CN105712406B - A kind of two-dimentional Fe2Mo3O8Nano-oxide and preparation method thereof - Google Patents
A kind of two-dimentional Fe2Mo3O8Nano-oxide and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8Nano-oxide and preparation method thereof, prepares the two-dimentional Fe grown using dynamics Controlling2Mo3O8, Oads/OlattRatio it is adjustable in the range of 0.17～0.61.Compared with prior art, the preparation method process is simple that the present invention is provided, synthesis condition are gentle, low production cost, easily operate；Any organic formwork agent, pollution-free, zero-emission are not introduced；The adjustable two-dimentional iron and molybdenum oxides of synthesized Lacking oxygen, while having two-dimentional high energy structure and the adjustable Lacking oxygen of concentration.
Description
Technical field
The invention belongs to new function material field, and in particular to a kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8Nano oxygen
Compound and preparation method thereof.
Background technology
Metal molybdate, because of its unique light, electricity, magnetic property, in fields such as environmental catalysis, optical material, magnetic materials
It is used widely, applies with immeasurable research and development value and market.It is as functional material, its chemical composition, micro-
See impact of the structure to its performance very notable.Numerous studies show, Lacking oxygen structure to the performance impact of these materials very
Significantly, especially as catalysis material, Lacking oxygen is more notable to its performance impact.
In order to prepared by the modulation for realizing Lacking oxygen structure, the preparation method for adopting at present focuses mostly in high temperature reduction method or true
Empty roasting method, not only complicated but also condition is harsh for operating process.Correlational study shows that ion doping method can realize oxygen in recent years
Room is constructed.However, by ion doping, constructing Lacking oxygen in high energy body structure surface and having not been reported.
Generally there is the material of high energy structure, with higher low coordination atom density, have than the material of low-energy configuration
More excellent process based prediction model.Two-dimensional nanostructure material is the high energy structural material of a quasi-representative, with very high
Chemism, generally with good performance.Therefore, a kind of effective synthetic method is developed, realizes that two-dimensional structure Surface Oxygen is empty
The modulation of position, with very high practical value.
The content of the invention
It is an object of the invention to provide a kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8Nano-oxide is one kind in gold
The two-dimentional Fe with a large amount of Lacking oxygens of growth in situ on category substrate2Mo3O8Nano-oxide.
Present invention also offers a kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8The preparation method of nano-oxide, is preparing
During do not introduce any template and harsh conditions, by introduce ammonium chloride, make iron-based piece in aqueous with controllable
Slow rate discharges iron ion, and iron ion is combined with molybdate with very low concentrations, with Growth kinetics control mode, realizes that two dimension is high
Can structure preparation；Meanwhile, during preparation, metal ion is introduced, under the hydrothermal condition of sealing, by metal ion and ferrum
Ion competition takes oxygen by force, forms the adjustable two-dimentional iron and molybdenum oxides of oxygen vacancy concentration.
The adjustable two-dimentional Fe of a kind of Lacking oxygen that the present invention is provided2Mo3O8The preparation method of nano-oxide, including it is following
Step：
A, with deionized water as solvent, add ammonium chloride and molybdenum source or ammonium chloride, molybdenum source and metal cation salt, stir molten
Xie Hou, obtains mixed solution；
B, iron plate is placed in mixed solution obtained by step a, heated sealed reaction, then takes out iron plate, rinse, drying,
Obtain final product the adjustable two-dimentional Fe of Lacking oxygen2Mo3O8Nano-oxide.
In step a, temperature is 18-30 DEG C, preferably 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 be 0.01～
0.20mmol/L。
Metal cation salt described in step a is selected from zinc source or nickel source, and the zinc source is selected from ZnCl2·4H2O, the nickel source
Selected from NiCl2·6H2O。
In step b, iron plate is 20# iron plates；
In step b, the volume of mixed solution with the surface area ratio of iron plate is：10～40 mL/cm2；
In step b, the reacting by heating is specifically：30～80 DEG C are reacted aging 12～72h.
In step b, the rinse is specially：The number of times of deionized water rinse is 5～6 times, and the drying is specially：Room
Temperature is dried 20-36h.
The adjustable two-dimentional Fe of a kind of Lacking oxygen that the present invention is provided2Mo3O8Nano-oxide, is prepared using said method.
