CN106111480A - A kind of preparation method of LBL self assembly thin-film material - Google Patents
A kind of preparation method of LBL self assembly thin-film material Download PDFInfo
- Publication number
- CN106111480A CN106111480A CN201610518397.2A CN201610518397A CN106111480A CN 106111480 A CN106111480 A CN 106111480A CN 201610518397 A CN201610518397 A CN 201610518397A CN 106111480 A CN106111480 A CN 106111480A
- Authority
- CN
- China
- Prior art keywords
- substrate
- reagent
- self assembly
- film material
- lbl self
- 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.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
Landscapes
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Measurement Of The Respiration, Hearing Ability, Form, And Blood Characteristics Of Living Organisms (AREA)
Abstract
The present invention relates to the preparation method of a kind of LBL self assembly thin-film material, soak including substrate being immersed in reagent A, take out substrate and use ethanol and deionized water rinsing successively after immersion, after flushing, nitrogen dries up；Substrate after drying up immerses in reagent B and soaks, and takes out substrate deionized water rinsing, then substrate immersed in reagent C and soak after immersion, takes out substrate deionized water rinsing after immersion, and this operation repeats 5～10 times；Obtain the thin-film material of stable LBL self assembly.Technique scheme, the method using negative ions compound LBL self assembly prepares a kind of novel LBL self assembly thin-film material, by changing the response group of compound, make ion present in material selectivity ground complex solution, thus there is the change of transmembrane potential, the LBL self assembly thin-film material of preparation is for ion transducer, and its detection signal is better than sensor prepared by monolayer polymer film, and response is fast, favorable reproducibility.
Description
Technical field
The present invention relates to the preparation field of thin-film material, be specifically related to the preparation side of a kind of LBL self assembly thin-film material
Method.
Background technology
Ion transducer has that miniaturization highly sensitive, easy, power consumption be little, the feature of low cost, in various fields by extensively
Application.Current thin film materials application is mainly monolayer polymer film in ion transducer, the sensor detection signal of preparation
Weak, unstable.Secondly a polymer thin-film sensor for large volume prepared by the method such as use droplet casting or rotary coating cannot be real
The most preferably respond repeatability.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of LBL self assembly thin-film material, it can effectively overcome above-mentioned
Defect, uses it for ion transducer and has good response repeatability, and the signal of sensor detection is strong.
For achieving the above object, present invention employs techniques below scheme:
A kind of preparation method of LBL self assembly thin-film material, including operating as follows:
S1: substrate immersed in reagent A and soak, takes out substrate and uses ethanol and deionized water rinsing successively after immersion,
After flushing, nitrogen dries up；
S2: the substrate after drying up immerses in reagent B and soaks, takes out substrate deionized water rinsing, then after immersion
Substrate is immersed in reagent C and soak, after immersion, take out substrate deionized water rinsing；
S3: operation S2 repeats 5～10 times, obtains the stable thin-film material replaced layer by layer；
Reagent A is to be dissolved with the alcohol-water mixture of 3-aminopropyl triethoxysilane, alcohol-water mixture by ethanol, water according to
The volume ratio mixed preparing of 95:5 obtains, and 3-aminopropyl triethoxysilane concentration in alcohol-water mixture is 0.8-
1.0mmol/L；Reagent B is 0.8-1.0mg/mL kayexalate aqueous solution, reagent C be 0.8-1.0mg/mL azepine-
Azepine-15-crown ether-5 hydrochloric acid solution of hexaoxacyclooctadecane-6-6 hydrochloric acid solution or 0.8-1.0mg/mL.
Concrete scheme is: substrate is the substrate of 10 × 10mm gold surface, and substrate soak time in reagent A is 8-
12h；Substrate soak time in reagent B is 15-20min；Substrate soak time in reagent C is 15-20min.
Technique scheme, uses the method for negative ions compound LBL self assembly to prepare a kind of novel successively from group
Dress thin-film material, by changing the response group of compound, makes ion present in material selectivity ground complex solution, thus sends out
The change of filming current potential.The LBL self assembly thin-film material of preparation is for ion transducer, and its detection signal is better than monolayer polymerization
The sensor of thing film preparation, and response is fast, favorable reproducibility.
