CN104624219A - In-situ transformation preparation method of efficient C3N4-CdS composite photocatalytic material - Google Patents
In-situ transformation preparation method of efficient C3N4-CdS composite photocatalytic material Download PDFInfo
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Abstract
The invention relates to an in-situ transformation preparation method of an efficient C3N4-CdS composite photocatalytic material. The in-situ transformation preparation method comprises the following steps that (1) tripolycyanamide is dispersed in deionized water to form a uniform solution; (2) cadmium sulfide powder is uniformly dispersed in the tripolycyanamide solution uniformly, the cadmium sulfide powder and the tripolycyanamide solution mixed fully to achieve that tripolycyanamide is uniformly absorbed on the surface of the cadmium sulfide powder; (3) liquid obtained in Step 2 is transferred to a blast drying oven to be dried, and tripolycyanamide modified cadmium sulfide powder is obtained; and (4) the tripolycyanamide modified cadmium sulfide powder is put in a tube furnace and calcined, and the efficient C3N4-CdS composite photocatalytic material is obtained. The in-situ transformation preparation method has the benefits of being simple efficient and green when being used for synthesizing the photocatalytic material with the surface uniformly loaded with C3N4-CdS; interface transmission and sharp separation of photon-generated carriers are further facilitated; and the photocatalysis performance is further improved. In addition, the synthetic method is simple to operate, and requirements on equipment are low.
Description
Technical field
The present invention relates to efficient C
3n
4the situ converting preparation method of-CdS composite photocatalyst material.
Background technology
In recent years, because the problems such as global energy anxiety are day by day serious, catalysis material has broad application prospects in photocatalytic hydrogen production by water decomposition.As everyone knows, CdS is wherein most important a kind of conductor photocatalysis material, and its energy gap is about 2.4eV, can 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), hydrogen ion that can be free in reductive water smoothly produces hydrogen, therefore, in solution energy problem, good effect can be played.But because the quantum efficiency of one pack system CdS is low, the easy compound of light induced electron and hole, greatly limit the efficiency of its photocatalysis performance.Many researchers promote hydrogen manufacturing performance and the stability of CdS, as addition agent modified, semiconductor coupling, precious metal surface deposition etc. by different processing modes.In above-mentioned various method, develop simple, efficient, cheap CdS semiconductor coupling material and be considered to one of method of most application potential in actual applications.
Different according to semiconductor property, couple semiconductor can be divided into inorganic semiconductor and organic semiconductor.Wherein, organic semiconductor (C
3n
4) there is the features such as synthesis is simple, cheap, stable chemical nature, responding to visible light and be subject to extensive concern.Meanwhile, C
3n
4there is the band structure of comparatively mating with CdS, and be easy to absorb visible ray simultaneously.When above-mentioned both carry out surface be coupled time, the light induced electron that respective semiconductor produces after optical excitation and hole can by interfaces between the two under the effect of internal electric field, successfully move to corresponding material surface, the recombination probability in light induced electron and hole is greatly reduced, thus significantly promotes hydrogen manufacturing performance.But, current C
3n
4mainly ultrasonic disperse solid C is passed through with the associated methods of CdS
3n
4, make C
3n
4solid transition becomes less sheet and is deposited on CdS surface with physisorption.Obviously there is C in said method
3n
4, C weak with CdS Interaction Force
3n
4uneven and the C in CdS surface distributed
3n
4the phenomenon that particle size is extremely uneven, and then cause the lifting of its Photocatalyzed Hydrogen Production performance very limited.Therefore, how cheap C
3n
4organic semiconductor on CdS surface, ensures C by a kind of simple mode uniform deposition simultaneously
3n
4and have 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, also not simple about utilization, in-situ transesterification political reform efficiently carrys out synthetic surface uniform load C at present
3n
4cdS catalysis material, to improve the report of CdS photocatalytic activity.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned prior art, proposes a kind of efficient C
3n
4modify the simple and easy situ converting preparation method of CdS catalysis material, to obtain surface uniform load C
3n
4cdS catalysis material.
