CN109647487A - The Cu of p-n junction structure2O@g-C3N4Nanocomposite, synthesis preparation method and its application - Google Patents

The Cu of p-n junction structure2O@g-C3N4Nanocomposite, synthesis preparation method and its application Download PDF

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CN109647487A
CN109647487A CN201910085056.4A CN201910085056A CN109647487A CN 109647487 A CN109647487 A CN 109647487A CN 201910085056 A CN201910085056 A CN 201910085056A CN 109647487 A CN109647487 A CN 109647487A
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junction structure
junction
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hydrogen production
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侯东芳
邓敏
田逢雨
乔秀清
李东升
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China Three Gorges University CTGU
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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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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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

本发明公开了一种p‑n结结构氧化亚铜与石墨相氮化碳纳米复合材料的制备及其在光催化产氢中的应用，属于纳米材料制备技术及能源开发领域。本发明采用两步法合成技术，首先利用尿素为原料，经过高温缩聚处理合成多孔石墨相氮化碳，然后将硝酸铜溶于DMF溶液中，加入不同量的石墨相氮化碳，经过特定的程序控温，溶剂热法得到Cu2O@g‑C3N4复合材料。该复合材料是由p型Cu2O中空纳米球和n型g‑C3N4纳米片组成的新型Cu2O@g‑C3N4 p‑n结光催化剂。其中，空心Cu2O纳米球不仅可以作为一种优良的光敏剂，而且还可以在腔内实现太阳光的多次反射，从而在内置p‑n结的协同作用下实现了较高的光催化分解。经实验发现，该纳米复合材料具有优异的光催化产氢活性。

The invention discloses the preparation of a p-n junction structure cuprous oxide and graphitic carbon nitride nanocomposite material and its application in photocatalytic hydrogen production, belonging to the fields of nanomaterial preparation technology and energy development. The invention adopts a two-step synthesis technology. First, urea is used as a raw material, and the porous graphitic carbon nitride is synthesized by high-temperature polycondensation treatment. Then, copper nitrate is dissolved in a DMF solution, and different amounts of graphitic carbon nitride are added. The Cu 2 O@g‑C 3 N 4 composite was obtained by programmed temperature control and solvothermal method. The composite material is a novel Cu 2 O@g-C 3 N 4 p-n junction photocatalyst composed of p-type Cu 2 O hollow nanospheres and n-type g-C 3 N 4 nanosheets. Among them, the hollow Cu 2 O nanospheres can not only serve as an excellent photosensitizer, but also can realize multiple reflections of sunlight in the cavity, thus achieving high photocatalysis under the synergistic effect of built-in p-n junctions break down. It was found by experiments that the nanocomposite has excellent photocatalytic hydrogen production activity.

