CN105712406A - Two-dimensional Fe2Mo3O8 nano oxide with adjustable oxygen vacancies and preparation method of nano oxide - Google Patents
Two-dimensional Fe2Mo3O8 nano oxide with adjustable oxygen vacancies and preparation method of nano oxide Download PDFInfo
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Abstract
The invention provides a two-dimensional Fe2Mo3O8 nano oxide with adjustable oxygen vacancies and a preparation method of the nano oxide. Two-dimensional Fe2Mo3O8 growing under the control of dynamics is prepared, and the ratio of Oads to Olatt is adjustable in the range of 0.17-0.61. Compared with the prior art, the nano oxide and the preparation method have the advantages as follows: the preparation method is simple in technology, mild in synthesis condition, low in production cost and easy to operate; no organic templates are introduced, and pollution-free and zero-emission effects are realized; the synthesized two-dimensional Fe2Mo3O8 oxide with the adjustable oxygen vacancies adopts the two-dimensional high-energy structure and has the oxygen vacancies with adjustable concentration.
Description
Technical field
The invention belongs to new function material field, be specifically related to a kind of Lacking oxygen adjustable two dimension Fe2Mo3O8Nano-oxide and preparation method thereof.
Background technology
Metal molybdate, because of optical, electrical, the magnetic property of its uniqueness, is used widely in fields such as environmental catalysis, optical material, magnetic materials, has immeasurable research and development and is worth and market application.As functional material, its chemical composition, microstructure are very notable on the impact of its performance.Big quantity research shows, Lacking oxygen structure is very notable to the performance impact of these materials, and especially as catalysis material, Lacking oxygen is more notable to its performance impact.
Prepared by the modulation in order to realize Lacking oxygen structure, the preparation method adopted at present focuses mostly in high temperature reduction method or vacuum baking method, and operating process is not only complicated but also condition is harsh.Correlational study shows in recent years, and ion doping method can realize Lacking oxygen and construct.But, by ion doping, construct Lacking oxygen at high energy body structure surface and have not been reported.
It is generally of the material of high energy structure, there is higher low coordination atom density, than the material of low-energy configuration, there is more excellent process based prediction model.Two-dimensional nanostructure material is the high energy structural material of a quasi-representative, has significantly high chemism, is generally of good performance.Therefore, a kind of effective synthetic method of exploitation, it is achieved the modulation in two-dimensional structure Surface Oxygen room, has significantly high practical value.
Summary of the invention
It is an object of the invention to provide a kind of Lacking oxygen adjustable two dimension Fe2Mo3O8Nano-oxide, for a kind of two-dimentional Fe with a large amount of Lacking oxygen of growth in situ on metal substrate2Mo3O8Nano-oxide.
Present invention also offers a kind of Lacking oxygen adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, the process of preparation does not introduce any template and harsh conditions, by introducing ammonium chloride, make iron-based sheet in aqueous with controlled slow rate Iron Release ion, iron ion is combined with molybdate with very low concentrations, with Growth kinetics control mode, it is achieved prepared by two dimension high energy structure；Meanwhile, in the process of preparation, introduce metal ion, under the hydrothermal condition sealed, metal ion take oxygen by force with iron ion competition, form oxygen vacancy concentration adjustable two dimension iron and molybdenum oxides.
A kind of Lacking oxygen provided by the invention adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, comprises the following steps:
A, with deionized water for solvent, add ammonium chloride and molybdenum source or ammonium chloride, molybdenum source and metal cation salt, after stirring and dissolving, obtain mixed solution；
B, being placed in by iron plate in step a gained mixed solution, heated sealed is reacted, and then takes out iron plate, rinse, dry, obtains Lacking oxygen adjustable two dimension Fe2Mo3O8Nano-oxide.
In step a, temperature is 18-30 DEG C, it is preferred that be 25 DEG C；
Molybdenum source described in step a is selected from Na2MoO4·2H2O；In mixed solution, the molar concentration of ammonium chloride is 0.01～2.0mmol/L；The molar concentration of sodium molybdate is 0.1～1.0mmol/L；The molar concentration of metal cation salt is 0.01～0.20mmol/L.
Metal cation salt described in step a is selected from zinc source or nickel source, and described zinc source is selected from ZnCl2·4H2O, described nickel source is selected from NiCl2·6H2O。
In step b, iron plate is 20# iron plate；
In step b, the volume of mixed solution and the surface area ratio of iron plate be: 10～40mL/cm2；
In step b, described reacting by heating specifically: 30～80 DEG C react aging 12～72h.
In step b, described rinse is particularly as follows: be 5～6 times with the number of times of deionized water rinse, described dry particularly as follows: drying at room temperature 20-36h.
A kind of Lacking oxygen provided by the invention adjustable two dimension Fe2Mo3O8Nano-oxide, adopts said method to prepare.
