CN108163883A - One kind has class " sea urchin " shape structure ZnO functional material and preparation method thereof - Google Patents
One kind has class " sea urchin " shape structure ZnO functional material and preparation method thereof Download PDFInfo
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- CN108163883A CN108163883A CN201711489508.2A CN201711489508A CN108163883A CN 108163883 A CN108163883 A CN 108163883A CN 201711489508 A CN201711489508 A CN 201711489508A CN 108163883 A CN108163883 A CN 108163883A
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- sea urchin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a type " sea urchin " shape ZnO functional materials and preparation method, the functional material under the action of Van der Waals force, is agglomerated into class " sea urchin " shape, has the characteristics that 3-D solid structure by ultra-thin ZnO nano piece.The present invention is with Zn (CH3COO)2•2H2O and NaOH is base stock, and required product is synthesized using hydro-thermal and high temperature sintering two-step method.The ZnO nano piece that hydro-thermal generates dispersion is first passed through, then under the high temperature conditions, three-dimensional flower-shaped structure is agglomerated under the action of Van der Waals force.Compared with other methods, this method is simple and effective, easy to operate, does not generate poisonous and hazardous by-product and pernicious gas, and raw material availability is high, adapts to the requirement of Modern Green production.As the electrode material of ultracapacitor, excellent chemical property is shown, in KOH electrolyte, there is apparent fake capacitance to generate, this unique structure can increase substantially the chemical property of material.
Description
Technical field
The present invention relates to a kind of " sea urchin " shape ZnO functional materials and preparation methods.Ultra-thin ZnO nano is prepared by hydro-thermal
Then piece is assembled into " sea urchin " shape structure by high temperature method.Using the material as the electrode material of ultracapacitor, have good
Capacitive property, the synthesis technology is simple and environmentally protective, and contamination-free and harmful by-products generate.Since metal oxide has
There is good fake capacitance to react, capacitive property can be significantly improved, it will play an important role in energy storage device field.
Background technology
With the progress of human sciences' technology, people are to the energy storage device with high power capacity and overlength service life cycle
Propose new requirement.Although ultracapacitor has higher power density and cyclical stability, ultracapacitor is deposited
The ability for storing up capacity is limited, an important factor for as its performance is influenced, electrode material received people extensive research and
Concern.Especially there is the metal oxide of good fake capacitance performance, due to its numerous excellent physical and chemical performance, evoke
The extensive enthusiasm of people.
Zinc oxide is a kind of oxide of zinc.ZnO is there are mainly four types of crystal structure, including zincblende lattce structure（With diamond
Structure is similar, can regard oxygen atom FCC arrangements as, and remaining 4 zinc atom occupies in diamond the four carbon atom in packet
Position）；Its excess-three kind structure includes NaCl structures, CsCl structures and wurtzite structure.The band gap of simultaneous oxidation zinc and swash
Sub- binding energy is larger, and transparency is high, has excellent room temperature luminescent properties, liquid crystal display, film crystal in semiconductor applications
There is application in the products such as pipe, light emitting diode.Zinc oxide is a kind of common chemical addition agent, be widely used in plastics,
The making of the products such as silicate product, synthetic rubber, lubricating oil, paint, ointment, adhesive, food, battery, fire retardant
In.
According to structures shape performance principle, ZnO nano piece, can be in the effect of Van der Waals force after high-temperature process
Under, for cluster into flower-shaped, which can improve the specific surface area of material, increase the contact area of material and electrolyte, improve from
Sub- transmission rate.Specific surface area larger simultaneously can also provide more fake capacitance reactivity sites.
Invention content
The object of the present invention is to provide a kind of ZnO of stabilization " sea urchin " structure, and as the capacitance material of ultracapacitor
Material has higher capacitance than the ZnO material of general pattern.The stable structure of products obtained therefrom, and with good electrochemistry
The material of energy.
