CN106353292A - Preparation method of dissolved oxygen sensing film - Google Patents
Preparation method of dissolved oxygen sensing film Download PDFInfo
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- CN106353292A CN106353292A CN201610876467.1A CN201610876467A CN106353292A CN 106353292 A CN106353292 A CN 106353292A CN 201610876467 A CN201610876467 A CN 201610876467A CN 106353292 A CN106353292 A CN 106353292A
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- preparation
- sensing film
- oxygen sensing
- solution
- dissolving
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 46
- 239000001301 oxygen Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000000593 microemulsion method Methods 0.000 claims abstract description 5
- 238000003980 solgel method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 46
- 239000000758 substrate Substances 0.000 claims description 40
- 238000001035 drying Methods 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 18
- 239000002077 nanosphere Substances 0.000 claims description 18
- 229910052707 ruthenium Inorganic materials 0.000 claims description 18
- 239000008346 aqueous phase Substances 0.000 claims description 17
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 16
- 239000004530 micro-emulsion Substances 0.000 claims description 16
- 239000012071 phase Substances 0.000 claims description 16
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 10
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 229940047670 sodium acrylate Drugs 0.000 claims description 10
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 150000004696 coordination complex Chemical class 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000000839 emulsion Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000703 high-speed centrifugation Methods 0.000 claims description 8
- HZBAVWLZSLOCFR-UHFFFAOYSA-N oxosilane Chemical compound [SiH2]=O HZBAVWLZSLOCFR-UHFFFAOYSA-N 0.000 claims description 8
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 claims description 8
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 7
- XETRDYSPPPDVAB-UHFFFAOYSA-N butan-1-ol;propan-1-ol Chemical compound CCCO.CCCCO XETRDYSPPPDVAB-UHFFFAOYSA-N 0.000 claims description 7
- 239000003269 fluorescent indicator Substances 0.000 claims description 7
- GWOGSJALVLHACY-UHFFFAOYSA-N 2-pyridin-2-ylpyridine;ruthenium Chemical compound [Ru].N1=CC=CC=C1C1=CC=CC=N1 GWOGSJALVLHACY-UHFFFAOYSA-N 0.000 claims description 5
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 5
- 235000010265 sodium sulphite Nutrition 0.000 claims description 5
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 239000003205 fragrance Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- -1 2- ethylhexyl Chemical group 0.000 claims description 2
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 claims description 2
- 241001597008 Nomeidae Species 0.000 claims description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 2
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical compound [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229910052756 noble gas Inorganic materials 0.000 claims description 2
- 150000002835 noble gases Chemical class 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- ZPIRTVJRHUMMOI-UHFFFAOYSA-N octoxybenzene Chemical compound CCCCCCCCOC1=CC=CC=C1 ZPIRTVJRHUMMOI-UHFFFAOYSA-N 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 125000000524 functional group Chemical group 0.000 abstract description 4
- 238000010791 quenching Methods 0.000 abstract description 4
- 230000000171 quenching effect Effects 0.000 abstract description 4
- 238000012423 maintenance Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 abstract 5
- 230000035945 sensitivity Effects 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000013019 agitation Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000011010 flushing procedure Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000004528 spin coating Methods 0.000 description 6
- 235000010290 biphenyl Nutrition 0.000 description 5
- 239000004305 biphenyl Substances 0.000 description 5
- 239000005357 flat glass Substances 0.000 description 5
- 238000007603 infrared drying Methods 0.000 description 5
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000306 component Substances 0.000 description 4
- 239000002563 ionic surfactant Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 229960004756 ethanol Drugs 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 125000001792 phenanthrenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C=CC12)* 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000013504 Triton X-100 Substances 0.000 description 1
- 229920004890 Triton X-100 Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 210000004247 hand Anatomy 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- OAUZHPPHFHTZCQ-UHFFFAOYSA-N propan-1-ol ruthenium Chemical compound C(CC)O.[Ru] OAUZHPPHFHTZCQ-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- JLGNHOJUQFHYEZ-UHFFFAOYSA-N trimethoxy(3,3,3-trifluoropropyl)silane Chemical compound CO[Si](OC)(OC)CCC(F)(F)F JLGNHOJUQFHYEZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
Landscapes
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Optics & Photonics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention belongs to the field of a surface thin film material for a dissolved oxygen sensor and in particular relates to a preparation method of a dissolved oxygen sensing film. Based on a fluorescence quenching principle, the invention provides the preparation method of the dissolved oxygen sensing film; a sol-gel method is mainly adopted and a lyophobic functional group with higher polarity is introduced; the service life of the sensing film is enhanced through the lyophobic functional group, so that the sensitivity is enhanced; single-dispersion nanoparticles carrying an indicator are prepared through a micro-emulsion method; the preparation method is simple; the oxytropism of a traditional dissolved oxygen sensing film and the stability of the indicator are improved; the maintenance period can be directly shortened and performances can be directly improved when the dissolved oxygen sensing film is applied to the dissolved oxygen sensor.
