CN105600814B - One kind prepares flower-like structure Cu2The method of O photoelectric materials - Google Patents
One kind prepares flower-like structure Cu2The method of O photoelectric materials Download PDFInfo
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- CN105600814B CN105600814B CN201610086902.0A CN201610086902A CN105600814B CN 105600814 B CN105600814 B CN 105600814B CN 201610086902 A CN201610086902 A CN 201610086902A CN 105600814 B CN105600814 B CN 105600814B
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- suspension
- flower
- deionized water
- photoelectric materials
- copper acetate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
Abstract
Flower-like structure Cu is prepared the invention provides one kind2The method of O photoelectric materials, by copper acetate and glucose powder in molar ratio 1:1‑1:4 and deionized water add in reaction vessel, and be stirred, obtain blue suspension；Deionized water is continuously added in above-mentioned suspension into suspension, and is stirred；Gained forerunner's liquid suspension is transferred in reactor, sealed；Reactor is put into Muffle stove heat, 50 90 DEG C of temperature, the h of soaking time 2 48, and furnace cooling to room temperature；After reaction terminates, supernatant liquor is removed, sediment is taken out, and with separation of ethanol 24 times, obtains red powder, preservation is spontaneously dried.The achievable Cu of the present invention2The green syt of O photoelectric materials, technique is simple, easy to operate, and products therefrom has the advantages that stability is good, purity is high, extends to the synthesis of other oxides.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of photoelectric material, specifically one kind prepares flower-like structure Cu2O
The method of photoelectric material.
Background technology
Solar energy is also paid close attention to as most development potentiality by everybody, and research meets the photoelectric material of environmental development, is
Develop the key of photoelectric energy.
There are a variety of solar cell materials, such as Si, CdSe, perovskite, organic matter at present.But these materials
The process for preparing flower-like structure of material can cause very big pollution or material to have very big bio-toxicity in itself, can not reach
To real clean energy resource.Therefore, low, the environment-friendly photoelectric material of exploitation abundant raw material, price be only solar cell can
The road of sustainable development.
Cuprous oxide (Cu2O) there is direct band structure, energy gap is 1.9-2.2eV, and its direct band gap is
2.17eV, with high fluidity, high carrier mobility, high absorptivity and it is with low cost the features such as, be widely used in light and urge
The field such as change and heterojunction solar battery.In addition, the pattern of cuprous oxide material and its absorbent properties and charge transport properties
It is closely related, so as to affect its application.
At present, the cuprous oxide that flower-like structure has gone out some patterns has been prepared using different synthetic methods, it is such as octahedra
Structure, octahedra core shell structure, nanocrystalline etc..But these prepare and use organic solvent flower-like structure method more, can cause ring
Border is polluted, and is unfavorable for human kind sustainable development.
The content of the invention
For above-mentioned technical problem of the prior art, flower-like structure Cu is prepared the invention provides one kind2O photoelectric materials
Method, it is described this to prepare flower-like structure Cu2The method of O photoelectric materials is solved prepares flower-like structure in the prior art
Cu2The method of O photoelectric materials can cause the technical problem of environmental pollution.
Flower-like structure Cu is prepared the invention provides one kind2The method of O photoelectric materials, comprises the following steps：
1) copper acetate is dissolved in the copper acetate solution that clear is obtained in deionized water；
2) glucose powder is added in copper acetate solution, the mol ratio of the copper acetate and glucose is 1:1-1:4, stir
Mix acquisition blue suspension；
3) deionized water is continuously added in above-mentioned suspension, the deionized water of addition is 0.4 ~ 2 times of suspension vol,
And stir, obtain forerunner's liquid suspension；
4) gained forerunner's liquid suspension is transferred in a reactor, sealed；
5) sealed reactor is put into a heater and heated, heating-up temperature is 50-90 DEG C, soaking time 2-48
H, and furnace cooling is to room temperature；
6) after reaction terminates, supernatant liquor is removed, sediment is taken out, and with separation of ethanol 2-4 times, acquisition red powder is
For flower-like structure Cu2O photoelectric materials.