Description

The Cu2O@g-C3N4 nanocomposite of p-n junction structure, synthesis preparation method and its Using
Technical field
The invention belongs to nano material preparation technology and energy development fields, and in particular to a kind of cuprous oxide and graphite-phase The preparation of azotized carbon nano composite material and its application in Photocatalyzed Hydrogen Production.
Background technique
Current social, energy crisis are increasingly sharpened with environmental pollution, and people show keen interest to new energy technology, And Hydrogen Energy is widely regarded as one of following most promising fossil fuel substitute as a kind of green regenerative energy sources, directly It connects then more simple and economical using sun photodegradation aquatic products hydrogen.Photocatalysis technology is can use of developing rapidly in recent years The sun can be carried out the new technology of the depollution of environment and energy conversion.Currently, photocatalysis technology is in environmental protection, health care, organic synthesis Etc. application study quickly grow, conductor photocatalysis becomes one of most active research field in the world.
g-C3N4As a kind of typically without metal-polymer semiconductor light-catalyst, there is good environment friendly, table Face is synthetic, good physical and chemical stability and unique characteristic electron.Cuprous oxide (Cu2O) have good environment can Acceptance, natural abundance and low energy gap (2.0 eV), it is considered to be enhancing g-C3N4The one of based nano composite material visible absorption The up-and-coming material of kind.With pure g-C3N4And Cu2O is compared, the Cu of preparation2O@g-C3N4P-n heterojunction has higher light Catalytic activity.This work is to realize the solar energy conversion of the non precious metal photocatalysis hetero-junctions of high activity and using before providing Scape.
Summary of the invention
The object of the present invention is to provide a kind of novel photocatalyst composite material and preparation methods, and are applied to light Catalysis produces hydrogen, and preparation method is rationally simple, and H2-producing capacity is obviously improved, with excellent Photocatalyzed Hydrogen Production activity.
The present invention is with three-dimensional hollow Cu2O nanosphere and g-C3N4Nanometer sheet is unit material, by Cu2O introduces g-C3N4 The Cu of the middle 3D or 2D for forming p-n knot2O@ g-C3N4Composite nano materials have synthesized the 3D/2D Cu of a series of novel2O@ g-C3N4Nanocomposite.During producing hydrogen using visible light photocatalysis, the introducing of Cu2O and g-C3N4 form p-n Knot, after the two fermi level reaches balance, so that the light induced electron of system and hole separate, while the presence of built in field The transfer for promoting carrier enables more photo-generated carriers to participate in effectively reacting, leads to the photocatalysis of catalyst Activity significantly improves.By SEM figure as can be seen that Cu2O nanosphere is uniformly embedded in duct and the interlayer of g-C3N4；g- C3N4 nanometer sheet and Cu2O nanosphere are successfully combined with each other, and contact is close between each other, forms heterojunction structure, It is advantageously implemented efficiently separating for electronics and hole, so that photocatalytic activity enhances.And Cu2O is in hollow structure, and it is this hollow Structure is conducive to the absorption of light, to improve photocatalysis performance, and has bigger specific surface area, can make photochemical catalyst exposure More active sites out, and bigger specific surface area during photocatalytic hydrogen production by water decomposition make catalyst with react molten The contact area of liquid becomes larger, to improve catalytic activity.
To achieve the above object, the technical solution that this discovery uses are as follows:
It is condensed to form graphite phase carbon nitride by high temperature sintering by presoma of urea first, then weighs different amounts of graphite-phase Carbonitride and nitric hydrate copper, its ratio be 1:0.5 ~ 3.5, obtained by solvent-thermal method by p-type Cu2O nanosphere and N-shaped g- C3N4The a series of new Cu of nanometer sheet composition2O@g-C3N4P-n junction photochemical catalyst, is tested by Photocatalyzed Hydrogen Production.
