CN102093890A - Tin dioxide composite nanomaterial for nano cataluminescence sensor and preparation method thereof - Google Patents
Tin dioxide composite nanomaterial for nano cataluminescence sensor and preparation method thereof Download PDFInfo
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- CN102093890A CN102093890A CN2010106158190A CN201010615819A CN102093890A CN 102093890 A CN102093890 A CN 102093890A CN 2010106158190 A CN2010106158190 A CN 2010106158190A CN 201010615819 A CN201010615819 A CN 201010615819A CN 102093890 A CN102093890 A CN 102093890A
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Abstract
The invention discloses a tin dioxide composite nanomaterial for a nano cataluminescence sensor. SnO2 nanoparticle layer is compounded on the surface of a carbon nanotube. The preparation method comprises the following steps of: adding 20mL of 25 to 35 percent nitric acid solution into a flask containing 5g of carbon nanotube, and fluxing and heating at the temperature of between 120 and 140DEG C for 24 hours under stirring of magnetons; adding 10 to 20g of SnCl2.2H2O into the flask, and performing ultrasonic treatment at room temperature for 1 to 3 hours; slowing adding 0.04 to 0.06g/mL NaOH or KOH solution into the flask with stirring, and regulating the pH value of the substance in the flask to be 9-11; filtering by using filter paper, washing a substance which is filtered out by using distilled water, and drying at the temperature of between 80 and 90DEG C for 1 to 2 hours; and heating the dried substance to the temperature of between 480 and 550DEG C in the air in a calcining furnace, introducing inert gas, keeping constant temperature for 0.5 to 3 hours, cooling in the inert gas to the temperature of between 20 and 30DEG C, and taking the dried substance out.
Description
Technical field:
The present invention relates to a kind of nano catalytic luminescence transmitter with nano material and preparation method, especially a kind of catalytic luminescence nano material specific surface area that increases, nano catalytic luminescence transmitter the tindioxide composite nano materials and the preparation method of raising luminous efficiency.
Background technology:
Existing nano-material surface-catalyzed luminescent detector is that the diameter that will scribble nano material is that to place diameter be that 12～20mm, length are in the silica tube of 100～150mm to 4～7mm electric ceramic rod, diagonally opposing corner is provided with injection port, drain on silica tube, corresponding spectral filter or grating, the photosignal transfer equipment (near ultraviolet sensitive spectroscopy measurement type Weak-luminescence survey meter, photomultiplier etc.) of being provided with nano material outside silica tube.During measurement, the electric ceramic rod heats nano material, sampling systems such as pneumatic pump enter silica tube with carrier gas from injection port with sample, the nano-material surface of flowing through is discharged from drain, the nano-material surface-catalyzed light that sends is behind spectral filter or grating removal stray light, become the electrical signal that is adapted to data processing units such as microcomputer through the photosignal transfer equipment again, carry out check and analysis.Catalytic luminescence is the phenomenon that the excited state product that produces in the catalytic reaction process radiates photon when turning back to ground state, and catalytic luminescence intensity becomes dependency with nano material, analytic target kind and concentration, detection efficiency etc.Nano material in the existing nano-material surface-catalyzed luminescent detector adopts nanoparticles such as aluminium sesquioxide, zinc oxide, ferric oxide and tindioxide usually, although also relevant for the report of composite nano materials, but all be that two kinds of nanoparticles are mixed mostly, the simple formed nano-material coating luminous efficiency of nanoparticle is relatively low.
Summary of the invention:
The present invention is in order to solve the above-mentioned technical problem of existing in prior technology, a kind of nano material specific surface area that increases to be provided, improving nano catalytic luminescence transmitter the tindioxide composite nano materials and the preparation method of luminous efficiency.
Technical solution of the present invention is: a kind of nano catalytic luminescence transmitter tindioxide composite nano materials is characterized in that it being that surface recombination at carbon nanotube has SnO
2Nanoparticle layers.
A kind of above-mentioned nano catalytic luminescence transmitter preparation method of tindioxide composite nano materials is characterized in that carrying out as follows successively:
A. be that 25～35% salpeter solution adds and fills in the flask of carbon nanotube with concentration, the ratio of salpeter solution and carbon nanotube is 200mL: 5g, under the magneton stirring, and 120～140 ℃ of reflux 24 hours;
B. with SnCl
22H
2O adds in the flask, and at room temperature supersound process is 1～3 hour, described SnCl
22H
2The mass ratio of O and carbon nanotube is 5: 10～20;
C. under agitation condition, slowly NaOH or the KOH solution with 0.04～0.06g/mL adds in the flask, and regulating vial pH value is 9～11, uses filter paper filtering, get leach thing with distilled water wash after 80～90 ℃ of dryings 1～2 hour;
D. dry thing is warming up to 480～550 ℃ in the calcining furnace air, fed rare gas element constant temperature 0.5～3 hour, in rare gas element, be cooled to 20～30 ℃, take out dry thing.
