CN110467215A - A kind of iron of morphology controllable, zinc ion codope cuprous oxide crystal preparation method - Google Patents
A kind of iron of morphology controllable, zinc ion codope cuprous oxide crystal preparation method Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of Fe, Zn of morphology controllable ion co-doped cuprous oxide crystal, it is related to technical field of nanometer material preparation, comprising steps of S100, by cupric salt and surfactant dissolution in deionized water, be sufficiently stirred to obtain the first solution；S200, it is added into the first solution and contains Fe3+And Zn2+Solution, and be stirred at room temperature to obtain the second solution；S300, the second solution is handled to obtain Primary product by alkaline solution and reducing agent, wherein the reducing agent is glucose solution；S400, the magnetic oxygenated cuprous powder that Primary product is centrifuged, is washed, is dried to obtain final product Fe, Zn doping.The preparation method at the nano cuprous oxide powder end of Fe, Zn doping provided by the invention is suitable for the industrial production of large-scale, and the nano cuprous oxide powder end of obtained Fe, Zn doping has good magnetic performance, has a good application prospect.
Description
Technical field
The present invention relates to the preparation technical fields of nano material more particularly to a kind of iron of morphology controllable, zinc ion to be co-doped with
The preparation method of miscellaneous cuprous oxide crystal.
Background technique
Cu2O is a kind of p-type semiconductor that forbidden bandwidth is 2.17eV, has a very big excitation energy 140meV, is predicted
For a kind of very promising host material.It is past in these years, a large amount of document report is in Cu2Gold is adulterated in O crystal
P-type or n-type semiconductor can be become by belonging to ion or nonmetallic ion.Therefore, research doping is to Cu2O crystallophy, chemistry
The influence of property is very important.Due to Doped ions and Cu+The spin state of ion is close, ionic radius is similar, in crystal
Identical position may be occupied in structure, therefore, the ion of these doping can modify Cu2Magnetics, optics, the electricity of O crystal
Etc. properties.Currently, using in Cu2The method that transiting state metal ion is adulterated in O crystal prepares dilute magnetic semiconductor and has caused
The broad interest of people.Has Cu reported in the literature2O nanometer rods mix magnetic element Fe, Co, Ni, Mn element, Cu2O crystal energy
It is changed into ferromagnet from diamagnetic body, and with the increase of doped chemical concentration, magnetism is gradually increased.Cu2The room of O crystal performance
Warm ferromagnetism is not only related with preparation method, also has certain relationship with the ionic species of doping.Related nanometer Cu2O adulterates magnetic
The preparation method of property element be concentrated mainly on hydro-thermal method perhaps this method of thermal oxidation method need under high temperature or hyperbaric environment into
Row, technique is relative complex, greatly constrains the large scale preparation of material.
Therefore, a kind of inexpensive and good template of controllability is developed, can be realized Cu2O appearance of nano material structure
Effective Regulation, to improve Cu2The magnetic performance of O nano material has great importance with its application is extended.Therefore, this field
Technical staff be dedicated to developing a kind of iron of morphology controllable, zinc ion codope cuprous oxide crystal preparation method.
Summary of the invention
In view of the above drawbacks of the prior art, technical problem to be solved by the invention is to provide a kind of morphology controllables
Iron, zinc ion codope cuprous oxide crystal preparation method so that the preparation method can be realized to Cu2O nano material
The Effective Regulation of appearance structure, to improve Cu2The magnetic performance of O nano material, and expand its application range.
To achieve the above object, the present invention provides the cuprous oxide of a kind of iron of morphology controllable, zinc ion codope is brilliant
The preparation method of body, comprising the following steps:
S100, cupric salt and surfactant are dissolved in deionized water, are sufficiently stirred to obtain the first solution,
In, the surfactant is ethylenediamine tetra-acetic acid；
S200, it is added into the first solution and contains Fe3+And Zn2+Solution, and be stirred at room temperature to obtain the second solution；
S300, the second solution is handled to obtain Primary product by alkaline solution and reducing agent, wherein the reducing agent is
Glucose solution；
S400, the magnetic oxygenated cuprous powder that Primary product is centrifuged, is washed, is dried to obtain final product Fe, Zn doping.
