CN106925300A - One kind synthesis CeO2The method of/CdS hetero-junctions - Google Patents
One kind synthesis CeO2The method of/CdS hetero-junctions Download PDFInfo
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- CN106925300A CN106925300A CN201710203093.1A CN201710203093A CN106925300A CN 106925300 A CN106925300 A CN 106925300A CN 201710203093 A CN201710203093 A CN 201710203093A CN 106925300 A CN106925300 A CN 106925300A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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Abstract
One kind synthesis CeO2The method of/CdS hetero-junctions, weigh a certain amount of terephthalic acid (TPA) and cysteine is dissolved in DMF and deionized water respectively, cerous nitrate is added in the DMF solution of terephthalic acid (TPA), cadmium nitrate is added in the aqueous solution of L cysteines, above two mixed solution is mixed, continue to stir so that solution is well mixed, the CeO of the polycrystalline structure of present invention synthesis2/ CdS hetero-junctions, has the advantages that good crystallinity, purity be high, good dispersion, the CeO of gained2/ CdS heterojunction composites have good application prospect.
Description
Technical field
The present invention relates to a kind of synthetic method of composite, more particularly to a kind of synthesis CeO2The side of/CdS hetero-junctions
Method.
Background technology
So far, why coordination polymer is always as the focus of field of scientific study, the crystal structure unique with it
Type and huge application value are undivided, and now, the synthetic technology of coordination polymer is very ripe, and it is except being employed
Outside each field, it is also used as preparing the presoma of the inorganic material such as metal oxide, nitride, sulfide, uses this side
The sample of method synthesis remains the pattern of coordination polymer, so performance can be more superior, similarly, it is also possible to utilize the different gold of double-core
Category coordination polymer prepares inorganic compounding functional material as presoma, and this method is in synthesizing inorganic composite functional material side
The brand-new approach that we provides is given in face, but this method also has many challenges in specific operation process, with
Correlation report it is also rare.
Semi-conducting material can utilize regenerated resources, and carbon dioxide is not produced directly, be widely used in photocatalysis hydrogen production side
Face, now, for photolysis water hydrogen photochemical catalyst based on semiconductor, such as CdS, TiO2, ZnO, Fe2O3.But they are big
Majority is the transition metal of greater band gap, can only absorb the light in ultraviolet band in sunshine, and utilization rate is very low, though
The band gap of right CdS is smaller, is 2.42eV, can absorb the visible ray in 400-550nm wave-length coverages, but urge in actual light
Change in reaction, it easily occurs photoetch effect, inhibits practical application, and in recent years, many improvement CdS light are urged
The method of the property changed emerges in an endless stream, and the method that CdS and transition metal oxide are combined together is maximally efficient method, but
Few reports on composite rare-earth oxide, rare earth oxide due to its unique 4f electron configuration, biological medicine,
The aspect such as catalysis, luminous is all widely used, and thus, CdS is combined with rare earth oxide may obtain unexpected
Performance, by taking CeO2 as an example, because its band gap is smaller (3.2eV), be used as in recent years degradation of dye pollutant catalyst and
Light-sensitive material etc., and effect is significant.Herein study on the basis of, our seminars be devoted to by calcine the homogeneous cerium of pattern-
Cadmium different metal coordination polymer integrates the CeO2/CdS nano composite materials of absorption and photocatalysis to synthesize.
It is combined into and property Quality Research is relatively fewer on CeO2/CdS is heterogeneous at present, there are several synthesis CeO2/CdS below
The method of hetero-junctions：Document [RSC.Advances 2011,1 (7):1207-1210.] et al. with cerous nitrate, cadmium nitrate and urea
It is raw material, the CeO2/CdS hetero-junctions of monodispersity is successfully prepared using an one-step electrochemistry method.The product photolysis water hydrogen
Activity is clearly enhanced, document [Dalton Trans.2015,44:19935-19941] with nitric hydrate cerium and cadmium nitrate as former
Material, CeO2 CdS hetero-junctions, the shortcoming of electrochemical process are prepared for electrochemical process, but above-mentioned electrochemical method is for material
Generation and the more difficult control of growth rate.
