CN109455706A - A kind of preparation method of sulfonated graphene load indium oxide gas sensitive - Google Patents
A kind of preparation method of sulfonated graphene load indium oxide gas sensitive Download PDFInfo
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- CN109455706A CN109455706A CN201811527036.XA CN201811527036A CN109455706A CN 109455706 A CN109455706 A CN 109455706A CN 201811527036 A CN201811527036 A CN 201811527036A CN 109455706 A CN109455706 A CN 109455706A
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention belongs to gas sensitive material technical fields, and in particular to a kind of preparation method of sulfonated graphene load indium oxide gas sensitive；Sulfonated graphene loads in the preparation process of indium oxide gas sensitive, it is sequentially prepared graphene oxide, redox graphene, sulfonated graphene, sulfonated graphene load indium oxide, manufacturing cost of the present invention is cheap, during preparing sulfonated graphene load indium oxide, generation is not polluted, in the sulfonated graphene load indium oxide gas sensitive being prepared, sulfonated graphene cooperates with mutually with indium oxide, possess preferable synergy, substantially increases the air-sensitive performance of gas sensitive.
Description
Technical field
The invention belongs to gas sensitive material technical fields, and in particular to a kind of sulfonated graphene load indium oxide air-sensitive material
The preparation method of material.
Background technique
In recent years, with the rapid emergence of China city automobile consumption market, environmental problem caused by emission of nitrogen oxide
It becomes increasingly conspicuous, nitrogen dioxide is not only to cause one of major pollutants of environmental problems such as acid rain, smog, and has to respiratory tract
Strong impulse effect, seriously threatens the health of citizen, therefore, carries out spirit to the content of nitrogen dioxide in living environment
Quick, accurate measurements are very necessary.
For indium oxide due to its lesser resistivity and higher catalytic activity, conductivity is very sensitive to external environment,
Be suitable as highly sensitive gas sensor, indium oxide as the principle of gas sensor be tested gas absorption and surface it is anti-
The variation for answering conductivity caused by process can measure the air-sensitive performance of material, due to being related to adsorbing by detecting electrical signal
The specific surface area reacted with surface, therefore increase gas sensitive is to improve an important channel of gas sensitive air-sensitive performance.
Graphene possesses biggish specific surface area, however single graphene is easy to appear due to the presence of Van der Waals force
The phenomenon that stacking, and graphene surface is not easy to metal oxide-loaded, in loading process, is easy to appear showing for reunion
As, and graphene usually contacted with the metal oxide of load it is bad, to influence the air-sensitive performance of gas sensitive.
Summary of the invention
It is an object of the invention to: a kind of preparation method of sulfonated graphene load indium oxide gas sensitive, this hair are provided
It is bright to load indium oxide gas sensitive by preparing sulfonated graphene, indium oxide is uniformly entrained in and possesses large specific surface area
Sulfonated graphene surface helps to improve the air-sensitive performance of gas sensitive.
A kind of preparation method of sulfonated graphene load indium oxide gas sensitive, includes the following steps:
The preparation of S1, graphene oxide: graphite, sodium nitrate, the concentrated sulfuric acid are persistently stirred under constant temperature conditions, thermostat temperature 1-
5 DEG C, mixing speed 800r/min, under conditions of temperature-resistant, mixing speed is constant, be added potassium permanganate, wherein graphite,
Sodium nitrate, potassium permanganate mass ratio be 4:3:12, the solid-to-liquid ratio of graphite and the concentrated sulfuric acid is 1g:50mL, and the concentration of the concentrated sulfuric acid is
98%, it is stirred to react 2-3h, then under the conditions of constant speed, is warming up to 40-45 DEG C, persistently stirs 2-3h, deionized water is added
And hydrogen peroxide, centrifuge separation, centrifugal rotational speed 12000-15000r/min, centrifugation time 10-20min, deionized water cleaning
It is 7 to PH, ultrasonic treatment, supersonic frequency 100-150W, ultrasonic time 10-20min are centrifugated after ultrasonic, most pass through afterwards
Vacuum drying is crossed, graphene oxide is prepared；
The preparation of S2, redox graphene: dispersing the step S1 graphene oxide being prepared in deionized water, is added dropwise
Sodium borohydride solution, isothermal reaction, reaction temperature 85- is added until dispersion liquid PH is 9 in the sodium carbonate liquor that concentration is 10%
