CN1908633A - Preparation of optical fiber pH sensor sensing membrane - Google Patents
Preparation of optical fiber pH sensor sensing membrane Download PDFInfo
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- CN1908633A CN1908633A CN 200610068522 CN200610068522A CN1908633A CN 1908633 A CN1908633 A CN 1908633A CN 200610068522 CN200610068522 CN 200610068522 CN 200610068522 A CN200610068522 A CN 200610068522A CN 1908633 A CN1908633 A CN 1908633A
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Abstract
The related preparation method for sensitive film of an optical fiber pH sensor comprises: selecting 30-50cm conventional fiber with inner and outer core diameter rate as 62.5/125mum, cutting 2-6cm segment on one end for sleeve and coating layer; corroding with HF to remove the package; activating the fiber core with 20-55% HNO3 for 10-60min to form active (OH)-; by sol-gel method and tetraethyl orthosilicate as precursor, fixing the pH indication molecule on fiber core. This invention is simple and reliable for remote detection.
Description
Technical field:
The invention belongs to the preparation method of the preparing technique process, particularly a kind of optical fiber pH sensor sensing membrane of a kind of sensor sensing material in the Fibre Optical Sensor pH value monitoring technical field.
Technical background:
Optical fiber sensing technology is a new branch that forms along with the development of Fibre Optical Communication Technology.It has: volume is little, in light weight, shape is flexible, anti-electromagnetic interference (EMI), and is good to the adaptability of environment; Belong to noncontact, non-destroyed measurement.That optical fiber sensing technology can be applicable to is inflammable, explosive, the detection under narrow space and corrosive gas, liquid environment and the ray contamination environment, it be methods such as existing machinery, electromagnetism, electronics can't realize or incomparable detection technique.A main method of traditional measurement pH value is potential electrode method (as a glass-membrane electrode), because electrode response time is long, poor stability, is difficult to measure the subtle change of pH value and variation rapidly; Simultaneously, the matrix volume is big, is not suitable for the online detection of microenvironment and biological living, more is difficult to adapt to the application in rugged surroundings.In addition, the pH test paper method can't monitor local pH value to be changed, and more can not monitor in real time.Optical fiber pH sensing technology mainly is that optical fiber sensing technology is combined with the colorimetric analysis technology, having overcome response time length in traditional pH value detection method, poor stability, be not suitable for the shortcomings such as online detection of microenvironment and biological living, is a new technology that develops rapidly in recent years.At present, the key point of this technology be on optical fiber surface is modified to the polymeric membrane of pH value sensitivity, conventional method is to be carrier with the macromolecular material, and the method for pH pH indicator by physically trapping or chemical bond combination is fixed on the fiber core surface.
The core of optical fiber pH sensing technology is the preparation method of research fiber core surface p H sensitive membrane, and core technology is the fixed form of indication agent molecule, and it is legal to be divided into physically trapping method and chemical bonded refractory.The former still can improve fixed effect by the collocation of selecting suitable carriers, optimization carrier and indicator because indicator easily runs off, and poor repeatability has limited its development; The latter has solved the problem that indicator runs off, but to the having relatively high expectations of process conditions, awaits further exploration.The physically trapping method is the method for present more or less freely enforcement, and wherein many is the immobilized indicator of carrier with the silicon gel, but its sensing range has only 2～4 pH values.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that exists in the prior art, seek to design a kind of architectural feature of optic fibre carrier of utilizing and prepare optical fiber pH sensor sensing membrane through chemistry and physical method, this sensitive membrane can be used for telemeasurement potential of hydrogen (pH value).The present invention has carried out compositely on the basis of optimized choice carrier and indicator collocation to indicator, increased the sensing range of prepared pH sensitive membrane.
The preparation method of optical fiber pH sensor sensing membrane, step is as follows:
1. get commercially available communication optical fiber 30-50cm, inside and outside core diameter is of a size of 62.5/125 μ m, and its inner structure is that fibre core is shaped on covering outward, and covering has overlay outward, and overlay is shaped on sheath outward.
2. cut the sheath and the overlay of optical fiber one end with blade, cutting length is 2-6cm.
3. exposed covering and core segment are corroded with 5%-40% hydrofluorite, to remove covering.Method is: corrode optical fiber in hydrofluoric acid solution, constantly monitor core diameter with spiral dial gauge (0-25mm range, resolution are 0.01mm), till it reached 50-60 μ m, etching time was 30 minutes to 5 hours 30 minutes.