Described carbon nanotube is a multi-walled carbon nano-tubes, and specific surface area is 200～300m
3/ g, average caliber is 20～40nm.
The heat-up rate of described d step is 4～6 ℃/minute; It is 1～4 liter/minute that described rare gas element feeds flow.
The present invention is under the condition that the nano-material coating area equates, can effectively increase the specific surface area of tindioxide composite nano materials, compare with simple tin dioxide nano-particle coating, luminous efficiency significantly improves, and then improved catalytic luminescence intensity, tested component contacts more abundant with nano-material surface simultaneously, time of response on nano material shortens greatly, signal response time is rapid, signal to noise ratio strengthens, the signal bands of a spectrum narrow down (similar sharp-pointed chromatogram elution curve), detection efficiency, resolving power and the sensitivity that can improve detector.
Description of drawings:
Fig. 1 is the sem photograph of the embodiment of the invention 1 tindioxide composite nano materials.
Fig. 2 is the Raman spectrogram of the embodiment of the invention 1 tindioxide composite nano materials.
Fig. 3 is the transmission electron microscope picture of the embodiment of the invention 1 tindioxide composite nano materials.
Fig. 4 is the X-ray diffractogram of the embodiment of the invention 1 tindioxide composite nano materials.
Fig. 5 is that the embodiment of the invention 1 tindioxide composite nano materials and tin dioxide nano-particle are to alcoholic acid catalytic luminescence intensity contrast figure.
Embodiment:
Embodiment 1:
The embodiment of the invention 1 is carried out as follows:
A. be that 25% salpeter solution adds and fills in the round-bottomed flask of 5g carbon nanotube with the concentration of the new preparation of 200mL, round-bottomed flask is placed the aluminum pot that fills silicone oil, under magneton stirs, 120 ℃ of reflux 24 hours; Described carbon nanotube is a multi-walled carbon nano-tubes, and specific surface area is 200m
3/ g, average caliber is 20nm.
B. with 10g SnCl
22H
2O adds in the flask, and at room temperature supersound process is 1 hour;
C. under agitation condition, slowly the NaOH solution with 0.04g/mL adds in the flask, and regulating vial pH value is 9, with the quantitative paper filtration, gets and leaches thing and remove Na with distilled water wash
+, 80 ℃ of dryings 2 hours more afterwards;
D. dry thing is warming up to 480 ℃ in the calcining furnace air, fed nitrogen constant temperature 0.5 hour, in rare gas element, be cooled to 20 ℃, take out dry thing; Described heat-up rate is 4 ℃/minute; It is 1 liter/minute that described rare gas element feeds flow.
The dry thing of gained is the tindioxide composite nano materials, is that the surfaces externally and internally at carbon nanotube is compounded with SnO
2Nanoparticle layers, the same prior art of using method.
The tindioxide composite nano materials sem photograph of embodiment 1 as shown in Figure 1.
The tindioxide composite nano materials Raman spectrogram of embodiment 1 as shown in Figure 2.
The tindioxide composite nano materials transmission electron microscope picture of embodiment 1 as shown in Figure 3.
The tindioxide composite nano materials X-ray diffractogram of embodiment 1 as shown in Figure 4.
Tindioxide composite nano materials and common tin dioxide nano-particle with the embodiment of the invention 1 are made the nano catalytic luminescence transmitter respectively, ethanol is test sample, to alcoholic acid catalytic luminescence intensity contrast as shown in Figure 5, show that the tindioxide composite nano materials obviously is better than common common tin dioxide nano-particle to alcoholic acid catalytic luminescence intensity.
The embodiment of the invention 2 is carried out as follows:
A. be that 35% salpeter solution adds and fills in the round-bottomed flask of 10g carbon nanotube with the concentration of the new preparation of 400mL, round-bottomed flask is placed the aluminum pot that fills silicone oil, under magneton stirs, 140 ℃ of reflux 24 hours; Described carbon nanotube is a multi-walled carbon nano-tubes, and specific surface area is 300m
3/ g, average caliber is 40nm.
