CN105905950B - A kind of quick response/recovery-type graphene CoTiO3The preparation method of composite sensitive material - Google Patents

A kind of quick response/recovery-type graphene CoTiO3The preparation method of composite sensitive material Download PDF

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CN105905950B
CN105905950B CN201610213611.3A CN201610213611A CN105905950B CN 105905950 B CN105905950 B CN 105905950B CN 201610213611 A CN201610213611 A CN 201610213611A CN 105905950 B CN105905950 B CN 105905950B
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卢靖
贾娜
程龙
黄剑锋
曹丽云
王勇
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Shaanxi University of Science and Technology
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Abstract

A kind of quick response/recovery-type graphene CoTiO3The preparation method of composite sensitive material, graphene oxide is dispersed in ethanol, graphene oxide ethanol solution is obtained, by Co (NO3)2·6H2O is dissolved in C2H5In OH, stirring at room temperature obtains red, transparent solution, and the pH value of regulation red, transparent solution is 2.0~5.0, obtains red tan solution；Red tan solution is added to Ti (OC4H9)4In, obtain red, transparent colloidal sol；Graphene oxide ethanol solution is added in red, transparent colloidal sol, colloidal sol is obtained after stirring；By colloidal sol drying after 1~3h of calcining at 600~700 DEG C.The present invention realizes CoTiO3With the chemical bond of graphene sheet layer, and the material can occasionally reach shortening response, the effect of recovery time.It the experiment proved that, the composite is sensitive to alcohol gas, and with quick response/recovery capability, can be used in sensitive material.

Description

A kind of quick response/recovery-type graphene-CoTiO3The preparation of composite sensitive material Method
Technical field
The present invention relates to a kind of preparation of sensitive material, and in particular to a kind of quick response/recovery-type graphene-CoTiO3 The preparation method of composite sensitive material.
Background technology
Gas sensitive refers to the class functional material that the resistance of material changes with the change of gaseous surrounding environment.Gas is passed Sensor plays critically important role in life, be just widely used in environmental monitoring, plant produced and safety monitoring and The fields such as medical diagnosis.[Varghese S S,Lonkar S,Singh K K,et al.Recent advances in graphene based gas sensors[J].Sensors and Actuators B:Chemical,2015,218:160- 183.]。
Ilmenite type compound CoTiO3With storage, record, catalysis and to the performance of alcohol sensible, can be applied to lithium from Sub- battery, magnetic recorder, catalyst and gas sensor domain.Wherein the gas sensing property of cobalt titanate is increasingly by the weight of people Depending on.Lu J have prepared nano Co TiO using sol-gal process3Gas sensitive, and its gas sensing property is studied, find CoTiO3Sensitivity to 104ppm ethanol is 17.9, and response and recovery time are respectively 13s and 10s.[Lu J,Jiang Y, Zhang Y,et al.Preparation of gas sensing CoTiO3nanocrystallites using EDTA as the chelating agent in a sol–gel process[J].Ceramics International,2015,41 (3):3714-3721.], cobalt titanate is as the subject matter that gas sensitive presently, there are：Operating temperature is higher, can detect Gas least concentration it is higher, the problems such as also response speed is slow.
The content of the invention
It is an object of the invention to provide a kind of quick response/recovery-type graphene-CoTiO3The preparation side of composite Method, easy to operate using sol-gel process, raw material proportioning controllability is strong, and particle size is uniform, the sensitive material of easily prepared nanoscale Material；Atmosphere heat treatment ensures graphene not oxidation by air, favourable graphene-CoTiO3The composition of composite air-sensitive material, structure Controllable preparation.
In order to achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of quick response/recovery-type graphene-CoTiO3The preparation method of composite sensitive material, comprises the following steps：
1) it is graphene oxide is dispersed in ethanol, graphene oxide ethanol solution is obtained, wherein, graphene oxide Concentration in ethanol is 0.5~1.5mg/mL；
2) by Co (NO3)2·6H2O is dissolved in C2H5In OH, stirring at room temperature obtains red, transparent solution, and regulation is red thoroughly The pH value of bright solution is 2.0~5.0, obtains red tan solution；Wherein, Co2+Concentration is 0.0003~0.0007mol/mL；
3) red tan solution is added to Ti (OC4H9)4In, stir, obtain red, transparent colloidal sol；Wherein, bronzing Co (NO in solution3)2·6H2O and Ti (OC4H9)4Mol ratio be (0.003~0.007) mol：(0.003~0.007) mol；
4) graphene oxide ethanol solution is added in red, transparent colloidal sol, colloidal sol is obtained after stirring；Wherein, stone is aoxidized Graphene oxide and Ti (OC in black alkene ethanol solution4H9)4Mass ratio be (3.125~50) mg：(1.02~2.38) g；
5) quick response/recovery is obtained after colloidal sol is dried in calcining 1~3h at 600~700 DEG C in nitrogen atmosphere stove Type graphene-CoTiO3Composite sensitive material.