The present invention solves the problems of the technologies described above adopted technical scheme: efficient C
3n
4the situ converting preparation method of-CdS composite photocatalyst material, is characterized in that comprising the following steps:
1) be scattered in deionized water by melamine, 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, fully stir 0.5-5h, make melamine uniform adsorption in cadmium sulfide powder surface;
3) by step 2) the cadmium sulfide suspension of the surface uniform of gained absorption melamine to be transferred in air dry oven in 30-100 DEG C of freeze-day with constant temperature, moisture evaporated completely and the final cadmium sulfide powder obtaining melamine and modify;
4) by step 3) the cadmium sulfide powder of surface uniform Supported Melamine that obtains is placed in tube furnace, in a nitrogen atmosphere in 250-850 DEG C of calcining 0.1-5h, namely obtains efficient C
3n
4-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 C
3n
4modify the simple and easy situ converting preparation method of CdS catalysis material, first by melamine solid dispersal in the aqueous solution, at a certain temperature (as 80 DEG C), melamine solid can be dissolved in the water completely; When adding CdS powder in the melamine aqueous solution, after stirring, evaporation water is until form pressed powder at relatively high temperatures, and now melamine can be deposited on CdS powder surface gradually along with water evaporation, and forms stronger interface coupling effect; When this melamine-CdS composite granule is in high-temperature calcination (as 550 DEG C) process, be deposited on the melamine at high temperature decomposition in situ formation C of CdS powder surface
3n
4, thus prepared C
3n
4-CdS composite photocatalyst material.Due to C
3n
4changed by the Molecular Adsorption of melamine-high-temp in-situ to form, the therefore C for preparing of this method
3n
4have on CdS surface evenly distribution and particle size, simultaneously can ensure C
3n
4good interface interaction alternate with CdS two, these are all conducive to the enhancing of Photocatalyzed Hydrogen Production performance.
C
3n
4the photocatalysis performance of-CdS composite photocatalyst material is by decomposing aquatic products hydrogen under visible light to assess.Experimentation is as follows: by 0.05g C
3n
4-CdS catalysis material is dispersed in and 80mL is housed contains 0.35M Na
2s and 0.25M Na
2sO
3in the three-neck flask of solution.Before illumination, first logical 30min nitrogen is in order to avoid the impact of oxygen in air, then seals bottleneck with rubber stopper.In whole During Illumination, get certain gaseous sample every 30min and detect hydrogen content by gas-chromatography (Shimadzu, GC-14C, Japan).
C
3n
4the structure characterization methods of-CdS catalysis material: observe pattern and granular size with field emission scanning electron microscope (FESEM), by X-ray diffraction (XRD) spectrum analysis crystallization situation, observe in conjunction with situation and crystal structure between composite with transmission electron microscope (TEM), with FTIR analyzing melamine, through calcination processing, whether successful conversion is C
3n
4.
Beneficial effect 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 C
3n
4cdS catalysis material, wherein C
3n
4content can by can also effectively obtain the simple regulation and control of presoma melamine concentration easily; Because presoma melamine is with molecular forms uniform adsorption in CdS surface in aqueous, the thus final C obtained
3n
4evenly can be coupled on CdS surface; In addition, due to C
3n
4that melamine molecule is at high temperature formed by situ converting, thus CdS and C
3n
4between interface coupling effect obviously stronger than the sample prepared by traditional ultrasonic delamination-absorption sedimentation, be more conducive to interface transmission and the quick separating of photo-generated carrier, be more conducive to the raising of photocatalysis performance.In addition, the operation of this synthetic method is very simple, equipment requirement is low, without the need to reaction units such as the various processing synthesis device of costliness and HTHPs, have advantages such as being easy to synthesis in enormous quantities, be expected to the Social and economic benef@that generation is good.
Accompanying drawing explanation
Fig. 1 is C in embodiment 1
3n
4the situ converting synthesis thinking of-CdS catalysis material;
Fig. 2 is CdS and C in embodiment 1
3n
4the XRD collection of illustrative plates of-CdS catalysis material;
Fig. 3 is CdS (a) and C in embodiment 1
3n
4the FESEM collection of illustrative plates of-CdS (b) catalysis material;
Fig. 4 is C in embodiment 1
3n
4the TEM collection of illustrative plates of-CdS catalysis material;
Fig. 5 is CdS (a), C in embodiment 1
3n
4-CdS (b) and C
3n
4the FTIR collection of illustrative plates of (c) catalysis material;
Fig. 6 is CdS (a) and C in embodiment 1
3n
4the activity performance of-CdS (b) catalysis material;
Fig. 7 is C in embodiment 1
3n
4the 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 can not be construed as limiting the invention.
Embodiment 1:
Efficient C
3n
4the situ converting preparation process of-CdS composite photocatalyst material is as follows: 1) be scattered in deionized water by melamine, and form homogeneous solution, 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, fully stir 2h, make melamine uniform adsorption in cadmium sulfide powder surface; 3) by step 2) the cadmium sulfide suspension of the surface uniform of gained absorption melamine to be transferred in air dry oven in 80 DEG C of freeze-day with constant temperature, moisture evaporated completely and the final cadmium sulfide powder obtaining melamine and modify; 4) by step 3) the cadmium sulfide powder of surface uniform Supported Melamine that obtains is placed in tube furnace, in a nitrogen atmosphere in 550 DEG C of calcining 0.5h, namely obtains C
3n
4content is the C of 1wt%
3n
4-CdS composite photocatalyst material.