Cu of the present invention with excellent Photocatalyzed Hydrogen Production performance2O-C3N4The preparation method packet of nanocomposite Include following steps:
(1) a certain amount of urea is weighed, is put into crucible (loading 70-80%) with cover, (the Muffle furnace in still air In) heating certain time, faint yellow fluffy g-C can be obtained3N4Nanometer sheet.
(2) by g-C obtained in step (1)3N4Nanometer sheet is fully ground in the agate mortar, nitric hydrate copper and g- C3N4Sample (the two ratio is 1:0.5 ~ 3.5) is dispersed in n,N-Dimethylformamide (DMF), and ultrasonic treatment forms uniform Solution.
(3) mixed solution that step (2) obtains is transferred in the ptfe autoclave liner of 50 ml, is covered close Envelope, is put into baking oven, and process control hydrothermal temperature is 100-250 DEG C, the hydro-thermal reaction time 20-30h.Hydro-thermal reaction is complete It is cooled to room temperature after, it is multiple with pure water and ethanol washing after obtained mixed liquor product is centrifuged in centrifuge, so It is dry in vacuum oven afterwards.
The present invention also provides a kind of by Cu2O-C3N4Research method of the nanocomposite applications on Photocatalyzed Hydrogen Production.Tool Body step includes the following: under visible light illumination, to have carried out hydrogen manufacturing experiment in closing quartz reaction system, passed through cooling cycle The temperature of reaction system is maintained at 6 DEG C by water, a certain amount of catalyst is dispersed in the aqueous solution of methanol, wherein methanol conduct Sacrifice agent is completely removed air with continuous stirring, with the 300W Xe arc lamp of 420 nm optical filters (CEL-HXF300) For light source, liberation of hydrogen analysis is carried out using online gas chromatography (FULI, GC-7920).It is tested by Photocatalyzed Hydrogen Production, it is known that CuCN150 H2-producing capacity is the most excellent.
Detailed description of the invention
Fig. 1: for catalyst Cu made from embodiment 12O、CuCN50、CuCN75、CuCN100、CuCN150、CuCN200、 The X-ray diffractogram of CuCN250.
Fig. 2: for catalyst g-C made from embodiment 13N4, Cu2The scanning electron microscope (SEM) photograph of O, CuCN150.
Fig. 3: for catalyst g-C made from embodiment 13N4,Cu2The transmission electron microscope picture of O, CuCN150.
Fig. 4: scheme for the XPS of catalyst CuCN150 made from embodiment 1.
Fig. 5: for catalyst g-C made from embodiment 13N4, Cu2O,CuCN50, CuCN75, CuCN100, CuCN150, The ultraviolet-visible diffuse reflectance spectrum figure of CuCN200, CuCN250.
Fig. 6: for catalyst Cu made from embodiment 12The Mott-Schottky of O schemes.
Fig. 7: for catalyst CuCN50, CuCN75, CuCN100, CuCN150, CuCN200, CuCN250 each in embodiment 2 Production hydrogen histogram.
Specific embodiment
It is arranged below with reference to specific implementation case, the present invention is further explained, it should be understood that these case study on implementation are merely to illustrate this It invents rather than limits the scope of the invention, after the present invention has been read, those skilled in the art are to of the invention various The modification of equivalent form falls within the application range as defined in the appended claims.
Embodiment 1
1) 10g urea is weighed, is put into crucible, is closed the lid.
2) crucible is placed in Muffle furnace, 4 h of heat condensation in 550 DEG C of still air, the rate of heat addition be 15 DEG C/ Min takes out after being down to room temperature naturally, and obtaining faint yellow fluffy product is porous g-C3N4。
3) g-C that will be obtained3N4Nanometer sheet is fully ground in the agate mortar.Weigh 73 mg nitric hydrate copper and certain The g-C of amount3N4Sample (0,50,75,100,150,200,250 mg) is dispersed in the n,N-Dimethylformamide (DMF) of 30 ml In, 30 min of ultrasonic treatment form uniform solution.Obtained mixed solution is transferred to the ptfe autoclave of 50 ml It in liner, seals, is put into baking oven, 24 h are heated at 150 DEG C, then 8 h of laser heating at 180 DEG C.