Compared with prior art, the preparation method process is simple that the present invention is provided, synthesis condition are gentle, low production cost,
Easily operate；Any organic formwork agent, pollution-free, zero-emission are not introduced；The adjustable two-dimentional ferrum molybdenum oxidation of synthesized Lacking oxygen
Thing, while having two-dimentional high energy structure and the adjustable Lacking oxygen of concentration.
Description of the drawings
Fig. 1 a are the adjustable two-dimentional Fe of Lacking oxygen prepared by embodiment 12Mo3O8The SEM figures of nano-oxide；
Fig. 1 b are the adjustable two-dimentional Fe of Lacking oxygen prepared by embodiment 22Mo3O8The SEM figures of nano-oxide；
Fig. 1 c are the adjustable two-dimentional Fe of Lacking oxygen prepared by embodiment 42Mo3O8The SEM figures of nano-oxide；
Fig. 2 is the adjustable two-dimentional Fe of Lacking oxygen prepared by embodiment 1,2 and 42Mo3O8The XRD figure of nano-oxide；A is real
Apply the XRD figure of example 1；XRD figure of the b for embodiment 2；XRD figure of the c for embodiment 4；
Fig. 3 is the adjustable two-dimentional Fe of Lacking oxygen prepared by embodiment 1,2 and 42Mo3O8The XPS of the O 1s of nano-oxide
Figure；Wherein：A is sample prepared by embodiment 1；B is sample prepared by embodiment 2；C is sample prepared by embodiment 4.
Specific embodiment
Below by embodiment, the invention will be further described.
Embodiment 1
A kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8The preparation method of nano-oxide, comprises the following steps：
(1) by ammonium chloride, Na2MoO4·2H2O is dissolved in deionized water, is obtained ammonium chloride, molybdic acid na concn and is respectively
The mixed solution of 0.01mmol/L and 0.1mmol/L；
(2) pipette the 40mL mixed solutions to seal in reactor to 100mL；Subsequent is 4cm by a surface area220# ferrum
Piece is also placed in the reactor, is put in water-bath, adjusts 50 DEG C of bath temperature, is placed 60h, is subsequently taken out, deionized water
The number of times of rinse is 5 times, and the time of drying at room temperature is 24h, obtains one layer of fine and close two dimension Fe on iron plate surface2Mo3O8Nano oxygen
Compound.
From Fig. 1 a, prepared iron and molybdenum oxides are two-dimensional sheet structure, and thickness is about 20nm；By shown in a in Fig. 2
XRD understand that synthesized product is Fe2Mo3O8Composite oxides；Shown in a in Fig. 3, the XPS analysis of O1s, synthesized
Product there is relatively low absorption oxygen content (Oads/Olatt=0.17), the relatively low oxygen vacancy concentration of correspondence.
Embodiment 2
A kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8The preparation method of nano-oxide, comprises the following steps：
(1) by ammonium chloride, Na2MoO4·2H2O、ZnCl2·4H2O is dissolved in deionized water, obtain ammonium chloride, sodium molybdate,
Zinc oxide concentration is respectively 2.0mmol/L, 1.0mmol/L and 0.20mmol/L mixed solution；
(2) pipette the 40mL mixed solutions to seal in reactor to 100mL；Subsequent is 1cm by a surface area220# ferrum
Piece is also placed in the reactor, is put in water-bath, is adjusted bath temperature and is caused 30 DEG C, places 12h, subsequently take out deionized water
The number of times of rinse is 6 times, and the time of drying at room temperature is 24h, obtains one layer of fine and close hexagon two dimension in ferrum substrate surface
Fe2Mo3O8Nano-oxide.
From Fig. 1 b, prepared iron and molybdenum oxides are hexagon two-dimensional sheet structure, and thickness is about 60nm；By Fig. 2
XRD shown in middle b understands that synthesized product is Fe2Mo3O8Composite oxides；By shown in b in Fig. 3, the XPS analysis of O1s can
Know, synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.55), the higher oxygen vacancy concentration of correspondence.
Embodiment 3
A kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8The preparation method of nano-oxide, comprises the following steps：
(1) by ammonium chloride, Na2MoO4·2H2O、ZnCl2·4H2O is dissolved in deionized water, obtain ammonium chloride, sodium molybdate,
Zinc oxide concentration is respectively the mixed solution of 0.01mmol/L, 0.1mmol/L and 0.01mmol/L；
(2) pipette the 40mL mixed solutions to seal in reactor to 100mL；Subsequent is 2cm by a surface area220# ferrum
Piece is also placed in the reactor, is put in water-bath, is adjusted bath temperature and is caused 60 DEG C, placing response 50h, subsequently take out spend from
The number of times of sub- water rinse is 5～6 times, and the time of drying at room temperature is 30h, can also obtain a layer thickness for 80nm in ferrum substrate surface
Hexagon two dimension Fe2Mo3O8Nano-oxide.