90 DEG C, reaction time 2-3h, redox graphene is prepared by being centrifugated, washing；
The preparation of S3, sulfonated graphene: p-aminobenzene sulfonic acid and sodium nitrite are added in hydrochloric acid solution, low-temp reaction, instead
Answering temperature is 0-10 DEG C, and diazonium salt is prepared, will be added to the redox graphene that step S2 is prepared to diazonium salt
In dispersion liquid, ice bath reacts 3h, and centrifuge separation, washing are scattered in deionized water, hydrazine hydrate, deionized water and water are added
Hydrazine volume ratio 1:2.5, isothermal reaction are closed, the isothermal reaction time is 25-30h, and isothermal reaction temperature is 90-95 DEG C, has been reacted
Cheng Hou, is added dropwise the sodium carbonate liquor that concentration is 10%, and sodium carbonate liquor and hydrazine hydrate volume ratio are 1:20, centrifuge separation, washing
Sulfonated graphene is prepared；
The preparation of S4, sulfonated graphene load indium oxide: deionized water is dispersed by the step S3 sulfonated graphene being prepared
In, sulfonated graphene and deionized water solid-to-liquid ratio are 5g:1L, and indium nitrate and carbamide, sulfonated graphene, indium nitrate, carbon is added
Amide mass ratio is 2:1:1, and boric acid sodium water solution and ethylenediamine are added in whipping process for uniform stirring, and wherein Boratex is water-soluble
Liquid concentration is 7-10%, and boric acid sodium water solution, ethylenediamine, deionized water volume ratio are 6:7:150, and hydro-thermal reaction, reaction temperature is
It 130-150 DEG C, reaction time 9-12h, after the reaction was completed, is sufficiently washed with dehydrated alcohol and deionized water, at 35-40 DEG C
It is dried, after the completion of dry, is placed under the conditions of helium, sintering processes, sintering temperature is 400-450 DEG C, when sintering
Between be 1-1.5h, be prepared sulfonated graphene load indium oxide.
Preferably, the hydrogen peroxide concentration of addition described in step S1 is 25-28%, the volume and dense sulphur that hydrogen peroxide is added
Acid, deionized water volume ratio are 20:1:10, and by addition hydrogen peroxide, remaining manganese dioxide and potassium permanganate are reduced to sulphur
Sour manganese.
Preferably, centrifugal rotational speed is first adjusted to 3000-3500r/ in centrifugal separation processes after ultrasound described in step S1
Min handles 4min, then centrifugal rotational speed is adjusted to 6000-6500r/min processing 10min, is first removed with low-speed centrifugal relatively large
Particulate matter, small pieces and the separation of large stretch of graphene oxide are obtained by large stretch of graphene oxide by high speed centrifugation later.
Preferably, sodium borohydride solution mass concentration described in step S2 is 30g/L, the sodium borohydride solution body of addition
Long-pending and deionized water volume ratio is 1:3-5, prereduction is carried out to graphene oxide by the way that sodium borohydride is added, to remove graphite
A large amount of oxygen-containing groups on alkene lamella.
Preferably, during preparing diazonium salt in step S3, p-aminobenzene sulfonic acid, sodium nitrite, hydrochloric acid molar ratio be
1:1.5:3-4, the excessive effect of hydrochloric acid are dissolution p-aminobenzene sulfonic acid, generation nitrous acid, the highly acid for maintaining medium in reaction.
Beneficial effect
(1) present invention is further to its to hydrazine hydrate is added after redox graphene progress carbonization treatment using diazonium salt
Reduction, further removes and remains remaining oxygen-containing group on its lamella, and finally obtains sulfonic acid group functionalization graphene, preparation
Obtained sulfonated graphene surface is smooth, is in partially pleated structure, between layers without agglomeration.
(2) sulfonic group on sulfonated graphene is a kind of drawing electron group, and graphene can be made to become further hole and mixed
It is miscellaneous, the doping level of graphene is improved, the sulfonated graphene for possessing better dispersion performance, and being prepared possesses higher
Specific surface area, more conducively indium oxide is uniformly entrained in sulfonated graphene surface, and the Uniform Doped of simultaneous oxidation indium can have
The phenomenon that effect prevents graphene from stacking reunion occurs.
(3) sulfonated graphene that the present invention is prepared possesses biggish specific surface area, can provide a large amount of active site,
Help to adsorb more gas molecules, n-type semiconductor indium oxide is loaded by p-type semiconductor sulfonated graphene, it is different to form P-N
Matter contact, substantially increases composite material to the response sensitivity of nitrogen dioxide.