4) the mixed liquor product obtained after 8000 r/min centrifuge separation, is washed respectively in centrifuge with pure water and ethyl alcohol It washs 3 times, collects product, then dry 10 h in 60 DEG C of baking ovens.Sample is labeled as Cu2O, CuCN50, CuCN75, CuCN100, CuCN150, CuCN200, CuCN250 are respectively corresponded and g-C are added3N4Weight is 0,50,75,100,150,200, Product when 250 mg.
Embodiment 2
1) composite catalyst obtained in embodiment 1 is carried out to the Photocatalyzed Hydrogen Production of visible light.
2) hydrogen manufacturing experiment under visible light illumination, has been carried out in closing quartz reaction system, it will by cooling circulating water The temperature of reaction system is maintained at 6 DEG C, 50 mg catalyst is dispersed in the aqueous solution (80 ml) of 8 ml methanol, wherein methanol As sacrifice agent, air is completely removed with continuous stirring, with 300 W Xe of 420 nm optical filters (CEL-HXF300) Arc lamp is light source, carries out liberation of hydrogen analysis using online gas chromatography (FULI, GC-7920).It is small every 1 after illumination starts When sampling it is primary, obtain producing hydrogen histogram shown in Fig. 7.It can be concluded that g-C3N4Product when weight is 150 mg is added CuCN150 hydrogen output is 637.5 μm of olh-1·g-1, this is than pure g-C3N4Hydrogen output is higher by more than 40 times.
The features of the present invention and advantage-Characteristics and preparation characteristic
g-C3N4(n-type semiconductor) and Cu2O(p type semiconductor) fermi level (Ef) respectively close to CB and VB, when they are mutual When contact, g-C3N4Fermi level move down, and Cu2The fermi level of O moves up, until the fermi level of the two is equal, is formed different Matter p-n junction.In the process, direction is by N-shaped g-C3N4It is directed toward p-type Cu2The built in field of O is established.When radiation of visible light, n Type g-C3N4Photohole in semiconductor valence band can be transferred to Cu2In the valence band of O, while p-type Cu2On O semiconductor conduction band Light induced electron can be transferred to g-C3N4Conduction band on.In the space-charge region of heterogeneous p-n, on built in field can promote State the transfer of light induced electron and photohole.Therefore in illumination space-charge region, light induced electron is gathered in n-type semiconductor one Side, and photohole is gathered in p-type semiconductor side, effectively inhibits the compound of photo-generate electron-hole pair.The result shows that p-type Cu2O and N-shaped g-C3N4The p-n junction formed between interface can efficiently separate Cu2O/g-C3N4Photo-induction in heterojunction structure is conductive Lotus, while the compound of electron-hole pair can be substantially reduced.In order to illustrate photocatalysis hydrogen production reaction mechanism, it is necessary to clearly hollow Cu2O nanosphere improves g-C by two kinds of effects3N4Activity: (1) p-n junction induction effective electron and hole separation；(2) Hollow nano-sphere is ideal visible photosensitizing agents.
The present invention selects three-dimensional hollow Cu2O nanosphere is candidate material, has synthesized a series of special 3D/2D Cu2O/g- C3N4Nanocomposite.Cu2O nanosphere is the g-C for being anchored on surface well or being wrapped in stratiform3N4In nanometer sheet, formed Close contact, is conducive to the transfer of carrier.Compared with previous research, Cu that this research obtains2O/g-C3N4Nanometer is multiple Condensation material shows excellent Photocatalyzed Hydrogen Production activity.It is considered that hollow Cu2O nanosphere acts not only as a kind of excellent Photosensitizer, and sunlight can be made in intracavitary carry out multiple reflections, to be realized under the synergistic effect of built-in p-n junction higher H2Photocatalysis is developed.The present invention is converted and is utilized as the solar energy for the non precious metal photocatalysis hetero-junctions for realizing high activity and mentions Prospect is supplied.

