CN105152202A - Preparation method for antimony-doped flower-ball-shaped tin dioxide gas-sensing material - Google Patents
Preparation method for antimony-doped flower-ball-shaped tin dioxide gas-sensing material Download PDFInfo
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- CN105152202A CN105152202A CN201510419003.3A CN201510419003A CN105152202A CN 105152202 A CN105152202 A CN 105152202A CN 201510419003 A CN201510419003 A CN 201510419003A CN 105152202 A CN105152202 A CN 105152202A
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Abstract
The invention provides a preparation method for an antimony-doped flower-ball-shaped tin dioxide gas-sensing material. The preparation method concretely comprises the following steps: with stannous chloride, antimony trichloride and sodium hydroxide as raw materials and hexadecyl trimethyl ammonium bromide as a surfactant, carrying out hydrothermal reaction and calcination treatment so as to obtain the antimony-doped flower-ball-shaped tin dioxide gas-sensing material. The obtained antimony-doped flower-ball-shaped tin dioxide gas-sensing material is flower-ball-shaped and is prepared by assembling a large number of two-dimensional nanometer sheets; meanwhile, antimony is doped into tin oxide crystal lattices, so good gas-sensing response to ethanol gas is realized. The method provided by the invention has the advantages of low cost, simple production process, high yield, no environmental pollution, and facilitation to large-scale industrial production.
Description
Technical field
The present invention relates to the preparation method relating to a kind of Sb doped flower ball-shaped tin dioxide gas-sensitive material, belong to advanced nano-functional material fabricating technology field.
Background technology
Stannic oxide (SnO
2) be a kind of n-type semiconductor of important broad-band gap, energy gap is 3.62eV.Because small-size effect and surface effects make nano tin dioxide have special photoelectric properties and air-sensitive performance, this makes it in gas sensor, stored material, electrode materials and solar cell etc., have potential application.Therefore to SnO
2the preparation of nano material and performance study thereof are quite active.The Morphology and structure of micro/nano structure functional materials is the principal element affecting its air-sensitive performance, and numerous scientific research personnel is devoted in preparation process, to control its Morphology and structure to realize the enhancing of air-sensitive performance.Three-dimensional hierarchical structure refers to the high-dimensional nanostructure assembled by low-dimensional nano structures such as such as nano particle, nanometer rod, nano wire, nanotube, nanometer sheet, makes it have the compages feature of nano material, mesopore/macropore material.In air-sensitive Application Areas, three-dimensional hierarchy construction particularly open hierarchy construction can not only suppress the reunion of nano particle to be grown up, retain nano material high-specific surface area, flourishing grading-hole passage (comprising mesoporous and macropore) can also be constructed simultaneously and strengthen the transmission of gas at material internal, be the ideal structure constructed highly sensitive and respond gas sensitive fast, day by day cause the concern of people.Meanwhile, research shows: in metal oxide preparation process, introduce additive (as precious metal element, transition metal oxide or other metal/non-metal oxide compounds), even seldom measure, a series of attributive character of body material also can change.Therefore, the three-dimensional hierarchical structure tin dioxide gas-sensitive material of other doped metallic oxides of controlledly synthesis, will effectively promote the raising of its performance in structure with composition two.