Compared with prior art, preparation method technique provided by the invention is simple, and synthesis condition is gentle, and production cost is low, it is easy to operation；Do not introduce any organic formwork agent, pollution-free, zero-emission；Synthesized Lacking oxygen adjustable two dimension iron and molybdenum oxides, has two-dimentional high energy structure and the adjustable Lacking oxygen of concentration simultaneously.
Accompanying drawing explanation
Fig. 1 a is the Lacking oxygen adjustable two dimension Fe of embodiment 1 preparation2Mo3O8The SEM figure of nano-oxide；
Fig. 1 b is the Lacking oxygen adjustable two dimension Fe of embodiment 2 preparation2Mo3O8The SEM figure of nano-oxide；
Fig. 1 c is the Lacking oxygen adjustable two dimension Fe of embodiment 4 preparation2Mo3O8The SEM figure of nano-oxide；
Fig. 2 is the Lacking oxygen adjustable two dimension Fe of embodiment 1,2 and 4 preparation2Mo3O8The XRD figure of nano-oxide；A is the XRD figure of embodiment 1；B is the XRD figure of embodiment 2；C is the XRD figure of embodiment 4；
Fig. 3 is the Lacking oxygen adjustable two dimension Fe of embodiment 1,2 and 4 preparation2Mo3O8The XPS figure of the O1s of nano-oxide；Wherein: a is the sample of embodiment 1 preparation；B is the sample of embodiment 2 preparation；C is the sample of embodiment 4 preparation.
Detailed description of the invention
The invention will be further described by the examples below.
Embodiment 1
A kind of Lacking oxygen adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, comprises the following steps:
(1) by ammonium chloride, Na2MoO4·2H2O is dissolved in deionized water, obtains the mixed solution of ammonium chloride, sodium molybdate concentration respectively 0.01mmol/L and 0.1mmol/L；
(2) this mixed solution of 40mL is pipetted to 100mL sealed reactor；It is 4cm by a surface area subsequently220# iron plate be also placed in this reactor, put in water-bath, regulate bath temperature 50 DEG C, place 60h, take out subsequently, be 5 times with the number of times of deionized water rinse, the time of drying at room temperature is 24h, namely obtains one layer of fine and close two dimension Fe on iron plate surface2Mo3O8Nano-oxide.
By Fig. 1 a it can be seen that prepared iron and molybdenum oxides is two-dimensional sheet structure, thickness is about 20nm；By the XRD shown in a in Fig. 2 it can be seen that synthesized product is Fe2Mo3O8Composite oxides；By the XPS analysis of O1s shown in a in Fig. 3 it can be seen that synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.17), corresponding relatively low oxygen vacancy concentration.
Embodiment 2
A kind of Lacking oxygen adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, comprises the following steps:
(1) by ammonium chloride, Na2MoO4·2H2O、ZnCl2·4H2O is dissolved in deionized water, obtains ammonium chloride, sodium molybdate, zinc oxide concentration respectively 2.0mmol/L, 1.0mmol/L and 0.20mmol/L mixed solution；
(2) this mixed solution of 40mL is pipetted to 100mL sealed reactor；It is 1cm by a surface area subsequently220# iron plate be also placed in this reactor, put in water-bath, regulate bath temperature cause 30 DEG C, place 12h, the number of times of taking-up deionized water rinse is 6 times subsequently, and the time of drying at room temperature is 24h, namely obtains one layer of fine and close hexagon two dimension Fe at ferrum substrate surface2Mo3O8Nano-oxide.
By Fig. 1 b it can be seen that prepared iron and molybdenum oxides is hexagon two-dimensional sheet structure, thickness is about 60nm；By the XRD shown in b in Fig. 2 it can be seen that synthesized product is Fe2Mo3O8Composite oxides；By the XPS analysis of O1s shown in b in Fig. 3 it can be seen that synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.55), corresponding higher oxygen vacancy concentration.
Embodiment 3
A kind of Lacking oxygen adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, comprises the following steps:
(1) by ammonium chloride, Na2MoO4·2H2O、ZnCl2·4H2O is dissolved in deionized water, obtains the mixed solution of ammonium chloride, sodium molybdate, zinc oxide concentration respectively 0.01mmol/L, 0.1mmol/L and 0.01mmol/L；
(2) this mixed solution of 40mL is pipetted to 100mL sealed reactor；It is 2cm by a surface area subsequently220# iron plate be also placed in this reactor, put in water-bath, regulate bath temperature cause 60 DEG C, placing response 50h, the number of times of taking-up deionized water rinse is 5～6 times subsequently, and the time of drying at room temperature is 30h, and also can obtain a layer thickness at ferrum substrate surface is 80nm hexagon two dimension Fe2Mo3O8Nano-oxide.