Preparation method of the invention compared with prior art, has the advantage that
(1) the preparation method preparation process at the nano cuprous oxide powder end of Fe, Zn provided by the invention doping simply, cost
It is cheap, and a nanometer Cu may be implemented by adjusting reaction time and ion doping concentration2The pattern of O crystal adjusts；
(2) preparation method at the nano cuprous oxide powder end of Fe, Zn doping provided by the invention is suitable for the work of large-scale
Industry production, and the nano cuprous oxide powder end of obtained Fe, Zn doping has good magnetic performance, has good application
Prospect.
It is described further below with reference to technical effect of the attached drawing to design of the invention, specific structure and generation, with
It is fully understood from the purpose of the present invention, feature and effect.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of a preferred embodiment of the present invention；
Fig. 2 (a)-Fig. 2 (e) is the nanometer Cu of presently preferred embodiments of the present invention preparation2The SEM of O powder schemes, wherein Fig. 2
(a) the nanometer Cu prepared for embodiment 12The SEM of O powder schemes；Fig. 2 (b) is nanometer Cu prepared by embodiment 22The SEM of O powder
Figure；Fig. 2 (c) is nanometer Cu prepared by embodiment 32The SEM of O powder schemes；Fig. 2 (d) is nanometer Cu prepared by embodiment 42O powder
SEM figure；Fig. 2 (e) is nanometer Cu prepared by embodiment 52The SEM of O powder schemes；
Fig. 3 is the Cu of Fe doping and Fe, Zn co-doped2The hysteresis loop of O crystal；
Fig. 4 is the Cu of Fe doping and Fe, Zn co-doped2The EPR map of O crystal；
Fig. 5 is the Cu of Zn doping and Fe, Zn co-doped2The hysteresis loop of O crystal；
Fig. 6 is undoped and Fe, Zn co-doped Cu2The photo-catalytic degradation of methyl-orange degradation rate figure of O crystal.
Specific embodiment
Multiple preferred embodiments of the invention are introduced below with reference to Figure of description, keep its technology contents more clear and just
In understanding.The present invention can be emerged from by many various forms of embodiments, and protection scope of the present invention not only limits
The embodiment that Yu Wenzhong is mentioned.
As shown in the preparation method flow chart of preferred embodiment Fig. 1 of the invention, comprising the following steps:
S100, cupric salt and surfactant are dissolved in deionized water, are sufficiently stirred to obtain the first solution,
In, the surfactant is ethylenediamine tetra-acetic acid；
S200, it is added into the first solution and contains Fe3+And Zn2+Solution, and be stirred at room temperature to obtain the second solution；
S300, the second solution is handled to obtain Primary product by alkaline solution and reducing agent, wherein the reducing agent is
Glucose solution；
S400, the magnetic oxygenated cuprous powder that Primary product is centrifuged, is washed, is dried to obtain final product Fe, Zn doping.
Wherein, cupric salt described in step S100 is one of copper nitrate, copper chloride, copper sulphate, copper acetate；
Contain Fe described in step S2003+Solution be one of ferric nitrate, iron chloride, ferric sulfate；It is described to contain Zn2+'s
Solution is one of zinc nitrate, zinc chloride, zinc sulfate；
In a preferred embodiment, Fe is contained described in step S2003+Solution molar concentration rate be 0.%~
3%；Contain Zn described in step S2002+Solution molar concentration rate be 0%~5%.
In a preferred embodiment, alkaline solution described in step S300 is one kind of sodium hydroxide, potassium hydroxide.
In a preferred embodiment, the step S300 further include:
S301, alkaline solution and the stirring that the second solution is heated in a water bath and instills 5~6mL 3M dropwise thereto
Obtain third solution；
S302, the glucose solution that 10~11mL molar concentration is 0.11M is instilled dropwise into third solution, 50~60
0.5~1.5h is reacted at DEG C, obtains Primary product.
In a preferred embodiment, the pattern of final product described in step S400 is nanometer truncated cube or receives
Rice cuts rib cube.
Below in conjunction with drawings and examples, technical scheme is described further.
