CN108204964A - A kind of quantum yield measuring method - Google Patents

A kind of quantum yield measuring method Download PDF

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CN108204964A
CN108204964A CN201810302648.2A CN201810302648A CN108204964A CN 108204964 A CN108204964 A CN 108204964A CN 201810302648 A CN201810302648 A CN 201810302648A CN 108204964 A CN108204964 A CN 108204964A
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程桂平
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6428Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material

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Abstract

A kind of quantum yield measuring method, including:Step 1:0.5 mL ammonium hydroxide and 2 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, is stirred 24 hours in 30 DEG C of reactions;Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 gram 3(Three ethoxy silylation)Propylsuccinic anhydride stirs 24 hours in 30 DEG C of reactions.

Description

A kind of quantum yield measuring method
Technical field
The present invention relates to a kind of quantum yield measuring methods.
Background technology
Quantum yield refers to the utilization rate of light quantum in photochemical reaction.
One photochemically reactive quantum yield can be defined as the molecule of reactant caused by one quantum of every absorption Number, for this is usually for specific wavelength, i.e., quantum yield=(Generate the molecular number of product)/(The quantum number of absorption).
To carbon doped silicon dioxide powder, there are no targetedly quantum yield test modes in the prior art.
Invention content
A kind of quantum yield measuring method, including:
Step 1:0.5 mL ammonium hydroxide and 2 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, in 30 DEG C of reaction stirrings 24 Hour;
Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;
Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 grams of 3-(Three ethoxy silylation)Propylsuccinic anhydride, 30 DEG C reaction stirring 24 hours;
Step 4:With alcohol washes 3 times;
Step 5:Gained powder is heat-treated, 400 DEG C is heated to the rate of heat addition of 2 DEG C/min, obtains flaxen carbon Doping silicon dioxide powder;
Step 6:Quantum yield, formula 1 are calculated according to formula 1:
Wherein Φ is quantum yield, and I is the overall emission intensity measured, and n is refraction coefficient, alcohol 1.36, and A is that optics is strong Degree, and subscript r refers to the reference fluorogen of known quantum yield.
The powder of the present invention is used as fluorescent material.
Inventive point is:1)Complete reaction process;2)Material used;3)Concrete component.
Specific embodiment
Embodiment 1
A kind of method for preparing carbon doped silicon dioxide powder, including:
Step 1:0.5 mL ammonium hydroxide and 2 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, in 30 DEG C of reaction stirrings 24 Hour;
Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;
Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 grams of 3-(Three ethoxy silylation)Propylsuccinic anhydride, 30 DEG C reaction stirring 24 hours;
Step 4:With alcohol washes 3 times;
Step 5:Gained powder is heat-treated, 400 DEG C is heated to the rate of heat addition of 2 DEG C/min, obtains flaxen carbon Doping silicon dioxide powder;
Step 6:Quantum yield, formula 1 are calculated according to formula 1:
Wherein Φ is quantum yield, and I is the overall emission intensity measured, and n is refraction coefficient, alcohol 1.36, and A is that optics is strong Degree, and subscript r refers to the reference fluorogen of known quantum yield.
The powder of the present invention is used as fluorescent material.
Embodiment 2
A kind of method for preparing carbon doped silicon dioxide powder, including:
Step 1:0.5 mL ammonium hydroxide and 2.1 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, in 30 DEG C of reaction stirrings 24 hours;
Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;
Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 grams of 3-(Three ethoxy silylation)Propylsuccinic anhydride, 30 DEG C reaction stirring 24 hours;
Step 4:With alcohol washes 3 times;
Step 5:Gained powder is heat-treated, 400 DEG C is heated to the rate of heat addition of 2 DEG C/min, obtains flaxen carbon Doping silicon dioxide powder;
Step 6:Quantum yield, formula 1 are calculated according to formula 1:
Wherein Φ is quantum yield, and I is the overall emission intensity measured, and n is refraction coefficient, alcohol 1.36, and A is that optics is strong Degree, and subscript r refers to the reference fluorogen of known quantum yield.
The powder of the present invention is used as fluorescent material.
Embodiment 3
A kind of method for preparing carbon doped silicon dioxide powder, including:
Step 1:0.5 mL ammonium hydroxide and 2.2 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, in 30 DEG C of reaction stirrings 24 hours;
Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;
Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 grams of 3-(Three ethoxy silylation)Propylsuccinic anhydride, 30 DEG C reaction stirring 24 hours;
Step 4:With alcohol washes 3 times;
Step 5:Gained powder is heat-treated, 400 DEG C is heated to the rate of heat addition of 2 DEG C/min, obtains flaxen carbon Doping silicon dioxide powder;
Step 6:Quantum yield, formula 1 are calculated according to formula 1:
Wherein Φ is quantum yield, and I is the overall emission intensity measured, and n is refraction coefficient, alcohol 1.36, and A is that optics is strong Degree, and subscript r refers to the reference fluorogen of known quantum yield.
The powder of the present invention is used as fluorescent material.
Embodiment 4
A kind of method for preparing carbon doped silicon dioxide powder, including:
Step 1:0.5 mL ammonium hydroxide and 2.3 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, in 30 DEG C of reaction stirrings 24 hours;
Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;
Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 grams of 3-(Three ethoxy silylation)Propylsuccinic anhydride, 30 DEG C reaction stirring 24 hours;
Step 4:With alcohol washes 3 times;
Step 5:Gained powder is heat-treated, 400 DEG C is heated to the rate of heat addition of 2 DEG C/min, obtains flaxen carbon Doping silicon dioxide powder;
Step 6:Quantum yield, formula 1 are calculated according to formula 1:
Wherein Φ is quantum yield, and I is the overall emission intensity measured, and n is refraction coefficient, alcohol 1.36, and A is that optics is strong Degree, and subscript r refers to the reference fluorogen of known quantum yield.
The powder of the present invention is used as fluorescent material.
Implement 5
A kind of method for preparing carbon doped silicon dioxide powder, including:
Step 1:0.5 mL ammonium hydroxide and 2.4 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, in 30 DEG C of reaction stirrings 24 hours;
Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;
Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 grams of 3-(Three ethoxy silylation)Propylsuccinic anhydride, 30 DEG C reaction stirring 24 hours;
Step 4:With alcohol washes 3 times;
Step 5:Gained powder is heat-treated, 400 DEG C is heated to the rate of heat addition of 2 DEG C/min, obtains flaxen carbon Doping silicon dioxide powder;
Step 6:Quantum yield, formula 1 are calculated according to formula 1:
Wherein Φ is quantum yield, and I is the overall emission intensity measured, and n is refraction coefficient, alcohol 1.36, and A is that optics is strong Degree, and subscript r refers to the reference fluorogen of known quantum yield.
The powder of the present invention is used as fluorescent material.