Embodiment 4
A kind of Lacking oxygen adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, comprises the following steps:
(1) by ammonium chloride, Na2MoO4·2H2O、NiCl2·6H2O is dissolved in deionized water, obtains the mixed solution of ammonium chloride, sodium molybdate, Nickel dichloride. concentration respectively 2.0mmol/L, 1.0mmol/L and 0.20mmol/L；
(2) this mixed solution of 40mL is pipetted to 100mL sealed reactor；It is 1cm by a surface area subsequently220# iron plate be also placed in this reactor, put in water-bath, regulate bath temperature cause 40 DEG C, place 50h, the number of times of taking-up deionized water rinse is 5～6 times subsequently, and the time of drying at room temperature is 30h, namely obtains the nano flower two dimension Fe of a lamellar structure composition on iron plate surface2Mo3O8Nano-oxide.
By Fig. 1 c it can be seen that prepared iron and molybdenum oxides is hexagon two-dimensional sheet structure, thickness is about 30nm；By the XRD shown in c in Fig. 2 it can be seen that synthesized product is Fe2Mo3O8Composite oxides；By the XPS analysis of O1s shown in c in Fig. 3 it can be seen that synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.61), corresponding significantly high oxygen vacancy concentration.
Embodiment 5
A kind of Lacking oxygen adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, comprises the following steps:
(1) by ammonium chloride, Na2MoO4·2H2O、NiCl2·6H2O is dissolved in deionized water, obtains the mixed solution of ammonium chloride, sodium molybdate, Nickel dichloride. concentration respectively 0.01mmol/L, 0.1mmol/L and 0.01mmol/L；
(2) this mixed solution of 40mL is pipetted to 100mL sealed reactor；It is 2cm by a surface area subsequently220# iron plate be also placed in this reactor, put in water-bath, regulate bath temperature and cause 80 DEG C, place 72h, the number of times of taking-up deionized water rinse is 5～6 times subsequently, the time of drying at room temperature is 36h, namely obtains, at ferrum substrate surface, the nano flower two dimension Fe that a layer thickness is 40nm laminated structure composition2Mo3O8Nano-oxide.
Claims (10)
1. a Lacking oxygen adjustable two dimension Fe2Mo3O8The preparation method of nano-oxide, it is characterised in that described preparation method comprises the following steps:
A, with deionized water for solvent, add ammonium chloride and molybdenum source or ammonium chloride, sodium molybdate and metal cation salt, after stirring and dissolving, obtain mixed solution；
B, being placed in by iron plate in step a gained mixed solution, heated sealed is reacted, and then takes out iron plate, rinse, dry, obtains Lacking oxygen adjustable two dimension Fe2Mo3O8Nano-oxide.
2. preparation method according to claim 1, it is characterised in that molybdenum source described in step a is selected from Na2MoO4·2H2O。
3. preparation method according to claim 1 and 2, it is characterised in that in step a in mixed solution, the molar concentration of ammonium chloride is 0.01～2.0mmol/L；The molar concentration of sodium molybdate is 0.1～1.0mmol/L.
4. preparation method according to claim 1 and 2, it is characterised in that in step a in mixed solution, the molar concentration of metal cation salt is 0.01～0.20mmol/L.
5. the preparation method according to claim 1 or 4, it is characterised in that metal cation salt described in step a is selected from zinc source or nickel source.
6. preparation method according to claim 5, it is characterised in that described zinc source is selected from ZnCl2·4H2O。
7. the preparation method according to claim 5 or 6, it is characterised in that described nickel source is selected from NiCl2·6H2O。
8. preparation method according to claim 2, it is characterised in that in step b, the volume of mixed solution and the surface area ratio of iron plate be: 10～40mL/cm2。
9. preparation method according to claim 2, it is characterised in that in step b, described reacting by heating specifically: 30～80 DEG C react aging 12～72h.
10. a Lacking oxygen adjustable two dimension Fe2Mo3O8Nano-oxide, it is characterised in that adopt the preparation method described in any one of claim 1-9 to prepare.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111807415A (en) * | 2020-07-23 | 2020-10-23 | 陕西科技大学 | Fe2Mo3O8Micron-sized hollow sphere and preparation method thereof |
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Non-Patent Citations (3)
| Title |
|---|
| T. KURUMAJI ET AL.: "Doping-Tunable Ferrimagnetic Phase with Large Linear Magnetoelectric Effect in a Polar Magnet Fe2Mo3O8", 《PHYSICAL REVIEW X》 * |
| YAZHONG WANG ET AL.: "Unveiling hidden ferrimagnetism and giant magnetoelectricity in polar magnet Fe2Mo3O8", 《SCIENTIFIC REPORTS》 * |
| 孙永明: "钼氧化物纳米结构的构筑及其储锂性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807415A (en) * | 2020-07-23 | 2020-10-23 | 陕西科技大学 | Fe2Mo3O8Micron-sized hollow sphere and preparation method thereof |
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