CN103626232B - A kind of flower pattern Ho-Bi 2wO 6nano-powder and its preparation method and application - Google Patents

A kind of flower pattern Ho-Bi 2wO 6nano-powder and its preparation method and application Download PDF

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CN103626232B
CN103626232B CN201310416351.6A CN201310416351A CN103626232B CN 103626232 B CN103626232 B CN 103626232B CN 201310416351 A CN201310416351 A CN 201310416351A CN 103626232 B CN103626232 B CN 103626232B
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谈国强
黄靖
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Yancheng modern green plant protection Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a kind of flower pattern Ho-Bi 2wO 6nano-powder and its preparation method and application, respectively by soluble in water by a certain percentage to five water Bismuth trinitrates, tungstate dihydrate acid sodium and six water holmium nitrates, after stirring, adjust ph obtains precursor liquid, obtains flower pattern Ho-Bi by microwave-hydrothermal method with the power of 300W at 140 DEG C-240 DEG C insulation 30-120min 2wO 6nano-powder, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Ho 3+.Morphology control is one of direction of Study on photocatalyst always, and present invention incorporates the advantage of microwave and hydrothermal method, technique is simple and easy to control, and preparation cycle is short, when without the flower pattern Ho-Bi preparing morphology controllable when any additive 2wO 6nano-powder, and this powder dispersity is good, pattern stable homogeneous, possesses good photocatalytic activity, can be used for degradation of organic substances.

Description

A kind of flower pattern Ho-Bi 2wO 6nano-powder and its preparation method and application
Technical field
The invention belongs to field of functional materials, relate to a kind of flower pattern Ho-Bi 2wO 6nano-powder and its preparation method and application.
Background technology
Nanoparticle is in the transitional region of atom and macroscopic material, and impart the special property being not only different from body phase material but also being different from individual molecule, such system is atypical microscopic system also atypical macrosystem both, is a kind of typical Mesoscopic structure.It has the physics-chem characteristic of series of novel usually, relates to basic Physico-Chemical Problems that is that ignore in body phase material or that do not have.Usually the specific performance of nano material is summed up as this few class of surface effects, small-size effect, quantum size effect and macro quanta tunnel effect, it optics, calorifics, electricity, magnetics, mechanics and chemical in character compare will have significant difference with bulk solid.
The semiconductor materials such as tungstate, because of its distinctive structure and physicochemical property, are subject to people's attention day by day, study very active.Systematically study the characteristics of luminescence and the relation of crystalline structure, the relation between pattern and photochemical catalysis of the semiconductor material system such as tungstate, can be advanced luminescent material and designing and developing of photocatalyst material provides theoretical foundation.
Bismuth tungstate has following characteristics as a kind of novel photocatalyst: the Uv and visible light response that (1) is good; (2) thermally-stabilised; (3) photochemical catalysis is stablized; (4) advantage of lower cost; (5) environmental friendliness.Therefore, Bi 2wO 6the research and development of photocatalyst material, for improving solar energy utilization ratio, will have potential practical value in environmental purification and new energy development.But simultaneously also just because of its energy gap relative narrower, the recombination probability of photo-generate electron-hole is increased, reduces the efficiency of photon, thus have influence on Bi 2wO 6photocatalysis performance.
Rare earth because its special electron structure, has the spectral response curve that general element is incomparable, and the 4f electronics with the compound that the rare earth atom of the 4f shell of underfilling or ion are formed can generation transition between f-f configuration or between f-d configuration.Therefore, rare-earth metal doped ion is the focus begun one's study in recent years.Some rare earth oxide itself is also hopeful to use as photocatalyst, but generally speaking, carries out considerably less using simple rare earth oxide as the research of photocatalyst.And doping content also has a great impact reactive behavior.
Tungstate photocatalyst is normally with the preparation of high-temperature calcination method.Calcining not only consumes a large amount of energy, and the particle size of the sample prepared is large, and the specific surface area of catalyzer reduces greatly, though can realize visible light-responded, photocatalysis efficiency is unsatisfactory.