Detailed description of the invention
In order to make objects and advantages of the present invention clearer, below in conjunction with embodiment, the present invention is carried out specifically
Bright.Should be appreciated that following word only in order to describe one or more specific embodiments of the present invention, not to the present invention
The protection domain of concrete request carries out considered critical.
Embodiment 1
The substrate of 10 × 10mm gold surface is positioned over soaked overnight in reagent A, then takes out substrate, successively with ethanol and
Several times, nitrogen dries up deionized water rinsing；Reagent A is to be dissolved with the alcohol-water mixture of 3-aminopropyl triethoxysilane, alcohol water
Mixed liquor is obtained according to the volume ratio mixed preparing of 95:5 by ethanol, water, and 3-aminopropyl triethoxysilane is at alcohol-water mixture
In concentration be 1.0mmol/L.
Substrate is immersed in 1mg/mL kayexalate (PSS) aqueous solution, wait 20min, spend after taking-up
Ionized water rinses, and is then immersed in 1mg/mL azepine-hexaoxacyclooctadecane-6-6 hydrochloric acid solution, continues 20min, takes out deionized water rinsing,
Repeat aforesaid operations 5～10 times, until forming stable thin-film material.
Being connected in the working electrode of electrochemical workstation by the above-mentioned thin-film material produced, reference electrode is Ag/AgCl
Electrode, is platinum wire to electrode.The sensor assembled is put into the tetrabutyl ammonium hexafluorophosphate-tetrahydrofuran solution of 0.1M
(Bu4NPF6-THF) in, it is subsequently adding 5.0mM Potassium Hexafluorophosphate (KPF6), uses cyclic voltammetry testing film respectively to potassium
The response of ion (K+).
Test result is: the thin film of nitrogen-containing hetero-hexaoxacyclooctadecane-6-6 compound is exposed to the tetrabutyl hexafluoro phosphorus that potassium ion exists
In acid ammonium-tetrahydrofuran solution, bigger spike potential displacement, negative electrode spike potential (Epc1) is had to move right 101 ± 13mV, negative electrode
Spike potential (Epc2) has moved right 128 ± 11mV；Anode spike potential (Epa1) has moved right 24 ± 6mV, anode spike potential
(Epa2) moved right 93 ± 15mV.
Embodiment 2
The substrate of 10 × 10mm gold surface is positioned over soaked overnight in reagent A, then takes out substrate, successively with ethanol and
Several times, nitrogen dries up deionized water rinsing；Reagent A is to be dissolved with the alcohol-water mixture of 3-aminopropyl triethoxysilane, alcohol water
Mixed liquor is obtained according to the volume ratio mixed preparing of 95:5 by ethanol, water, and 3-aminopropyl triethoxysilane is at alcohol-water mixture
In concentration be 0.8mmol/L.
Substrate is immersed in 1mg/mL kayexalate (PSS) aqueous solution, wait 20min, spend after taking-up
Ionized water rinses, and is then immersed in azepine-15-crown ether-5 hydrochloric acid solution of 1mg/mL, continues 20min, takes out deionized water punching
Wash, repetition aforesaid operations 5～10 times, until forming stable self-assembled film material.
Being connected in the working electrode of electrochemical workstation by the above-mentioned thin-film material produced, reference electrode is Ag/AgCl
Electrode, is platinum wire to electrode.The sensor assembled is put into the tetrabutyl ammonium hexafluorophosphate-tetrahydrofuran solution of 0.1M
(Bu4NPF6-THF), in, it is subsequently adding 5.0mM sodium hexafluoro phosphate (NaPF6), use cyclic voltammetry to test multilamellar absorption respectively
The thin film response to sodium ion (Na+).