Summary of the invention
The object of the invention is to, overcome the deficiencies in the prior art, a kind of preparation method of Sb doped flower ball-shaped tin dioxide gas-sensitive material is provided.Have cost low, production technique is simple, and productive rate is high, non-environmental-pollution, is easy to the feature of industrialization scale operation.A kind of Sb doped flower ball-shaped of gained tin dioxide gas-sensitive material regular appearance, has excellent air-sensitive performance, can be used for the fields such as gas sensor.The technical scheme realizing the object of the invention is: a kind of preparation method of Sb doped flower ball-shaped tin dioxide gas-sensitive material, it is characterized in that: with tin protochloride, butter of antimony and sodium hydroxide for raw material, take cetyl trimethylammonium bromide as tensio-active agent, through hydro-thermal reaction, calcination processing, obtain Sb doped flower ball-shaped tin dioxide gas-sensitive material.Products therefrom is flower ball-shaped, assembled, and Sb doped enters stannic oxide lattice by a large amount of two-dimensional nano sheet, has the response of good air-sensitive to alcohol gas.Present method cost is low, and production technique is simple, and productive rate is high, non-environmental-pollution, is easy to industrialization scale operation.Concrete synthesis step is as follows:
(1) take a certain amount of tin protochloride and butter of antimony, be dissolved in deionized water, wherein the concentration of tin protochloride is 0.1-0.2mol/L, and the concentration of butter of antimony is 0.001-0.01mol/L, and the mol ratio controlling tin protochloride and butter of antimony is 100:1-5;
(2) a certain amount of sodium hydroxide and cetyl trimethylammonium bromide is taken, be dissolved in deionized water, wherein the concentration of sodium hydroxide is 0.4-0.8mol/L, the concentration of cetyl trimethylammonium bromide is 0.1-0.2mol/L, and the mol ratio controlling tin protochloride and sodium hydroxide is 1:4, the mol ratio of tin protochloride and cetyl trimethylammonium bromide is 1:1;
(3) by step (1) and the mixing of step (2) gained solution, it is in the hydrothermal reaction kettle of tetrafluoroethylene that gained mixing solutions moves to liner, at 140-180 DEG C of temperature, carry out hydro-thermal reaction 16-24 hour, again the product utilization whizzer after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(4) be positioned in loft drier by step (3) gained solid product, 60 DEG C of dryings 24 hours, be then placed in alumina crucible and put into retort furnace, thermal treatment 3 hours at 500 DEG C, obtains Sb doped flower ball-shaped tin dioxide gas-sensitive material.
Accompanying drawing explanation
The XRD figure spectrum of Fig. 1 Sb doped flower ball-shaped tindioxide
The low power FESEM collection of illustrative plates of Fig. 2 Sb doped flower ball-shaped tin dioxide gas-sensitive material
The high power FESEM collection of illustrative plates of Fig. 3 Sb doped flower ball-shaped tin dioxide gas-sensitive material
Fig. 4 Sb doped flower ball-shaped tin dioxide gas-sensitive material EDS power spectrum
The low power TEM figure of Fig. 5 Sb doped flower ball-shaped tin dioxide gas-sensitive material
The high power TEM figure of Fig. 6 Sb doped flower ball-shaped tin dioxide gas-sensitive material
Under Fig. 7 optimum operating voltage, Sb doped flower ball-shaped tin dioxide gas-sensitive material is to the sensitivity curve comparison diagram of the alcohol gas of 50-1000ppm.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
(1) take a certain amount of tin protochloride and butter of antimony, be dissolved in deionized water, wherein the concentration of tin protochloride is 0.1mol/L, and the concentration of butter of antimony is 0.003mol/L;
(2) take a certain amount of sodium hydroxide and cetyl trimethylammonium bromide, be dissolved in deionized water, wherein the concentration of sodium hydroxide is 0.4mol/L, and the concentration of cetyl trimethylammonium bromide is 0.1mol/L;
(3) by step (1) and the mixing of step (2) gained solution, it is in the hydrothermal reaction kettle of tetrafluoroethylene that gained mixing solutions moves to liner, at 160 DEG C of temperature, carry out hydro-thermal reaction 24 hours, again the product utilization whizzer after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(4) be positioned in loft drier by step (3) gained solid product, 60 DEG C of dryings 24 hours, be then placed in alumina crucible and put into retort furnace, thermal treatment 3 hours at 500 DEG C, obtains Sb doped flower ball-shaped tin dioxide gas-sensitive material.