Further, described heater is Muffle furnace.
Specifically, described ethanol is absolute ethyl alcohol.
The key problem in technology of the present invention is reaction raw materials, the selection of reaction temperature, material rate is adjusted, in magnetic stirring apparatus
Stirring to obtain unit for uniform suspension, and move on in reactor and uniformly heated, the flower-shaped Cu of acquisition2O photoelectric materials.
The flower-shaped Cu of the present invention2O photoelectric materials are obtained based on hydro-thermal method, and reaction raw materials are nontoxic, and reaction dissolvent is deionization
Water.Meanwhile, Cu of the invention2O photoelectric materials are carried out in reactor, and course of reaction is safe and reliable, does not discharge pernicious gas；Behaviour
Facilitate, synthetic method is simple, and gained reaction product stability is good, purity is high.
In the preparation process of the present invention, using magnetic stirrer, it is ensured that the physics of whole reaction suspension is uniform
Property, it is Cu2The synthesis of O photoelectric materials provides good forming core and growing environment.
In the preparation process of the present invention, using deionized water as reaction dissolvent, without other additives.Meanwhile, in reaction
During will not produce pernicious gas, with environment-friendly characteristic.
In the preparation process of the present invention, when reaction temperature is more than 90 DEG C, reaction response product is elemental copper and Cu2O
Mixture；When reaction temperature is less than 50 DEG C, most of reaction raw materials can not be converted completely, and conversion rate of products is low.Therefore close
It is advisable into temperature range with 50 DEG C -90 DEG C.In this temperature range, flower-shaped Cu can be obtained2O photoelectric materials.
In the preparation process of the present invention, the reaction time is 2-48 h.When being less than 2 h between when reacted, most of reaction
Raw material can not be converted completely, and conversion rate of products is extremely low, when reacted between be more than 48 h, gained sample size is larger, flower-like structure
Become club shaped structure.Therefore generated time scope is advisable with 2 h-48 h.In this temperature range, flower-shaped Cu can be obtained2O light
Electric material.
In the preparation process of the present invention, using Muffle stove heat, it is ensured that the uniformity of reactor temperature.
The present invention is compared with prior art, and its technological progress is significant.Cu can be realized by the method for the present invention2O light
The green syt of electric material, technique is simple, easy to operate, and products therefrom has the advantages that stability is good, purity is high, extends to
The synthesis of other oxides.
Brief description of the drawings
Fig. 1 is the Cu obtained by the method for the present invention2The X-ray diffraction pattern of O samples.
Fig. 2 is the Cu obtained by the method for the present invention2The SEM figures of O samples.
The X-ray diffraction pattern of gained sample under Fig. 3 different temperatures.
Embodiment
Below by embodiment, the present invention is further elaborated, but does not limit the protection domain of patent of the present invention.
Embodiment 1
2 mmol copper acetates are dissolved in after the copper acetate solution that deionized water obtains clear, 2 mmol Portugals are continuously added
Grape Icing Sugar end, stirring to obtain blue suspension；Deionized water is added in above-mentioned suspension, overall solution volume is 40 ml；In magnetic
Stir after 30 min, all moved on in 50 ml tetrafluoro reactors in the presence of power agitator, and be heated in Muffle furnace 50
DEG C, and it is incubated 12 h.After reaction terminates, supernatant liquor is removed, sediment is taken out, and with separation of ethanol 2-4 time, acquisition red powder
End, spontaneously dries and preserves.
Embodiment 2
Except for the following differences, other are such as be the same as Example 1, the Cu of the acquisition present invention2O photoelectric materials.
