CN104624219B - Efficiently C3n4the situ converting preparation method of-CdS composite photocatalyst material - Google Patents
Efficiently C3n4the situ converting preparation method of-CdS composite photocatalyst material Download PDFInfo
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Abstract
The present invention relates to efficient C3N4The situ converting preparation method of CdS composite photocatalyst material, comprises the following steps: 1) tripolycyanamide is scattered in deionized water, form homogeneous solution；2) evenly spread to, in melamine solution, be sufficiently stirred for by cadmium sulfide powder, make tripolycyanamide uniform adsorption in cadmium sulfide powder surface；3) it is transferred in air dry oven be dried, it is thus achieved that the cadmium sulfide powder body that tripolycyanamide is modified；4) it is placed in tube furnace, calcining, i.e. obtains efficient C3N4CdS composite photocatalyst material.The beneficial effects of the present invention is: the present invention proposes a kind of simple, efficient and green in-situ transesterification political reform and carrys out synthetic surface uniform load C3N4CdS catalysis material；It is more beneficial for interface transmission and the sharp separation of photo-generated carrier, is more beneficial for the raising of photocatalysis performance.Additionally, the operation of this synthetic method is very simple, equipment requirements is low.
Description
Technical field
The present invention relates to efficient C3N4The situ converting preparation method of-CdS composite photocatalyst material.
Background technology
In recent years, owing to the problems such as global energy anxiety are day by day serious, catalysis material has broad application prospects in terms of photocatalytic hydrogen production by water decomposition.It is known that CdS is most important of which one conductor photocatalysis material, its energy gap is about 2.4eV, it is possible to responding to visible light；CdS is after excited by visible light, and the light induced electron of generation transfers to material surface, and has stronger reducing power (-0.51V, vs.SHE), it is possible in reductive water, free hydrion produces hydrogen, therefore smoothly, solving in energy problem, good effect can played.But, owing to the quantum efficiency of one pack system CdS is low, light induced electron is easily combined with hole, greatly limit the efficiency of its photocatalysis performance.Many researcheres promote hydrogen manufacturing performance and the stability of CdS by different processing modes, such as addition agent modified, semiconductor coupling, precious metal surface deposition etc..In above-mentioned various methods, develop one of the method that simple, efficient, cheap CdS semiconductor coupling material is considered as the most most application potential.
Different according to semiconductor property, couple semiconductor can be divided into inorganic semiconductor and organic semiconductor.Wherein, organic semiconductor (C3N4) there is the features such as synthesis simple, cheap, stable chemical nature, responding to visible light and receive significant attention.Meanwhile, C3N4There is the band structure relatively mated with CdS, and be prone to absorb visible ray simultaneously.When above-mentioned both carry out surface coupling time, light induced electron and hole that each quasiconductor produces after light excites can be by interfaces between the two under the effect of internal electric field, successfully move to corresponding material surface, light induced electron is greatly reduced with the recombination probability in hole, thus is obviously improved hydrogen manufacturing performance.But, current C3N4It is mainly by ultrasonic disperse solid C with the associated methods of CdS3N4, make C3N4Solid transition becomes less lamellar and is deposited on CdS surface with physisorption.Said method is clearly present C3N4, C weak with CdS Interaction Force3N4Uneven and the C in CdS surface distributed3N4The phenomenon that particle size is the most uneven, and then cause the lifting of its Photocatalyzed Hydrogen Production performance extremely limited.Therefore, how cheap C3N4Organic semiconductor on CdS surface, ensures C by one simple mode uniform deposition simultaneously3N4And having stronger adhesion between CdS, this is significant for the hydrogen manufacturing performance and development high-efficiency photocatalysis material promoting CdS catalysis material further.But as far as we know, there is presently no about utilizing in-situ transesterification political reform simple, efficient to carry out synthetic surface uniform load C3N4CdS catalysis material, to improve the report of CdS photocatalytic activity.