The content of the invention
Semi-conducting material can utilize regenerated resources, and carbon dioxide is not produced directly, be widely used in photocatalysis hydrogen production side
Face, now, for photolysis water hydrogen photochemical catalyst based on semiconductor, such as CdS, TiO2、ZnO、Fe2O3Deng, although the band of CdS
Gap is smaller, is 2.42eV, can absorb the visible ray in 400-550nm wave-length coverages, but in actual light-catalyzed reaction,
Easily there is photoetch effect in it, inhibit practical application, in recent years, the side of many improvement CdS photocatalytics
Method emerges in an endless stream, and the method that CdS and transition metal oxide are combined together is maximally efficient method, CeO2/ CdS is combined
Material may have the performance for integrating absorption and photocatalysis.
It is an object of the invention to provide one kind synthesis CeO2The method of/CdS hetero-junctions, the method is not required to addition surface and lives
Property agent, synthetic method succinctly efficiently, synthesizes under reactor airtight condition, and synthesis step is simple, and can to the pattern of product and
Size carries out precise control.
The present invention with terephthalic acid (TPA) (PTA) and cysteine (CYS) as part, by the hot method of mixed solvent obtain cerium-
Cadmium double-core different metal coordination polymer nanosphere, then obtains CeO in the calcining of Muffle furnace high temperature2/ CdS hetero-junctions.
The invention provides one kind synthesis CeO2The method of/CdS hetero-junctions, its synthesis step is：It is closed in reactor
Under the conditions of, cerium-cadmium different metal coordination polymer nanosphere first using solvent structure, then in the protection of nitrogen atmosphere
Under calcined, obtained the CeO of polycrystalline structure2/ CdS hetero-junctions.
It is as follows that the present invention implements step：
Step one：Weigh terephthalic acid (TPA) (PTA) and cysteine (CYS) is dissolved in DMF and deionized water respectively, will
Cerous nitrate is added in the DMF solution of terephthalic acid (TPA), and cadmium nitrate is added in the aqueous solution of Cys, by above-mentioned two
Plant mixed solution to mix, continue to stir so that solution is well mixed；
Step 2：Mixed solution is transferred into reactor, is put into 100 DEG C of baking ovens and is heated 12 hours, after reaction terminates
Centrifuge washing, 60 DEG C of vacuum drying obtain cerium-cadmium double-core different metal coordination polymer nanosphere；
Step 3：Dry cerium-cadmium double-core different metal coordination polymer nanosphere is placed in tube furnace, in nitrogen
Respectively at 4h is calcined at 550 DEG C and 600 DEG C in atmosphere, CeO is obtained after being cooled to room temperature2/ CdS hetero-junctions.
With terephthalic acid (TPA) (PTA), cysteine (CYS), cerous nitrate, cadmium nitrate as raw material, DMF, deionized water are molten
Agent, first reaction obtains cerium-cadmium double-core different metal coordination polymer nanosphere in a kettle., is then calcined in tube furnace high temperature
Obtain CeO2/ CdS hetero-junctions.
The present invention by the selection to composition of raw materials, with terephthalic acid (TPA) (PTA) and cysteine (CYS) as organic linking
Body, part when distinguishing mainly due to them containing O and containing S, using mixed ligand and hybrid metal ion in solvent heat condition
Under be assembled 3d-4f metal coordinating polymers, i.e. cerium-cadmium different metal coordination polymer, because Cys and right
The mixed ligand of phthalic acid combination possesses multiple coordination sites, for the coordination of rare earth and transition metal ions provides possibility, by
This, adds cerous nitrate and cadmium nitrate in the environment of sealing, and cerium-cadmium different metal coordination polymerization has been synthesized using the hot method of mixed solvent
Thing nanosphere.
The present invention is needed by solvent heat and simple thermal treatment process, and baking oven reaction temperature is 80-160 DEG C, reaction time
It is 2-24h；550-1000 DEG C of calcining heat in tube furnace, calcination time 1-4h.