(4) manufacturing cost of the present invention is cheap, during preparing sulfonated graphene load indium oxide, does not pollute generation,
In the sulfonated graphene load indium oxide gas sensitive being prepared, sulfonated graphene cooperates with mutually with indium oxide, possesses preferably
Synergy.
Detailed description of the invention
A, b are respectively graphene oxide TEM figure, the SEM figure that step S1 is prepared in Fig. 1；
Fig. 2 is the sulfonated graphene XPS figure that step S3 is prepared；
Fig. 3 is the sulfonated graphene SEM figure that step S3 is prepared；
Fig. 4 is that the sulfonated graphene that step S4 is prepared loads indium oxide TEM figure；
A, b, c respectively correspond the sulfonated graphene load indium oxide that embodiment 1, embodiment 2, embodiment 3 are prepared in Fig. 5
Gas sensitive sensitivity characteristic curve graph measured in the nitrogen dioxide gas atmosphere that concentration is 15ppm；
Fig. 6 is that the sulfonated graphene that embodiment 2 is prepared loads indium oxide gas sensitive in the titanium dioxide nitrogen of various concentration
Measured sensitivity characteristic curve graph in body atmosphere；
Fig. 7 is the reperformance test curve for applying the sulfonated graphene load indium oxide gas sensitive that example 2 is prepared.
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated；It should be understood that these embodiments are merely to illustrate the present invention
Rather than the claimed range of the limitation present invention；It will further be understood that read the content lectured of the present invention it
Afterwards, those skilled in the art can make various changes or modification to the present invention, and such equivalent forms are equally fallen within appended by the application
Claims limited range.
Embodiment 1-3
A kind of preparation method of sulfonated graphene load indium oxide gas sensitive, includes the following steps:
The preparation of S1, graphene oxide: graphite, sodium nitrate, the concentrated sulfuric acid are persistently stirred under constant temperature conditions, it is temperature-resistant,
Under conditions of mixing speed is constant, be added potassium permanganate, wherein graphite, sodium nitrate, potassium permanganate mass ratio be 4:3:12, stone
The solid-to-liquid ratio of ink and the concentrated sulfuric acid is 1g:50mL, and the concentration of the concentrated sulfuric acid is 98%, is stirred to react, then under the conditions of constant speed, by it
It heats up and continues to stir, deionized water and hydrogen peroxide is added, the volume that hydrogen peroxide is added is with the concentrated sulfuric acid, deionized water volume ratio
20:1:10, centrifuge separation, it is 7 that deionized water, which is cleaned to PH, ultrasonic treatment, is centrifugated after ultrasound, finally dry by vacuum
It is dry, graphene oxide is prepared；
The preparation of S2, redox graphene: dispersing the step S1 graphene oxide being prepared in deionized water, is added dropwise
The sodium carbonate liquor that concentration is 10%, until dispersion liquid PH is 9, addition sodium borohydride solution, isothermal reaction, by being centrifugated,
Redox graphene is prepared in washing；
The preparation of S3, sulfonated graphene: p-aminobenzene sulfonic acid and sodium nitrite are added in hydrochloric acid solution, low-temp reaction, system
It is standby to obtain diazonium salt, diazonium salt will be added in the redox graphene dispersion liquid that step S2 is prepared, ice bath reaction,
Centrifuge separation, washing, are scattered in deionized water, and hydrazine hydrate, deionized water and hydrazine hydrate volume ratio 1:2.5 is added, permanent
Sodium carbonate liquor is added dropwise after the reaction was completed in temperature reaction, and sulfonated graphene is prepared in centrifuge separation, washing；
The preparation of S4, sulfonated graphene load indium oxide: deionized water is dispersed by the step S3 sulfonated graphene being prepared
In, it is added indium nitrate and carbamide, boric acid sodium water solution and ethylenediamine is added in whipping process, wherein Boratex in uniform stirring
Aqueous solution, ethylenediamine, deionized water volume ratio are 6:7:150, hydro-thermal reaction, after the reaction was completed, with dehydrated alcohol and deionization
Water sufficiently washs, and is dried, and after the completion of dry, is placed under the conditions of helium, sulfonated graphite is prepared in sintering processes
Alkene loads indium oxide.
It is lasting stirred under constant temperature described in step S1 in embodiment as the present invention more preferred embodiment
Cheng Zhong, thermostat temperature are 1-5 DEG C, mixing speed 800r/min.
As the present invention more preferred embodiment, during being stirred to react described in step S1 in embodiment, stirring
Reaction time is 2-3h.