Summary of the invention
The technical problem to be solved is for above-mentioned prior art, proposes a kind of efficiently C3N4Modify the simple situ converting preparation method of CdS catalysis material, to obtain surface uniform load C3N4CdS catalysis material.
The present invention solves above-mentioned technical problem and be the technical scheme is that efficient C3N4The situ converting preparation method of-CdS composite photocatalyst material, it is characterised in that comprise the following steps:
1) being scattered in deionized water by tripolycyanamide, form homogeneous solution, wherein melamine concentration is 0.0001-0.1g/mL；
2) 0.2g cadmium sulfide powder is evenly spread to step 1) in the 9mL melamine solution that configures, in 30-100 DEG C of water bath with thermostatic control, it is sufficiently stirred for 0.5-5h, makes tripolycyanamide uniform adsorption in cadmium sulfide powder surface；
3) by step 2) the cadmium sulfide suspension of the surface uniform adsorption tripolycyanamide of gained is transferred in air dry oven in 30-100 DEG C of freeze-day with constant temperature, and make moisture evaporate completely and finally obtain the cadmium sulfide powder body that tripolycyanamide is modified；
4) by step 3) the cadmium sulfide powder body of surface uniform load tripolycyanamide that obtains is placed in tube furnace, calcines 0.1-5h in 250-850 DEG C in a nitrogen atmosphere, i.e. obtain efficient C3N4-CdS composite photocatalyst material.
By such scheme, step 1) described in melamine concentration be 0.0005-0.05g/mL.
By such scheme, step 2) described in bath temperature be 60-100 DEG C, mixing time is 1-2h.
By such scheme, step 3) described in baking temperature be 80-100 DEG C.
By such scheme, step 4) described in calcining heat be 400-600 DEG C, calcination time is 0.5-2h.
The present invention proposes efficient C3N4Modifying the simple situ converting preparation method of CdS catalysis material, be first scattered in aqueous solution by tripolycyanamide solid, at a certain temperature (such as 80 DEG C), tripolycyanamide solid can be dissolved completely in water；When adding CdS powder body in tripolycyanamide aqueous solution, after stirring, evaporation water is until forming pressed powder at relatively high temperatures, and now tripolycyanamide can gradually be deposited on CdS powder surface along with water evaporation, and forms stronger interface coupling effect；When this tripolycyanamide-CdS composite granule is during high-temperature calcination (such as 550 DEG C), the tripolycyanamide at high temperature decomposition in situ being deposited on CdS powder surface forms C3N4, thus it is prepared for C3N4-CdS composite photocatalyst material.Due to C3N4It is to be changed by the Molecular Adsorption of tripolycyanamide-high-temp in-situ to form, the C that therefore prepared by this method3N4There is on CdS surface distribution evenly and particle size, can guarantee that C simultaneously3N4Good interface interaction alternate with CdS two, these are all conducive to the enhancing of Photocatalyzed Hydrogen Production performance.
C3N4The photocatalysis performance of-CdS composite photocatalyst material is estimated by decomposing Aquatic product hydrogen under visible light.Experimentation is as follows: by 0.05g C3N4-CdS catalysis material is dispersed in and contains 0.35M Na equipped with 80mL2S and 0.25M Na2SO3In the three-neck flask of solution.Before illumination, first lead to 30min nitrogen in order to avoid the impact of oxygen in air, then seal bottleneck with rubber closure.In whole During Illumination, take certain gaseous sample every 30min and detect hydrogen content by gas chromatogram (Shimadzu, GC-14C, Japan).