Description
Technical field
The invention belongs to the surface film Material Field used by dissolved oxygen sensor, particularly to a kind of dissolving the oxygen sensing film
Preparation method.
Background technology
With the development of optical fiber technology, the fibre optic chemical sensor of the Fluorescence Quenching Principle based on transition metal complex is not
Disconnected be applied, and based on the quenching attenuation using fluorescence intensity more than the dissolved oxygen sensor of Fluorescence Quenching Principle,
And fluorescence lifetime, as the intrinsic characteristics of fluorophor, is less susceptible to external interference, therefore, photochemical based on fluorescence lifetime detection
Learn oxygen sensor and there is more preferable using value.And the core component of photochemistry oxygen sensor is exactly to dissolve the oxygen sensing film, it contains
The quick indicator of aerobic and solid matrix, the stability of indicator has important impact to the performance of sensor, but is using process
In be susceptible to leak；Or for keeping stability to be fixed in substrate by the method for chemical bonding, but this chemistry
The method of bonding can a certain degree of optical characteristics reducing indicator.
Content of the invention
For above-mentioned problem, the present invention provides a kind of preparation method of dissolving the oxygen sensing film, from material surface property
Handss, using sol-gel process, introduce the higher hydrophobic atom functional group of polarity, and are increased by changing medium polarity and acids type
Strong hydrolyzation catalysis effect, utilizes template (microemulsion method) preparation to wrap up the nanoparticle of certain dosis indicators simultaneously, obtain stable and
Sensitive dissolving the oxygen sensing film.
The purpose of the present invention is achieved by the following technical programs:
A kind of preparation method of dissolving the oxygen sensing film, comprises the following steps:
S1. utilize sol-gel process preparation sensing film sol: by tetraethoxysilane, trifluoromethyl front three oxosilane, water and
Propanol-butanol mixed solution is put in reactor, adds some organic acid, controls ph scope between 1 and 2, sealing stirring, so
Add metal complex fluorescent indicator propanol solution, ultrasonic disperse afterwards, put into lucifuge interior ageing 24h-48h.
S2. coating base is processed: is substrate using glass or piezoid, uses the potassium hydroxide of 2mol/l-4mol/l successively
Solution, Organic Alcohol solution soaking, are then rinsed with dehydrated alcohol, then with pure water rinsing, last dried for standby.
S3. take out the substrate handled well in s2, the colloidal sol preparing is adjusted according to the surface nature viscosity-controlling agent of substrate
Section viscosity, loads sol evenning machine, is spin-coated on substrate surface, then carries out heat treatment drying with the method for heated drying, places after drying
More than 100h, for using, keeps vacuum lucifuge to process after drying course and drying.
S4. utilize the nanosphere of microemulsion method preparation parcel indicator: at 25 DEG C -50 DEG C, oil phase, aqueous phase solution are used
Magnetic agitation is mixed, and forms microemulsion, wherein oil phase component be double (2- ethylhexyl) Disodium sulfosuccinate (aot),
Triton X-100 (triton), decane, liquid mass ratio compatible with water is 10:90-22:78；Then Deca is drawn in right amount
Send out agent solution, be passed through noble gases, introduce sulfur dioxide, isothermal reaction 1 hour, add demulsifier, high speed centrifugation, the receiving of acquirement
After rice ball pure water, it is dried.
S5. prepare dissolving the oxygen sensing film: add the nanosphere containing indicator to carry out disperseing simultaneously in the colloidal sol of s3 preparation
Film, is spin-coated on precondition substrate with sol evenning machine, is vacuum dried 3 days under light protected environment.
Preferably, in s1, the volume ratio of propanol and butanol mixed liquid is 1:4-6:1.
