CN109663600A - One-step preparation method of multiphase uniform load - Google Patents
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Abstract
本发明公开了一种多相均匀负载物的一步制备方法，涉及多相负载物制备技术领域。该多相均匀负载物的一步制备方法包括将多个挥发物分别放置在石英管的不同温区；向石英管通入辅助气体，并在石英管内的辅助气体的流向的下游煅烧形成多相均匀负载物。并具体地将利用CdS和MoO3挥发温度相似，且可随气流吹出的特点，将二者共挥发并在高温区反应，得到CdS纳米颗粒在超薄六边形MoO2纳米片上均匀负载的复合物，并且具有很好的光催化产氢性能。此方法用于多相负载具有制备方法简单，制备成本低廉，且不会产生对环境不利的副产物，负载均匀，性能优异等特点，在能源环境中对于一些两相材料的制备具有很好的应用前景。
The invention discloses a one-step preparation method of a multiphase uniform load, and relates to the technical field of the preparation of a multiphase load. The one-step preparation method of the multi-phase uniform load comprises placing a plurality of volatiles in different temperature zones of a quartz tube respectively; introducing auxiliary gas into the quartz tube, and calcining downstream of the flow direction of the auxiliary gas in the quartz tube to form a multi-phase uniform load. Specifically, the characteristics of CdS and MoO 3 that have similar volatilization temperatures and can be blown out with the airflow will be co-volatile and reacted in the high temperature region to obtain a composite of CdS nanoparticles uniformly supported on ultra-thin hexagonal MoO 2 nanosheets. and has good photocatalytic hydrogen production performance. This method for multiphase loading has the characteristics of simple preparation method, low preparation cost, no by-products that are unfavorable to the environment, uniform loading, excellent performance, etc. It is very suitable for the preparation of some two-phase materials in the energy environment. application prospects.
Description
Technical field
The present invention relates to the preparation technical fields of multiphase load object, and an in particular to a kind of step of multiphase uniform load object
Preparation method.
Background technique
Nowadays, energy crisis is still a great problem of world's progress and development, development clean reproducible hydrogen energy source at
For the big hot spot developed now, due to many non-renewable energy resources of traditional hydrogen producing technology consumption and pollution can be generated, so
Photocatalytic hydrogen production by water decomposition technology just becomes the hot spot of nowadays energy technology.The basic demand of photocatalytic semiconductor is to lead first
Band position is more negative than zero, and valence band location is greater than 1.23ev, i.e., forbidden bandwidth will across and be greater than 1.23ev, be likely to for light
Water is catalytically decomposed, secondly common semiconductor titanium dioxide can only absorb ultraviolet light, and ultraviolet accounts for the 4% of sunlight, to open up
The utilization for opening up sunlight, needs the semiconductor of suitable forbidden bandwidth, wherein most typically CdS.But CdS also has lacking for it
Point is exactly photoetch problem first, furthermore be it photo-generate electron-hole be easy it is compound again, reduce photocatalytic speed.It is common
Improved method be load cocatalyst on the semiconductor, improve the separation of electron hole, or prepare two semiconductors
Heterojunction structure, problem above is improved by the level-density parameter of the two.Two-phase complex method generally there are prepare it is more complicated or
The problems such as person's load is uneven, and can generate and much be unfavorable for environmental-friendly by-product, so that many composite constructions is difficult to structure
It makes.
Summary of the invention
The purpose of the present invention is to provide an a kind of one step preparation method of multiphase uniform load object, this method can step preparation
Uniform multiphase load object is obtained, preparation method is simple, and preparation cost is cheap, and will not generate the by-product unfavorable to environment,
Load Balanced the features such as haveing excellent performance, has a good application prospect the preparation of some two phase materials in energy environment.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes an a kind of one step preparation method of multiphase uniform load object comprising:
Multiple volatile matters are individually positioned in the different warm areas of quartz ampoule；
It is passed through auxiliary gas to quartz ampoule, and the downstream of the flow direction of the auxiliary gas in quartz ampoule calcines that form multiphase equal
Even loaded article.
