CN106904659B - A kind of preparation method of multi-layer hollow stannic oxide flower-like nanometer piece surface growth di-iron trioxide nanometer rods - Google Patents
A kind of preparation method of multi-layer hollow stannic oxide flower-like nanometer piece surface growth di-iron trioxide nanometer rods Download PDFInfo
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- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
The present invention is a kind of preparation method of Heteroepitaxy di-iron trioxide on multi-layer hollow flower-like nanometer piece stannic oxide surface, belong to the technical field of nano material preparation, this method first prepares multi-layer hollow flower-like nanometer piece stannic oxide, then using multi-layer hollow flower-like nanometer piece stannic oxide as presoma, it is dispersed in aqueous solution, sal glauberi and ferric chloride (FeCl36H2O) is added, pass through hydro-thermal reaction at a certain temperature, its reaction is set to generate the predecessor of di-iron trioxide nanometer rods, and the Heteroepitaxy on the multi-layer hollow of preparation graduation flower-like nanometer piece stannic oxide surface, it is annealed 2 hours by 450 degree, obtain the composite material of Heteroepitaxy di-iron trioxide on multi-layer hollow flower-like nanometer piece stannic oxide surface.The present invention provides a kind of novel semiconductor nanometer composite material preparation methods, are grown by Heterogeneous Composite, stannic oxide and di-iron trioxide are combined with each other, can show excellent air-sensitive performance.
Description
Technical field
The invention belongs to the technical fields of nano material preparation, and in particular to a kind of multi-layer hollow stannic oxide flower-like nanometer
Piece surface grows the preparation method of di-iron trioxide nanometer rods, such composite material shows excellent in gas sensor field
Air-sensitive performance, have potential using value.
Background technique
In recent years, with the rapid development of social economy and industrial production technology, people are faced with the environment got worse
Pollution problem, people more pay attention to the monitoring and detection to toxic and harmful gas, flammable explosive gas and atmosphere pollution.
Gas sensor is as a kind of effective gas detection tool in industrial production monitoring, home environment safety, atmospheric monitoring, medical treatment
And the fields such as national defence are widely used.Therefore, the development of good, high sensitivity the gas sensor of selectivity has become closely
The hot spot studied both at home and abroad over year.
Stannic oxide is a kind of important n-type semiconductor inorganic material, due to its unique physics and chemical property,
The fields such as gas sensor, photocatalysis, dye-sensitized solar cells, lithium ion battery and transparent electrode, which have, widely answers
With.SnO2It is a kind of adsorption control type gas sensitive, many because being known as of its air-sensitive performance is influenced, such as SnO2Material internal
Microstructure, the size of particle, the specific surface area of material, surface defect etc..Prepare the micro-nano structure SnO of complex topography2Tool
There are the characteristics such as small crystallite dimension, big specific surface area, high surface activity, adsorbed gas ability are strong and gas reaction is fast, it can pole
The earth improves its air-sensitive performance.It can also make SnO by adulterating different metal and metal oxide simultaneously2Gas sensor work
Make temperature decline, response to gas and recovery time shorten, and improve its selectivity under test gas, make its sensitivity and
Stability greatly improves.
By a large amount of literature survey, di-iron trioxide has excellent air-sensitive performance, has extensively for gas sensor
Application.In addition, existing template (hard template, soft template) synthesis cost is high, goes the nanometer that the process of template is cumbersome, synthesizes
Material is largely by the limitation of formwork structure, the defects of existing gas sensitive still has poor selectivity, and operating temperature is high.It is non-
Ball shaped nano material compares ball shaped nano material, significantly reduces the contact resistance between particle, promotes the gas sensing property of material
It can performance.
Summary of the invention
The technical problem to be solved by the present invention is to, overcome background technique there are the shortcomings that, provide it is a kind of low cost, operation letter
A kind of single, fast, environmental-friendly, low-carbon high-efficiency three oxidation of multi-layer hollow stannic oxide flower-like nanometer piece surface growth of reaction rate
The preparation method of two iron nanometer rods.