Fig. 1 is C in embodiment 1
3n
4the situ converting preparation process schematic diagram of-CdS catalysis material.First synthetic CdS powder is dispersed in the melamine aqueous solution, by the content of melamine regulating the concentration of melamine can change CdS adsorption; Process 1 is that melamine molecule uniform adsorption is surperficial at CdS, can ensure the uniform load on CdS surface like this; Process 2 is that 550 DEG C of high-temperature calcination process make melamine molecule be C at CdS surface favourable conversions
3n
4, and CdS and C
3n
4between interface at high temperature there is strong coupling, be conducive to photo-generated carrier interface transmission and quick separating.
Fig. 2 is CdS and C in embodiment 1
3n
4the XRD collection of illustrative plates of-CdS catalysis material.As can be seen from Figure 2, through C
3n
4after finishing, the characteristic diffraction peak of products therefrom is consistent with the XRD peak modifying front CdS sample, and C is described
3n
4finishing does not affect crystal structure and the crystallization degree of CdS; Meanwhile, due to C
3n
4content in composite sample seldom (1wt%), XRD figure can not demonstrate corresponding C
3n
4diffraction maximum.
Fig. 3 is CdS (a) and C in embodiment 1
3n
4the FESEM collection of illustrative plates of-CdS (b) catalysis material.As can be seen from Fig. 3 a, the size of CdS particle is 100-200nm; Through C
3n
4after finishing (Fig. 3 b), the size of corresponding composite photo-catalyst particle does not have significant change, and C is described
3n
4modification can't cause the significant change of CdS particle size and pattern.
Fig. 4 is C in embodiment 1
3n
4the TEM collection of illustrative plates of-CdS catalysis material.Can clearly be seen that from Fig. 4 (a), the particle of CdS is approximately 100-200nm, and its result is identical with FESEM; Meanwhile, many C
3n
4nanostructured is modified at CdS catalysis material surface equably, consistent with the formation schematic diagram that in Fig. 1, we propose.Can more clearly find out from Fig. 4 (b), (c) and (d), CdS surface is by C
3n
4evenly coated, and and C
3n
4formation is combined closely.
Fig. 5 is CdS (a), C in embodiment 1
3n
4-CdS (b) and C
3n
4the FTIR collection of illustrative plates of (c) catalysis material.As can be seen from the figure, the absorption spectrum that shows of sample (a), (c) respectively with CdS and C of standard
3n
4absorption spectrum is consistent, and the absworption peak potential energy that sample (b) occurs is enough good owing to CdS and C
3n
4combination, although its intensity due to content different and distinguish to some extent.Therefore, in conjunction with the interpretation of result of TEM and FTIR, can show that melamine is after high-temperature heat treatment, can converted in-situ be successfully C
3n
4and strong bonded is on CdS surface.
Fig. 6 is CdS (a) and C in embodiment 1
3n
4the activity performance of-CdS (b) catalysis material.As can be seen from the figure, independent CdS hydrogen manufacturing performance is more satisfactory, and its hydrogen generation efficiency is 2258 μm of ol h
-1g
-1.Through C
3n
4after success load, the photocatalysis performance of CdS obtains larger enhancing, and its hydrogen generation efficiency reaches 5303 μm of ol h
-1g
-1.Meanwhile, after 4 photocatalysis circular responses, C
3n
4the inactivation rate (12%) of-CdS hydrogen manufacturing performance of photocatalyst, far below the inactivation performance (23%) of pure CdS, illustrates through C
3n
4after modification, the photocatalysis stability of CdS can be significantly improved.
Fig. 7 is C in embodiment 1
3n
4the photocatalytic mechanism figure of-CdS catalysis material.Due to C
3n
4with the band structure that CdS mates between the two mutually, the photohole of CdS under the effect of internal electric field can fast transfer to C
3n
4valence band location, and C
3n
4light induced electron effectively can 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 reduce greatly; Meanwhile, due to C
3n
4that melamine molecule is at high temperature formed by situ converting, thus CdS and C
3n
4between interface close coupling effect be more conducive to photo-generated carrier interface transmission and quick separating, be more conducive to the raising of photocatalysis performance.