As the present invention more preferred embodiment, in embodiment in centrifugal separation processes described in step S1, centrifugation
Revolving speed is 12000-15000r/min, centrifugation time 10-20min.
As the present invention more preferred embodiment, in embodiment in ultrasonication described in step S1, ultrasound
Frequency is 100-150W, ultrasonic time 10-20min.
As the present invention more preferred embodiment, centrifugal separation processes after ultrasound described in step S1 in embodiment
In, centrifugal rotational speed is first adjusted to 3000-3500r/min processing 4min, then centrifugal rotational speed is adjusted to 6000-6500r/min processing
10min。
As the present invention more preferred embodiment, sodium borohydride solution mass concentration described in step S2 in embodiment
For 30g/L, the sodium borohydride solution volume and deionized water volume ratio of addition are 1:3-5.
As the present invention more preferred embodiment, in embodiment in ice bath reaction process described in step S3, ice bath
Reaction time is 3h.
As the present invention more preferred embodiment, isothermal reaction described in step S3 in embodiment, when isothermal reaction
Between be 25-30h, isothermal reaction temperature be 90-95 DEG C.
As the present invention more preferred embodiment, sodium carbonate liquor concentration described in step S3 is 10% in embodiment,
Sodium carbonate liquor and hydrazine hydrate volume ratio are 1:20.
As the present invention more preferred embodiment, sulfonated graphene and deionized water described in step S4 in embodiment
Solid-to-liquid ratio is 5g:1L.
As the present invention more preferred embodiment, sulfonated graphene, indium nitrate, carbon described in step S4 in embodiment
Amide mass ratio is 2:1:1.
It is dry in embodiment in drying process process described in step S4 as the present invention more preferred embodiment
Temperature is 35-40 DEG C.
Wherein, in the preparation process of embodiment 1-3 sulfonated graphene load indium oxide gas sensitive, step S1 graphite oxide
In the preparation process of alkene, the hydrogen peroxide concentration of addition is A%, under the conditions of constant speed, is warming up to B DEG C and continues mixing time and be
Ch, in the preparation process of step S2 redox graphene, isothermal reaction temperature is D DEG C, and the isothermal reaction time is Eh, step S3
In the preparation process of sulfonated graphene, p-aminobenzene sulfonic acid, sodium nitrite, hydrochloric acid molar ratio be 1:1.5:F, low-temp reaction
Temperature is G DEG C, and step S4 sulfonated graphene loads in the preparation process of indium oxide, and Boratex concentration of aqueous solution is H%, and hydro-thermal is anti-
Answering temperature is I DEG C, reaction time Jh, and sintering temperature is K DEG C, sintering time Lh, and specific each step related data is detailed in table
1。
Each step related data of table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| A% | 25 | 27 | 28 |
| B℃ | 40 | 43 | 45 |
| Ch | 2 | 2.5 | 3 |
| D℃ | 85 | 87 | 90 |
| Eh | 2 | 2.5 | 3 |
| F | 3 | 4 | 3 |
| G℃ | 5 | 0 | 10 |
| H% | 8 | 7 | 10 |
| I℃ | 150 | 140 | 130 |
| Jh | 10 | 9 | 12 |
| K℃ | 425 | 400 | 450 |
| Lh | 1 | 1.5 | 1.3 |
Graphene oxide that step S1 is prepared as shown in Figure 1, a, b are respectively graphene oxide TEM figure, SEM figure in Fig. 1,
By the graphene oxide TEM figure, the SEM figure that are prepared it can be seen that the surface of graphene oxide that is prepared of the present embodiment compared with
Be it is smooth, be in film-form, possess stratiform, pleated structure.
The sulfonated graphene XPS that step S3 is prepared schemes, SEM figure is as shown in Figure 2 and Figure 3 respectively, by sulfonation is prepared
Graphene XPS figure, containing carbon, oxygen, element sulphur, shows graphene success sulphur it can be seen that in the sulfonated graphene being prepared
Change；By sulfonated graphene SEM figure is prepared it can be seen that the sulfonated graphene surface that is prepared of the present embodiment is compared to oxygen
Graphite alkene surface is more smooth, possesses stratiform, pleated structure.
The sulfonated graphene load indium oxide TEM that step S4 is prepared schemes the sulfonation stone as shown in figure 4, by being prepared
Black alkene load indium oxide TEM figure is it can be seen that the indium oxide being prepared is in bulk, and indium oxide is successfully sulfonated graphene and bears
It carries.