The solution have the advantages that：The present invention is closed using the method that coordination polymer presoma is calcined in the atmosphere of nitrogen
Into CeO2/ CdS hetero-junctions, synthesizes under reactor airtight condition, and synthesis step is simple, and the pattern of product and size can be entered
Row precise control, the present invention uses solvent structure presoma, due to the closed environment of reactor, can be in the condition without template
Lower formation cerium-cadmium double-core different metal coordination polymer nanosphere, the presoma is uniform in size, dispersed preferable micron ball,
The CeO of the polycrystalline structure of present invention synthesis2/ CdS hetero-junctions, has the advantages that good crystallinity, purity be high, good dispersion, gained
CeO2/ CdS heterojunction composites have good application prospect.
Brief description of the drawings
Fig. 1 is the CeO after calcining at different temperatures2The XRD spectrum of/CdS compounds.
Fig. 2 is the CeO after calcining2The TEM of/CdS compounds, HRTEM and SAED scheme.
Specific embodiment
The present invention is described in detail below in conjunction with accompanying drawing embodiment to be had the advantage that, it is intended to help reader more preferable
Ground understands essence of the invention, but can not constitute any restriction to implementation of the invention and protection domain.
Reference picture 1, XRD diffraction patterns Rigaku/Max-3A X-ray diffractometers determine (CuK α radiation), transmission electron micrograph is obtained on Japanese JEM-2100 transmission electron microscopes.
Reference picture 1, is the CeO after calcining at different temperatures2The XRD spectrum of/CdS compounds, most diffraction maximum
With the CeO of fluorite Emission in Cubic2The CdS (JCPDS 77-2306) of (JCPDS 43-1002) and hexagonal crystal phase matches, and does not have substantially
There are other miscellaneous peaks, the corresponding diffraction maximums of CdS are very sharp in figure, CeO2Diffraction maximum it is relatively weak, thus illustrate this
CeO2CdS has preferable crystallinity in/CdS compounds, additionally, compare two respectively being obtained at 550 DEG C and 600 DEG C
CeO2The collection of illustrative plates of/CdS, when finding 600 DEG C, CeO2Diffraction maximum become strong, and died down with the corresponding diffraction maximum of CdS, this
Individual phenomenon shows a liter high-temperature, CeO2Crystallinity become big, and CdS starts slow decomposition, it can thus be appreciated that the appropriate heat of selection
Treatment temperature is particularly important, and thus the sample after explanation calcining is fully converted to CeO2/ CdS compounds.
Reference picture 2, is the CeO after calcining2The TEM of/CdS compounds, HRTEM and SAED scheme, and (a), (b) are TEM in Fig. 2
Figure, (c), (d) are respectively CeO in Fig. 22The SAED figures and HREM figures of/CdS compound micron balls, (a), (b) show in Fig. 2
CeO2/ CdS compounds are still nanosphere, and simply by high temperature, decomposition and the burning of organic ligand cause the loose of ball interior
With it is porous, the diffracted electrons ring of (c) shows that product is the good polycrystalline structure of crystallinity in Fig. 2, in high definition transmission plot 2 (d)
Can be clear that there are two kinds of closely adjacent lattice fringes in figure, wherein spacing of lattice is the lattice fringe correspondence of 0.312nm
The CeO of Emission in Cubic2(111) crystal face, another spacing of lattice is the CdS of the lattice fringe correspondence hexagonal crystal phase of 0.334nm
(002) crystal face, therefore, based on the above results understand the product be a heterojunction structure.