C3N4The structure characterization methods of-CdS catalysis material: observe pattern and granular size with field emission scanning electron microscope (FESEM), situation is crystallized with X-ray diffraction (XRD) spectrum analysis, observing with transmission electron microscope (TEM) and combine situation and crystal structure between composite, with FTIR analyzing melamine, through calcination processing, whether successful conversion is C3N4。
The beneficial effects of the present invention is: the present invention proposes a kind of simple, efficient and green in-situ transesterification political reform and carrys out synthetic surface uniform load C3N4CdS catalysis material, wherein C3N4Content can be by obtaining the simple regulation and control of presoma melamine concentration easily and effectively；Owing to presoma tripolycyanamide is in CdS surface in aqueous with molecular forms uniform adsorption, thus the final C obtained3N4Uniformly can couple on CdS surface；Additionally, due to C3N4It is that melamine molecule is at high temperature formed by situ converting, thus CdS and C3N4Between interface coupling effect obviously higher than the sample prepared by traditional ultrasonic delamination-absorption sedimentation, be more beneficial for photo-generated carrier interface transmission and sharp separation, be more beneficial for the raising of photocatalysis performance.Additionally, the operation of this synthetic method is very simple, equipment requirements is low, without reaction units such as expensive various processing synthesis devices and High Temperature High Pressure, there is advantages such as being prone to high-volume synthesis, be expected to produce good Social and economic benef@.
Accompanying drawing explanation
Fig. 1 is C in embodiment 13N4The situ converting synthesis thinking of-CdS catalysis material；
Fig. 2 is CdS and C in embodiment 13N4The XRD figure spectrum of-CdS catalysis material；
Fig. 3 is CdS (a) and C in embodiment 13N4The FESEM collection of illustrative plates of-CdS (b) catalysis material；
Fig. 4 is C in embodiment 13N4The TEM collection of illustrative plates of-CdS catalysis material；
Fig. 5 is CdS (a), C in embodiment 13N4-CdS (b) and C3N4The FTIR collection of illustrative plates of (c) catalysis material；
Fig. 6 is CdS (a) and C in embodiment 13N4The activity performance of-CdS (b) catalysis material；
Fig. 7 is C in embodiment 13N4The photocatalytic mechanism figure of-CdS catalysis material.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described in detail, but this explanation will not be construed as limiting the invention.
Embodiment 1:
Efficiently C3N4The situ converting preparation process of-CdS composite photocatalyst material is as follows: 1) be scattered in deionized water by tripolycyanamide, forms homogeneous solution, and wherein melamine concentration is 0.002g/mL；2) 0.2g cadmium sulfide powder is evenly spread to step 1) in the 9mL melamine solution that configures, in 85 DEG C of waters bath with thermostatic control, it is sufficiently stirred for 2h, makes tripolycyanamide uniform adsorption in cadmium sulfide powder surface；3) by step 2) the cadmium sulfide suspension of the surface uniform adsorption tripolycyanamide of gained is transferred in air dry oven in 80 DEG C of freeze-day with constant temperature, and make moisture evaporate completely and finally obtain the cadmium sulfide powder body that tripolycyanamide is modified；4) by step 3) the cadmium sulfide powder body of surface uniform load tripolycyanamide that obtains is placed in tube furnace, calcines 0.5h in 550 DEG C in a nitrogen atmosphere, i.e. obtain C3N4Content is the C of 1wt%3N4-CdS composite photocatalyst material.
Fig. 1 is C in embodiment 13N4The situ converting preparation process schematic diagram of-CdS catalysis material.First synthetic CdS powder body is dispersed in tripolycyanamide aqueous solution, the content of melamine of CdS surface adsorption can be changed by the concentration of regulation tripolycyanamide；Process 1 be melamine molecule uniform adsorption on CdS surface, so can ensure that the uniform load on CdS surface；Process 2 is that 550 DEG C of high-temperature calcinations process that to make melamine molecule be C at CdS surface favourable conversions3N4, and CdS and C3N4Between interface at high temperature have strong coupling, beneficially photo-generated carrier interface transmission and sharp separation.
Fig. 2 is CdS and C in embodiment 13N4The XRD figure spectrum of-CdS catalysis material.From figure 2 it can be seen that through C3N4After surface is modified, the characteristic diffraction peak of products therefrom is consistent with the XRD peak modifying front CdS sample, and C is described3N4Crystal structure and the crystallization degree having no effect on CdS is modified on surface；Simultaneously as C3N4Content in composite sample seldom (1wt%), can not demonstrate corresponding C in XRD figure3N4Diffraction maximum.