ZnO material in the present invention, ZnO purity is higher, is generated substantially without impurity, and has good crystallinity,
Crystalline phase corresponds to PDF standard cards：36-1451.As shown in Figure 1.
ZnO material in the present invention, have " sea urchin " shape structure, be by ultra-thin ZnO nano piece Van der Waals force work
Under, the structure that assembles has apparent gap between nanometer sheet.As shown in Figure 2.
" sea urchin " the shape ZnO material of the present invention has good chemical property, has compared to general ZnO material aobvious
The raising of work.The use of the KOH solution of 1mol/L is electrolyte as the electrode material of ultracapacitor, is assembled into symmetrical
The ultracapacitor of formula, test voltage range recycle survey in -0.8-0.2 V, sweep speed in 10 to 50mV/s CV curves
In examination, CV curves have good symmetrical performance, and show apparent redox peaks, it was demonstrated that the structure ZnO material shows
Go out excellent power and volumetric properties.As shown in Figure 3.
Realize that the technical solution adopted in the present invention is：A kind of ZnO functional materials pass through Mr.'s hydro-thermal method slabbing ZnO
Material then under conditions of high-temperature process, is self-assembly of cluster structure, has the advantages of simple for process, green non-pollution,
Its electrode material had into good chemical property, preparation process is as follows：
（1）Weigh 4 g（0.1 mol）NaOH solids, be dissolved in the deionized water of 100ml, be configured to 1mol/L's
NaOH alkaline solutions are in case subsequent experimental uses；
（2）Weigh 2.195g（0.01 mol）Zn (CH3COO)2•2H2O is added in the deionized water of 100ml, continuing magnetic force
Stirring is configured to the Zn (CH of 0.1 mol/L3COO)2•2H2Then O solution takes 10ml steps（1）The middle alkaline solution being configured,
Under the premise of magnetic force is stirred continuously, it is added dropwise to the Zn (CH being configured3COO)2•2H2In O solution, the cotton-shaped of white is formed
Mixed solution is then heated to 90 DEG C, and keeps the temperature 2h by object, is cooled to and is formed wet gel at room temperature；
（3）By step（2）The wet gel of middle formation is placed in 90 DEG C of vacuum drying chambers, dry to form xerogel state for 24 hours, with
30min is ground with agate mortar afterwards, is worn into white powder；
（4）By step（3）In white powder be put into porcelain boat, be put into tube furnace, under Ar gas inert atmospheres, with 2
DEG C/heating rate of min is warming up to 400 DEG C, and keep the temperature 2h, last cooled to room temperature is collected after being ground with agate mortar,
As final product.
Step（2）Middle Zn (CH3COO)2•2H2O:NaOH=1:1（Molar ratio）.
Step（2）In NaOH solution be added dropwise rather than all be directly added into.
Step（4）In heating rate be 2 DEG C/min.
Description of the drawings
Fig. 1 is the XRD diagram of ultra-thin ZnO nano piece.
Fig. 2 is that the SEM of ultra-thin ZnO nano piece schemes.
Fig. 3 is CV curve graph of the ultra-thin ZnO nano piece under different scanning rates.
Specific embodiment
（1）Weigh 4 g（0.1 mol）NaOH solids, be dissolved in the deionized water of 100ml, be configured to 1mol/
The NaOH alkaline solutions of L are in case subsequent experimental uses.
（2）Weigh 2.195g（0.01 mol）Zn (CH3COO)2•2H2O is added in the deionized water of 100ml, is continued
Magnetic agitation is configured to the Zn (CH of 0.1 mol/L3COO)2•2H2Then O solution takes 10ml steps（1）The middle alkalinity being configured
Solution under the premise of magnetic force is stirred continuously, is added dropwise to the Zn (CH being configured3COO)2•2H2In O solution, white is formed
Floccule, mixed solution is then heated to 90 DEG C, and keep the temperature 2h, is cooled to and forms wet gel at room temperature.