4. the fibre core of optical fiber is made by quartz material, and the fibre core after the corrosion activates 10-60 minute with the nitric acid of 20%-55%, makes the fibre core surface form the hydroxyl of activation.
5. the employing sol-gal process is a presoma with the tetraethyl orthosilicate, the pH indicator molecules is fixed on the fiber core surface forms sensitive membrane.Method is: tetraethyl orthosilicate (TEOS) is mixed with the part by weight of ethanol according to 1: 1, and add bromophenol blue successively, cresol red and chlorophenol red, concentration is respectively 1-5mg/ml, 0.1-2mg/ml and 0.1-2mg/ml.Then solution is placed 20-80 ℃ stirred in water bath 60 minutes, after treating that solution is cooled to room temperature, to remove covering and activated optical fiber impregnated in the solution, make it optical fiber surface film forming 30 minutes, in the dipping film forming procedure, drag optical fiber back and forth with certain speed, to guarantee the homogeneity of film.Tetraethyl orthosilicate (TEOS) forms silicon dioxide (SiO2) 3-D solid structure with polymerization oxo bridge through hydrolysis, condensation, with the Stationary pH indicator.
The present invention compared with prior art has the following advantages: the optical fiber that at first will have the pH sensitive membrane is immersed in the hydrochloric acid solution of pH=4.5, adjust the pH value of solution by adding the pH=14 sodium hydroxide solution, in the process that record pH value increases gradually, optical output power reduces gradually along with the increase of pH value, the process of pH value from 4.5 to 13, optical output power becomes 6.87 μ W by 6.99 μ W, and its variation tendency is basic and the pH value is linear.The optical fiber that secondly will have the pH sensitive membrane is immersed in the mixed phosphate salt buffer solution of pH=6.90, treat that it transfers to 9.28 with the pH value of solution after stable, and then make the pH value of solution return 6.90, so repeat several times, when the pH value changes between 6.90 and 9.28, after the circulation, optical output power all changes between 7.164 μ W and 7.138 μ W, illustrates that prepared optical fiber pH sensor has good reversibility each time.This method principle is reliable, and processing step is easy, and the operation technology of preparing requires low, and product stability is good, long service life.
Embodiment:
Specific implementation method of the present invention can have following example to further describe.
Embodiment:
1. get commercially available communication optical fiber 40cm, inside and outside core diameter is of a size of 62.5/125 μ m.
2. cut optical fiber jacket and overlay with blade, cutting length is 4cm.
3. exposed covering and core segment are corroded with 15% hydrofluorite, to remove covering.Method is: corrode optical fiber in hydrofluoric acid solution, constantly monitor core diameter with spiral dial gauge (0-25mm range, resolution are 0.01mm), till reaching 60 μ m, etching time is 4 hours.
4. the fibre core of optical fiber is made by quartz material, and the fibre core after the corrosion activates 30 minutes with 35% nitric acid, makes the fibre core surface form the hydroxyl of activation.
5. measuring 5mL tetraethyl orthosilicate (TEOS) joins in the 5mL ethanol, add 10mg bromophenol blue, 4mg cresol red and 4mg chlorophenol red more successively, solution placed 30 ℃ water-bath heated and stirred 60 minutes, after treating that solution is cooled to room temperature, to remove covering and activated optical fiber and impregnated in the solution 30 minutes, and make it in the optical fiber surface film forming, in the dipping film forming procedure, drag optical fiber back and forth with certain speed, to guarantee the homogeneity of film.
Claims (3)
1. the preparation method of an optical fiber pH sensor sensing membrane, it is characterized in that choosing earlier inside and outside core diameter is the commercially available optical fiber 30-50cm of 62.5/125 μ m, going length in the one end-grain cutting is sheath and the overlay of 2-6cm; Use hydrofluorite erosion removal covering again; Fibre core after the corrosion activates 10-60 minute with the nitric acid of 20%-55%, makes the fibre core surface form the hydroxyl of activation; Using sol-gal process then, is presoma with the tetraethyl orthosilicate, the pH indicator molecules is fixed on the fiber core surface forms pH value sensitive membrane.