Embodiment 4
It is right respectively in order to investigate the air-sensitive performance for the sulfonated graphene load indium oxide gas sensitive that embodiment 1-3 is prepared
Gas sensor is made in the sulfonated graphene load indium oxide gas sensitive that embodiment 1-3 is prepared, at room temperature, right
15ppm nitrogen dioxide carries out sensitivity test, and Fig. 5 is the dioxy that graphene-supported indium oxide gas sensitive is 15ppm in concentration
Change sensitivity characteristic curve graph measured in nitrogen atmosphere, a, b, c respectively correspond embodiment 1, embodiment 2, implement in Fig. 5
The sulfonated graphene that example 3 is prepared loads indium oxide gas sensitive sensitivity characteristic curve graph, as seen from Figure 5: embodiment
1, the sulfonated graphene load indium oxide gas sensitive that embodiment 2, embodiment 3 are prepared rings 15ppm nitrogen dioxide gas
Answering sensitivity is respectively 124.1%, 150.7%, 114.7%, therefore the sulfonated graphene load indium oxide gas that embodiment 2 is prepared
Quick material property is best；It is dense to difference in order to investigate the sulfonated graphene load indium oxide gas sensitive that embodiment 2 is prepared
The nitrogen dioxide sensitivity test of degree, Fig. 6 are sensitivity characteristic curve measured in the nitrogen dioxide gas atmosphere of various concentration
Figure, as seen from Figure 6: sulfonated graphene that embodiment 2 is prepared load indium oxide gas sensitive to 0.2ppm,
The response sensitivity of 0.35ppm, 0.5ppm nitrogen dioxide gas is respectively 7.2%, 16.9%, 23.4%, dense with nitrogen dioxide
Degree increases, and the sulfonated graphene load indium oxide gas sensitive sensitivity being prepared is higher, while nitrogen dioxide gas concentration
Minimum is 0.2ppm, at this point, sound of the sulfonated graphene load indium oxide gas sensitive being prepared to nitrogen dioxide gas
Answering sensitivity is 7.2%.
Embodiment 5
In order to investigate whether the sulfonated graphene load indium oxide gas sensitive that embodiment 2 is prepared possesses spirit steady in a long-term
Sensitivity, the sulfonated graphene that embodiment 2 is prepared load sensor made of indium oxide gas sensitive, are repeatedly placed in concentration
In the nitrogen dioxide gas atmosphere of 15ppm, to record its dynamic test curve, Fig. 7 is the sulfonated graphene applying example 2 and being prepared
The reperformance test curve of indium oxide gas sensitive is loaded, as seen from Figure 7: the sulfonated graphene that embodiment 2 is prepared
Sensor made of load indium oxide gas sensitive is placed in the nitrogen dioxide gas atmosphere that concentration is 15ppm, responds tendency phase
Together, after sulfonated graphene load indium oxide gas sensitive leaves nitrogen dioxide gas atmosphere, that is, it is restored to basic resistance value, repeatedly
The sensitivity of test is identical, biggish variation does not occur, shows that sulfonated graphene load indium oxide gas sensitive performance is stablized,
Possess preferable repeatability.
The above, only of the invention illustrates embodiment, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, that makes several changes
It also should be regarded as protection scope of the present invention into supplement；All those skilled in the art, do not depart from spirit of that invention and
In the case where range, using the equivalent variations of a little change, modification and differentiation that disclosed above technology contents are made, it is
Equivalent embodiment of the invention；Meanwhile any equivalent variations that all substantial technologicals according to the present invention do above-described embodiment
Change, modification and differentiation, still fall within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive, which comprises the steps of:
The preparation of S1, graphene oxide: being that 98% concentrated sulfuric acid persistently stirs under constant temperature conditions by graphite, sodium nitrate, concentration, permanent
Temperature is 1-5 DEG C, mixing speed 800r/min, and under conditions of temperature-resistant, mixing speed is constant, permanganic acid is added
Potassium is stirred to react 2-3h, then under the conditions of constant speed, is heated up and continues to stir, and deionized water and hydrogen peroxide, centrifugation is added
Separation, centrifugal rotational speed 12000-15000r/min, centrifugation time 10-20min, it is 7 that deionized water, which is cleaned to PH, at ultrasound
Reason, supersonic frequency 100-150W, ultrasonic time 10-20min are centrifugated after ultrasound, first will be from centrifugal separation processes
Heart revolving speed is adjusted to 3000-3500r/min processing 4min, then centrifugal rotational speed is adjusted to 6000-6500r/min processing 10min, finally