Preferably, in s1 organic acid be maleic acid, succinic acid, citric acid, benzenesulfonic acid derivant therein a kind of or several
Kind.
Preferably, metal complex fluorescent indicator is three (2,2 '-bipyridyl) ruthenium () complex, three (1,10- is adjacent
Phenanthroline) ruthenium () complex, three (4,7- diphenyl -1,10- o-phenanthroline) ruthenium () complex, three (1,10- is adjacent luxuriant and rich with fragrance
Sieve quinoline) ruthenium (), one or more of three (5- amino -1,10- Phen) ruthenium.
Preferably, the particle size range of nanosphere is 20nm-100nm.
Preferably, aqueous phase solution is formulated by water, acrylamide, sodium acrylate and metal complex fluorescent indicator,
Acrylamide and sodium acrylate mol ratio are 4:1-6:1, and metal complex fluorescent indicator mass fraction in aqueous phase is 1%-
0.1%.
Preferably, initiator solution is aqueous solution or decane solution, and mass concentration is 0.2%-1.5%.
It is highly preferred that aqueous solution is potassium peroxydisulfate and sodium sulfite mixed aqueous solution, mass concentration scope is 0.05%-
0.5%.
It is highly preferred that decane solution contains azodiisobutyronitrile or 2,2'-Azobis(2,4-dimethylvaleronitrile).
Preferably, in microemulsion, emulsion particle diameter is 20nm-50nm.
Preferably, demulsifier is ionic surfactant, and its water oil content hlb value is between 13-16.
Preferably, heated drying method is infrared drying and/or microwave drying.
Beneficial effects of the present invention are that the present invention sets about from material surface property, using sol-gel process, introduce polarity
Higher hydrophobic atom functional group, and strengthen hydrolyzation catalysis effect by changing medium polarity and acids type, raising is formed
The hydrophobicity of material surface and stability, and wrap up receiving of certain dosis indicators using gentle template (microemulsion method) preparation
The grain of rice, had both ensured the optical of indicator, and during being also prevented from using, indicator is revealed.Preparation method of the present invention is simple, carries
The high stability of the oxytropism of conventional solution the oxygen sensing film and indicator, is applied to can directly reduce in solvent oxygen sensor
Maintenance period and improving performance.
Specific embodiment
To further illustrate the present invention below in conjunction with specific embodiment, but embodiment does not limit to the scope of the present invention
System.All equivalents made without departing from basic idea of the present invention, belong to protection scope of the present invention.
Embodiment 1
The trifluoromethyl front three oxosilane of the tetraethoxysilane of 1 volume and 1 volume is put in reactor, adds 0.2 volume
The propanol of water and 2 volumes and the mixed solution of butanol, add maleic acid, control ph scope to 1.0, seal stirring 3 hours, add
Three (2,2 '-bipyridyl) ruthenium () complex propanol solution of 0.5 volume, ultrasonic disperse 20min, puts into lucifuge interior ageing
24h.
At 25 DEG C, the oil phase for 12:88 for the mass ratio is mixed with magnetic agitation with aqueous phase, formed microemulsion.Oil
Phase component is aot, triton, decane, and aqueous phase consists of acrylamide, sodium acrylate and three (2,2 '-bipyridyl) ruthenium () network
Compound.Form the emulsion particle diameter after microemulsion and control in 20nm, then Deca appropriate initiator solution (potassium peroxydisulfate and sulfurous acid
Hydrogen sodium mixed aqueous solution, concentration is 0.1%), it is passed through nitrogen 1h, introduce sulfur dioxide, isothermal reaction 1 hour, add ion-type table
Face activating agent (hlb=13), high speed centrifugation, after the nanosphere pure water of acquirement, it is dried.
Add nanosphere and carry out dispersion film in colloidal sol, the substrate using film is piezoid, first adopts before film
Soaked with the potassium hydroxide solution of 3mol/l, then soak 10min with propanol solution, then with dehydrated alcohol flushing three times,
Use twice of pure water rinsing afterwards, be then placed in drying baker dried for standby.Before film, take out the substrate handled well, by the colloidal sol preparing
Viscosity is adjusted according to the surface nature viscosity-controlling agent of substrate, loads sol evenning machine, spin coating under conditions of 5000r/min, 20s
In substrate surface, then carry out heat treatment drying with the method for microwave drying, place more than 100h after drying for using.
