CN107121454B - A kind of difference element doping graphene quantum dot is respectively with molecular engram compound gas sensitive and the preparation method and application thereof - Google Patents
A kind of difference element doping graphene quantum dot is respectively with molecular engram compound gas sensitive and the preparation method and application thereof Download PDFInfo
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- CN107121454B CN107121454B CN201710247622.8A CN201710247622A CN107121454B CN 107121454 B CN107121454 B CN 107121454B CN 201710247622 A CN201710247622 A CN 201710247622A CN 107121454 B CN107121454 B CN 107121454B
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Abstract
The invention discloses a kind of different element doping graphene quantum dots respectively with molecular engram compound gas sensitive and the preparation method and application thereof.The different element doping graphene quantum dots include respectively raw material B-GQDs, N-GQDs, S-GQDs, Cl-GQDs, MIALFO through being prepared with molecular engram compound gas sensitive, and wherein B-GQDs and MIALFO material quality ratio is (0.005~0.05): 1；N-GQDs and MIALFO material quality ratio is (0.01~0.05): 1；S-GQDs and MIALFO material quality ratio is (0.005~0.05): 1；Cl-GQDs and MIALFO material quality ratio is (0.005~0.03): 1.Preparation method has mixed solution, microwave reaction, ultrasonic vibration, drying, grinding and sintering.The application in formaldehyde, acetone, benzene and methanol gas sensor or air-sensitive tester is being prepared using for compound gas sensitive.The present invention is based on provided raw materials and proportion to provide a kind of method for preparing different element doping GQDs respectively with MIALFO compound gas sensitive, obtains a kind of gas sensor that can be worked at a lower temperature.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of element doping graphene quantum dot respectively with molecular engram
Compound gas sensitive and the preparation method and application thereof.
Background technique
In recent years, with the rapid development of our country's economy, especially improvement of living standard, and thus in bring room
The high speed development of decorations industry, the pollution caused by building materials, decorations have become indoor environmental pollution it is main Lai
Source.In addition for energy conservation, building structure usually has good sealing function, more exacerbates the deterioration of indoor air quality.Mesh
In the pollution greatly of preceding indoor formaldehyde, benzene and benzene homologues, ammonia and radioactivity four, harm is maximum, be most difficult to radical cure is formaldehyde pollution and benzene
Pollution.Secondly there is also some volatile organic matters being harmful to the human body for the room air of some laboratories and factory.Acetone and
Methanol is the common two kinds of solvents in laboratory, and acetone is still used to clean effective detergent of some glass apparatus, in laboratory
It can be widely used with some factories.However acetone and methanol are harmful, hematological system and mind of the methanol to human body to human body
Harmful through system, new researches show that it is also harmful to optic nerve and retina；And acetone is mainly Central nervous system
System has inhibition, anesthetic effect, and high concentration contact may have damage to liver, kidney and pancreas.The detection of acetone can also be applied to
To determine whether the people suffers from diabetes in the detection of the exhaled gas of people.The temperature of conductor oxidate gas sensor work at present
It spends higher, is 200-400 DEG C, operating temperature high in this way has made when making devices manufacture craft complicated and needed very
High energy consumption and cost, is unfavorable for practical application.Therefore, develop it is a kind of maintain high sensitivity and selectivity, while can be
The gas sensor even to work at room temperature under lower temperature is very important.
Summary of the invention
The first object of the present invention be to provide a kind of different element doping graphene quantum dots (GQDs) respectively with molecule
Trace Ag-LaFeO3(molecular imprinted Ag-LaFeO3, MIALFO) and compound gas sensitive；Second purpose is
There is provided the different element doping graphene quantum dots (GQDs) respectively with molecular engram Ag-LaFeO3(molecular
imprinted Ag-LaFeO3, MIALFO) compound gas sensitive preparation method；Third be designed to provide it is described not
With element doping graphene quantum dot (GQDs) respectively with molecular engram Ag-LaFeO3(molecular imprinted Ag-
LaFeO3, MIALFO) compound gas sensitive application.