2 mmol copper acetates are dissolved in after the copper acetate solution that deionized water obtains clear, 4 mmol Portugals are continuously added
Grape Icing Sugar end, stirring to obtain blue suspension；Deionized water is added in above-mentioned suspension, overall solution volume is 40 ml；In magnetic
Stir after 30 min, all moved on in 50 ml tetrafluoro reactors in the presence of power agitator, and be heated in Muffle furnace 60
DEG C, and it is incubated 6 h.After reaction terminates, supernatant liquor is removed, sediment is taken out, and with separation of ethanol 2-4 time, acquisition red powder
End, spontaneously dries and preserves.
Embodiment 3
Except for the following differences, other are such as be the same as Example 1, the Cu of the acquisition present invention2O photoelectric materials.
5 mmol copper acetates are dissolved in after the copper acetate solution that deionized water obtains clear, 5 mmol Portugals are continuously added
Grape Icing Sugar end, stirring to obtain blue suspension；Deionized water is added in above-mentioned suspension, overall solution volume is 40 ml；In magnetic
Stir after 30 min, all moved on in 50 ml tetrafluoro reactors in the presence of power agitator, and be heated in Muffle furnace 80
DEG C, and it is incubated 2 h.After reaction terminates, supernatant liquor is removed, sediment is taken out, and with separation of ethanol 2-4 time, acquisition red powder
End, spontaneously dries and preserves.
Embodiment 4
Except for the following differences, other are such as be the same as Example 1, the Cu of the acquisition present invention2O photoelectric materials.
2 mmol copper acetates are dissolved in after the copper acetate solution that deionized water obtains clear, 4 mmol Portugals are continuously added
Grape Icing Sugar end, stirring to obtain blue suspension；Deionized water is added in above-mentioned suspension, overall solution volume is 40 ml；In magnetic
Stir after 30 min, all moved on in 50 ml tetrafluoro reactors in the presence of power agitator, and be heated in Muffle furnace 90
DEG C, and it is incubated 24 h.After reaction terminates, supernatant liquor is removed, sediment is taken out, and with separation of ethanol 2-4 time, acquisition red powder
End, spontaneously dries and preserves.
According to above-described embodiment, final gained sample characterizes its phase structure by x-ray diffraction, with Cu2O mark
Quasi- card (JCPDS NO.05-0667) corresponds；And pass through ESEM（SEM）Its shape characteristic is characterized, flower is obtained
Shape structure.
Fig. 1 illustrates Cu2The X-ray diffraction pattern of O samples, by Jade software analysis, its diffraction maximum and Cu2O standard
Card (JCPDS NO.05-0667) is corresponded.The θ of the angle of diffraction 2 is 29.49o、37.55o、42.45o、52.37o、62.5o、
74.45oWhen, correspond respectively to cubic crystal structure cuprous oxide（110）、(111)、(200)、（211）、(220)、(311)
Crystal face.In addition, other dephasigns in addition to cuprous oxide are also not observed, it was demonstrated that gained sample is brilliant for pure cuprous oxide
Body；Narrow and sharp diffraction maximum shows that this sample has very high crystallinity.
Fig. 2 illustrates the stereoscan photograph of gained cuprous oxide sample.From SEM low power pictures（Fig. 2 a）In can observe
Constituted to sample by being uniformly distributed flower-like structure.Further multiplication factor, from SEM high power picture 2b, it is clear that
The flower-like structure is formed by connecting by six branches, and the length of each branch is 10 μm of 2 μ m, and the surface relatively light of branch
It is sliding.
Fig. 3 illustrates the X-ray diffraction pattern of gained sample under different temperatures.It was found from being analyzed from figure, when temperature is less than 90
DEG C, gained sample is pure Cu2O；When temperature continues to raise, the diffraction maximum of elemental copper is occurred in that in sample, its content is with temperature
The rise of degree and increase.