The specific technical solution that the present invention takes is as follows：
A kind of preparation method of multi-layer hollow stannic oxide flower-like nanometer piece surface growth di-iron trioxide nanometer rods
The first step：ZnSn(OH)6The synthesis of flower-like nanometer piece template, by the SnCl of the ZnO of 13mg, 70~210mg4·
5H20, the NaOH and CTAB of 240mg is dissolved in the deionized water of 40mL, and 60r/s stirs 10min.Mixed solution is put into
In the reaction kettle of polytetrafluoroethylliner liner, react 12h in the environment of 180~190 DEG C, by the precipitating after reaction spend respectively from
Sub- water and each eccentric cleaning of dehydrated alcohol three times, the drying in oven at 60 DEG C is dry later and collects sample.
Second step：Graded structure multi-layer hollow Sn02The synthesis of flower-like nanometer piece, the ZnSn that will be prepared in the first step
(OH)6Template is annealed 30min at 850 DEG C, is cooled to room temperature and is obtained Zn2Sn04/Sn02Mixed phase template.After taking 10mg to anneal
Sample is dissolved in the HN0 that 9mL concentration is 8M3In solution, static 8~for 24 hours after eccentric cleaning and collect precipitating.
Third step：Ferric oxide coated graded structure multilayer stannic oxide flower-like nanometer piece takes 10~30 milligram
The stannic oxide prepared in two steps is put into 100 milliliters of beaker, measures 40 ml deionized waters with liquid-transfering gun and beaker is added
In, beaker is put into magnetic stirring apparatus and is stirred, then weigh 30~90 milligrams sal glauberi be added stirring solution in, most
20~75 milligrams of ferric chloride (FeCl36H2O)s are weighed afterwards to be added in the solution of stirring, solution are continued to be stirred at room temperature 10 minutes, then will be molten
It is transferred in 40 milliliters of autoclaves, is put into baking oven, be raised to 110~120 degrees Celsius by room temperature, heat preservation 0.5~1.5 is small
When, natural cooling stands, reactant is taken out, centrifuge washing, dry.The complete reactant of drying is put into tube furnace by room
Temperature is heated to 400~450 degrees Celsius with 5 degree every point of heating rate, keeps the temperature 2~3 hours, natural cooling simultaneously collects sample.
Operating procedure of the invention is mainly in two stages：First stage is to prepare graded structure multi-layer hollow titanium dioxide
The synthesis process of tin flower-like nanometer piece, first passes through hydro-thermal reaction, regulates hydrothermal temperature and hydro-thermal time, and CTAB is added as table
Face activating agent passes through reactant ZnO, SnCl4·5H20, the reaction of NaOH forms flower-shaped ZnSn (OH)6Multi-layer nano piece, then
Method by annealing, etching forms the flower-shaped hollow tin dioxide nanosheet of multilayer of pure phase.Second stage is multi-layer hollow two
Tin oxide flower-like nanometer piece surface grows di-iron trioxide nanometer rod motion, using aqueous solution as solvent, in 120 degrees Celsius of hydro-thermal
Under the conditions of, by the way that sal glauberi and ferric chloride (FeCl36H2O) is added as reactant, reacts it under hydrothermal conditions, keep it anti-
The predecessor of di-iron trioxide nanometer rods should be generated, and in the multi-layer hollow of preparation graduation flower-like nanometer piece stannic oxide table
Heteroepitaxy on face is annealed 2~3 hours by 400~450 degree, is obtained on multi-layer hollow flower-like nanometer piece stannic oxide surface
The composite material of Heteroepitaxy di-iron trioxide can more improve the performance of combination product in this way, further increase a nanometer material
The specific surface area of material has excellent air-sensitive performance.
The invention has the following beneficial effects：
1, the nanocomposite of composite structure excellent stannic oxide and di-iron trioxide, not easy to reunite, anisotropy,
There are large specific surface area and higher chemical activity, there are a large amount of face contacts between particle, air-sensitive performance is excellent.
2, environmental-friendly, in whole experiment process, no toxic pharmaceuticals addition avoids the pollution to environment.
3, the nanocomposite of stannic oxide and di-iron trioxide prepared by the present invention have large specific surface area and compared with
High chemical activity.
Detailed description of the invention
Fig. 1 is the scanned photograph figure of multi-layer hollow stannic oxide flower-like nanometer piece prepared by embodiment 1.
Fig. 2 is the transmission photo figure of multi-layer hollow stannic oxide flower-like nanometer piece prepared by embodiment 1.
Fig. 3 is the X-ray diffractogram of multi-layer hollow stannic oxide flower-like nanometer piece prepared by embodiment 1.