Fig. 3 is CdS (a) and C in embodiment 13N4The FESEM collection of illustrative plates of-CdS (b) catalysis material.It can be seen that the size of CdS particle is 100-200nm from Fig. 3 a；Through C3N4After the modification of surface (Fig. 3 b), the size of corresponding composite photo-catalyst particle does not has significant change, C is described3N4Modification can't cause the significant change of CdS particle size and pattern.
Fig. 4 is C in embodiment 13N4The TEM collection of illustrative plates of-CdS catalysis material.From Fig. 4 (a) it can be clearly seen that the granule of CdS is about 100-200nm, its result is identical with FESEM；Meanwhile, many C3N4Nanostructured is modified on CdS catalysis material surface equably, with in Fig. 1 it is proposed that formation schematic diagram consistent.Can be seen more clearly from from Fig. 4 (b), (c) and (d), CdS surface is by C3N4Uniformly cladding, and and C3N4Formation is combined closely.
Fig. 5 is CdS (a), C in embodiment 13N4-CdS (b) and C3N4The FTIR collection of illustrative plates of (c) catalysis material.It can be seen that the absorption spectrum that shown of sample (a), (c) respectively with CdS and C of standard3N4Absorption spectrum is consistent, and the absworption peak potential energy that sample (b) is occurred is enough preferably owing to CdS and C3N4Combination, although its intensity is different and otherwise varied due to content.Therefore, in conjunction with the interpretation of result of TEM and FTIR, it can be deduced that tripolycyanamide after high-temperature heat treatment, can converted in-situ be successfully C3N4And it is firmly bonded to CdS surface.
Fig. 6 is CdS (a) and C in embodiment 13N4The activity performance of-CdS (b) catalysis material.It can be seen that individually CdS hydrogen manufacturing performance is more satisfactory, its hydrogen generation efficiency is 2258 μm ol h-1g-1.Through C3N4After success loads, the photocatalysis performance of CdS obtains bigger enhancing, and its hydrogen generation efficiency reaches 5303 μm ol h-1g-1.Meanwhile, after 4 photocatalysis circular response, C3N4The inactivation rate (12%) of-CdS hydrogen manufacturing performance of photocatalyst inactivation performance (23%) far below pure CdS, illustrates through C3N4After modification, the photocatalysis stability of CdS can be obviously improved.
Fig. 7 is C in embodiment 13N4The photocatalytic mechanism figure of-CdS catalysis material.Due to C3N4The band structure being mutually matched between the two with CdS, the photohole of CdS under the effect of internal electric field can fast transfer to C3N4Valence band location, and C3N4Light induced electron can effectively be transferred to the conduction band positions of CdS under the effect of internal electric field, thus the recombination probability of photo-generated carrier can be greatly reduced；Simultaneously as C3N4It is that melamine molecule is at high temperature formed by situ converting, thus CdS and C3N4Between interface close coupling effect be more beneficial for photo-generated carrier interface transmission and sharp separation, be more beneficial for the raising of photocatalysis performance.
Embodiment 2:
In order to check melamine concentration to C3N4The impact of-CdS photocatalyst photocatalysis performance, in addition to melamine concentration difference, other reaction conditions such as water-bath temperature (85 DEG C), mixing time (2h), baking temperature (80 DEG C), calcining heat (550 DEG C), calcination time (0.5h) etc. are the most same as in Example 1.Result shows: when melamine concentration is 0.0001g/mL, owing to melamine concentration is the lowest, it is thus achieved that C3N4C in-CdS photocatalyst3N4Content is relatively low, and Photocatalyzed Hydrogen Production performance boost is inconspicuous, and its performance is 2310 μm ol h-1g-1；When melamine concentration is respectively 0.0005,0.002 and 0.05g/mL, it is thus achieved that C3N4The photocatalysis performance of-CdS photocatalyst promotes substantially, all at 5000-5500 μm ol h-1g-1；When melamine solution concentration is 0.1g/mL, owing to tripolycyanamide solid can not be completely dissolved, experiment cannot obtain the equally distributed C in surface3N4-CdS photocatalyst.Therefore, at C3N4In the preparation process of-CdS photocatalyst, optimal melamine concentration is 0.0005-0.05g/mL.