Step 1) in disperse be by ultrasonic power be 40~80Hz under, 1~3h of ultrasound realization.
PH value analyzes what pure glacial acetic acid was realized by being added into red, transparent solution.
Step 4) in the speed of stirring be 60~90r/min, time of stirring is 22~25h.
Drying actual conditions is：5~8h is dried at 60~90 DEG C.
The flow velocity that nitrogen is passed through into nitrogen atmosphere stove is 100~200mL/min.
Compared with prior art, beneficial effects of the present invention are：Because graphene is that a kind of have high specific surface area, good Unique physically and electrically property such as good thermal conductivity, high thermal stability, high optical transmittance and quick carrier mobility Material, so, the present invention is with graphene oxide, CoTiO3For raw material, CoTiO is prepared using sol-gal process first3Colloidal sol Presoma, then adds a certain amount of graphene oxide solution, dries and is calcined in atmosphere furnace after it forms gel, it is intended to Prepare CoTiO3Nano particle is equably layered on the structure on graphene film, realizes CoTiO3With the chemical bond of graphene sheet layer, And the material can occasionally reach shortening response, the effect of recovery time.It the experiment proved that, the composite is quick to alcohol gas Sense, and with quick response/recovery capability, can be used in sensitive material.In addition, this method to nanocomposite constituents can Control property is strong, easy to operate, and cobalt titanate is nano-scale particle in product, meets the microstructure demand of gas sensitive.
Brief description of the drawings
Fig. 1 is graphene-CoTiO made from the embodiment of the present invention 43The SEM figures of composite air-sensitive material；
Fig. 2 is graphene-CoTiO made from the embodiment of the present invention 43The Raman figures of composite air-sensitive material；
Fig. 3 is graphene-CoTiO made from the embodiment of the present invention 43Composite air-sensitive material and CoTiO3To 100ppm ethanol Response/recovery curve.
Embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
Embodiment 1：
1) 3.125mg graphene oxide is added in 3.125mL ethanol, the concentration of graphene oxide in ethanol It is 1mg/mL, ultrasonic 1.5h, ultrasonic power is 60Hz, graphene oxide is dispersed in ethanol, obtain graphene oxide Ethanol solution.
2) by 0.005molCo (NO3)2·6H2O is dissolved completely in 15mL C2H5In OH, stirring at room temperature obtains uniform Red, transparent solution, is designated as A, now Co2+Concentration is 0.00033mol/mL.
3) the 1 pure glacial acetic acid of drop analysis is added into A, regulation solution ph is 2.0, obtains red tan solution, is designated as B.
4) B is poured slowly into the analytically pure Ti (OC of 0.005mol4H9)4In, and be stirred continuously, red, transparent colloidal sol is obtained, It is designated as C.
5) 3.125mL graphene oxide ethanol solution is slowly added in above-mentioned red, transparent colloidal sol, stirs 24h, stir Speed is mixed for 70r/min, colloidal sol is obtained；
6) above-mentioned colloidal sol is put into drying box in drying 7h at 80 DEG C, forms it into xerogel.Then xerogel is put into In calcining 2h at 650 DEG C in nitrogen atmosphere stove, the flow velocity that nitrogen is passed through into nitrogen atmosphere stove is 100~200mL/min, is obtained Quick response/recovery-type graphene-CoTiO3Composite air-sensitive material.
Embodiment 2：
1) 12.5mg graphene oxide is added in 12.5mL ethanol, the concentration of graphene oxide in ethanol is 1mG/mL, ultrasonic 1.5h, ultrasonic power is 60Hz, and graphene oxide is dispersed in ethanol, obtains graphene oxide second Alcoholic solution.
