present invention is to be immersed in expanded PTFE substrate
In dehydrated alcohol, after ultrasonic cleaning, drying, then it is immersed in 8 ~ 12h in the NaOH solution of 1 ~ 5mol/L, spontaneously dried.
Preparation process of the present invention is simple, easy to operate, it is easy to accomplish.In preparation process, expanded PTFE substrate warp
Over cleaning can remove expanded PTFE especially by ultrasonic cleaning and the immersion treatment of NaOH aqueous slkali well
The adsorbate of substrate surface, avoids impurity from introducing.The processing of using plasma method, greatly improves expanded PTFE
The wetability of substrate, and then enhance the titania nanoparticles of later period hydro-thermal formation and the binding force of the substrate.The present invention
Used in solvent be dehydrated alcohol and deionized water, it is low in cost, it is non-toxic.In addition, making titanium dioxide using hydro-thermal method
Nano particle balanced heating during being nucleated and growing up is formed by film even compact.The film has good biological
Compatibility and optical Response have potential application in the fields such as photocatalytic self-cleaning and organizational project.
Detailed description of the invention
Fig. 1 is the titanium dioxide nano-film shape appearance figure in the preparation of expanded PTFE surface.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
Embodiment 1
(1) expanded PTFE substrate is immersed in dehydrated alcohol, is cleaned by ultrasonic 20min, then takes out substrate and exist
60 DEG C of dryings, then it is immersed in 10h in the NaOH solution of 3mol/L, it spontaneously dries；
(2) oxygen is passed through in plasma reactor, will cleaning, it is dry after expanded PTFE substrate be placed in away from
From the plasma discharge region position 10cm, 10s is handled；
(3) by butyl titanate and dehydrated alcohol, 1:1 is mixed and stirred for uniformly, obtaining solution A by volume；
(4) solution A of 20ul is added dropwise, on step 2 treated expanded PTFE substrate with 7000r/min's
Revolving speed spin coating 30s, 60 DEG C of dryings obtain butyl titanate film；
(5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermals
2h is handled, obtains titanium dioxide nano-film in expanded PTFE substrate surface.
Film surface appearance made from this example is shown in Fig. 1, it can be seen that the TiO in film2Nano particle even compact is passing through
It crosses after UV365 irradiation 15min, film contacts angle amplitude of variation is 50。.This film is firm in conjunction with expanded PTFE substrate
Gu titania nanoparticles are not fallen off after ultrasonic vibration 5min.
Embodiment 2
(1) expanded PTFE substrate is immersed in dehydrated alcohol, is cleaned by ultrasonic 20min, then takes out substrate and exist
60 DEG C of dryings, then it is immersed in 8h in the NaOH solution of 1mol/L, it spontaneously dries；
(2) oxygen is passed through in plasma reactor, will cleaning, it is dry after expanded PTFE substrate be placed in away from
From the plasma discharge region position 15cm, 20s is handled；
(3) by butyl titanate and dehydrated alcohol, 1:2 is mixed and stirred for uniformly, obtaining solution A by volume；
(4) solution A of 22ul is added dropwise, on step 2 treated expanded PTFE substrate with 7000r/min's
Revolving speed spin coating 32s, 60 DEG C of dryings obtain butyl titanate film；
(5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermals
2h is handled, obtains titanium dioxide nano-film in expanded PTFE substrate surface.
The TiO in film is made in this example2Nano particle even compact, after UV365 irradiation 15min, film is connect
Feeler amplitude of variation is 45。.This film is firmly combined with expanded PTFE substrate, after ultrasonic vibration 5min, titanium dioxide
Nano particle is not fallen off.
Embodiment 3
(1) expanded PTFE substrate is immersed in dehydrated alcohol, is cleaned by ultrasonic 20min, then takes out substrate and exist
60 DEG C of dryings, then it is immersed in 10h in the NaOH solution of 3mol/L, it spontaneously dries；
(2) oxygen is passed through in plasma reactor, will cleaning, it is dry after expanded PTFE substrate be placed in away from
From the plasma discharge region position 20cm, 30s is handled；
(3) by butyl titanate and dehydrated alcohol, 1:3 is mixed and stirred for uniformly, obtaining solution A by volume；
(4) solution A of 24ul is added dropwise, on step 2 treated expanded PTFE substrate with 7000r/min's
Revolving speed spin coating 34s, 60 DEG C of dryings obtain butyl titanate film；
(5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermals
3h is handled, obtains titanium dioxide nano-film in expanded PTFE substrate surface.
The TiO in film is made in this example2Nano particle even compact, after UV365 irradiation 15min, film is connect
Feeler amplitude of variation is 35。.This film is firmly combined with expanded PTFE substrate, after ultrasonic vibration 5min, titanium dioxide
Nano particle is not fallen off.
Embodiment 4
(1) expanded PTFE substrate is immersed in dehydrated alcohol, is cleaned by ultrasonic 20min, then takes out substrate and exist
60 DEG C of dryings, then it is immersed in 10h in the NaOH solution of 3mol/L, it spontaneously dries；
(2) oxygen is passed through in plasma reactor, will cleaning, it is dry after expanded PTFE substrate be placed in away from
From the plasma discharge region position 20cm, 40s is handled；
(3) by butyl titanate and dehydrated alcohol, 1:4 is mixed and stirred for uniformly, obtaining solution A by volume；
(4) solution A of 26ul is added dropwise, on step 2 treated expanded PTFE substrate with 7000r/min's
Revolving speed spin coating 36s, 60 DEG C of dryings obtain butyl titanate film；
(5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermals
3h is handled, obtains titanium dioxide nano-film in expanded PTFE substrate surface.