Embodiment 1
1) by the CuSO of 2mmol4It is dissolved in 40mL deionized water with ethylenediamine tetra-acetic acid (EDTA) powder of 1mmol,
It is sufficiently stirred, dissolution completely, obtains clear solution；
2) this solution does not do doping treatment；
3) heat in a water bath, when reaction temperature be 55 DEG C when, respectively by 5mL molar concentration be 3M NaOH solution dropwise
Instill solution.After being vigorously agitated again 5min, the glucose solution that 10mL molar concentration is 0.11M is added dropwise respectively into above-mentioned reaction
In solution, 1h is reacted under conditions of 55 DEG C, obtains the mixed solution containing red precipitate substance.
4) the mixed solution centrifuge washing by prepared containing red precipitate substance for several times, and by red deposit
It is placed in dry 12h in vacuum oven, obtains final product nano cuprous oxide powder end.
Shown in the pattern such as Fig. 2 (a) at the nano cuprous oxide powder end that embodiment 1 obtains, when there is no Fe3+And Zn2+It is existing
In the case of, which is uniform Cu2O cube is made of 6 { 100 } crystal faces, and size is at 1.2 μm or so.
Embodiment 2
1) by the CuSO of 2mmol4It is dissolved in 40mL deionized water with ethylenediamine tetra-acetic acid (EDTA) powder of 1mmol,
It is sufficiently stirred, dissolution completely, obtains clear solution；
2) Fe (NO that molar concentration ratio is 3% is added in acquired solution3)33h is stirred at room temperature in solution, obtains phase
Answer solution.
3) heat in a water bath, when reaction temperature be 55 DEG C when, respectively by 5mL molar concentration be 3M KOH solution dropwise
Instill solution.After being vigorously agitated again 5min, the glucose solution that 10mL molar concentration is 0.11M is added dropwise respectively into above-mentioned reaction
In solution, 1h is reacted under conditions of 55 DEG C, obtains the mixed solution containing red precipitate substance；
4) the mixed solution centrifuge washing by prepared containing red precipitate substance for several times, and by red deposit
It is placed in dry 12h in vacuum oven, obtains the nano cuprous oxide powder end of final product Fe ion doping.
Shown in the pattern such as Fig. 2 (b) at the nano cuprous oxide powder end that embodiment 2 obtains, it can be seen that a certain amount of when adding
Fe3+When ion, product remains as cube, but size, at 2 μm or so, this illustrates Fe3+Ion mainly influences the ruler of product
It is very little, do not change the pattern of product.
Embodiment 3
1) by the CuSO of 2mmol4It is dissolved in 40mL deionized water with ethylenediamine tetra-acetic acid (EDTA) powder of 1mmol,
It is sufficiently stirred, dissolution completely, obtains clear solution；
2) Fe (NO that molar concentration ratio is 3% is added in acquired solution3)3, 1% Zn (NO3)2Solution, at room temperature
3h is stirred, corresponding solution is obtained.
3) heat in a water bath, when reaction temperature be 55 DEG C when, respectively by 5.5mL molar concentration be 3M NaOH solution by
Drop instills solution.After being vigorously agitated again 5min, the glucose solution that 10.5mL molar concentration is 0.11M is added dropwise respectively into above-mentioned
In reaction solution, 1h is reacted under conditions of 55 DEG C, obtains the mixed solution containing red precipitate substance；
4) the mixed solution centrifuge washing by prepared containing red precipitate substance for several times, and by red deposit
It is placed in dry 12h in vacuum oven, obtains final product Fe, the nano cuprous oxide powder end of Zn ion doping.
Shown in the pattern such as Fig. 2 (c) at the nano cuprous oxide powder end that embodiment 3 obtains, it can be seen that Zn2+Ion molar ratio
When example is 1%, product is uniform truncated cube, and newly-increased crystal face is 8 { 111 } crystal faces.