Embodiment 2
(1) take a certain amount of tin protochloride and butter of antimony, be dissolved in deionized water, wherein the concentration of tin protochloride is 0.1mol/L, and the concentration of butter of antimony is 0.001mol/L;
(2) take a certain amount of sodium hydroxide and cetyl trimethylammonium bromide, be dissolved in deionized water, wherein the concentration of sodium hydroxide is 0.4mol/L, and the concentration of cetyl trimethylammonium bromide is 0.1mol/L;
(3) by step (1) and the mixing of step (2) gained solution, it is in the hydrothermal reaction kettle of tetrafluoroethylene that gained mixing solutions moves to liner, at 180 DEG C of temperature, carry out hydro-thermal reaction 16 hours, again the product utilization whizzer after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(4) be positioned in loft drier by step (3) gained solid product, 60 DEG C of dryings 24 hours, be then placed in alumina crucible and put into retort furnace, thermal treatment 3 hours at 500 DEG C, obtains Sb doped flower ball-shaped tin dioxide gas-sensitive material.
Embodiment 3
(1) take a certain amount of tin protochloride and butter of antimony, be dissolved in deionized water, wherein the concentration of tin protochloride is 0.2mol/L, and the concentration of butter of antimony is 0.006mol/L;
(2) take a certain amount of sodium hydroxide and cetyl trimethylammonium bromide, be dissolved in deionized water, wherein the concentration of sodium hydroxide is 0.8mol/L, and the concentration of cetyl trimethylammonium bromide is 0.2mol/L;
(3) by step (1) and the mixing of step (2) gained solution, it is in the hydrothermal reaction kettle of tetrafluoroethylene that gained mixing solutions moves to liner, at 160 DEG C of temperature, carry out hydro-thermal reaction 20 hours, again the product utilization whizzer after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(4) be positioned in loft drier by step (3) gained solid product, 60 DEG C of dryings 24 hours, be then placed in alumina crucible and put into retort furnace, thermal treatment 3 hours at 500 DEG C, obtains Sb doped flower ball-shaped tin dioxide gas-sensitive material.
Embodiment 4
(1) take a certain amount of tin protochloride and butter of antimony, be dissolved in deionized water, wherein the concentration of tin protochloride is 0.15mol/L, and the concentration of butter of antimony is 0.0045mol/L;
(2) take a certain amount of sodium hydroxide and cetyl trimethylammonium bromide, be dissolved in deionized water, wherein the concentration of sodium hydroxide is 0.6mol/L, and the concentration of cetyl trimethylammonium bromide is 0.15mol/L;
(3) by step (1) and the mixing of step (2) gained solution, it is in the hydrothermal reaction kettle of tetrafluoroethylene that gained mixing solutions moves to liner, at 160 DEG C of temperature, carry out hydro-thermal reaction 22 hours, again the product utilization whizzer after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(4) be positioned in loft drier by step (3) gained solid product, 60 DEG C of dryings 24 hours, be then placed in alumina crucible and put into retort furnace, thermal treatment 3 hours at 500 DEG C, obtains Sb doped flower ball-shaped tin dioxide gas-sensitive material.
Embodiment 5
(1) take a certain amount of tin protochloride and butter of antimony, be dissolved in deionized water, wherein the concentration of tin protochloride is 0.1mol/L, and the concentration of butter of antimony is 0.001mol/L;
(2) take a certain amount of sodium hydroxide and cetyl trimethylammonium bromide, be dissolved in deionized water, wherein the concentration of sodium hydroxide is 0.4mol/L, and the concentration of cetyl trimethylammonium bromide is 0.1mol/L;
(3) by step (1) and the mixing of step (2) gained solution, it is in the hydrothermal reaction kettle of tetrafluoroethylene that gained mixing solutions moves to liner, at 170 DEG C of temperature, carry out hydro-thermal reaction 18 hours, again the product utilization whizzer after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(4) be positioned in loft drier by step (3) gained solid product, 60 DEG C of dryings 24 hours, be then placed in alumina crucible and put into retort furnace, thermal treatment 3 hours at 500 DEG C, obtains Sb doped flower ball-shaped tin dioxide gas-sensitive material.
test-results
The Sb doped flower ball-shaped tindioxide prepared by embodiment 1 is composed through the XRD figure of X-ray diffractometer test gained, as shown in Figure 1; Through high power and the low power FESEM picture of field emission scanning electron microscope shooting gained, as shown in Figures 2 and 3; EDS energy spectrum analysis is utilized to analyze its component, shown in its result and Fig. 4; The high power that Sb doped flower ball-shaped tindioxide is taken through transmission electron microscope and low power TEM picture, as shown in Figure 5 and Figure 6; Fig. 7 be in embodiment 1 Sb doped flower ball-shaped tin dioxide gas-sensitive material to the dynamic response recovery curve of different concentration ethanol gas.