The TiO in film is made in this example2Nano particle even compact, after UV365 irradiation 15min, film is connect
Feeler amplitude of variation is 30。.This film is firmly combined with ePTFE substrate, and after ultrasonic vibration 5min, titania nanoparticles are not
It falls off.
Embodiment 5
(1) expanded PTFE substrate is immersed in dehydrated alcohol, is cleaned by ultrasonic 20min, then takes out substrate and exist
60 DEG C of dryings, then it is immersed in 12h in the NaOH solution of 5mol/L, it spontaneously dries；
(2) oxygen is passed through in plasma reactor, will cleaning, it is dry after expanded PTFE substrate be placed in away from
From the plasma discharge region position 25cm, 50s is handled；
(3) by butyl titanate and dehydrated alcohol, 1:5 is mixed and stirred for uniformly, obtaining solution A by volume；
(4) solution A of 28ul is added dropwise, on step 2 treated expanded PTFE substrate with 7000r/min's
Revolving speed spin coating 38s, 60 DEG C of dryings obtain butyl titanate film；
(5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermals
4h is handled, obtains titanium dioxide nano-film in expanded PTFE substrate surface.
The TiO in film is made in this example2Nano particle even compact, after UV365 irradiation 15min, film is connect
Feeler amplitude of variation is 20。.This film is firmly combined with expanded PTFE substrate, after ultrasonic vibration 5min, titanium dioxide
Nano particle is not fallen off.
Embodiment 6
(1) expanded PTFE substrate is immersed in dehydrated alcohol, is cleaned by ultrasonic 20min, then takes out substrate and exist
60 DEG C of dryings, then it is immersed in 12h in the NaOH solution of 5mol/L, it spontaneously dries；
(2) oxygen is passed through in plasma reactor, will cleaning, it is dry after expanded PTFE substrate be placed in away from
From the plasma discharge region position 30cm, 60s is handled；
(3) by butyl titanate and dehydrated alcohol, 1:6 is mixed and stirred for uniformly, obtaining solution A by volume；
(4) solution A of 30ul is added dropwise, on step 2 treated expanded PTFE substrate with 7000r/min's
Revolving speed spin coating 40s, 60 DEG C of dryings obtain butyl titanate film；
(5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermals
4h is handled, obtains titanium dioxide nano-film in expanded PTFE substrate surface.
The TiO in film is made in this example2Nano particle even compact, after UV365 irradiation 15min, film is connect
Feeler amplitude of variation is 10。.This film is firmly combined with expanded PTFE substrate, after ultrasonic vibration 5min, titanium dioxide
Nano particle is not fallen off.
Claims (2)
1. a kind of method for preparing titanium dioxide nano-film on expanded PTFE surface, it is characterised in that including walking as follows
It is rapid:
1) expanded PTFE substrate is cleaned, substrate surface adsorbate is removed, is spontaneously dried；
2) it is passed through oxygen in plasma reactor, the expanded PTFE substrate after cleaning, drying is placed in distance etc.
The plasma discharge area position 10 ~ 30cm handles 10 ~ 60s；
3) by butyl titanate and dehydrated alcohol, 1:1 ~ 1:6 is mixed and stirred for uniformly, obtaining solution A by volume；
4) 20 ul ~ 30ul solution A is added dropwise on step 2 treated expanded PTFE substrate, with 7000r/min
30 ~ 40s of revolving speed spin coating, 60 DEG C of dryings obtain butyl titanate film；
5) by butyl titanate membranes submerged made from step 4) in the hydro-thermal tank for filling deionized water, 140 DEG C of hydro-thermal process 2
~ 4h obtains titanium dioxide nano-film in expanded PTFE substrate surface.
2. the method according to claim 1 for preparing titanium dioxide nano-film on expanded PTFE surface, special
Sign is cleaning expanded PTFE substrate described in step 1), is that expanded PTFE substrate is immersed in dehydrated alcohol
In, after ultrasonic cleaning, drying, then it is immersed in 8 ~ 12h in the NaOH solution of 1 ~ 5mol/L, spontaneously dried.
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| CN113527760A (en) * | 2020-04-20 | 2021-10-22 | 江苏泛亚微透科技股份有限公司 | Method for manufacturing expanded polytetrafluoroethylene (ePTFE) -silicon dioxide aerogel composite heat-insulating film material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718411A (en) * | 2012-06-12 | 2012-10-10 | 华南理工大学 | Natural super-hydrophilic porous TiO2/SiO2 composite thin film and preparation method thereof |
| CN103421200A (en) * | 2013-09-06 | 2013-12-04 | 成都同明新材料技术有限公司 | Method for improving teflon adhesive property and method for producing pressure-sensitive adhesive tape |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718411A (en) * | 2012-06-12 | 2012-10-10 | 华南理工大学 | Natural super-hydrophilic porous TiO2/SiO2 composite thin film and preparation method thereof |
| CN103421200A (en) * | 2013-09-06 | 2013-12-04 | 成都同明新材料技术有限公司 | Method for improving teflon adhesive property and method for producing pressure-sensitive adhesive tape |
Non-Patent Citations (1)
| Title |
|---|
| "Low Temperature Preparation of High Refractive Index and Mechanically Resistant Sol-gel TiO2 Films for Multilayer Antireflective Coating Applications";M. LANGLET et al.;《Journal of Sol-Gel Science and Technology》;20011231;第22卷;第139-150页 |
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