An one step preparation method of multiphase uniform load object, passes through quick and easy one-step method provided by the embodiment of the present invention
Multiphase load object can be prepared, and the compound of the controllable multiphase load of loading process is used for Photocatalyzed Hydrogen Production, has very big
Application prospect.Also, in an embodiment of the present invention, by MoO3As presoma, MoO3Under certain reducing atmosphere, pass through
Control air-flow can prepare ultra-thin hexagon MoO2Nanometer sheet utilizes CdS and MoO3Volatilization temperature is similar, and can be with air-flow
The two is total to volatilization and reacted in high-temperature region, obtains CdS nano particle in ultra-thin hexagon MoO by the characteristics of blowout2In nanometer sheet
The compound of uniform load, and there is good Photocatalyzed Hydrogen Production performance.The method has preparation method for two phase loads
Simply, preparation cost is cheap, and will not generate the by-product unfavorable to environment, Load Balanced, the features such as haveing excellent performance, in the energy
The preparation of some two phase materials is had a good application prospect in environment.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the preparation-obtained CdS/MoO of the embodiment of the present invention 12SEM figure；
Fig. 2 is the preparation-obtained CdS/MoO of the embodiment of the present invention 22SEM figure；
Fig. 3 is the preparation-obtained CdS/MoO of the embodiment of the present invention 32SEM figure；
Fig. 4 is the preparation-obtained CdS/MoO of the embodiment of the present invention2XRD diagram；
Fig. 5 is the properties of sample figure for the different CdS load capacity that the embodiment of the present invention 1~3 provides.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
An one step preparation method of the multiphase uniform load object of the embodiment of the present invention is specifically described below.
An a kind of one step preparation method of multiphase uniform load object comprising:
Multiple volatile matters are individually positioned in the different warm areas of quartz ampoule；
It is passed through auxiliary gas to quartz ampoule, and the downstream of the flow direction of the auxiliary gas in quartz ampoule calcines that form multiphase equal
Even loaded article.
In detail, multiphase load object, and the multiphase that loading process is controllable can be prepared by quick and easy one-step method
The compound of load is used for Photocatalyzed Hydrogen Production, there is very big application prospect.
Further, in the preferred embodiment, multiple volatile matters are individually positioned in the not equality of temperature of quartz ampoule
Area specifically includes: two volatile matters are individually positioned in the different warm areas of quartz ampoule.Certainly, in the other embodiment of the present invention
In, the number of volatile matter can also be it is multiple, be not limited in two, can also for three, it is four or even more, it is of the invention
Embodiment is without limitation.
Further, in the preferred embodiment, one of volatile matter is CdS in two volatile matters, another
A volatile matter is MoO3.Certainly, in other embodiments of the invention, the type of volatile matter can also be selected according to demand
It selects, is not limited in CdS and MoO3.Wherein, it is passed through auxiliary gas to quartz ampoule, so that CdS and MoO3It is calcined in quartz ampoule
Multiphase uniform load object is formed, multiphase uniform load object is CdS/MoO2Loaded article.Obtained compound has good light
It is catalyzed H2-producing capacity.CdS/MoO is prepared by this method2Loaded article, simple process is feasible, environmental-friendly, solves biography
The problem that amount in the case of system calcining is uncontrollable and the compound uniformity of two-phase is bad, and there is good Photocatalyzed Hydrogen Production
Energy.
Further, in the preferred embodiment, 780~795 DEG C of the temperature of the present position of CdS, MoO3's
795~805 DEG C of the temperature of present position.Preferably, 790 DEG C of the temperature of the present position of CdS, MoO3Present position temperature
800℃.Certainly, in other embodiments of the invention, the temperature of the present position of CdS can also be near 790 DEG C, MoO3
The temperature of present position can also be near 800 DEG C, the embodiment of the present invention is without limitation.By MoO3As presoma, MoO3
Under certain reducing atmosphere, ultra-thin hexagon MoO can be prepared by controlling air-flow2Nanometer sheet utilizes CdS and MoO3
Volatilization temperature is similar, and the characteristics of can blow out with air-flow, and the two is total to volatilization and is reacted in high-temperature region, CdS nano particle is obtained
In ultra-thin hexagon MoO2The compound of uniform load in nanometer sheet, and there is good Photocatalyzed Hydrogen Production performance.The method
Have preparation method simple for two phase loads, preparation cost is cheap, and will not generate the by-product unfavorable to environment, and load is equal
It is even, the features such as haveing excellent performance, the preparation of some two phase materials is had a good application prospect in energy environment.