The dissolving the oxygen sensing film being obtained is arranged on dissolved oxygen sensor and is tested.
Embodiment 2
1 volume tetraethoxysilane and 1 volume trifluoromethyl front three oxosilane are put in reactor, add 0.2 volume of water and 2 bodies
Long-pending propanol-butanol mixed solution, adds succinic acid, controls ph scope to 2.0, seals stirring 1 hour, add the three of 0.5 volume
(5- amino -1,10- Phen) ruthenium propanol solution, ultrasonic disperse 10min, puts into lucifuge interior ageing 48h.
At 25 DEG C, the oil phase for 16:84 for the mass ratio is mixed with magnetic agitation with aqueous phase, formed microemulsion, its
Middle oil phase component is aot, triton, decane, and aqueous phase consists of acrylamide, sodium acrylate and three, and (5- amino -1,10- is adjacent luxuriant and rich with fragrance
Sieve quinoline) ruthenium () complex.Form the emulsion particle diameter after microemulsion and control in 50nm, then Deca appropriate initiator solution (mistake
Potassium sulfate and sodium sulfite mixed aqueous solution, concentration is 0.5%), it is passed through nitrogen 1h, introduces sulfur dioxide, isothermal reaction 1 is little
When, add ionic surfactant (hlb=15), high speed centrifugation, after the nanosphere pure water of acquirement, be dried.
Add nanosphere and carry out dispersion film in colloidal sol, the substrate using film is piezoid, first adopts before film
Soaked with the potassium hydroxide solution of 4mol/l, then soak 20min with propanol solution, then with dehydrated alcohol flushing three times,
Use twice of pure water rinsing afterwards, be then placed in drying baker dried for standby.Before film, take out the substrate handled well, by the colloidal sol preparing
Viscosity is adjusted according to the surface nature viscosity-controlling agent of substrate, loads sol evenning machine, spin coating under conditions of 3000r/min, 20s
In substrate surface, then carry out heat treatment drying with the method for infrared drying, place more than 200h after drying for using.
The dissolving the oxygen sensing film being obtained is arranged on dissolved oxygen sensor and is tested.
Embodiment 3
1 volume tetraethoxysilane and 1 volume trifluoromethyl front three oxosilane are put in reactor, add 0.2 volume of water and 2 bodies
Long-pending propanol-butanol mixed solution, adds benzene sulfonic derivative, controls ph scope to 1.8, seals stirring 2.5 hours, add 0.5
Three (4,7- diphenyl -1,10- o-phenanthroline) ruthenium () complex propanol solution of volume, ultrasonic disperse 20min, puts into
Lucifuge interior ageing 36h.
At 50 DEG C, the oil phase for 20:80 for the mass ratio is mixed with magnetic agitation with aqueous phase, formed microemulsion, its
Middle oil phase component be aot, triton, decane, aqueous phase consist of acrylamide, sodium acrylate and three (4,7- diphenyl -1,
10- o-phenanthroline) ruthenium () complex.Form the emulsion particle diameter after microemulsion and control in 40nm, then Deca appropriate initiator
Solution (potassium peroxydisulfate and sodium sulfite mixed aqueous solution, concentration is 0.05%), is passed through nitrogen 1h, introduces sulfur dioxide, constant temperature
Reaction 1 hour, adds ionic surfactant (hlb=16), high speed centrifugation, after the nanosphere pure water of acquirement, does
Dry.
Add nanosphere and carry out dispersion film in colloidal sol, the substrate using film is sheet glass, first adopts before film
Soaked with the potassium hydroxide solution of 2mol/l, then soak 20min with propanol solution, then with dehydrated alcohol flushing three times,
Use twice of pure water rinsing afterwards, be then placed in drying baker dried for standby.Before film, take out the substrate handled well, by the colloidal sol preparing
Viscosity is adjusted according to the surface nature viscosity-controlling agent of substrate, loads sol evenning machine, spin coating under conditions of 4000r/min, 20s
In substrate surface, then first use infrared drying, then the method for microwave drying carries out heat treatment drying, place after drying 150h with
Upper for use.
The dissolving the oxygen sensing film being obtained is arranged on dissolved oxygen sensor and is tested.