Embodiment 4
1) by the CuSO of 2mmol4It is dissolved in 40mL deionized water with ethylenediamine tetra-acetic acid (EDTA) powder of 1mmol,
It is sufficiently stirred, dissolution completely, obtains clear solution；
2) Fe (NO that molar concentration ratio is 3% is added in acquired solution3)3, 3% Zn (NO3)2Solution, at room temperature
3h is stirred, corresponding solution is obtained.3) it heats in a water bath, is respectively 3M's by 5mL molar concentration when reaction temperature is 55 DEG C
NaOH solution instills solution dropwise.After being vigorously agitated again 5min, the glucose solution that 10mL molar concentration is 0.11M is dripped respectively
It adds in above-mentioned reaction solution, reacts 1h under conditions of 55 DEG C, obtain the mixed solution containing red precipitate substance；
4) the mixed solution centrifuge washing by prepared containing red precipitate substance for several times, and by red deposit
It is placed in dry 12h in vacuum oven, obtains final product Fe, the nano cuprous oxide powder end of Zn ion doping.
Shown in the pattern such as Fig. 2 (d) at the nano cuprous oxide powder end that embodiment 4 obtains, it can be seen that work as Zn2+Ion rubs
When your ratio is 3%, product is that rescinded angle section rib cube 12 { 110 } crystal faces occurs that is, on the basis of original pattern.
Embodiment 5
1) by the CuSO of 2mmol4It is dissolved in 40mL deionized water with ethylenediamine tetra-acetic acid (EDTA) powder of 1mmol,
It is sufficiently stirred, dissolution completely, obtains clear solution；
2) Fe (NO that molar concentration ratio is 3% is added in acquired solution3)3, 5% Zn (NO3)2Solution, at room temperature
3h is stirred, corresponding solution is obtained.3) it heats in a water bath, is respectively 3M's by 5mL molar concentration when reaction temperature is 55 DEG C
NaOH solution instills solution dropwise.After being vigorously agitated again 5min, the glucose solution that 10mL molar concentration is 0.11M is dripped respectively
It adds in above-mentioned reaction solution, reacts 1h under conditions of 55 DEG C, obtain the mixed solution containing red precipitate substance；
4) the mixed solution centrifuge washing by prepared containing red precipitate substance for several times, and by red deposit
It is placed in dry 12h in vacuum oven, obtains final product Fe, the nano cuprous oxide powder end of Zn ion doping.
Shown in the pattern such as Fig. 2 (e) at the nano cuprous oxide powder end that embodiment 5 arrives, it can be seen that work as Zn2+Mole of ion
When ratio is further increased to 5%, the pattern of product does not have obvious significant change, but has larger size, and { 110 } are brilliant
Ratio of the face in entire crystal significantly increases.
In summary it is found that Fe3+Ion doping mainly affects the size of product, and Zn2+The doping of ion then causes ruler
A series of very little and pattern variations.
Fig. 3 is the Cu of Fe doping and Fe, Zn co-doped2The hysteresis loop of O crystal, it can be seen that at room temperature,
All samples all have certain ferromagnetism.As only 3% Fe3+When ion doping, sample display goes out the iron of room temperature
Magnetism, saturation magnetization 0.0125emu/g.It is worth noting that, micro Zn2+The addition of ion will cause magnetic
Fe is worked as in significant change3+The content of ion remains unchanged, with Zn2+The increase of ion concentration, the doping of Fe increases in product,
Its magnetism is caused to gradually increase.As the Zn that addition molar ratio is 1%, 3% and 5% respectively2+When ion, saturated magnetization is strong
Degree is respectively increased to 0.0237,0.0525 and 0.1008emu/g, and this variation tendency and Al, Cu for being previously reported doping ZnO are
It is consistent.Simultaneously it was noted that hysteresis loop does not reach saturation state when maximum field, show at this time also
Many ferromagnetic magnetic moments and paramagnetic magnetic moment coexist.It can be inferred that Zn from result above2+The concentration of ion is to Fe, Zn codope
Cu2The magnetic performance of O crystal plays an important role.