Test result is: the thin film of nitrogen-containing hetero-15-crown ether-5 compound is exposed to the tetrabutyl hexafluoro phosphorus that sodium ion exists
In acid ammonium-tetrahydrofuran solution, bigger spike potential displacement, negative electrode spike potential (Epc1) is had to move right 79 ± 9mV, negative electrode peak
Current potential (Epc2) has moved right 95 ± 11mV；Anode spike potential (Epa1) has moved right 33 ± 7mV, anode spike potential
(Epa2) moved right 54 ± 7mV.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, after knowing content described in the present invention, under the premise without departing from the principles of the invention, it is also possible to it is made some
Equal conversion and replacement, these convert on an equal basis and substitute and also should be regarded as belonging to protection scope of the present invention.
Claims (5)
1. a preparation method for LBL self assembly thin-film material, including operating as follows:
S1: substrate immersed in reagent A and soak, takes out substrate and successively with ethanol and deionized water rinsing, rinses after immersion
Rear nitrogen dries up；
S2: the substrate after drying up immerses in reagent B and soaks, takes out substrate deionized water rinsing, then by base after immersion
Matter immerses in reagent C and soaks, and takes out substrate deionized water rinsing after immersion；
S3: operation S2 repeats 5～10 times, obtains the thin-film material of stable LBL self assembly；
Reagent A is to be dissolved with the alcohol-water mixture of 3-aminopropyl triethoxysilane, alcohol-water mixture by ethanol, water according to 95:5
Volume ratio mixed preparing obtain, 3-aminopropyl triethoxysilane concentration in alcohol-water mixture is 0.8-1.0mmol/L；
Reagent B is the kayexalate aqueous solution of 0.8-1.0mg/mL, and reagent C is the azepine-hexaoxacyclooctadecane-6-6 of 0.8-1.0mg/mL
Azepine-15-crown ether-5 hydrochloric acid solution of hydrochloric acid solution or 0.8-1.0mg/mL.
The preparation method of LBL self assembly thin-film material the most according to claim 1, it is characterised in that: substrate is in reagent A
Soak time be 8-12h.
The preparation method of LBL self assembly thin-film material the most according to claim 1, it is characterised in that: substrate is in reagent B
Soak time be 15-20min.
The preparation method of LBL self assembly thin-film material the most according to claim 1, it is characterised in that: substrate is in reagent C
Soak time be 15-20min.
The preparation method of LBL self assembly thin-film material the most according to claim 1, it is characterised in that: substrate is 10 × 10mm
The substrate of gold surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610518397.2A CN106111480A (en) | 2016-07-04 | 2016-07-04 | A kind of preparation method of LBL self assembly thin-film material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610518397.2A CN106111480A (en) | 2016-07-04 | 2016-07-04 | A kind of preparation method of LBL self assembly thin-film material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106111480A true CN106111480A (en) | 2016-11-16 |
Family
ID=57469206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610518397.2A Pending CN106111480A (en) | 2016-07-04 | 2016-07-04 | A kind of preparation method of LBL self assembly thin-film material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106111480A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060124573A (en) * | 2005-05-31 | 2006-12-05 | 경북대학교 산학협력단 | Crown ether derivatives and process for immobilization of biomolecules and process for recognizing molecules by using the same |
| CN101294927A (en) * | 2007-04-27 | 2008-10-29 | 株式会社日立高新技术 | Ion concentration measuring device and ion concentration measuring element |
| CN101462388A (en) * | 2009-01-13 | 2009-06-24 | 四川大学 | Compound film enhanced by inclusion complex of ring molecule and polymer and preparation method thereof |
| CN103030305A (en) * | 2012-12-17 | 2013-04-10 | 哈尔滨工业大学 | Phospholipid bilayer membrane array fabricated by multilayer polyelectrolyte membrane substrate and fabrication method |
| CN105080814A (en) * | 2014-04-22 | 2015-11-25 | 马德里高等材料研究院 | Polyelectrolyte nanometer flame-retardant coating by adoption of layer-by-layer assembly and preparation method thereof |
-
2016