In recent years, hydrothermal method was adopted to prepare Bi 2wO 6nanocrystal becomes a focus of research.But, in traditional hydrothermal synthesis method, shortcomings such as adopting common conduction often, this type of heating has that heating rate is slow, long reaction time, heat distribution are uneven, thermograde is large, has had a strong impact on the character of synthetic powder, particle scale etc.It is controlled that microwave-hydrothermal method has condition, with low cost, environment gentleness waits many merits, be considered to the synthetic method of nearly Green Chemistry, and microwave hydrothermal method is to inorganic reaction and the size of inorganic photocatalyst material that generates thus, pattern, structure, crystallinity presents special effect, particularly can make inorganic photocatalyst material surface metastable structure, the effective group of Atomic Arrangement and surface is conducive to the photocatalysis performance of material greatly, be suitable for being generalized in large-scale industrial production and go, in nano materials, good development momentum and wide application prospect is shown in the fields such as stupalith.
Summary of the invention
The object of the present invention is to provide a kind of flower pattern Ho-Bi 2wO 6nano-powder and its preparation method and application, this preparation method's reaction times is short, and technical process is simple, obtained flower pattern Ho-Bi 2wO 6nano-powder possesses good photocatalytic activity.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of flower pattern Ho-Bi 2wO 6the preparation method of nano-powder, comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o and Na 2wO 42H 2o puts into container according to the mol ratio of Bi:W=2:1, and by Ho (NO 3) 36H 2o joins in container, wherein the add-on x=2%-20% of Ho, x=n ho/ (n bi+ n ho) × 100%, n biand n hobe respectively the molar weight of Bi and Ho;
Step 2: water is joined in container, stirred at ambient temperature is even, and be mixed with mixing solutions, adjust ph is 1.5-2.0, obtains precursor liquid;
Step 3: precursor liquid is moved in microwave hydrothermal reaction kettle, then microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stopped reaction be incubated 30-120min at 140 DEG C-240 DEG C after;
Step 4: after question response temperature is down to room temperature, takes out microwave hydrothermal reaction kettle, isolates throw out wherein, then obtain flower pattern Ho-Bi by after throw out washing, ultrasonic disperse, freeze-day with constant temperature 2wO 6nano-powder.
Bi (NO in the mixing solutions of described step 2 3) 35H 2the concentration of O is 0.1mol/L-0.6mol/L, Na 2wO 42H 2the concentration of O is 0.05mol/L-0.3mol/L.
The required time that stirs in described step 2 is 30-60min.
In described step 3, the compactedness of microwave hydrothermal reaction kettle is 40%-70%.
In described step 3, the liner of microwave hydrothermal reaction kettle is tetrafluoroethylene material.
In order to use deionized water and dehydrated alcohol, washing precipitate is extremely neutral respectively in washing in described step 4.
The time of the ultrasonic disperse in described step 4 is 30-60min.
The drying temperature of the freeze-day with constant temperature in described step 4 is 75-85 DEG C, and time of drying is 12-24h.
Described flower pattern Ho-Bi 2wO 6the flower pattern Ho-Bi that the preparation method of nano-powder obtains 2wO 6nano-powder, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Ho 3+, wherein the content of Ho is x=2%-20%, and it has the flower pattern pattern be assembled into by nanometer sheet.
Described flower pattern Ho-Bi 2wO 6the flower pattern Ho-Bi that the preparation method of nano-powder obtains 2wO 6the application of nano-powder in degradation of organic substances.