Embodiment 3:
In order to check bath temperature to C3N4The impact of-CdS photocatalyst photocatalysis performance, in addition to bath temperature difference, other reaction conditions such as melamine concentration (0.002g/mL), mixing time (2h), baking temperature (80 DEG C), calcining heat (550 DEG C), calcination time (0.5h) etc. are the most same as in Example 1.Result shows: when melamine solution bath temperature is 30 DEG C, and tripolycyanamide solid can not dissolve substantially, therefore cannot obtain the equally distributed C in surface3N4-CdS photocatalyst；When melamine solution bath temperature is respectively 60,85 and 100 DEG C, it is possible to obtain uniform melamine solution, thus the equally distributed C in surface can be obtained3N4-CdS photocatalyst.Therefore, at C3N4In the preparation process of-CdS photocatalyst, optimal bath temperature is 60-100 DEG C.
Embodiment 4:
In order to check mixing time to C3N4The impact of-CdS photocatalyst photocatalysis performance, in addition to mixing time difference, other reaction conditions such as melamine concentration (0.002g/mL), water-bath temperature (85 DEG C), baking temperature (80 DEG C), calcining heat (550 DEG C), calcination time (0.5h) etc. are the most same as in Example 1.Result shows: when the stirring and adsorbing time is 0.5h, tripolycyanamide is not completely dissolved, and causes CdS surface on the low side to the adsorbance of tripolycyanamide, it is thus achieved that C3N4C in-CdS photocatalyst3N4Content is relatively low, and photocatalysis performance promotes inconspicuous；When the stirring and adsorbing time is 1-2h, tripolycyanamide can be completely dissolved and adsorb on CdS surface, can obtain uniform C3N4-CdS composite photo-catalyst so that its photocatalysis performance is improved significantly；When the stirring and adsorbing time is 5h, although tripolycyanamide can adsorb completely on CdS surface, but prepared C3N4The H2-producing capacity of-CdS composite photo-catalyst is not changed in substantially.Therefore, at C3N4In the preparation process of-CdS photocatalyst, the optimal stirring and adsorbing time is 1-2h.
Embodiment 5:
In order to check baking temperature to C3N4The impact of-CdS photocatalyst photocatalysis performance, in addition to baking temperature difference, other reaction conditions such as melamine concentration (0.002g/mL), water-bath temperature (85 DEG C), mixing time (2h), calcining heat (550 DEG C), calcination time (0.5h) etc. are the most same as in Example 1.Result shows: when baking temperature is 30 DEG C, and the little molecule of tripolycyanamide in solution can the most gradually separate out from solution, causes tripolycyanamide solid at CdS surface nonuniform deposition so that it is photocatalysis performance promotes inconspicuous；When baking temperature is 80-100 DEG C, on the one hand melamine molecule can uniform dissolution in the solution, and be gradually and uniformly distributed to CdS surface along with evaporation of water, the highest temperature is more beneficial for the quickly volatilization of water to improve preparation efficiency.Therefore, at C3N4In the preparation process of-CdS photocatalyst, optimum drying temperature is 80-100 DEG C.