Embodiment 4
1 volume tetraethoxysilane and 1 volume trifluoromethyl front three oxosilane are put in reactor, add 0.2 volume of water and 2 bodies
Long-pending propanol-butanol mixed solution, adds citric acid, controls ph scope to 1.5, sealing stirring 3 hours, add 0.5 volume three (1,
10- o-phenanthroline) ruthenium () complex propanol solution, ultrasonic disperse 10min, puts into lucifuge interior ageing 48h.
At 50 DEG C, liquid compatible with water for the oil phase for 13:87 for the mass ratio is mixed with magnetic agitation, formed microemulsion
Liquid.Wherein oil phase consists of aot, triton, decane, and aqueous phase consists of acrylamide, sodium acrylate and three, and (1,10- adjacent phenanthrene is coughed up
Quinoline) ruthenium () complex.Form the emulsion particle diameter after microemulsion and control in 25nm, then Deca appropriate initiator solution (azo
Bis-isobutyronitrile solution, concentration is 1.5%), it is passed through nitrogen 1h, introduce sulfur dioxide, isothermal reaction 1 hour, add ion-type surface
Activating agent (hlb=13), high speed centrifugation, after the nanosphere pure water of acquirement, it is dried.
Add nanosphere and carry out dispersion film in colloidal sol, the substrate using film is sheet glass, first adopts before film
Soaked with the potassium hydroxide solution of 2mol/l, then soak 20min with propanol solution, then with dehydrated alcohol flushing three times,
Use twice of pure water rinsing afterwards, be then placed in drying baker dried for standby.Before film, take out the substrate handled well, by the colloidal sol preparing
Viscosity is adjusted according to the surface nature viscosity-controlling agent of substrate, loads sol evenning machine, spin coating under conditions of 2000r/min, 20s
In substrate surface, then first use microwave drying, then the method for infrared drying carries out heat treatment drying, place after drying 200h with
Upper for use.
The dissolving the oxygen sensing film being obtained is arranged on dissolved oxygen sensor and is tested.
Embodiment 5
1 volume tetraethoxysilane and 1 volume trifluoromethyl front three oxosilane are put in reactor, add 0.2 volume of water and 2 bodies
Long-pending propanol-butanol mixed solution, adds maleic acid, controls ph scope to 1.1, seals stirring 2.5 hours, add 0.5 volume three
(1,10- o-phenanthroline) ruthenium () complex propanol solution, ultrasonic disperse 15min, puts into lucifuge interior ageing 28h.
At 40 DEG C, the oil phase for 21:79 for the mass ratio and aqueous phase solution are mixed with magnetic agitation, formed microemulsion
Liquid.Wherein oil phase consists of aot, triton, decane, and aqueous phase consists of acrylamide, sodium acrylate and three, and (1,10- adjacent phenanthrene is coughed up
Quinoline) ruthenium () complex.Form the emulsion particle diameter after microemulsion and control in 35nm, then Deca appropriate initiator solution (azo
Bis-isobutyronitrile solution, concentration is 0.5%), it is passed through nitrogen 1h, introduce sulfur dioxide, isothermal reaction 1 hour, add ion-type surface
Activating agent (hlb=16), high speed centrifugation, after the nanosphere pure water of acquirement, it is dried.
Add nanosphere and carry out dispersion film in colloidal sol, the substrate using film is sheet glass, first adopts before film
Soaked with the potassium hydroxide solution of 3mol/l, then use alcohol solution dipping 15min, then with dehydrated alcohol flushing three times,
Use twice of pure water rinsing afterwards, be then placed in drying baker dried for standby.Before film, take out the substrate handled well, by the colloidal sol preparing
Viscosity is adjusted according to the surface nature viscosity-controlling agent of substrate, loads sol evenning machine, spin coating under conditions of 3500r/min, 20s
In substrate surface, then the method for infrared drying carries out heat treatment drying, places more than 180h for use after drying.
The dissolving the oxygen sensing film being obtained is arranged on dissolved oxygen sensor and is tested.
Embodiment 6
1 volume tetraethoxysilane and 1 volume trifluoromethyl front three oxosilane are put in reactor, add 0.2 volume of water and 2 bodies
Long-pending propanol-butanol mixed solution, adds citric acid, controls ph scope to 1.3, seals stirring 1.5 hours, add 0.5 volume three
(2,2 '-bipyridyl) ruthenium () complex propanol solution, ultrasonic disperse 15min, puts into lucifuge interior ageing 28h.