Compared with prior art, the present invention has following beneficial effect:
Flower pattern Ho-Bi provided by the invention 2wO 6the preparation method of nano-powder, with five water Bismuth trinitrate (Bi (NO 3) 35H 2o) be Bi source, tungstate dihydrate acid sodium (Na 2wO 42H 2o) be W source, six water holmium nitrate (Ho (NO 3) 36H 2o) be Ho source, by soluble in water again after three kinds of raw material mixing, be made into precursor liquid, then carry out microwave hydrothermal reaction, by Ho 3+introduce Bi 2wO 6in, obtain flower pattern Ho-Bi 2wO 6nano-powder.The microwave-hydrothermal method that the present invention adopts combines the heat characteristic of microwave uniqueness and the advantage of hydrothermal method, do not need to add other additive, energy one-step synthesis product, speed of response is fast, generated time is short, reaction conditions is gentle, reaction efficiency is high, environmental friendliness, technique are simple and easy to control, preparation cycle is short, save the energy, and can be obtained the flower pattern Ho-Bi of the morphology controllable with excellent photocatalysis performance by Controlling Technology parameter 2wO 6nano-powder.
Flower pattern Ho-Bi provided by the invention 2wO 6nano-powder is orthorhombic phase structure, even particle size distribution, and narrow diameter distribution, pattern stable homogeneous, purity are higher, have visible light-responded performance, and be a kind of visible light responsible photocatalytic material with high catalytic activity, its main component is Bi 2wO 6, and Bi 2wO 6in containing Ho 3+.Flower pattern Ho-Bi provided by the invention 2wO 6nano-powder has the flower pattern pattern be assembled into by nanometer sheet, and has good visible light photocatalysis active, shows good photocatalysis performance, can be used in degradation of organic substances, have a good application prospect when degradating organic dye rhodamine B.
Accompanying drawing explanation
Fig. 1 is flower pattern Ho-Bi prepared by the embodiment of the present invention 2 2wO 6the XRD figure of nano-powder;
Fig. 2 is flower pattern Ho-Bi prepared by the embodiment of the present invention 2 2wO 6the SEM figure of nano-powder, wherein the magnification of a is 10k times, and the magnification of b is 200k times;
Fig. 3 is flower pattern Ho-Bi prepared by the embodiment of the present invention 2 2wO 6the absorbancy change curve of nano-powder rhodamine B degradation under different time.
Embodiment
Be described further the present invention below in conjunction with drawings and Examples, raw material is analytical pure.
Embodiment 1:
Flower pattern Ho-Bi 2wO 6the preparation method of nano-powder, comprises the following steps:
Step 1: take Bi (NO respectively according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, and takes a certain amount of Ho (NO 3) 36H 2o joins in beaker, wherein the add-on x=2% of Ho, x=n ho/ (n bi+ n ho) × 100%, n biand n hobe respectively the molar weight of Bi and Ho;
Step 2: measure deionized water and join in beaker, stirred at ambient temperature 30min fully dissolves to raw material and forms white suspension liquid, is mixed with mixing solutions, wherein Bi (NO 3) 35H 2the concentration of O is 0.6mol/L, Na 2wO 42H 2the concentration of O is 0.3mol/L, and adjust ph is 1.6, obtains precursor liquid;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the compactedness controlling microwave hydrothermal reaction kettle is 40%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stopped reaction be incubated 120min at 220 DEG C after;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate throw out wherein, after deionized water and absolute ethanol washing throw out to neutrality, ultrasonic disperse 60min is to reduce the reunion of nano-powder again, then obtains flower pattern Ho-Bi after freeze-day with constant temperature 24h at 75 DEG C 2wO 6nano-powder.
Obtained flower pattern Ho-Bi 2wO 6nano-powder, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Ho 3+, wherein the content of Ho is x=2%, and it has the flower pattern pattern be assembled into by nanometer sheet.