Fig. 4 illustrates the EPR map of doped samples at room temperature, it can be seen from the figure that in pure Cu2O is brilliant
There is no the signal of unpaired electronics in body, this has further showed that the sample does not show magnetism externally.When only Fe doping
In the case of, which shows a weak resonance signal, and g value is 2.0041, this and previous document report are consistent.When
Under conditions of Fe, Zn co-doped, EPR shows apparent resonance signal, and with Zn2+The concentration of ion increases
Greatly, resonance signal is stronger.The Cu that wherein Fe 3%Zn 1%, Fe 3%Zn 3% and Fe 3%Zn 5% is adulterated2The g of O crystal
Value is respectively 2.0064,2.0083 and 2.0083, these values show that these resonance signals originate from the hole Vo all close to 2.0, this
It is to cause the defect density of cation sufficiently high due to its low formation energy, these concentration for being higher than required threshold value can be into one
Its ferromagnetic long-range order of the adjusting of step.
Fig. 5 is the Zn of doping2+When ion concentration is constant, the Fe of various concentration3+The Cu of ion doping2The magnetic hysteresis of O crystal is returned
Line, it can be seen that Zn2+Ion concentration is constant, with Fe3+The increase of ion concentration, magnetism are also to gradually increase, wherein Fe
The Cu that 1%Zn 5%, Fe 2%Zn 5%, Fe 3%Zn 5% and Fe 4%Zn 5% are adulterated2The corresponding saturated magnetization of O crystal
Intensity is respectively 0.00453,0.04983,0.07729 and 0.0954emu/g.Simultaneously when maximum field, the intensity of magnetization
Also do not reach saturation state, show also in paramagnetic and the ferromagnetic state coexisted.Experimental result has absolutely proved Fe3+Ion
Concentration also plays a role the magnetism of final product.
Fig. 6 is undoped and Fe, Zn co-doped Cu2The photo-catalytic degradation of methyl-orange degradation rate figure of O crystal, Cong Tuzhong
It can be seen that as light-catalyzed reaction 2h, the Cu of Fe, Zn codope2O crystal degrades methyl orange 88%, and undoped pure
Cu2O crystal only degrades methyl orange 59%, shows 26 face body Cu of Fe, Zn codope2O crystal is than undoped pure Cu2O crystal
With better Photocatalytic activity.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be within the scope of protection determined by the claims.
Claims (9)
1. a kind of preparation method of the cuprous oxide crystal of iron of morphology controllable, zinc ion codope, the method includes following
Step:
S100, cupric salt and surfactant are dissolved in deionized water, is sufficiently stirred to obtain the first solution, wherein institute
Stating surfactant is ethylenediamine tetra-acetic acid；
S200, it is added into the first solution and contains Fe3+And Zn2+Solution, and be stirred at room temperature to obtain the second solution；
S300, the second solution is handled to obtain Primary product by alkaline solution and reducing agent, wherein the reducing agent is grape
Sugar juice；
S400, the magnetic oxygenated cuprous powder that Primary product is centrifuged, is washed, is dried to obtain final product Fe, Zn doping.
2. the method for claim 1, wherein preferred, cupric salt described in step S100 is copper nitrate, chlorination
One of copper, copper sulphate, copper acetate.
3. the method for claim 1, wherein containing Fe described in step S2003+Solution be ferric nitrate, iron chloride, sulphur
One of sour iron.
4. the method for claim 1, wherein containing Zn described in step S2002+Solution be zinc nitrate, zinc chloride, sulphur
One of sour zinc.
5. the method for claim 1, wherein containing Fe described in step S2003+Solution molar concentration rate be 0~
3%.
6. the method for claim 1, wherein containing Zn described in step S2002+Solution molar concentration rate be 0%~
5%.
7. the method for claim 1, wherein alkaline solution described in step S300 is sodium hydroxide, potassium hydroxide
It is a kind of.
8. the method for claim 1, wherein step S300 further include:
S301, the second solution is heated in a water bath and instills the alkaline solution of 5~6mL 3M dropwise thereto and stirs to get
Third solution；
S302, the glucose solution that 10~11mL molar concentration is 0.11M is instilled dropwise into third solution, at 50~60 DEG C
0.5~1.5h is reacted, Primary product is obtained.
9. the method for claim 1, wherein the pattern of final product described in step S400 is nanometer truncated cube
Or nanometer cuts rib cube.
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Cited By (1)
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| CN111151262A (en) * | 2020-01-14 | 2020-05-15 | 西安理工大学 | Mn-Cu2O-modified photocatalyst and preparation method thereof |
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