2. the preparation method of optical fiber pH sensor sensing membrane according to claim 1, it is characterized in that removing covering, promptly in hydrofluoric acid solution, corrode optical fiber, constantly monitor core diameter with the spiral dial gauge, till it reached 50-60 μ m, etching time was 30 minutes to 330 minutes.
3. the preparation method of optical fiber pH sensor sensing membrane according to claim 1, the step that it is characterized in that forming sensitive membrane is that tetraethyl orthosilicate (TEOS) is mixed with the part by weight of ethanol according to 1: 1, and adding bromophenol blue, cresol red and chlorophenol red successively, concentration is respectively 1-5mg/ml, 0.1-2mg/ml and 0.1-2mg/ml; Then solution is placed 20-80 ℃ stirred in water bath 60 minutes, after treating that solution is cooled to room temperature, to remove covering and activated optical fiber impregnated in the solution, make it optical fiber surface film forming 30 minutes, in the dipping film forming procedure, drag optical fiber back and forth with certain speed, to guarantee the homogeneity of mould; Tetraethyl orthosilicate (TEOS) forms silicon dioxide (SiO2) 3-D solid structure with polymerization oxo bridge through hydrolysis, condensation, with the Stationary pH indicator.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610068522 CN1908633A (en) | 2006-08-17 | 2006-08-17 | Preparation of optical fiber pH sensor sensing membrane |
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| CN 200610068522 CN1908633A (en) | 2006-08-17 | 2006-08-17 | Preparation of optical fiber pH sensor sensing membrane |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982760A (en) * | 2010-09-20 | 2011-03-02 | 北京邮电大学 | Optical fiber pH meter |
| CN103278182A (en) * | 2013-03-25 | 2013-09-04 | 海龙核材科技（江苏）有限公司 | Manufacturing method for optical fiber sensor |
| CN103293137A (en) * | 2013-06-08 | 2013-09-11 | 中国船舶重工集团公司第七二五研究所 | Preparation method of optical fiber iron ion sensitive film |
| CN103410007A (en) * | 2013-08-07 | 2013-11-27 | 东华大学 | Sol-gel pH discoloration finishing method for fabric |
| CN103543150A (en) * | 2013-09-03 | 2014-01-29 | 郑州大学 | Gel-based pH sensor preparation method thereof |
| CN103645141A (en) * | 2013-11-16 | 2014-03-19 | 中山欧麦克仪器设备有限公司 | Optical fiber pH meter |
| CN103675061A (en) * | 2013-12-16 | 2014-03-26 | 南京市第二医院 | Anatase type TiO2 nano particle based pH sensor and pH value detection method |
-
2006
- 2006-08-17 CN CN 200610068522 patent/CN1908633A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982760A (en) * | 2010-09-20 | 2011-03-02 | 北京邮电大学 | Optical fiber pH meter |
| CN103278182A (en) * | 2013-03-25 | 2013-09-04 | 海龙核材科技（江苏）有限公司 | Manufacturing method for optical fiber sensor |
| CN103278182B (en) * | 2013-03-25 | 2016-03-02 | 江苏海龙核科技股份有限公司 | A kind of method for making of Fibre Optical Sensor |
| CN103293137A (en) * | 2013-06-08 | 2013-09-11 | 中国船舶重工集团公司第七二五研究所 | Preparation method of optical fiber iron ion sensitive film |
| CN103410007A (en) * | 2013-08-07 | 2013-11-27 | 东华大学 | Sol-gel pH discoloration finishing method for fabric |
| CN103410007B (en) * | 2013-08-07 | 2016-01-06 | 东华大学 | A kind of sol-gel pH variable color method for sorting of textiles |
| CN103543150A (en) * | 2013-09-03 | 2014-01-29 | 郑州大学 | Gel-based pH sensor preparation method thereof |
| CN103543150B (en) * | 2013-09-03 | 2015-11-04 | 郑州大学 | A kind of gel base pH sensor and preparation method thereof |
| CN103645141A (en) * | 2013-11-16 | 2014-03-19 | 中山欧麦克仪器设备有限公司 | Optical fiber pH meter |
| CN103645141B (en) * | 2013-11-16 | 2016-04-27 | 中山欧麦克仪器设备有限公司 | A kind of optical fiber pH meter |
| CN103675061A (en) * | 2013-12-16 | 2014-03-26 | 南京市第二医院 | Anatase type TiO2 nano particle based pH sensor and pH value detection method |
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