Embodiment 2:
Flower pattern Ho-Bi 2wO 6the preparation method of nano-powder, comprises the following steps:
Step 1: take Bi (NO respectively according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, and takes a certain amount of Ho (NO 3) 36H 2o joins in beaker, wherein the add-on x=10% of Ho, x=n ho/ (n bi+ n ho) × 100%, n biand n hobe respectively the molar weight of Bi and Ho;
Step 2: measure deionized water and join in beaker, stirred at ambient temperature 60min fully dissolves to raw material and forms white suspension liquid, is mixed with mixing solutions, wherein Bi (NO 3) 35H 2the concentration of O is 0.1mol/L, Na 2wO 42H 2the concentration of O is 0.05mol/L, and adjust ph is 1.8, obtains precursor liquid;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the compactedness controlling microwave hydrothermal reaction kettle is 60%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stopped reaction be incubated 90min at 240 DEG C after;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate throw out wherein, after deionized water and absolute ethanol washing throw out to neutrality, ultrasonic disperse 40min is to reduce the reunion of nano-powder again, then obtains flower pattern Ho-Bi after freeze-day with constant temperature 24h at 80 DEG C 2wO 6nano-powder.
Obtained flower pattern Ho-Bi 2wO 6nano-powder, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Ho 3+, wherein the content of Ho is x=10%, and it has the flower pattern pattern be assembled into by nanometer sheet.
Fig. 1 is flower pattern Ho-Bi prepared by the embodiment of the present invention 2 2wO 6the XRD figure of nano-powder, as can be seen from the figure, the flower pattern Ho-Bi of preparation 2wO 6all diffraction peaks of nano-powder are consistent with PDF card (JCPDSNO.39-0256), are orthorhombic phase Bi 2wO 6structure, diffraction peak is comparatively sharp-pointed, does not have dephasign to generate, has stronger degree of crystallinity.
Fig. 2 is flower pattern Ho-Bi prepared by the embodiment of the present invention 2 2wO 6the SEM figure of nano-powder, as can be seen from the figure, the flower pattern Ho-Bi of preparation 2wO 6nano-powder all has the flower pattern pattern be assembled into by nanometer sheet.
Fig. 3 is flower pattern Ho-Bi prepared by the embodiment of the present invention 2 2wO 6the absorbancy change curve of nano-powder rhodamine B degradation under different time, the unit a.u. of ordinate zou represents arbitrary unit, experiment adopts 350W xenon lamp as visible lamp source, along with the carrying out of photocatalytic degradation, the absorbancy of rhodamine B is more and more lower, shows its concentration also more and more lower, along with the prolongation of time, absorbancy reduces, and rhodamine B reduces also blue shift gradually in the characteristic peak intensity of 554nm, finally reduces to straight line.This shows that the rhodamine B in solution is well degraded, and flower pattern Ho-Bi provided by the invention is described 2wO 6nano-powder has good degradation effect to rhodamine B, proves flower pattern Ho-Bi 2wO 6nano-powder has higher photocatalytic activity, can be used in degradation of organic substances.
Embodiment 3
Flower pattern Ho-Bi 2wO 6the preparation method of nano-powder, comprises the following steps:
Step 1: take Bi (NO respectively according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, and takes a certain amount of Ho (NO 3) 36H 2o joins in beaker, wherein the add-on x=15% of Ho, x=n ho/ (n bi+ n ho) × 100%, n biand n hobe respectively the molar weight of Bi and Ho;
Step 2: measure deionized water and join in beaker, stirred at ambient temperature 40min fully dissolves to raw material and forms white suspension liquid, is mixed with mixing solutions, wherein Bi (NO 3) 35H 2the concentration of O is 0.2mol/L, Na 2wO 42H 2the concentration of O is 0.1mol/L, and adjust ph is 2.0, obtains precursor liquid;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the compactedness controlling microwave hydrothermal reaction kettle is 70%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stopped reaction be incubated 30min at 180 DEG C after;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate throw out wherein, after deionized water and absolute ethanol washing throw out to neutrality, ultrasonic disperse 50min is to reduce the reunion of nano-powder again, then obtains flower pattern Ho-Bi after freeze-day with constant temperature 12h at 85 DEG C 2wO 6nano-powder.
Obtained flower pattern Ho-Bi 2wO 6nano-powder, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Ho 3+, wherein the content of Ho is x=15%, and it has the flower pattern pattern be assembled into by nanometer sheet.