Embodiment 1：
Step one：Weigh terephthalic acid (TPA) (PTA) and cysteine (CYS) is dissolved in DMF and deionized water respectively, will
Cerous nitrate is added in the DMF solution of terephthalic acid (TPA), and cadmium nitrate is added in the aqueous solution of Cys, by above-mentioned two
Plant mixed solution to mix, continue to stir so that solution is well mixed；
Step 2：Mixed solution is transferred into reactor, is put into 100 DEG C of baking ovens and is heated 12 hours, after reaction terminates
Centrifuge washing, 60 DEG C of vacuum drying obtain cerium-cadmium double-core different metal coordination polymer nanosphere；
Step 3：Dry typical sample is placed in tube furnace, respectively at 550 DEG C and 600 in the atmosphere of nitrogen
4h is calcined at DEG C, CeO is obtained after being cooled to room temperature2/ CdS hetero-junctions.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to model of the invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, those of ordinary skill in the art are to technical side of the invention
Various modifications and improvement that case is made, all should fall into the protection domain of claims of the present invention determination.
Claims (2)
1. it is a kind of to synthesize CeO2The method of/CdS hetero-junctions, it is characterised in that step one：Weigh a certain amount of terephthalic acid (TPA) and
Cysteine is dissolved in DMF and deionized water respectively, and cerous nitrate is added in the DMF solution of terephthalic acid (TPA), by nitric acid
Cadmium is added in the aqueous solution of Cys, and above two mixed solution is mixed, and continues to stir so that solution is mixed
Close uniform；Step 2：Mixed solution is transferred into reactor, is put into 100 DEG C of baking ovens and is heated 12 hours, reaction terminate after from
The heart is washed, and 60 DEG C of vacuum drying obtain cerium-cadmium double-core different metal coordination polymer nanosphere；Step 3：By dry cerium-cadmium
Double-core different metal coordination polymer nanosphere is placed in tube furnace, respectively at calcination at 550 DEG C and 600 DEG C in the atmosphere of nitrogen
4h, CeO is obtained after being cooled to room temperature2/ CdS hetero-junctions.
2. the one kind described in a claim 1 synthesizes CeO2The method of/CdS hetero-junctions, it is characterised in that with terephthalic acid (TPA), half
Cystine, cerous nitrate, cadmium nitrate are raw material, and DMF, deionized water are solvent, and it is different that first reaction in a kettle. obtains cerium-cadmium double-core
Metal coordinating polymer nanosphere, then obtains CeO in the calcining of tube furnace high temperature2/ CdS hetero-junctions.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710203093.1A CN106925300A (en) | 2017-03-30 | 2017-03-30 | One kind synthesis CeO2The method of/CdS hetero-junctions |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108176407A (en) * | 2017-12-13 | 2018-06-19 | 江苏大学 | A kind of Ce-In composite material photocatalysts and preparation method and purposes |
| CN109364949A (en) * | 2018-09-25 | 2019-02-22 | 武汉大学苏州研究院 | Ultraviolet-visible-near infrared light response PbS/TiO2Nanotube reunion microballoon hetero-junctions, preparation method and use |
| CN115888656A (en) * | 2022-11-29 | 2023-04-04 | 四川轻化工大学 | Hydrothermal synthesis method of metal organic framework Cys-MIL-101 adsorbent |
| CN116851006A (en) * | 2023-07-07 | 2023-10-10 | 江苏大学 | Preparation method of leaf-shaped Ce-doped CdS photocatalyst and application of photocatalyst in preparing fuel by mineralizing organic matters |
-
2017
- 2017-03-30 CN CN201710203093.1A patent/CN106925300A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 马丹阳: "含O和S配位聚合物微/纳米结构的合成与转化", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108176407A (en) * | 2017-12-13 | 2018-06-19 | 江苏大学 | A kind of Ce-In composite material photocatalysts and preparation method and purposes |
| CN109364949A (en) * | 2018-09-25 | 2019-02-22 | 武汉大学苏州研究院 | Ultraviolet-visible-near infrared light response PbS/TiO2Nanotube reunion microballoon hetero-junctions, preparation method and use |
| CN115888656A (en) * | 2022-11-29 | 2023-04-04 | 四川轻化工大学 | Hydrothermal synthesis method of metal organic framework Cys-MIL-101 adsorbent |
| CN116851006A (en) * | 2023-07-07 | 2023-10-10 | 江苏大学 | Preparation method of leaf-shaped Ce-doped CdS photocatalyst and application of photocatalyst in preparing fuel by mineralizing organic matters |
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