Further, in the preferred embodiment, MoO3Dosage be 5g, the dosage of CdS is 0.6~2g.It is logical
Overregulate the CdS and MoO of addition early period3Amount, the compound of different proportion can be obtained, to meet various production requirements.
Further, in the preferred embodiment, the dosage of CdS is specifically as follows appointing in 0.6g, 1g, 2g
One.Certainly, in other embodiments of the invention, the dosage of CdS can also be adjusted according to demand, implementation of the invention
Example is without limitation.
Further, in the preferred embodiment, auxiliary gas is reducibility gas.Reducibility gas is in this hair
It is mainly used for reduction in bright embodiment for MoO3At MoO2.Certainly, in other embodiments of the invention, according to variety classes
Volatile matter property, can also will auxiliary gas be selected as other kinds of gas, such as inert gas, oxidizing gas
Deng the embodiment of the present invention is without limitation.
Further, in the preferred embodiment, reducibility gas can be 10%Ar/H2.Certainly, at this
In the other embodiments of invention, the specifically type of reducibility gas can also be selected according to demand, implementation of the invention
Example is without limitation.
Further, in the preferred embodiment, the flow velocity of reducibility gas is 180~220sccm.Pass through
The selection of the dosage of the setting of flow velocity and each volatile matter can effectively synthesize the multiphase uniform load object of high quality.
Further, in the preferred embodiment, CdS/MoO2Loaded article with a thickness of 1~1.5nm.This scheme
Utilize MoO3The characteristics of volatilizing altogether with CdS, the MoO prepared2Nanometer sheet is very thin, and thickness only has several nanometers of about 1.1nm, CdS particle
When being supported in nanometer sheet, particle very little is very uniform, and two-phase contacts form interfacial structure well, comes into full contact with hydrone.
By adjusting the CdS and MoO that are added early period3The compound object amount of both amount regulations.The two-phase compound of formation sufficiently combines two
The advantage of kind substance, has absorbing properties and Photocatalyzed Hydrogen Production performance well.It is multiple compared to traditional two-phase photochemical catalyst
It closing, the method preparation process is simple, and it is low in cost, it is environmentally friendly, and have excellent performance.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
Present embodiments provide a kind of one one step preparation method of multiphase uniform load object, comprising the following steps:
S1: respectively by the MoO of 5g3The different warm areas in quartz ampoule, and the present position of CdS are placed in the CdS of 0.6g
780~795 DEG C of temperature, MoO3795~805 DEG C of temperature of present position；
S2: being passed through auxiliary gas to quartz ampoule, so that CdS and MoO3Calcining forms CdS/MoO in quartz ampoule2Loaded article.
Embodiment 2
Present embodiments provide a kind of one one step preparation method of multiphase uniform load object, comprising the following steps:
S1: respectively by the MoO of 5g3The different warm areas in quartz ampoule, and the present position of CdS are placed in the CdS of 1.0g
790 DEG C of temperature, MoO3800 DEG C of temperature of present position；
S2: being passed through auxiliary gas to quartz ampoule, so that CdS and MoO3Calcining forms CdS/MoO in quartz ampoule2Loaded article.
Embodiment 3
Present embodiments provide a kind of one one step preparation method of multiphase uniform load object, comprising the following steps:
S1: respectively by the MoO of 5g3The different warm areas in quartz ampoule are placed in the CdS of 2g, and the present position of CdS
795 DEG C of temperature, MoO3805 DEG C of temperature of present position；
S2: being passed through auxiliary gas to quartz ampoule, so that CdS and MoO3Calcining forms CdS/MoO in quartz ampoule2Loaded article.
Experimental example
Embodiment 1 is recorded to the preparation-obtained difference CdS/MoO of embodiment 32SEM figure and XRD diagram, by changing
The amount for becoming CdS prepares three samples of different loads amount, as above schemes, Fig. 1-3 is different CdS/MoO respectively2The SEM of ratio
Figure, Fig. 1 show CdS when loading on a small quantity, and a small amount of nano particle is supported on ultrathin nanometer on piece, with gradually increasing for CdS,
MoO2The nano particle loaded in nanometer sheet gradually increases increase, evengranular until as shown in figure 3, under ultimate load
It is supported on ultrathin nanometer on piece.The XRD of Fig. 4 shows that No. 1 sample principal crystalline phase under a small amount of CdS load is MoO2And Cd
(MoO4), No. 2 No. 3 samples are mainly CdS and MoO2With Cd (MoO4), and No. 3 crystallinity are more preferable.It can be proved that MoO2With
The generation of CdS, and form Cd (MoO4) interface, it is therefore more likely that being MoO2/CdS/Cd(MoO4) three-phase system propose its performance
It is high.It is the properties of sample figure of different CdS load capacity shown in Fig. 5, as shown, No. 3 big properties of sample of CdS load capacity are optimal, reach
To 39.08umol/ (mgh).