Claims (2)

1. a kind of quantum yield measuring method, including:
Step 1:0.5 mL ammonium hydroxide and 2 grams of tetraethyl orthosilicates are added in 20 mL isopropanol solvents, in 30 DEG C of reaction stirrings 24 Hour;
Step 2:3 gram of four fourth oxosilane and 2ml normal propyl alcohols are added in, is stirred 12 hours in 50 DEG C of reactions;
Step 3:Add in 1 gram of aminopropyltriethoxywerene werene and 3 grams of 3-(Three ethoxy silylation)Propylsuccinic anhydride, 30 DEG C reaction stirring 24 hours;
Step 4:With alcohol washes 3 times;
Step 5:Gained powder is heat-treated, 400 DEG C is heated to the rate of heat addition of 2 DEG C/min, obtains flaxen carbon Doping silicon dioxide powder;
Step 6:Quantum yield, formula 1 are calculated according to formula 1:
Wherein Φ is quantum yield, and I is the overall emission intensity measured, and n is refraction coefficient, alcohol 1.36, and A is that optics is strong Degree, and subscript r refers to the reference fluorogen of known quantum yield.
2. the powder of the present invention is used as fluorescent material.
CN201810302648.2A 2018-04-05 2018-04-05 A kind of quantum yield measuring method Withdrawn CN108204964A (en)

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CN108204964A true CN108204964A (en) 2018-06-26

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