The present invention realizes flower-shaped Cu based on hydro-thermal method2The synthesis of O photoelectric materials, from reaction raw materials to course of reaction not
There is poisonous and hazardous material, realize environment-friendly technology path.The method technique that the present invention is used is simple and convenient to operate
And it is environment-friendly, and the advantage such as products therefrom performance stabilization, purity height, reduce synthesis cost.The present invention extends to it
The synthesis of its oxide.
Claims (2)
1. one kind prepares flower-like structure Cu2The method of O photoelectric materials, it is characterised in that comprise the following steps：
1）Copper acetate is dissolved in the copper acetate solution that clear is obtained in deionized water；
2）Glucose powder is added in copper acetate solution, the mol ratio of the copper acetate and glucose is 1:1-1:4, stirring is obtained
Obtain blue suspension；
3）Deionized water is continuously added in above-mentioned suspension, the deionized water of addition is 0.4 ~ 2 times of suspension vol, and is stirred
Mix uniform, obtain forerunner's liquid suspension；
4）Gained forerunner's liquid suspension is transferred in a reactor, sealed；
5）Sealed reactor is put into a heater and heated, heating-up temperature is 50-90 DEG C, soaking time 2-48 h,
And furnace cooling is to room temperature；
6）After reaction terminates, supernatant liquor is removed, sediment is taken out, and with separation of ethanol 2-4 times, acquisition red powder is flower
Shape structure C u2O photoelectric materials, described flower-like structure is formed by connecting by six branches, and the length of each branch is 2 μ ms
10 μm, and the surface smoother of branch.
2. prepare flower-like structure Cu as claimed in claim 12The method of O photoelectric materials, it is characterised in that described heater
For Muffle furnace.
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| CN201610086902.0A CN105600814B (en) | 2016-02-16 | 2016-02-16 | One kind prepares flower-like structure Cu2The method of O photoelectric materials |
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| CN201610086902.0A CN105600814B (en) | 2016-02-16 | 2016-02-16 | One kind prepares flower-like structure Cu2The method of O photoelectric materials |
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| CN105600814B true CN105600814B (en) | 2017-11-03 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109956493B (en) * | 2019-04-18 | 2021-09-07 | 上海电力学院 | Preparation method of cerium or/and zinc doped cuprous oxide nano material |
| CN111252800A (en) * | 2020-01-21 | 2020-06-09 | 上海电力大学 | Preparation method of nano cuprous oxide photoelectric material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412530A (en) * | 2008-10-31 | 2009-04-22 | 浙江理工大学 | Preparation with organic addition for controlling external morphology of cuprous oxide crystal |
| CN102583499A (en) * | 2012-01-11 | 2012-07-18 | 哈尔滨工业大学 | Preparation method for cuprous oxide micron/nano crystal with controllable morphology |
| CN103373739A (en) * | 2012-04-18 | 2013-10-30 | 宁波大学 | Hydrothermal preparation method of cuprous oxide crystal |
| CN103449499A (en) * | 2013-08-23 | 2013-12-18 | 上海应用技术学院 | Snowflake-shaped cuprous oxide micro/nano particle and preparation method thereof |
-
2016
- 2016-02-16 CN CN201610086902.0A patent/CN105600814B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412530A (en) * | 2008-10-31 | 2009-04-22 | 浙江理工大学 | Preparation with organic addition for controlling external morphology of cuprous oxide crystal |
| CN102583499A (en) * | 2012-01-11 | 2012-07-18 | 哈尔滨工业大学 | Preparation method for cuprous oxide micron/nano crystal with controllable morphology |
| CN103373739A (en) * | 2012-04-18 | 2013-10-30 | 宁波大学 | Hydrothermal preparation method of cuprous oxide crystal |
| CN103449499A (en) * | 2013-08-23 | 2013-12-18 | 上海应用技术学院 | Snowflake-shaped cuprous oxide micro/nano particle and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 葡萄糖还原Cu(II)制备超细Cu2O;宋超等;《五邑大学学报（自然科学版）》;20101130;第24卷(第4期);第39-44页 * |
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