The first object of the present invention be achieved in that the different element doping graphene quantum dot GQDs respectively with
Molecular engram Ag-LaFeO3(molecular imprinted Ag-LaFeO3, MIALFO) and compound gas sensitive includes raw material
Boron doping graphene quantum dot (B-GQDs), nitrogen-doped graphene quantum dot (N-GQDs), sulfur doping graphene quantum dot (S-
GQDs), chlorine doped graphene quantum dot (Cl-GQDs), MIALFO be through being prepared, wherein B-GQDs and MIALFO material quality
Than for (0.005 ~ 0.05): 1；N-GQDs and MIALFO material quality ratio is (0.01 ~ 0.05): 1；S-GQDs and MIALFO raw material
Mass ratio is (0.005 ~ 0.05): 1；Cl-GQDs and MIALFO material quality ratio is (0.005 ~ 0.03): 1.
The second object of the present invention be achieved in that the following steps are included:
A, by the B-GQDs of formulation ratio and MIALFO；N-GQDs and MIALFO；S-GQDs and MIALFO；Cl-GQDs and
MIALFO is added 10-100mL deionized water after mixing respectively and obtains mixture a；
B, mixture a is ultrasonically treated under 70-250w power 30-90min, stirs 6- on magnetic stirring apparatus later
48h is mixed them thoroughly；
C, the mixture a after being sufficiently mixed is imported in microwave synthesizer in the case where pressure is normal pressure, and temperature is at 50-90 DEG C
React 2-8h；
D, mixture a drying to moisture content is obtained into object for 2 ~ 15%.
The third object of the present invention be achieved in that the different element doping graphene quantum dots respectively with molecule
Trace compound gas sensitive is preparing the application in formaldehyde, acetone, benzene and methanol gas sensor or air-sensitive tester.
In numerous metal-oxide semiconductor (MOS)s, perovskite ABO3Type LaFeO3Good conductivity, thermal stability are good, prepare
Simply, it is considered as a kind of potential gas sensitive that preparation cost is low, uses Ag+The La of replacement A is adulterated to it3+After can be into one
Step reduces the resistance of material, and the vacancy for adulterating introducing is also that certain space has been vacateed in adsorbed gas, is conducive to mentioning for air-sensitive performance
It is high.Reported in literature shows, LaFeO3Air-sensitive performance compared with ZnO, SnO2、In2O3Good more of equal single oxides.Therefore the present invention selects
Use Ag-LaFeO3(ALFO) this ideal gas sensitive is further modified, using molecular imprinting technology to its selectivity
It is adjusted, obtains formaldehyde, acetone, benzene and the methanol gas sensitive (hereinafter referred to as MIALFO) based on ALFO.
GQDs is that three dimensions are all that nanoscale 0 ties up material, the high electron mobility of graphene is inherited, due to its ruler
It is very little in 20nm hereinafter, energy band is opened, be a kind of novel semiconductor material.Also it is provided with quantum confined effect and edge effect
It answers, is easy the upper different functional group of grafting on it, becomes a kind of outstanding gas sensitive.The present invention is using outermost layer electricity
The GQDs for the element (B, N, S, Cl) pair that subnumber successively increases is doped, to obtain the different doping GQDs of semiconductor property,
And the MIALFO of synthesis early period is modified respectively with these doping GQDs, obtain the doping with different semiconductor properties
Influence of the GQDs to the electric property and air-sensitive performance of MIALFO, and obtained the increasing with doped chemical outermost electron number
Add, the rule that these influences follow.
After outermost electron number is doped GQDs less than the B element of carbon group element, obtained B-GQDs is p-type doping
GQDs, otherwise obtained N-GQDs, S-GQDs and Cl-GQDs are the GQDs of n-type doping after other three kinds of element doping GQDs.