- 2016-07-04 CN CN201610518397.2A patent/CN106111480A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060124573A (en) * | 2005-05-31 | 2006-12-05 | 경북대학교 산학협력단 | Crown ether derivatives and process for immobilization of biomolecules and process for recognizing molecules by using the same |
| CN101294927A (en) * | 2007-04-27 | 2008-10-29 | 株式会社日立高新技术 | Ion concentration measuring device and ion concentration measuring element |
| CN101462388A (en) * | 2009-01-13 | 2009-06-24 | 四川大学 | Compound film enhanced by inclusion complex of ring molecule and polymer and preparation method thereof |
| CN103030305A (en) * | 2012-12-17 | 2013-04-10 | 哈尔滨工业大学 | Phospholipid bilayer membrane array fabricated by multilayer polyelectrolyte membrane substrate and fabrication method |
| CN105080814A (en) * | 2014-04-22 | 2015-11-25 | 马德里高等材料研究院 | Polyelectrolyte nanometer flame-retardant coating by adoption of layer-by-layer assembly and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘育等: ""冠醚的分子设计及其识别性质研究进展"", 《有机化学》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10871463B2 (en) | Preparation method based on simultaneous package of target substance and synthesis of MOFs with redox activity | |
| CN109187688B (en) | A kind of light-operated polymer sensitive membrane electrochemical detection method and its device | |
| CN105717174B (en) | The electrochemical detection method of modified graphene oxide composite modified electrode trace heavy metal ion in water body is detected | |
| Moretto et al. | Electrochemiluminescence of Ru (bpy) 32+ loaded in Nafion Langmuir–Blodgett films: Role of the interfacial ultrathin film | |
| Abramova et al. | Solid contact ion sensor with conducting polymer layer copolymerized with the ion-selective membrane for determination of calcium in blood serum | |
| CN103243367B (en) | The preparation method of streptavidin molecular imprinting biosensor | |
| CN103926294A (en) | Preparation and application of CS/IL-GR modified bovine serum albumin molecular imprinting electrode | |
| Luo et al. | Voltammetric determination of ferulic acid by didodecyldimethyl-ammonium bromide/Nafion composite film-modified carbon paste electrode | |
| CN107367534A (en) | A kind of method of dimethyl diaminophenazine chloride metal/composite material modified electrode detection cysteine | |
| Gao et al. | Permeability controllable overoxidised polypyrrole film modified glassy carbon electrodes | |
| Zhang et al. | Determination of dopamine in the presence of ascorbic acid using a poly (amidosulfonic acid) modified glassy carbon electrode | |
| CN103063718B (en) | Solid nitrate ion electrode based on conductive polyaniline and preparing method thereof | |
| CN105606678A (en) | Doped polyaniline based solid acid radical electrode and preparation method thereof | |
| CN106111480A (en) | A kind of preparation method of LBL self assembly thin-film material | |
| Zhang et al. | Electrochemical behaviors of roxithromycin at poly (3, 4-ethylenedioxythiophene) modified gold electrode and its electrochemical determination | |
| CN102393412B (en) | Modified electrode and preparation method thereof | |
| Yadav et al. | Electro-kinetic investigations and voltammetric detection of anti-ulcer drug cinitapride at low-cost pencil graphite electrode | |
| IWASAKI et al. | Coulometric determination of perfluoroalkyl substances (PFAS) with the thin-layer electrolysis flow cell for the ion transfer | |
| CN103063725B (en) | Solid ammonium ion electrode based on conductive polyaniline and preparing method thereof | |
| CN103063723B (en) | Solid hydrogen ion concentration electrode based on conductive polyaniline and preparing method thereof | |
| Xu et al. | The electrochemical oxidation of pentachlorophenol and its sensitive determination at chitosan modified carbon paste electrode | |
| CN105136892B (en) | A kind of electrochemical sensor cellulose heteropoly acid PEM and its preparation method | |
| CN108107091A (en) | A kind of preparation method and application of chirality MOF membrane materials | |
| CN103063722B (en) | Solid calcium ion electrode based on conductive polyaniline and preparing method thereof | |
| CN103063721B (en) | Solid nitrite ion electrode based on conductive polyaniline and preparing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161116 |
|
| WD01 | Invention patent application deemed withdrawn after publication |