At 30 DEG C, the oil phase for 18:82 for the mass ratio and aqueous phase solution are mixed with magnetic agitation, formed microemulsion
Liquid.Wherein oil phase consists of aot, triton, decane, and aqueous phase consists of acrylamide, sodium acrylate and three (2,2 '-connection pyrroles
Pyridine) ruthenium () complex.Form the emulsion particle diameter after microemulsion and control in 45nm, then Deca appropriate initiator solution (over cure
Sour potassium and sodium sulfite mixed aqueous solution, its concentration is 0.25%), it is passed through nitrogen 1h, introduces sulfur dioxide, isothermal reaction 1 is little
When, add ionic surfactant (hlb=14), high speed centrifugation, after the nanosphere pure water of acquirement, be dried.
Add nanosphere and carry out dispersion film in colloidal sol, the substrate using film is sheet glass, first adopts before film
Soaked with the potassium hydroxide solution of 4mol/l, then soak 20min with butanol solution, then with dehydrated alcohol flushing three times,
Use twice of pure water rinsing afterwards, be then placed in drying baker dried for standby.Before film, take out the substrate handled well, by the colloidal sol preparing
Viscosity is adjusted according to the surface nature viscosity-controlling agent of substrate, loads sol evenning machine, spin coating under conditions of 4500r/min, 20s
In substrate surface, then the method for microwave drying carries out heat treatment drying, places more than 150h for use after drying.
The dissolving the oxygen sensing film being obtained is arranged on dissolved oxygen sensor and is tested.
Comparative example 1
The tetraethoxysilane of 2 volumes is put in reactor, adds the water of 0.5 volume and the alcohol mixed solution of 2 volumes, adds
Hydrochloric acid, controls ph scope to 2, seals stirring 1 hour, add three (4,7- diphenyl -1,10- o-phenanthrolines) of 0.5 volume
Ruthenium () complex ethanol solution, ultrasonic disperse 10min, puts into lucifuge interior ageing 48h, obtains colloidal sol.
After colloidal sol obtains, carry out dispersion film, the substrate using film is sheet glass, before film, first adopt 2mol's
Sodium hydroxide solution soaks, and then use alcohol solution dipping 30min, finally uses twice of pure water rinsing, is then placed in drying baker dry
Dry stand-by.Before film, take out the substrate handled well, the colloidal sol preparing is loaded sol evenning machine, under conditions of 5000r/min, 20s
It is spin-coated on substrate surface, is then dried and dries, place more than 48h after drying for using.Then will obtain dissolving the oxygen sensing film dress
Enter sensor to be tested.
Comparative example 2
The trifluoro propyl trimethoxy silane of the tetraethoxysilane of 1 volume and 1 volume is put in reactor, adds 0.5 volume
Water and 2 volume ethanol mixed solutions, add hydrochloric acid, control ph scope to 2, sealing stirring 1 hour, add 0.5 volume three (4,
7- diphenyl -1,10- o-phenanthroline) ruthenium () complex indicator ethanol solution, ultrasonic disperse 10min, puts into lucifuge room
Interior ageing 48h, obtains colloidal sol.
Then dispersion film are carried out, the substrate using film is piezoid, first adopts the sodium hydroxide of 3mol before film
Solution soaking, then uses alcohol solution dipping 20min, finally uses twice of pure water rinsing, is then placed in drying baker dried for standby.Apply
Before film, take out the substrate handled well, the colloidal sol preparing is loaded sol evenning machine, is spin-coated on base under conditions of 4000r/min, 20s
Piece surface, is then dried and dries, and places more than 48h for using after drying.Finally will obtain dissolving the oxygen sensing film loading sensor
Tested.