MIALFO is a kind of typical p-type semiconductor in air, above-mentioned four kinds of doping GQDs obtained after being modified to MIALFO with
Draw a conclusion: B-GQDs-MIALFO resistance reduces, N-GQDs-MIALFO, S-GQDs-MIALFO and Cl-GQDs-MIALFO resistance
Increase, and its resistance has such rule: N-GQDs-MIALFO < S-GQDs-MIALFO < Cl-GQDs-MIALFO.Reason
It is two kinds of materials energy under the premise of two kinds of semiconductors cannot form p-n junction, with semiconductor property of the same race because collaboration is made
With reducing the resistance of system, and then reduce the operating temperature of gas sensor made from the material.Similarly, for some n
Semiconductor gas sensors the material such as ZnO, SnO of type2、In2O3GQDs Deng then optional n-type doping further decreases resistance to be modified.
The present invention is to provide the raw material and proportion of preparation doping GQDs and MIALFO compound first, and based on provided
Raw material and proportion provide a kind of method for preparing doping GQDs and MIALFO compound gas sensitive, and provide a kind of with difference
Semiconductor property adulterates GQDs to the affecting laws of current oxide semiconductor gas sensitive resistance, so that obtaining can subtract
Method of the low gas sensitive resistance to reduce operating temperature.
The sensor of doping GQDs and MIALFO compound gas sensitive preparation provided by the invention has following positive effect
Fruit:
(1) operating temperature is low: after B-GQDs and MIALFO are compound, made device operating temperature can be reduced to 55 DEG C.
(2) sensitivity of PARA FORMALDEHYDE PRILLS(91,95) gas is higher: by the MIALFO gas sensitive with B-GQDs after compound, can detect that
Low concentration formaldehyde, acetone, benzene and the methanol gas of 0.1ppm.
(3) selectivity is good: B-GQDs-MIALFO gas sensitive is to formaldehyde under same concentrations, acetone, benzene and methanol gas
Sensitivity is much higher than the sensitivity to toluene or gasoline or water or ammonium hydroxide.
(4) the response-recovery time is fast: B-GQDs-MIALFO gas sensitive, PARA FORMALDEHYDE PRILLS(91,95), acetone, benzene and methanol gas sound
Answer-recovery time is below 1 minute, it is suitble to quickly examine the above pernicious gas.
To sum up, the sensibility of MIALFO gas sensitive PARA FORMALDEHYDE PRILLS(91,95) gas of the present invention by B-GQDs after compound, especially
Operating temperature and sensitivity are all higher than the technical level of currently known sensor, and have raising by a relatively large margin, can directly use
It makes formaldehyde, acetone, benzene and methanol gas sensor.
Detailed description of the invention
Fig. 1 be the present invention prepared by B-GQDs, GQDs, N-GQDs, S-GQDs and Cl-GQDs respectively with MIALFO- first
After aldehyde gas sensitive is compound, PARA FORMALDEHYDE PRILLS(91,95), toluene, the sensitivity of the gases such as ammonium hydroxide；
X-axis is gaseous species in figure, and y-axis is gas sensitive type, and z-axis is sensitivity；
Fig. 2 is sensitivity of the prepared B-GQDs-MIALFO- formaldehyde gas sensitive material to various concentration formaldehyde；
Abscissa is the time in figure, and unit s, ordinate is sensitivity；
Fig. 3 is 5 loop tests of the prepared B-GQDs-MIALFO- formaldehyde gas sensitive material to 10ppm formaldehyde；
Abscissa is the time in figure, and unit s, ordinate is sensitivity；As can be seen from the figure the device is stablized very well,
5 times test result is almost consistent.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is further illustrated, but is not subject in any way to the present invention
Limitation, based on present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
Difference element doping graphene quantum dot GQDs of the present invention respectively with molecular engram Ag-LaFeO3
(molecular imprinted Ag-LaFeO3, MIALFO) and compound gas sensitive includes raw material boron doping graphene quantum
Point (B-GQDs), nitrogen-doped graphene quantum dot (N-GQDs), sulfur doping graphene quantum dot (S-GQDs), chlorine doped graphene
Quantum dot (Cl-GQDs), MIALFO are through being prepared, and wherein B-GQDs and MIALFO material quality ratio is (0.005 ~ 0.05):
1；N-GQDs and MIALFO material quality ratio is (0.01 ~ 0.05): 1；S-GQDs and MIALFO material quality ratio be (0.005 ~
0.05): 1；Cl-GQDs and MIALFO material quality ratio is (0.005 ~ 0.03): 1.