By vacuum drying, graphene oxide is prepared；
The preparation of S2, redox graphene: dispersing the step S1 graphene oxide being prepared in deionized water, is added dropwise
The sodium carbonate liquor that concentration is 10% is added the sodium borohydride solution that mass concentration is 30g/L, is added until dispersion liquid PH is 9
Sodium borohydride solution volume and deionized water volume ratio be 1:3-5, isothermal reaction is prepared by being centrifugated, washing
Redox graphene；
The preparation of S3, sulfonated graphene: p-aminobenzene sulfonic acid and sodium nitrite are added in hydrochloric acid solution, low-temp reaction, system
It is standby to obtain diazonium salt, diazonium salt is added in the redox graphene dispersion liquid that step S2 is prepared, ice bath reacts 3h,
Centrifuge separation, washing, are scattered in deionized water, and hydrazine hydrate, deionized water and hydrazine hydrate volume ratio 1:2.5 is added, permanent
Temperature reaction, isothermal reaction time are 25-30h, and isothermal reaction temperature is 90-95 DEG C, and after the reaction was completed, it is 10% that concentration, which is added dropwise,
Sodium carbonate liquor, sodium carbonate liquor and hydrazine hydrate volume ratio are 1:20, and sulfonated graphene is prepared in centrifuge separation, washing；
The preparation of S4, sulfonated graphene load indium oxide: deionized water is dispersed by the step S3 sulfonated graphene being prepared
In, sulfonated graphene and deionized water solid-to-liquid ratio are 5g:1L, and indium nitrate and carbamide, sulfonated graphene, indium nitrate, carbon is added
Amide mass ratio is 2:1:1, and boric acid sodium water solution and ethylenediamine are added in whipping process for uniform stirring, and wherein Boratex is water-soluble
Liquid, ethylenediamine, deionized water volume ratio are 6:7:150, and hydro-thermal reaction is filled with dehydrated alcohol and deionized water after the reaction was completed
Divide washing, be dried at 35-40 DEG C, after the completion of dry, is placed under the conditions of helium, sintering processes are prepared
Sulfonated graphene loads indium oxide.
2. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive according to claim 1, feature exist
It is 4:3:12 in the mass ratio of, graphite in step S1, sodium nitrate, potassium permanganate, the solid-to-liquid ratio of graphite and the concentrated sulfuric acid is 1g:
50mL。
3. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive according to claim 1, feature exist
In, heated up and continued in whipping process in step S1, warming temperature be 40-45 DEG C, mixing time 2-3h.
4. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive according to claim 1, feature exist
In the hydrogen peroxide concentration being added in step S1 is 25-28%, and the volume that hydrogen peroxide is added is with the concentrated sulfuric acid, deionized water volume ratio
20:1:10.
5. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive according to claim 1, feature exist
During step S2 isothermal reaction, reaction temperature is 85-90 DEG C, reaction time 2-3h.
6. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive according to claim 1, feature exist
In, during step S3 prepares diazonium salt, p-aminobenzene sulfonic acid, sodium nitrite, hydrochloric acid molar ratio be 1:1.5:3-4, low temperature
Reaction temperature is 0-10 DEG C.
7. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive according to claim 1, feature exist
In step S4 Boratex concentration of aqueous solution is 7-10%.
8. a kind of preparation method of sulfonated graphene load indium oxide gas sensitive according to claim 1, feature exist
In in step S4 hydrothermal reaction process, reaction temperature is 130-150 DEG C, reaction time 9-12h.
9. according to a kind of preparation method of sulfonated graphene load indium oxide gas sensitive described in claim 1, which is characterized in that
During step S4 sintering processes, sintering temperature is 400-450 DEG C, sintering time 1-1.5h.
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| CN111115619A (en) * | 2019-12-30 | 2020-05-08 | 深圳烯创先进材料研究院有限公司 | Preparation method of functionalized graphene with gas-sensitive performance and gas-sensitive ink |
| CN112625625A (en) * | 2020-12-09 | 2021-04-09 | 安徽腾龙泵阀制造有限公司 | Preparation method of low-temperature adhesive for low-temperature pump activated carbon adsorption material |
| CN113686928A (en) * | 2021-08-24 | 2021-11-23 | 华北电力大学 | GO/In2O3Composite nano material and preparation and application thereof |
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| CN113686928A (en) * | 2021-08-24 | 2021-11-23 | 华北电力大学 | GO/In2O3Composite nano material and preparation and application thereof |
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