2) 0.005molCo (NO will be weighed3)2·6H2O is dissolved completely in 15mL C2H5In OH, stirring at room temperature is obtained Even red, transparent solution, is designated as A, now Co2+Concentration is 0.00033mol/mL.
3) the 1 pure glacial acetic acid of drop analysis is added into A, regulation solution ph is 3.0, obtains red tan solution, is designated as B.
4) B is poured slowly into the analytically pure Ti (OC of 0.005mol4H9)4In, and be stirred continuously, red, transparent colloidal sol is obtained, It is designated as C.
5) 12.5mL graphene oxide ethanol solution amount is slowly added in above-mentioned red, transparent colloidal sol, stirs 24h, stir Speed is mixed for 70r/min, colloidal sol is obtained；
6) above-mentioned colloidal sol is put into drying box in drying 7h at 80 DEG C, forms it into xerogel.Then xerogel is put into In calcining 2h at 650 DEG C in nitrogen atmosphere stove, the flow velocity that nitrogen is passed through into nitrogen atmosphere stove is 200mL/min, obtains quick Response/recovery-type graphene-CoTiO3Composite air-sensitive material.
Embodiment 3：
1) graphene oxide for weighing 31.25mg is added in 31.25mL ethanol, graphene oxide is in ethanol 'sIt is denseIt is 1mg/mL to spend scope, and ultrasonic 1.5h, ultrasonic power is 60Hz, and graphene oxide is dispersed in ethanol, obtains oxygen Graphite alkene ethanol solution.
2) 0.005molCo (NO will be weighed3)2·6H2O is dissolved completely in 15mL C2H5In OH, stirring at room temperature is obtained Even red, transparent solution, is designated as A, now Co2+Concentration is 0.00033mol/mL.
3) the 1 pure glacial acetic acid of drop analysis is added into A, regulation solution ph is 4.0, obtains red tan solution, is designated as B.
4) B is poured slowly into the analytically pure Ti (OC of 0.005mol4H9)4In, and be stirred continuously, red, transparent colloidal sol is obtained, It is designated as C.
5) 31.25mL graphene oxide solution amount is slowly added in above-mentioned red, transparent colloidal sol, stirs 24h, stirring Speed is 70r/min, obtains colloidal sol；
6) above-mentioned colloidal sol is put into drying box in drying 7h at 80 DEG C, forms it into xerogel.Then xerogel is put into In calcining 2h at 650 DEG C in nitrogen atmosphere stove, the flow velocity that nitrogen is passed through into nitrogen atmosphere stove is 150mL/min, obtains quick Response/recovery-type graphene-CoTiO3Composite air-sensitive material.
Embodiment 4：
1) 50mg graphene oxide is added in 50mL ethanol, the concentration range of graphene oxide in ethanol is 1mg/mL, ultrasonic 1.5h, ultrasonic power is 60Hz, and graphene oxide is dispersed in ethanol, obtains graphene oxide second Alcoholic solution.
2) by 0.005molCo (NO3)2·6H2O is dissolved completely in 15mL C2H5In OH, stirring at room temperature obtains uniform Red, transparent solution, is designated as A, now Co2+Concentration is 0.00033mol/mL.
3) the 1 pure glacial acetic acid of drop analysis is added into A, regulation solution ph is 5.0, obtains red tan solution, is designated as B.
4) B is poured slowly into the analytically pure Ti (OC of 0.005mol4H9)4In, and be stirred continuously, red, transparent colloidal sol is obtained, It is designated as C.
5) 50mL graphene oxide solution amount is slowly added in above-mentioned red, transparent colloidal sol, stirs 24h, stir speed (S.S.) For 70r/min, colloidal sol is obtained；
6) above-mentioned colloidal sol is put into drying box in drying 7h at 80 DEG C, forms it into xerogel.Then xerogel is put into In calcining 2h at 650 DEG C in nitrogen atmosphere stove, the flow velocity that nitrogen is passed through into nitrogen atmosphere stove is 120mL/min, obtains quick Response/recovery-type graphene-CoTiO3Composite air-sensitive material.
Graphene-CoTiO made from the present embodiment is detected using voltage test method3Composite air-sensitive material is at different temperatures Sensitivity characteristic.
As shown in Figure 1, graphene-CoTiO made from the embodiment of the present invention 43Composite air-sensitive material is nanoscale CoTiO3 Grain is evenly dispersed in the structure on graphene sheet layer.