The outermost electron number of the element of the doped graphene quantum dot GQDs is 3,5,6,7, is sequentially increased.
The element of the doping GQDs is boron, nitrogen, sulphur, chlorine.
The different element doping graphene quantum dot GQDs include simultaneously p-type doping and n-type doping.
The different element doping graphene quantum dots electric property with molecular engram compound gas sensitive respectively
With air-sensitive performance in regularity variation.
The difference element doping graphene quantum dot of the present invention system with molecular engram compound gas sensitive respectively
Preparation Method, comprising the following steps:
A, by the B-GQDs of formulation ratio and MIALFO；N-GQDs and MIALFO；S-GQDs and MIALFO；Cl-GQDs and
MIALFO is added 10-100mL deionized water after mixing respectively and obtains mixture a；
B, mixture a is ultrasonically treated under 70-250w power 30-90min, stirs 6- on magnetic stirring apparatus later
48h is mixed them thoroughly；
C, the mixture a after being sufficiently mixed is imported in microwave synthesizer in the case where pressure is normal pressure, and temperature is at 50-90 DEG C
React 2-8h；
D, mixture a drying to moisture content is obtained into object for 2 ~ 15%.
Difference element doping graphene quantum dot of the present invention is answered with molecular engram compound gas sensitive respectively
Formaldehyde, third are being prepared with molecular engram compound gas sensitive respectively with for the different element doping graphene quantum dots
Application in ketone, benzene and methanol gas sensor or air-sensitive tester.
Case is embodied, the present invention will be further described below:
Embodiment 1
Material composition is B-GQDs, MIALFO- formaldehyde gas sensitive material, and the corresponding mass ratio of the material composition is 0.01:1.
Weigh the B-GQDs 0.01g and MIALFO- formaldehyde gas sensitive material 1g prepared be added after mixing 30mL go from
Sub- water obtains mixture a；Mixture a is ultrasonically treated 50min under 150w power, is stirred for 24 hours on magnetic stirring apparatus later
It mixes them thoroughly；Mixture a after being sufficiently mixed is imported in microwave synthesizer in the case where pressure is normal pressure, and temperature is at 80 DEG C
4 h are reacted, it is dry to obtain object to moisture content for 10%.
Embodiment 2
Material composition is N-GQDs, MIALFO- benzene gas sensitive, and the corresponding mass ratio of the material composition is 0.015:1.
Weigh the N-GQDs 0.015g and MIALFO- benzene gas sensitive 1g prepared be added after mixing 25mL go from
Sub- water obtains mixture a；Mixture a is ultrasonically treated 60min under 120w power, stirs 30h on magnetic stirring apparatus later
It mixes them thoroughly；Mixture a after being sufficiently mixed is imported in microwave synthesizer in the case where pressure is normal pressure, and temperature is at 75 DEG C
5h is reacted, it is dry to obtain object to moisture content for 12%.
Embodiment 3
Material composition is S-GQDs, MIALFO- acetone air-sensitive material, and the corresponding mass ratio of the material composition is 0.02:1.