Embodiment 4
A kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8The preparation method of nano-oxide, comprises the following steps：
(1) by ammonium chloride, Na2MoO4·2H2O、NiCl2·6H2O is dissolved in deionized water, obtain ammonium chloride, sodium molybdate,
Chlorination nickel concentration is respectively the mixed solution of 2.0mmol/L, 1.0mmol/L and 0.20mmol/L；
(2) pipette the 40mL mixed solutions to seal in reactor to 100mL；Subsequent is 1cm by a surface area220# ferrum
Piece is also placed in the reactor, is put in water-bath, is adjusted bath temperature and is caused 40 DEG C, places 50h, subsequently take out deionized water
The number of times of rinse is 5～6 times, and the time of drying at room temperature is 30h, obtains the nanometer of a lamellar structure composition on iron plate surface
Spend two-dimentional Fe2Mo3O8Nano-oxide.
From Fig. 1 c, prepared iron and molybdenum oxides are hexagon two-dimensional sheet structure, and thickness is about 30nm；By Fig. 2
XRD shown in middle c understands that synthesized product is Fe2Mo3O8Composite oxides；By shown in c in Fig. 3, the XPS analysis of O1s can
Know, synthesized product has relatively low absorption oxygen content (Oads/Olatt=0.61), the very high oxygen vacancy concentration of correspondence.
Embodiment 5
A kind of adjustable two-dimentional Fe of Lacking oxygen2Mo3O8The preparation method of nano-oxide, comprises the following steps：
(1) by ammonium chloride, Na2MoO4·2H2O、NiCl2·6H2O is dissolved in deionized water, obtain ammonium chloride, sodium molybdate,
Chlorination nickel concentration is respectively the mixed solution of 0.01mmol/L, 0.1mmol/L and 0.01mmol/L；
(2) pipette the 40mL mixed solutions to seal in reactor to 100mL；Subsequent is 2cm by a surface area220# ferrum
Piece is also placed in the reactor, is put in water-bath, is adjusted bath temperature and is caused 80 DEG C, places 72h, subsequently take out deionized water
The number of times of rinse is 5～6 times, and the time of drying at room temperature is 36h, obtains a layer thickness in ferrum substrate surface and ties for 40nm lamellars
The nano flower two dimension Fe of structure composition2Mo3O8Nano-oxide.
Claims (9)
1. a kind of two-dimentional Fe2Mo3O8The preparation method of nano-oxide, it is characterised in that the preparation method includes following step
Suddenly：
A, with deionized water as solvent, add ammonium chloride and molybdenum source or ammonium chloride, sodium molybdate and metal cation salt, stirring and dissolving
Afterwards, obtain mixed solution；
B, iron plate is placed in mixed solution obtained by step a, heated sealed reaction then takes out iron plate, and rinse, drying are obtained final product
Two-dimentional 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, ammonium chloride are rubbed
Your concentration 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, metal cation salt
Molar concentration be 0.01～0.20mmol/L.
5. preparation method according to claim 1, it is characterised in that metal cation salt described in step a be selected from zinc source or
Person's nickel source.
6. preparation method according to claim 5, it is characterised in that the zinc source is selected from ZnCl2·4H2O。
7. preparation method according to claim 5, it is characterised in that the 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 table of iron plate
Area ratio is：10～40mL/cm2。
9. preparation method according to claim 2, it is characterised in that in step b, the reacting by heating is specifically：30～
80 DEG C are reacted aging 12～72h.
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Non-Patent Citations (3)
| Title |
|---|
| Doping-Tunable Ferrimagnetic Phase with Large Linear Magnetoelectric Effect in a Polar Magnet Fe2Mo3O8;T. Kurumaji et al.;《PHYSICAL REVIEW X》;20150915;第5卷;第031034（1-7）页 * |
| Unveiling hidden ferrimagnetism and giant magnetoelectricity in polar magnet Fe2Mo3O8;Yazhong Wang et al.;《Scientific Reports》;20150721;第5卷;第1-8页 * |
| 钼氧化物纳米结构的构筑及其储锂性能研究;孙永明;《中国博士学位论文全文数据库 工程科技I辑》;20120815(第8期);第B020-38页 * |
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