As can be seen from Figure 1, adopt the position of all diffraction peaks of the XRD figure of the sample prepared by the present invention spectrum to be consistent with international diffraction data standard card JCPDSNo.710652, degree of crystallinity is good, there is no weisspiessglanz diffraction peak and occurs.
Can find out that gained sample is flower ball-shaped from Fig. 2 low power FESEM picture, size is about 4-5 micron, and this bouquet is assembled by numerous two-dimensional sheet structure, regular appearance; As can be seen from Fig. 3 high power FESEM picture, the two-dimensional sheet diameter of movement of composition bouquet is about 1 micron, and thickness is about 20 nanometers, is made up of a large amount of tiny nano particle; The EDS energy spectrum analysis of Fig. 4 demonstrates the existence of Sb element, in conjunction with XRD figure spectrum analysis, shows that weisspiessglanz enters in tindioxide crystalline network.
It is the three-dimensional structure bouquet that numerous nanometer sheet assembles that the TEM picture of Fig. 5 more clearly can observe gained sample, is typical three-dimensional hierarchical structure; Fig. 6 high power TEM picture shows that the tin oxide nano particles that nanometer sheet is about 10-20 nanometer by diameter is formed, and there is a large amount of hole, and this will be conducive to improving its air-sensitive performance.
Fig. 7 be in embodiment 1 Sb doped flower ball-shaped tin dioxide gas-sensitive material to the dynamic response recovery curve of different concentration ethanol gas, can find out: along with the increase of alcohol concn, the sensitivity of Sb doped flower ball-shaped tin dioxide gas-sensitive material also increases gradually, 25 are reached to the sensitivity of 50ppm ethanol, and response, time of recovery all within 20 seconds, demonstrate good ethanol air-sensitive performance.
Claims (1)
1. a preparation method for Sb doped flower ball-shaped tin dioxide gas-sensitive material, concrete synthesis step is as follows:
(1) take a certain amount of tin protochloride and butter of antimony, be dissolved in deionized water, wherein the concentration of tin protochloride is 0.1-0.2mol/L, and the concentration of butter of antimony is 0.001-0.01mol/L, and the mol ratio controlling tin protochloride and butter of antimony is 100:1-5;
(2) a certain amount of sodium hydroxide and cetyl trimethylammonium bromide is taken, be dissolved in deionized water, wherein the concentration of sodium hydroxide is 0.4-0.8mol/L, the concentration of cetyl trimethylammonium bromide is 0.1-0.2mol/L, and the mol ratio controlling tin protochloride and sodium hydroxide is 1:4, the mol ratio of tin protochloride and cetyl trimethylammonium bromide is 1:1;
(3) by step (1) and the mixing of step (2) gained solution, it is in the hydrothermal reaction kettle of tetrafluoroethylene that gained mixing solutions moves to liner, at 140-180 DEG C of temperature, carry out hydro-thermal reaction 16-24 hour, again the product utilization whizzer after hydro-thermal reaction is carried out solid-liquid separation, and with deionized water and ethanol, gained solid product is repeatedly washed;
(4) be positioned in loft drier by step (3) gained solid product, 60 DEG C of dryings 24 hours, be then placed in alumina crucible and put into retort furnace, thermal treatment 3 hours at 500 DEG C, obtains Sb doped flower ball-shaped tin dioxide gas-sensitive material.
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| JP2020106445A (en) * | 2018-12-28 | 2020-07-09 | 国立研究開発法人産業技術総合研究所 | Bridge-shaped tin oxide-containing sheet and method of manufacturing the same |
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