Embodiment 2:
In order to check melamine concentration to C
3n
4the impact of-CdS photochemical catalyst photocatalysis performance, except melamine concentration difference, other reaction conditions are as all identical with embodiment 1 in water-bath temperature (85 DEG C), mixing time (2h), baking temperature (80 DEG C), calcining heat (550 DEG C), calcination time (0.5h) etc.Result shows: when melamine concentration is 0.0001g/mL, because melamine concentration is too low, and the C of acquisition
3n
4c in-CdS photochemical catalyst
3n
4content is lower, and Photocatalyzed Hydrogen Production performance boost is not obvious, and its performance is 2310 μm of ol h
-1g
-1; When melamine concentration is respectively 0.0005,0.002 and 0.05g/mL, the C of acquisition
3n
4the photocatalysis performance of-CdS photochemical catalyst promotes obviously, all at 5000-5500 μm of ol h
-1g
-1; When melamine solution concentration is 0.1g/mL, because melamine solid can not dissolve completely, experiment cannot obtain the C of surface uniform distribution
3n
4-CdS photochemical catalyst.Therefore, at C
3n
4in the preparation process of-CdS photochemical catalyst, best melamine concentration is 0.0005-0.05g/mL.
Embodiment 3:
In order to check bath temperature to C
3n
4the impact of-CdS photochemical catalyst photocatalysis performance, except bath temperature difference, other reaction conditions are as all identical with embodiment 1 in melamine concentration (0.002g/mL), mixing time (2h), baking temperature (80 DEG C), calcining heat (550 DEG C), calcination time (0.5h) etc.Result shows: when melamine solution bath temperature is 30 DEG C, melamine solid can not dissolve substantially, therefore cannot obtain the C of surface uniform distribution
3n
4-CdS photochemical catalyst; When melamine solution bath temperature is respectively 60,85 and 100 DEG C, uniform melamine solution can be obtained, thus can obtain the C of surface uniform distribution
3n
4-CdS photochemical catalyst.Therefore, at C
3n
4in the preparation process of-CdS photochemical catalyst, best bath temperature is 60-100 DEG C.
Embodiment 4:
In order to check mixing time to C
3n
4the impact of-CdS photochemical catalyst photocatalysis performance, except mixing time difference, other reaction conditions are as all identical with embodiment 1 in 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.Result shows: when the stirring and adsorbing time is 0.5h, melamine does not dissolve completely, causes CdS surface on the low side to the adsorbance of melamine, the C of acquisition
3n
4c in-CdS photochemical catalyst
3n
4content is lower, and photocatalysis performance promotes not obvious; When the stirring and adsorbing time is 1-2h, melamine can dissolve completely and be adsorbed on CdS surface, can obtain uniform C
3n
4-CdS composite photo-catalyst, makes its photocatalysis performance be improved significantly; When the stirring and adsorbing time is 5h, although melamine can be adsorbed on CdS surface completely, prepared C
3n
4the H2-producing capacity of-CdS composite photo-catalyst does not change substantially.Therefore, at C
3n
4in the preparation process of-CdS photochemical catalyst, the best stirring and adsorbing time is 1-2h.
Embodiment 5:
In order to check baking temperature to C
3n
4the impact of-CdS photochemical catalyst photocatalysis performance, except baking temperature difference, other reaction conditions are as all identical with embodiment 1 in melamine concentration (0.002g/mL), water-bath temperature (85 DEG C), mixing time (2h), calcining heat (550 DEG C), calcination time (0.5h) etc.Result shows: when baking temperature is 30 DEG C, and the melamine Small molecular in solution can be separated out in solid form gradually from solution, causes melamine solid at CdS surface nonuniform deposition, its photocatalysis performance is promoted not obvious; When baking temperature is 80-100 DEG C, on the one hand melamine molecule can uniform dissolution in the solution, and along with evaporation of water gradually and be distributed to CdS surface equably, higher temperature is more conducive to the quick volatilization of water to improve preparation efficiency on the other hand.Therefore, at C
3n
4in the preparation process of-CdS photochemical catalyst, optimum drying temperature is 80-100 DEG C.