As seen from Figure 2, composite made from the embodiment of the present invention 4 is graphene-CoTiO3Composite.
As seen from Figure 3, graphene-CoTiO made from the embodiment of the present invention 43Composite air-sensitive material is to 100ppm second The response of alcohol and recovery time are respectively 1s and 1s, possess response/regeneration rate more faster than simple cobalt titanate.
Embodiment 5：
1) graphene oxide is dispersed in ethanol, under 40Hz, ultrasonic 3h obtains graphene oxide ethanol solution, Wherein, the concentration of graphene oxide in ethanol is 0.5mg/mL；
2) by Co (NO3)2·6H2O is dissolved in C2H5In OH, stirring at room temperature obtains red, transparent solution, to red, transparent The pH value that the pure glacial acetic acid regulation red, transparent solution of analysis is added in solution is 2.0, obtains red tan solution；Wherein, Co2+Concentration For 0.0003mol/mL；
3) red tan solution is added to Ti (OC4H9)4In, stir, obtain red, transparent colloidal sol；Wherein, bronzing Co (NO in solution3)2·6H2O and Ti (OC4H9)4Mol ratio be 0.003mol：0.007mol；
4) graphene oxide ethanol solution is added in red, transparent colloidal sol, obtains molten after stirring 25h under 60r/min Glue；Wherein, graphene oxide and Ti (OC in graphene oxide ethanol solution4H9)4Mass ratio be 3.125mg：1.02g；
5) colloidal sol is dried at 90 DEG C after 5h in nitrogen atmosphere stove in calcining 3h at 600 DEG C, obtains quick response/extensive Replica graphene-CoTiO3Composite sensitive material.Wherein, nitrogen is passed through into nitrogen atmosphere stove, and nitrogen flow rate is 100mL/ min。
Embodiment 6：
1) graphene oxide is dispersed in ethanol, under 80Hz, ultrasonic 1h obtains graphene oxide ethanol solution, Wherein, the concentration of graphene oxide in ethanol is 1.5mg/mL；
2) by Co (NO3)2·6H2O is dissolved in C2H5In OH, stirring at room temperature obtains red, transparent solution, to red, transparent The pH value that the pure glacial acetic acid regulation red, transparent solution of analysis is added in solution is 3.0, obtains red tan solution；Wherein, Co2+Concentration For 0.0007mol/mL；
3) red tan solution is added to Ti (OC4H9)4In, stir, obtain red, transparent colloidal sol；Wherein, bronzing Co (NO in solution3)2·6H2O and Ti (OC4H9)4Mol ratio be 0.007mol：0.004mol；
4) graphene oxide ethanol solution is added in red, transparent colloidal sol, obtains molten after stirring 22h under 90r/min Glue；Wherein, graphene oxide and Ti (OC in graphene oxide ethanol solution4H9)4Mass ratio be 50mg：1.5g；
5) colloidal sol is dried at 60 DEG C after 8h in nitrogen atmosphere stove in calcining 2h at 620 DEG C, obtains quick response/extensive Replica graphene-CoTiO3Composite sensitive material.Wherein, nitrogen is passed through into nitrogen atmosphere stove, and nitrogen flow rate is 200mL/ min。
Embodiment 7：
1) graphene oxide is dispersed in ethanol, under 70Hz, ultrasonic 1.5h obtains graphene oxide ethanol molten Liquid, wherein, the concentration of graphene oxide in ethanol is 0.8mg/mL；
2) by Co (NO3)2·6H2O is dissolved in C2H5In OH, stirring at room temperature obtains red, transparent solution, to red, transparent The pH value that the pure glacial acetic acid regulation red, transparent solution of analysis is added in solution is 5.0, obtains red tan solution；Wherein, Co2+Concentration For 0.0005mol/mL；
3) red tan solution is added to Ti (OC4H9)4In, stir, obtain red, transparent colloidal sol；Wherein, bronzing Co (NO in solution3)2·6H2O and Ti (OC4H9)4Mol ratio be 0.005mol：0.003mol；
4) graphene oxide ethanol solution is added in red, transparent colloidal sol, obtains molten after stirring 24h under 70r/min Glue；Wherein, graphene oxide and Ti (OC in graphene oxide ethanol solution4H9)4Mass ratio be 20mg：2.38g；
5) colloidal sol is dried at 70 DEG C after 6h in nitrogen atmosphere stove in calcining 1h at 700 DEG C, obtains quick response/extensive Replica graphene-CoTiO3Composite sensitive material.Wherein, nitrogen is passed through into nitrogen atmosphere stove, and nitrogen flow rate is 100mL/ min。