Weigh the S-GQDs 0.02g and MIALFO- acetone air-sensitive material 1g prepared be added after mixing 40mL go from
Sub- water obtains mixture a；Mixture a is ultrasonically treated 80min under 200w power, stirs 36h on magnetic stirring apparatus later
It mixes them thoroughly；Mixture a after being sufficiently mixed is imported in microwave synthesizer in the case where pressure is normal pressure, and temperature is at 60 DEG C
2h is reacted, it is dry to obtain object to moisture content for 8%.
Embodiment 4
Material composition is Cl-GQDs, MIALFO- methanol gas sensitive, and the corresponding mass ratio of the material composition is 0.008:
1。
It weighs the Cl-GQDs 0.008g and MIALFO- methanol gas sensitive 1g prepared and 20mL is added after mixing
Ionized water obtains mixture a；Mixture a is ultrasonically treated 90min under 100w power, is stirred on magnetic stirring apparatus later
48h is mixed them thoroughly；Mixture a after being sufficiently mixed is imported in microwave synthesizer in the case where pressure is normal pressure, temperature 40
7h is reacted at DEG C, it is dry to obtain object to moisture content for 5%.
Claims (3)
1. a kind of element doping graphene quantum dot and molecular engram Ag-LaFeO3Compound gas sensitive, it is characterised in that described
Element doping graphene quantum dot is boron doping graphene quantum dot B-GQDs, nitrogen-doped graphene quantum dot N-GQDs, sulphur are mixed
Miscellaneous graphene quantum dot S-GQDs or chlorine doped graphene quantum dot Cl-GQDs；B-GQDs and molecular engram Ag-LaFeO3Raw material
Mass ratio is (0.005 ~ 0.05): 1, N-GQDs and molecular engram Ag-LaFeO3Material quality ratio is (0.01 ~ 0.05): 1, S-
GQDs and molecular engram Ag-LaFeO3Material quality ratio is (0.005 ~ 0.05): 1, Cl-GQDs and molecular engram Ag-LaFeO3It is former
Expect that mass ratio is (0.005 ~ 0.03): 1.
2. element doping graphene quantum dot described in a kind of claim 1 and molecular engram Ag-LaFeO3Compound gas sensitive
Preparation method, it is characterised in that the following steps are included:
A, by the element doping graphene quantum dot of formulation ratio and molecular engram Ag-LaFeO3Raw material is uniformly mixed, and is then added
10-100mL deionized water obtains mixture a；
B, mixture a is ultrasonically treated 30-90min under 70-250W power, 6-48h is stirred on magnetic stirring apparatus later makes
It is sufficiently mixed；
C, the mixture a after being sufficiently mixed, which is imported in microwave synthesizer, reacts 2-8h at normal pressure, 50-90 DEG C；
D, step C reactants dry to moisture content is obtained into object for 2 ~ 15%.
3. element doping graphene quantum dot described in a kind of claim 1 and molecular engram Ag-LaFeO3Compound gas sensitive exists
Prepare the application in formaldehyde, acetone, benzene, methanol gas sensor or air-sensitive tester.
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| CN110736770B (en) * | 2019-10-16 | 2022-04-19 | 郑州大学 | N-GQDs modified 3DOM In2O3Composite material and preparation method and application thereof |
| CN112680210A (en) | 2019-10-17 | 2021-04-20 | 三星电子株式会社 | Core-shell quantum dot, method for manufacturing same, quantum dot composite including same, quantum dot composition, display device, and electronic device |
| KR20210045948A (en) | 2019-10-17 | 2021-04-27 | 삼성전자주식회사 | Core shell quantum dot, production method thereof electronic device including the same |
| CN110887875A (en) * | 2019-11-25 | 2020-03-17 | 陕西科技大学 | Preparation method of sensitive material with specificity to formaldehyde gas |
| CN113189064B (en) * | 2021-04-22 | 2022-12-09 | 西安交通大学 | Glycopeptide-based fluorescent molecularly imprinted polymer, preparation method and application in screening and detecting glycoprotein |
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