（3）By step（2）The wet gel of middle formation is placed in 90 DEG C of vacuum drying chambers, and drying for 24 hours, forms xerogel shape
State then grinds 30min with agate mortar, is worn into white powder.
（4）By step（3）In white powder be put into porcelain boat, be put into tube furnace, under Ar gas inert atmospheres,
400 DEG C are warming up to, and keep the temperature 2h with the heating rate of 2 DEG C/min, last cooled to room temperature is received after being ground with agate mortar
Collection, becomes final product.
Claims (4)
- A 1. type " sea urchin " shape ZnO functional materials, it is characterised in that：The material agglomerates into " sea by ultra-thin ZnO nano piece Courage " shape structure, has the characteristics that 3-D solid structure, is with Zn (CH3COO)2•2H2O and NaOH is base stock, using hydro-thermal Required product is synthesized with high temperature sintering two-step method.
- 2. the preparation method of one kind " sea urchin " shape ZnO material as described in right 1, it is characterised in that including following preparation process：（1）Weigh 4 g（0.1 mol）NaOH solids, be dissolved in the deionized water of 100ml, be configured to 1mol/L's NaOH alkaline solutions are in case subsequent experimental uses；（2）Weigh 2.195g（0.01 mol）Zn (CH3COO)2•2H2O is added in the deionized water of 100ml, continuing magnetic force Stirring is configured to the Zn (CH of 0.1 mol/L3COO)2•2H2Then O solution takes 10ml steps（1）The middle alkaline solution being configured, Under the premise of magnetic force is stirred continuously, it is added dropwise to the Zn (CH being configured3COO)2•2H2In O solution, the cotton-shaped of white is formed Mixed solution is then heated to 90 DEG C, and keeps the temperature 2h by object, is cooled to and is formed wet gel at room temperature；（3）By step（2）The wet gel of middle formation is placed in 90 DEG C of vacuum drying chambers, dry to form xerogel state for 24 hours, 30min then is ground with agate mortar, is worn into white powder；（4）By step（3）In white powder be put into porcelain boat, be put into tube furnace, under Ar gas inert atmospheres, with 2 DEG C/heating rate of min is warming up to 400 DEG C, and keep the temperature 2h, last cooled to room temperature is collected after being ground with agate mortar, As final product；The preparation method of one kind " sea urchin " shape ZnO material as described in power 1, it is characterised in that：Step（2）Middle Zn (CH3COO)2•2H2O:NaOH=1:1（Molar ratio）.
- 3. the preparation method of one kind " sea urchin " shape ZnO material as described in right 1, it is characterised in that：Step（2）In NaOH it is molten Liquid is to be added dropwise rather than be all directly added into.
- 4. the preparation method of one kind " sea urchin " shape ZnO material as described in right 1, it is characterised in that：Step（4）In heating speed Rate is 2 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711489508.2A CN108163883A (en) | 2017-12-29 | 2017-12-29 | One kind has class " sea urchin " shape structure ZnO functional material and preparation method thereof |
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| CN201711489508.2A CN108163883A (en) | 2017-12-29 | 2017-12-29 | One kind has class " sea urchin " shape structure ZnO functional material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220081312A1 (en) * | 2020-09-16 | 2022-03-17 | Industry-Academic Cooperation Foundation, Yonsei University | Method for preparing sea urchin-shaped zinc oxide nanowire |
-
2017
- 2017-12-29 CN CN201711489508.2A patent/CN108163883A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220081312A1 (en) * | 2020-09-16 | 2022-03-17 | Industry-Academic Cooperation Foundation, Yonsei University | Method for preparing sea urchin-shaped zinc oxide nanowire |
| US11685665B2 (en) * | 2020-09-16 | 2023-06-27 | Industry-Academic Cooperation Foundation, Yonsei University | Method for preparing sea urchin-shaped zinc oxide nanowire |
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Application publication date: 20180615 |