Embodiment 4
Flower pattern Ho-Bi 2wO 6the preparation method of nano-powder, comprises the following steps:
Step 1: take Bi (NO respectively according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, and takes a certain amount of Ho (NO 3) 36H 2o joins in beaker, wherein the add-on x=20% of Ho, x=n ho/ (n bi+ n ho) × 100%, n biand n hobe respectively the molar weight of Bi and Ho;
Step 2: measure deionized water and join in beaker, stirred at ambient temperature 50min fully dissolves to raw material and forms white suspension liquid, is mixed with mixing solutions, wherein Bi (NO 3) 35H 2the concentration of O is 0.4mol/L, Na 2wO 42H 2the concentration of O is 0.2mol/L, and adjust ph is 1.5, obtains precursor liquid;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the compactedness controlling microwave hydrothermal reaction kettle is 50%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stopped reaction be incubated 60min at 140 DEG C after;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate throw out wherein, after deionized water and absolute ethanol washing throw out to neutrality, ultrasonic disperse 30min is to reduce the reunion of nano-powder again, then obtains flower pattern Ho-Bi after freeze-day with constant temperature 16h at 80 DEG C 2wO 6nano-powder.
Obtained flower pattern Ho-Bi 2wO 6nano-powder, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Ho 3+, wherein the content of Ho is x=20%, and it has the flower pattern pattern be assembled into by nanometer sheet.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of those of ordinary skill in the art by reading specification sheets of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.

Claims (7)

1. a flower pattern Ho-Bi 2wO 6the preparation method of nano-powder, is characterized in that, comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o and Na 2wO 42H 2o puts into container according to the mol ratio of Bi:W=2:1, and by Ho (NO 3) 36H 2o joins in container, wherein the add-on x=2%-20% of Ho, x=n ho/ (n bi+ n ho) × 100%, n biand n hobe respectively the molar weight of Bi and Ho;
Step 2: water is joined in container, stirred at ambient temperature is even, and be mixed with mixing solutions, adjust ph is 1.5-2.0, obtains precursor liquid; Wherein Bi (NO in mixing solutions 3) 35H 2the concentration of O is 0.1mol/L-0.6mol/L, Na 2wO 42H 2the concentration of O is 0.05mol/L-0.3mol/L
Step 3: precursor liquid is moved in microwave hydrothermal reaction kettle, then microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stopped reaction be incubated 30-120min at 140 DEG C-240 DEG C after;
Step 4: after question response temperature is down to room temperature, takes out microwave hydrothermal reaction kettle, isolates throw out wherein, then obtains flower pattern Ho-Bi by after throw out washing, ultrasonic disperse 30-60min, 75-85 DEG C freeze-day with constant temperature 12-24h 2wO 6nano-powder.
2. flower pattern Ho-Bi according to claim 1 2wO 6the preparation method of nano-powder, is characterized in that: the required time that stirs in described step 2 is 30-60min.
3. flower pattern Ho-Bi according to claim 1 2wO 6the preparation method of nano-powder, is characterized in that: in described step 3, the compactedness of microwave hydrothermal reaction kettle is 40%-70%.
4. flower pattern Ho-Bi according to claim 1 2wO 6the preparation method of nano-powder, is characterized in that: in described step 3, the liner of microwave hydrothermal reaction kettle is tetrafluoroethylene material.
5. flower pattern Ho-Bi according to claim 1 2wO 6the preparation method of nano-powder, is characterized in that: washing precipitate is extremely neutral respectively in order to use deionized water and dehydrated alcohol for the washing in described step 4.
6. according to the flower pattern Ho-Bi in claim 1-5 described in any one 2wO 6the flower pattern Ho-Bi that the preparation method of nano-powder obtains 2wO 6nano-powder, is characterized in that: its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Ho 3+, wherein the content of Ho is x=2%-20%, and it has the flower pattern pattern be assembled into by nanometer sheet.
7. according to the flower pattern Ho-Bi in claim 1-5 described in any one 2wO 6the flower pattern Ho-Bi that the preparation method of nano-powder obtains 2wO 6the application of nano-powder in degradation of organic substances.
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