Fig. 4 is growth di-iron trioxide nanometer rods in multi-layer hollow stannic oxide flower-like nanometer piece surface prepared by embodiment 2
Scanned photograph figure.
Fig. 5 is growth di-iron trioxide nanometer rods in multi-layer hollow stannic oxide flower-like nanometer piece surface prepared by embodiment 2
Transmission photo figure.
Fig. 6 is growth di-iron trioxide nanometer rods in multi-layer hollow stannic oxide flower-like nanometer piece surface prepared by embodiment 2
X-ray diffractogram.
Specific embodiment
Embodiment 1：
The stannic oxide flower-like nanometer piece for first preparing multi-layer hollow, then uses multi-layer hollow flower-like nanometer piece as before
Body is driven, using aqueous solution as solvent, under 120 degrees Celsius of hydrothermal condition, by the way that sal glauberi and ferric chloride (FeCl36H2O) is added
It as reactant, reacts it under hydrothermal conditions, at a certain temperature by hydro-thermal reaction, its reaction is made to generate three oxidations two
The predecessor of iron nanometer rods, and the Heteroepitaxy on the multi-layer hollow of preparation graduation flower-like nanometer piece stannic oxide surface,
It is annealed 2 hours by 450 degree, obtains answering for Heteroepitaxy di-iron trioxide on multi-layer hollow flower-like nanometer piece stannic oxide surface
Condensation material, specific preparation process is as follows：
The first step：ZnSn(OH)6The synthesis of flower-like nanometer piece template, by the SnCl of ZnO, 105mg of 13mg4·5H20、
The NaOH and CTAB of 240mg is dissolved in the deionized water of 40mL, and 60r/s stirs 10min, and mixed solution is put into polytetrafluoro
In the reaction kettle of ethylene liner, 12h is reacted in the environment of 180 DEG C, the precipitating after reaction is used into deionized water and anhydrous respectively
Each eccentric cleaning of ethyl alcohol three times, the drying in oven at 60 DEG C is dry later and collects sample；
Second step：Graded structure multi-layer hollow Sn02The synthesis of flower-like nanometer piece, the ZnSn that will be prepared in the first step
(OH)6Template is annealed 30min at 850 DEG C, is cooled to room temperature and is obtained Zn2Sn04/Sn02Mixed phase template, after taking 10mg to anneal
Sample is dissolved in the HN0 that 9mL concentration is 8M3Eccentric cleaning and precipitating is collected in solution, after static 8h；
Third step：Ferric oxide coated graded structure multilayer stannic oxide flower-like nanometer piece, takes 20 milligrams of second steps
In the stannic oxide for preparing be put into 100 milliliters of beaker, measure 40 ml deionized waters with liquid-transfering gun and be added in beaker, will
Beaker is put into magnetic stirring apparatus and stirs, then weigh 85.8 milligrams sal glauberi be added stirring solution in, finally weigh
71.6 milligrams of ferric chloride (FeCl36H2O)s are added in the solution of stirring, solution are continued to be stirred at room temperature 10 minutes, then be transferred to 40 for molten
It in milliliter autoclave, is put into baking oven, is raised to 120 degrees Celsius by room temperature, keeps the temperature 1.5 hours, natural cooling is stood, will
Reactant takes out, centrifuge washing, dry.The complete reactant of drying is put into tube furnace by room temperature with 5 degree every point of heating speed
Rate is heated to 450 degrees Celsius, keeps the temperature 2 hours, natural cooling simultaneously collects sample.
Embodiment 2：
By the SnCl of ZnO, 105mg of 13mg4·5H20, the NaOH and CTAB of 240mg is dissolved in the deionized water of 40mL
In, by hydro-thermal reaction, synthesize ZnSn (OH)6Flower-like nanometer piece, by the ZnSn prepared (OH)6Template is annealed at 850 DEG C
30min is cooled to room temperature and obtains Zn2Sn04/Sn02Mixed phase template.It is 8M's that sample, which is dissolved in 9mL concentration, after taking 10mg to anneal
HN03In solution, after static 8h, eccentric cleaning simultaneously collects precipitating, obtains multi-layer hollow stannic oxide flower-like nanometer piece, scanning
Photo figure, transmission photo figure and X-ray diffractogram are shown in attached drawing 1, attached drawing 2 and attached drawing 3 respectively.Crystal structure crystallinity is fine, with
The standard card (JCPDS 41-1445) of stannic oxide is completely corresponding, without any miscellaneous peak, illustrates that sample is the dioxy of high-purity
Change tin.