Embodiment 6:
In order to check calcining heat to C
3n
4the impact of-CdS photochemical catalyst photocatalysis performance, except calcining heat difference, other reaction conditions are as all identical with embodiment 1 in melamine concentration (0.002g/mL), water-bath temperature (85 DEG C), mixing time (2h), baking temperature (80 DEG C), calcination time (0.5h) etc.Result shows: when calcining heat is 250 DEG C, because melamine molecule effectively can not be converted into C
3n
4, efficient C can not be obtained
3n
4-CdS photochemical catalyst; When temperature is 400-600 DEG C, melamine successfully can be converted into C
3n
4, meanwhile, higher heat treatment temperature can strengthen C
3n
4and the interface binding power between CdS, makes its photocatalysis performance be further enhanced, and its hydrogen generation efficiency all reaches 5000 μm of ol h
-1g
-1; When temperature is 850 DEG C, due to C
3n
4lim-ited temperature stability, be easy to be decomposed to form organic molecule and lose.Therefore, at C
3n
4in the preparation process of-CdS photochemical catalyst, optimum calcinating temperature is 400-600 DEG C.
Embodiment 7:
In order to check calcination time to C
3n
4the impact of-CdS photochemical catalyst photocatalysis performance, except calcination time difference, other reaction conditions are as all identical with embodiment 1 in 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.Result shows: time upon calcination for 0.1h, melamine is not converted into C completely
3n
4, the C of acquisition
3n
4also containing unconverted melamine in-CdS catalysis material, cause the obvious reduction of photocatalysis performance; When being upon calcination 0.5-2h, melamine can favourable conversions be C
3n
4, surface uniform load C can be obtained
3n
4cdS photochemical catalyst, its hydrogen generation efficiency can reach 5000 μm of ol h
-1g
-1; When being upon calcination 5h, prepared C
3n
4the H2-producing capacity of-CdS catalysis material drops to 4150 μm of ol h
-1g
-1, possible cause is that the long meeting of calcination time causes C
3n
4with the phase counterdiffusion between CdS, thus form new complex centre.Therefore, at C
3n
4in the preparation process of-CdS photochemical catalyst, best calcination time is 0.5-2h.
Claims (5)
1. efficient C
3n
4the situ converting preparation method of-CdS composite photocatalyst material, is characterized in that comprising the following steps:
1) be scattered in deionized water by melamine, 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, fully stir 0.5-5h, make melamine uniform adsorption in cadmium sulfide powder surface;
3) by step 2) the cadmium sulfide suspension of the surface uniform of gained absorption melamine to be transferred in air dry oven in 30-100 DEG C of freeze-day with constant temperature, moisture evaporated completely and the final cadmium sulfide powder obtaining melamine and modify;
4) by step 3) the cadmium sulfide powder of surface uniform Supported Melamine that obtains is placed in tube furnace, in a nitrogen atmosphere in 250-850 DEG C of calcining 0.1-5h, namely obtains efficient C
3n
4-CdS composite photocatalyst material.
2. efficient C according to claim 1
3n
4the situ converting preparation method of-CdS composite photocatalyst material, is characterized in that step 1) described in melamine concentration be 0.0005-0.05g/mL.
3. efficient C according to claim 1
3n
4the situ converting preparation method of-CdS composite photocatalyst material, is characterized in that step 2) described in bath temperature be 60-100 DEG C, mixing time is 1-2h.
4. efficient C according to claim 1
3n
4the situ converting preparation method of-CdS composite photocatalyst material, is characterized in that step 3) described in baking temperature be 80-100 DEG C.
5. efficient C according to claim 1
3n
4the situ converting preparation method of-CdS composite photocatalyst material, is characterized in that step 4) described in calcining heat be 400-600 DEG C, calcination time is 0.5-2h.
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| CN105562055A (en) * | 2016-01-14 | 2016-05-11 | 天津理工大学 | Method for preparing cadmium sulfide graphite-like carbon nitride compound photocatalyst |
| CN107008484A (en) * | 2017-04-17 | 2017-08-04 | 武汉理工大学 | A kind of binary metal sulfide/carbonitride composite photocatalyst material and preparation method thereof |
| CN107008484B (en) * | 2017-04-17 | 2020-08-25 | 武汉理工大学 | Binary metal sulfide/carbon nitride composite photocatalytic material and preparation method thereof |
| CN110787821A (en) * | 2019-09-10 | 2020-02-14 | 温州大学 | Graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nanocomposite material with burr-like structure and preparation method and application thereof |
| CN110787821B (en) * | 2019-09-10 | 2022-06-03 | 温州大学 | Graphite-phase nitrogen carbide/cadmium sulfide photocatalytic nano composite material with burred spherical structure and preparation method and application thereof |
| CN113117718A (en) * | 2021-03-29 | 2021-07-16 | 安徽建筑大学 | NiCoP-g-C3N4/CdS composite photocatalyst, preparation method and application thereof |
| CN113117718B (en) * | 2021-03-29 | 2023-03-14 | 安徽建筑大学 | NiCoP-g-C 3 N 4 CdS composite photocatalyst, preparation method and application thereof |
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