Claims (8)

1.p-n结结构的Cu2O@g-C3N4纳米复合材料，其特征在于，该材料将Cu2O 引入g-C3N4 中形成p-n 结的3D或2D的 Cu2O@ g-C3N4复合纳米材料。1. Cu 2 O@gC 3 N 4 nanocomposite material with pn junction structure, characterized in that the material introduces Cu 2 O into g-C3N4 to form a 3D or 2D Cu 2 O@gC 3 N 4 composite of pn junction nanomaterials. 2.根据权利要求1所述的p-n结结构的Cu2O@g-C3N4纳米复合材料，其特征在于，所述的Cu2O为空心纳米球颗粒，该Cu2O空心纳米球颗粒均匀的镶嵌在g-C3N4 的孔道及层间。2 . The Cu 2 O@gC 3 N 4 nanocomposite material with pn junction structure according to claim 1 , wherein the Cu 2 O is hollow nanosphere particles, and the Cu 2 O hollow nanosphere particles are uniform. 3 . are embedded in the channels and interlayers of g-C3N4. 3.根据权利要求1或2所述的p-n结结构的Cu2O@g-C3N4纳米复合材料的制备方法，其特征在于，包括如下步骤：3. The preparation method of the Cu 2 O@gC 3 N 4 nanocomposite material of pn junction structure according to claim 1 or 2, characterized in that, comprising the following steps: （1）将尿素放入带盖的坩埚中，在静态空气中的马弗炉中，500-600℃下缩(1) Put urea into a crucible with a lid, shrink it in a muffle furnace in static air at 500-600°C 合反应3-5h，得到淡黄色蓬松g-C3N4纳米片；The combined reaction was carried out for 3-5 h to obtain pale yellow fluffy gC 3 N 4 nanosheets; （2）将步骤（1）中得到的g-C3N4纳米片在玛瑙研钵中充分研磨，将水合硝(2) The gC 3 N 4 nanosheets obtained in step (1) are fully ground in an agate mortar, and the hydrated nitrate 酸铜和g-C3N4纳米片样品分散在N，N-二甲基甲酰胺中，超声处理以形成均匀的混合溶液；The copper acid and gC3N4 nanosheet samples were dispersed in N,N - dimethylformamide and sonicated to form a homogeneous mixed solution; （3）将步骤（2）得到的混合溶液转移到聚四氟乙烯反应釜内衬中，加盖密(3) Transfer the mixed solution obtained in step (2) into the lining of the polytetrafluoroethylene reactor, and seal it tightly. 封，放入烘箱中程控加热进行水热反应，冷却至室温，用纯水和乙醇洗涤多次，然后在烘箱中干燥，即可得到p-n结结构的Cu2O@g-C3N4纳米复合材料。sealed, placed in an oven for program-controlled heating for hydrothermal reaction, cooled to room temperature, washed with pure water and ethanol for several times, and then dried in an oven to obtain Cu 2 O@gC 3 N 4 nanocomposites with pn junction structure . 4.根据权利要求1所述的p-n结结构的Cu2O@g-C3N4纳米复合材料的制备方法，其特征在于，步骤（1）中水合硝酸铜与g-C3N4纳米片的质量比为1：0.5~3.5。4 . The preparation method of Cu 2 O@gC 3 N 4 nanocomposite material with pn junction structure according to claim 1, wherein the mass ratio of hydrated copper nitrate to gC 3 N 4 nanosheets in step (1) is It is 1:0.5~3.5. 5.根据权利要求1所述的p-n结结构的Cu2O@g-C3N4纳米复合材料的制备方法，其特征在于，步骤（2）中水热反应温度为100-250℃，水热反应时间为20-30h。5 . The method for preparing Cu 2 O@gC 3 N 4 nanocomposites with pn junction structure according to claim 1 , wherein in step (2), the hydrothermal reaction temperature is 100-250° C., and the hydrothermal reaction The time is 20-30h. 6.根据权利要求1或2所述的p-n结结构的Cu2O@g-C3N4纳米复合材料在光催化产氢上的应用。6 . The application of the Cu 2 O@gC 3 N 4 nanocomposite with pn junction structure according to claim 1 or 2 in photocatalytic hydrogen production. 7 . 7.根据权利要求6所述的应用，其特征在于，具体步骤包括如下：在可见光照射下，在封闭石英反应***中进行了制氢实验，通过冷却循环水将反应体系的温度保持在3-8℃，将p-n结结构的Cu2O@g-C3N4纳米复合材料分散在甲醇的水溶液中，在连续搅拌下将其完全除去空气，以附以大于420 nm截止滤光片CEL-HXF300的300 W Xe弧光灯为光源，即可得到氢气。7. application according to claim 6, is characterized in that, concrete steps comprise as follows: under visible light irradiation, carried out hydrogen production experiment in closed quartz reaction system, by cooling circulating water, the temperature of reaction system is kept at 3- The Cu 2 O@gC 3 N 4 nanocomposites with pn junction structure were dispersed in an aqueous solution of methanol at 8 °C, and the air was completely removed under continuous stirring to attach a larger than 420 nm cut-off filter CEL-HXF300. A 300 W Xe arc lamp is used as the light source to obtain hydrogen gas. 8.根据权利要求7所述的应用，其特征在于，甲醇作为牺牲剂，浓度为5%-30%。8. application according to claim 7 is characterized in that, methanol is used as sacrificial agent, and the concentration is 5%-30%.
CN201910085056.4A 2019-01-18 2019-01-18 The Cu of p-n junction structure2O@g-C3N4Nanocomposite, synthesis preparation method and its application Pending CN109647487A (en)

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CN110523421A (en) * 2019-06-17 2019-12-03 湖南大学 A kind of photocatalyst and its preparation method and application
CN110586135A (en) * 2019-09-24 2019-12-20 河南师范大学 Containing Mn0.5Cd0.5S and Cu2Preparation method of O-supported photocatalyst
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CN114768844A (en) * 2022-03-23 2022-07-22 桂林电子科技大学 Preparation method and application of ultra-thin porous sheet g-C3N4 photocatalyst
CN117696100A (en) * 2024-02-06 2024-03-15 太原科技大学 A kind of g-C3N4/FeOOH/Cu2O nano-heterojunction photocatalyst and its preparation method and application

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