Embodiment 8：
1) graphene oxide is dispersed in ethanol, under 50Hz, ultrasonic 2h obtains graphene oxide ethanol solution, Wherein, the concentration of graphene oxide in ethanol is 1mg/mL；
2) by Co (NO3)2·6H2O is dissolved in C2H5In OH, stirring at room temperature obtains red, transparent solution, to red, transparent The pH value that the pure glacial acetic acid regulation red, transparent solution of analysis is added in solution is 4.0, obtains red tan solution；Wherein, Co2+Concentration For 0.0004mol/mL；
3) red tan solution is added to Ti (OC4H9)4In, stir, obtain red, transparent colloidal sol；Wherein, bronzing Co (NO in solution3)2·6H2O and Ti (OC4H9)4Mol ratio be 0.006mol：0.005mol；
4) graphene oxide ethanol solution is added in red, transparent colloidal sol, obtains molten after stirring 23h under 80r/min Glue；Wherein, graphene oxide and Ti (OC in graphene oxide ethanol solution4H9)4Mass ratio be 40mg：2g；
5) by colloidal sol at 80 DEG C dry 6h after in nitrogen atmosphere stove in calcining 1.5h at 650 DEG C, obtain quick response/ Recovery-type graphene-CoTiO3Composite sensitive material.Wherein, nitrogen is passed through into nitrogen atmosphere stove, and nitrogen flow rate is 100mL/min。
It is of the invention that nanoscale graphite alkene-CoTiO is specifically synthesized using combination of sol-gel atmosphere heat treatment method3It is compound Sensitive material, cobalt titanate is combined with the sensitivity characteristic of graphene, using sol-gal process combination atmosphere heat treatment legal system Standby graphene-CoTiO3Composite, reaches shortening response, the effect of recovery time.Possesses quick response/extensive to alcohol gas Multiple characteristic.Shorten response, the advantage of recovery time for having in sensitive material.

Claims (4)

1. a kind of quick response/recovery-type graphene-CoTiO3The preparation method of composite sensitive material, it is characterised in that including with Lower step：
1) it is graphene oxide is dispersed in ethanol, graphene oxide ethanol solution is obtained, wherein, graphene oxide is in second Concentration in alcohol is 0.5~1.5mg/mL；
2) by Co (NO3)2·6H2O is dissolved in C2H5In OH, stirring at room temperature obtains red, transparent solution, and regulation red, transparent is molten The pH value of liquid is 2.0~5.0, obtains red tan solution；Wherein, Co2+Concentration is 0.0003~0.0007mol/mL；
3) red tan solution is added to Ti (OC4H9)4In, stir, obtain red, transparent colloidal sol；Wherein, red tan solution Middle Co (NO3)2·6H2O and Ti (OC4H9)4Mol ratio be (0.003~0.007) mol：(0.003~0.007) mol；
4) graphene oxide ethanol solution is added in red, transparent colloidal sol, colloidal sol is obtained after stirring；Wherein, graphene oxide Graphene oxide and Ti (OC in ethanol solution4H9)4Mass ratio be (3.125~50) mg：(1.02~2.38) g；
5) quick response/recovery-type stone is obtained after colloidal sol is dried in calcining 1~3h at 600~700 DEG C in nitrogen atmosphere stove Black alkene-CoTiO3Composite sensitive material；
Step 1) in disperse be by ultrasonic power be 40~80Hz under, 1~3h of ultrasound realization；
Step 4) in the speed of stirring be 60~90r/min, time of stirring is 22~25h.
2. quick response according to claim 1/recovery-type graphene-CoTiO3The preparation method of composite sensitive material, its It is characterised by, pH value analyzes what pure glacial acetic acid was realized by being added into red, transparent solution.
3. quick response according to claim 1/recovery-type graphene-CoTiO3The preparation method of composite sensitive material, its It is characterised by, drying actual conditions is：5~8h is dried at 60~90 DEG C.
4. quick response according to claim 1/recovery-type graphene-CoTiO3The preparation method of composite sensitive material, its It is characterised by, the flow velocity that nitrogen is passed through into nitrogen atmosphere stove is 100~200mL/min.
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