Stannic oxide obtained above is dissolved into 40 ml deionized waters, then weighs 85.8 milligrams of sal glauberi
Be added in the solution of stirring, finally weigh 71.6 milligrams of ferric chloride (FeCl36H2O)s and be added in the solution of stirring, then in an oven into
120 DEG C water thermal response of row keeps the temperature 1.5 hours, and natural cooling stands, reactant taken out, centrifuge washing, dry.It will do
Dry complete reactant is put into tube furnace at 450 degrees Celsius, keeps the temperature 2 hours, natural cooling simultaneously collects sample.Obtain multi-layer hollow
Stannic oxide flower-like nanometer piece surface grows di-iron trioxide nanometer rod composite material, scanned photograph figure, transmission photo figure and X
X ray diffration pattern x is shown in attached drawing 4, attached drawing 5 and attached drawing 6 respectively.
Claims (1)
1. a kind of preparation method of multi-layer hollow stannic oxide flower-like nanometer piece surface growth di-iron trioxide nanometer rods, first prepares
The stannic oxide flower-like nanometer piece of multi-layer hollow out, uses multi-layer hollow flower-like nanometer piece as presoma, then with aqueous solution
Reaction is used as by the way that sal glauberi and ferric chloride (FeCl36H2O) is added under 110~120 degrees Celsius of hydrothermal condition for solvent
Object reacts it under hydrothermal conditions, at a certain temperature by hydro-thermal reaction, its reaction is made to generate di-iron trioxide nanometer rods
Predecessor, and the Heteroepitaxy on the multi-layer hollow of preparation graduation flower-like nanometer piece stannic oxide surface, by 400~
450 degree are annealed 2~3 hours, and answering for Heteroepitaxy di-iron trioxide on multi-layer hollow flower-like nanometer piece stannic oxide surface is obtained
Condensation material, specific preparation process is as follows：
The first step：ZnSn(OH)6The synthesis of flower-like nanometer piece template, by the SnCl of the ZnO of 13mg, 70~210mg4·5H20、
The NaOH and CTAB of 240mg is dissolved in the deionized water of 40mL, and 60r/s stirs 10min, and mixed solution is put into polytetrafluoro
In the reaction kettle of ethylene liner, react 12h in the environment of 180~190 DEG C, by the precipitating after reaction use respectively deionized water and
Each eccentric cleaning of dehydrated alcohol three times, the drying in oven at 60 DEG C is dry later and collects sample；
Second step：Graded structure multi-layer hollow Sn02The synthesis of flower-like nanometer piece, by the ZnSn prepared in the first step (OH)6
Template is annealed 30min at 850 DEG C, is cooled to room temperature and is obtained Zn2Sn04/Sn02Mixed phase template, sample is molten after taking 10mg to anneal
Solution is in the HN0 that 9mL concentration is 8M3In solution, static 8~for 24 hours after eccentric cleaning and collect precipitating；
Third step：Ferric oxide coated graded structure multilayer stannic oxide flower-like nanometer piece, takes 10~30 milligrams of second steps
In the stannic oxide for preparing be put into 100 milliliters of beaker, measure 40 ml deionized waters with liquid-transfering gun and be added in beaker, will
Beaker is put into magnetic stirring apparatus and stirs, then weigh 30~90 milligrams sal glauberi be added stirring solution in, finally claim
It takes 20~75 milligrams of ferric chloride (FeCl36H2O)s to be added in the solution of stirring, solution is continued to be stirred at room temperature 10 minutes, then solution is turned
It moves on in 40 milliliters of autoclaves, is put into baking oven, be raised to 110~120 degrees Celsius by room temperature, keep the temperature 0.5~1.5 hour,
Natural cooling stands, reactant is taken out, centrifuge washing, dry, by the complete reactant of drying be put into tube furnace by room temperature with
5 degree every point of heating rate is heated to 400~450 degrees Celsius, keeps the temperature 2~3 hours, natural cooling simultaneously collects sample.
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| CN110697777A (en) * | 2019-10-09 | 2020-01-17 | 西北工业大学 | Preparation method of tin molybdenum disulfide with hollow structure |
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