Embodiment 6:
In order to check calcining heat to C3N4The impact of-CdS photocatalyst photocatalysis performance, in addition to calcining heat difference, other reaction conditions such as melamine concentration (0.002g/mL), water-bath temperature (85 DEG C), mixing time (2h), baking temperature (80 DEG C), calcination time (0.5h) etc. are the most same as in Example 1.Result shows: when calcining heat is 250 DEG C, owing to melamine molecule can not be efficiently converted into C3N4, it is impossible to obtain efficient C3N4-CdS photocatalyst；When temperature is 400-600 DEG C, tripolycyanamide can successfully be converted into C3N4, meanwhile, higher heat treatment temperature can strengthen C3N4And the interface binding power between CdS so that it is photocatalysis performance is further enhanced, its hydrogen generation efficiency all reaches 5000 μm ol h-1g-1；When temperature is 850 DEG C, due to C3N4Lim-ited temperature stability, it is easy to be decomposed to form organic molecule and lose.Therefore, at C3N4In the preparation process of-CdS photocatalyst, optimum calcinating temperature is 400-600 DEG C.
Embodiment 7:
In order to check calcination time to C3N4The impact of-CdS photocatalyst photocatalysis performance, in addition to calcination time difference, other reaction conditions such as melamine concentration (0.002g/mL), water-bath temperature (85 DEG C), mixing time (2h), baking temperature (80 DEG C), calcining heat (550 DEG C) etc. are the most same as in Example 1.Result shows: time between upon calcination for 0.1h, tripolycyanamide is not fully converted to C3N4, it is thus achieved that C3N4Possibly together with unconverted tripolycyanamide in-CdS catalysis material, cause the obvious reduction of photocatalysis performance；When being 0.5-2h between upon calcination, tripolycyanamide can favourable conversions be C3N4, surface uniform load C can be obtained3N4CdS photocatalyst, its hydrogen generation efficiency can reach 5000 μm ol h-1g-1；When being 5h between upon calcination, prepared C3N4The H2-producing capacity of-CdS catalysis material drops to 4150 μm ol h-1g-1, possible cause is that the long meeting of calcination time causes C3N4With the phase counterdiffusion between CdS, thus form new complex centre.Therefore, at C3N4In the preparation process of-CdS photocatalyst, optimal calcination time is 0.5-2h.
Claims (4)
1. efficient C3N4The situ converting preparation method of-CdS composite photocatalyst material, it is characterised in that comprise the following steps:
1) being scattered in deionized water by tripolycyanamide, form homogeneous solution, wherein melamine concentration is 0.0005-0.05g/mL；
2) 0.2g cadmium sulfide powder is evenly spread to step 1) in the 9mL melamine solution that configures, in 30-100 DEG C of thermostatted water
Bath is sufficiently stirred for 0.5-5h, makes tripolycyanamide uniform adsorption in cadmium sulfide powder surface, it is thus achieved that surface uniform adsorption tripolycyanamide
Cadmium sulfide suspension；
3) by step 2) the cadmium sulfide suspension of the surface uniform adsorption tripolycyanamide of gained is transferred in air dry oven in 30-100 DEG C
Freeze-day with constant temperature, makes moisture evaporate completely and finally obtains the cadmium sulfide powder body that tripolycyanamide is modified；
4) by step 3) the cadmium sulfide powder body modified of the tripolycyanamide that obtains is placed in tube furnace, in a nitrogen atmosphere in 250-850 DEG C
Calcining 0.1-5h, i.e. obtains efficient C3N4-CdS composite photocatalyst material.
Efficient C the most according to claim 13N4The situ converting preparation method of-CdS composite photocatalyst material, it is characterised in that
Step 2) described in bath temperature be 60-100 DEG C, mixing time is 1-2h.
Efficient C the most according to claim 13N4The situ converting preparation method of-CdS composite photocatalyst material, it is characterised in that
Step 3) described in baking temperature be 80-100 DEG C.
Efficient C the most according to claim 13N4The situ converting preparation method of-CdS composite photocatalyst material, it is characterised in that
Step 4) described in calcining heat be 400-600 DEG C, calcination time is 0.5-2h.
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| CN103191766A (en) * | 2013-04-15 | 2013-07-10 | 南京理工大学 | CdS/g-C3N4 composite visible light catalyst, preparation method and application |
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