Embodiment is as follows: with comparative example test parameter and Comparative result
Claims (11)
1. a kind of preparation method of dissolving the oxygen sensing film is it is characterised in that comprise the following steps:
S1. utilize sol-gel process preparation sensing film sol: by tetraethoxysilane, trifluoromethyl front three oxosilane, water and
Propanol-butanol mixed solution is put in reactor, adds some organic acid, controls ph scope between 1 and 2, sealing stirring, so
Add metal complex fluorescent indicator propanol solution, ultrasonic disperse afterwards, put into lucifuge interior ageing 24h-48h；
S2. coating base is processed: is substrate using glass or piezoid, uses the potassium hydroxide of 2mol/l-4mol/l molten successively
Liquid, Organic Alcohol solution soaking, are then rinsed with dehydrated alcohol, then with pure water rinsing, last dried for standby；
S3. take out the substrate handled well in s2, the colloidal sol preparing is adjusted with viscosity-controlling agent according to the surface nature of substrate glutinous
Degree, loads sol evenning machine, is spin-coated on substrate surface, then carries out heat treatment drying with the method for heated drying, places 100h after drying
Above for using, after drying course and drying, vacuum lucifuge is kept to process；
S4. utilize the nanosphere of microemulsion method preparation parcel indicator: at 25 DEG C -50 DEG C, by oil phase, aqueous phase solution magnetic force
Stirring is mixed, and forms microemulsion, wherein oil phase component is double (2- ethylhexyl) Disodium sulfosuccinate (aot), poly- second
Glycol octyl phenyl ether (triton), decane, liquid mass ratio compatible with water is 10:90-22:78；Then Deca appropriate initiator
Solution, is passed through noble gases, introduces sulfur dioxide, isothermal reaction 1-3 hour, adds demulsifier, high speed centrifugation, the nanometer of acquirement
After ball pure water, it is dried；
S5. prepare dissolving the oxygen sensing film: add the nanosphere containing indicator to be disperseed and apply in the colloidal sol of s3 preparation
Film, is spin-coated on precondition substrate with sol evenning machine, is vacuum dried 1-3 days under light protected environment.
2. according to claim 1 the preparation method of dissolving the oxygen sensing film it is characterised in that described propanol and butanol mixed liquid
Volume ratio be 1:4-6:1.
3. according to claim 2 dissolving the oxygen sensing film preparation method it is characterised in that described organic acid be maleic acid,
Succinic acid, citric acid, benzenesulfonic acid derivant therein one or more.
4. dissolve the preparation method of the oxygen sensing film according to claim 3 it is characterised in that described metal complex fluorescent refers to
Show agent be three (2,2 '-bipyridyl) ruthenium () complex, three (1,10- o-phenanthroline) ruthenium () complex, three (4,7- bis-
Phenyl -1,10- o-phenanthroline) ruthenium () complex, three (1,10- Phen) ruthenium (), three (5- amino -1,10- is adjacent luxuriant and rich with fragrance
One or more of sieve quinoline) ruthenium.
5. according to claim 1 the preparation method of dissolving the oxygen sensing film it is characterised in that the particle size range of described nanosphere
For 20nm-100nm.
6. according to claim 1 dissolving the oxygen sensing film preparation method it is characterised in that described aqueous phase solution by water, third
Acrylamide, sodium acrylate and metal complex fluorescent indicator are formulated, and acrylamide and sodium acrylate mol ratio are 4:1-
6:1, metal complex fluorescent indicator mass fraction in aqueous phase is 1%-0.1%.
7. dissolve the preparation method of the oxygen sensing film according to claim 4 it is characterised in that described initiator solution is water-soluble
Liquid or decane solution.
8. dissolve the preparation method of the oxygen sensing film according to claim 7 it is characterised in that described aqueous solution is potassium peroxydisulfate
With sodium sulfite mixed aqueous solution, mass concentration is 0.05%-0.5%.
9. dissolve the preparation method of the oxygen sensing film according to claim 7 it is characterised in that described decane solution contains azo
Bis-isobutyronitrile or 2,2'-Azobis(2,4-dimethylvaleronitrile), mass concentration is 0.2%-1.5%.
10. dissolve the preparation method of the oxygen sensing film according to any one of claim 1-9 it is characterised in that described microemulsion
Middle emulsion particle diameter is 20nm-50nm.
11. preparation methoies dissolving the oxygen sensing film according to claim 10 are it is characterised in that described demulsifier is ion-type
Surfactant, its water oil content hlb value is between 13-16.
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| CN111398239B (en) * | 2020-05-19 | 2022-11-25 | 威海精讯畅通电子科技有限公司 | Dissolved oxygen measuring device based on fluorescence quenching method |
| CN114414536A (en) * | 2021-10-15 | 2022-04-29 | 上海蓝长自动化科技有限公司 | Preparation method of dissolved oxygen sensitive film based on fluorescence |
| CN115308183A (en) * | 2022-08-29 | 2022-11-08 | 兰州大学 | Optical fiber oxygen sensing system based on fluorescence quenching mechanism and coherent detection principle |
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