In conclusion an one step preparation method of the multiphase uniform load object of the embodiment of the present invention, passes through quick and easy one
Footwork can be prepared multiphase load object, and the compound of the controllable multiphase load of loading process is used for Photocatalyzed Hydrogen Production, has very
Big application prospect.Also, in an embodiment of the present invention, by MoO3As presoma, MoO3Under certain reducing atmosphere,
Ultra-thin hexagon MoO can be prepared by controlling air-flow2Nanometer sheet utilizes CdS and MoO3Volatilization temperature is similar, and can be with
The two is total to volatilization and reacted in high-temperature region, obtains CdS nano particle in ultra-thin hexagon MoO by the characteristics of air-flow is blown out2Nanometer
The compound of on piece uniform load, and there is good Photocatalyzed Hydrogen Production performance.The method has preparation for two phase loads
Method is simple, and preparation cost is cheap, and will not generate the by-product unfavorable to environment, Load Balanced, the features such as haveing excellent performance,
The preparation of some two phase materials is had a good application prospect in energy environment.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. an a kind of one step preparation method of multiphase uniform load object, characterized in that it comprises:
Multiple volatile matters are individually positioned in the different warm areas of quartz ampoule；
It is passed through auxiliary gas to the quartz ampoule, and shape is calcined in the downstream of the flow direction of the auxiliary gas in the quartz ampoule
At multiphase uniform load object.
2. an one step preparation method of multiphase uniform load object according to claim 1, which is characterized in that described waved multiple
Hair object is individually positioned in the different warm areas of quartz ampoule, specifically includes:
Two volatile matters are individually positioned in the different warm areas of quartz ampoule.
3. an one step preparation method of multiphase uniform load object according to claim 2, it is characterised in that:
One of them described volatile matter is CdS in two volatile matters, another described volatile matter is MoO3；
Wherein, Xiang Suoshu quartz ampoule is passed through auxiliary gas, so that the CdS and MoO3Calcining forms multiphase in the quartz ampoule
Uniform load object, the multiphase uniform load object are CdS/MoO2Loaded article.
4. an one step preparation method of multiphase uniform load object according to claim 3, it is characterised in that:
780~795 DEG C of the temperature of the present position of the CdS, the MoO3795~805 DEG C of temperature of present position.
5. an one step preparation method of multiphase uniform load object according to claim 4, it is characterised in that:
The MoO3Dosage be 5g, the dosage of the CdS is 0.6~2g.
6. an one step preparation method of multiphase uniform load object according to claim 5, it is characterised in that:
The dosage of the CdS is specifically as follows any of 0.6g, 1g, 2g.
7. an one step preparation method of multiphase uniform load object according to claim 3, it is characterised in that:
The auxiliary gas is reducibility gas.
8. an one step preparation method of multiphase uniform load object according to claim 7, it is characterised in that:
The reducibility gas can be 10%Ar/H2。
9. an one step preparation method of multiphase uniform load object according to claim 7, it is characterised in that:
The flow velocity of the reducibility gas is 180~220sccm.
10. an one step preparation method of multiphase uniform load object according to claim 3, which is characterized in that:
The CdS/MoO2Loaded article with a thickness of 1~1.5nm.
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| CN110586137A (en) * | 2019-09-24 | 2019-12-20 | 河南师范大学 | Containing Mn0.5Cd0.5Preparation method of S and Au supported photocatalyst |
| CN115318307A (en) * | 2022-08-29 | 2022-11-11 | 四川启睿克科技有限公司 | Method for designing high-performance hydrogen production cocatalyst by introducing galvanic couple layer and constructing snowflake-shaped CuNi @ EDL/CdS catalyst |
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