B. with 20g SnCl
22H
2O adds in the flask, and at room temperature supersound process is 3 hours;
C. under agitation condition, slowly the KOH solution with 0.06g/mL adds in the flask, and regulating vial pH value is 11, with the quantitative paper filtration, gets and leaches thing and remove K with distilled water wash
+, 90 ℃ of dryings are 1 hour afterwards;
D. dry thing is warming up to 550 ℃ in the calcining furnace air, fed helium constant temperature 3 hours, in rare gas element, be cooled to 30 ℃, take out dry thing; Described heat-up rate is 6 ℃/minute; It is 4 liters/minute that described rare gas element feeds flow.
The dry thing of gained is the tindioxide composite nano materials, is that the surfaces externally and internally at carbon nanotube is compounded with SnO
2Nanoparticle layers, the same prior art of using method.
Claims (4)
1. nano catalytic luminescence transmitter tindioxide composite nano materials is characterized in that it being that surface recombination at carbon nanotube has SnO
2Nanoparticle layers.
2. the described nano catalytic luminescence transmitter of a claim 1 is characterized in that carrying out as follows successively with the preparation method of tindioxide composite nano materials:
A. be that 25～35% salpeter solution adds and fills in the flask of carbon nanotube with concentration, the ratio of salpeter solution and carbon nanotube is 200mL: 5g, under the magneton stirring, and 120～140 ℃ of reflux 24 hours;
B. with SnCl
22H
2O adds in the flask, and at room temperature supersound process is 1～3 hour, described SnCl
22H
2The mass ratio of O and carbon nanotube is 5: 10～20;
C. under agitation condition, slowly NaOH or the KOH solution with 0.04～0.06g/mL adds in the flask, and regulating vial pH value is 9～11, uses filter paper filtering, get leach thing with distilled water wash after 80～90 ℃ of dryings 1～2 hour;
D. dry thing is warming up to 480～550 ℃ in the calcining furnace air, fed rare gas element constant temperature 0.5～3 hour, in rare gas element, be cooled to 20～30 ℃, take out dry thing.
3. nano catalytic luminescence transmitter according to claim 2 is characterized in that with the preparation method of tindioxide composite nano materials described carbon nanotube is a multi-walled carbon nano-tubes, and specific surface area is 200～300m
3/ g, average caliber is 20～40nm.
4. the nano catalytic luminescence transmitter according to claim 3 preparation method of tindioxide composite nano materials, the heat-up rate that it is characterized in that described d step is 4～6 ℃/minute; It is 1～4 liter/minute that described rare gas element feeds flow.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106505188A (en) * | 2015-09-06 | 2017-03-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tinbase nano-particle-carbon composite and preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005094231A2 (en) * | 2004-03-19 | 2005-10-13 | The Regents Of The University Of California | Methods for fabrication of positional and compositionally controlled nanostructures on substrate |
| CN101439855A (en) * | 2008-12-24 | 2009-05-27 | 北京科技大学 | Microwave assisted hydrothermal process for synthesizing nano-SnO2-MWCNTs |
| CN101704504A (en) * | 2009-12-03 | 2010-05-12 | 中国科学院宁波材料技术与工程研究所 | In-situ synthesis method for nano tin dioxide/carbon nano tube composite material |
-
2010
- 2010-12-31 CN CN2010106158190A patent/CN102093890A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005094231A2 (en) * | 2004-03-19 | 2005-10-13 | The Regents Of The University Of California | Methods for fabrication of positional and compositionally controlled nanostructures on substrate |
| CN101439855A (en) * | 2008-12-24 | 2009-05-27 | 北京科技大学 | Microwave assisted hydrothermal process for synthesizing nano-SnO2-MWCNTs |
| CN101704504A (en) * | 2009-12-03 | 2010-05-12 | 中国科学院宁波材料技术与工程研究所 | In-situ synthesis method for nano tin dioxide/carbon nano tube composite material |
Non-Patent Citations (2)
| Title |
|---|
| NGUYEN VAN HIEU等: "Gas-sensing properties of tin oxide doped with metal oxides and carbonnanotubes: A competitive sensor for ethanol and liquid petroleum gas", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
| YONG JIA等: "Preparation of Porous Tin Oxide Nanotubes Using Carbon Nanotubes as Templates and Their Gas-Sensing Properties", 《J. PHYS. CHEM. C》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106505188A (en) * | 2015-09-06 | 2017-03-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tinbase nano-particle-carbon composite and preparation method and application |
| CN106505188B (en) * | 2015-09-06 | 2019-10-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Tinbase nano particle-carbon composite and the preparation method and application thereof |
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Application publication date: 20110615 |