CN106830086B - A kind of tungsten oxide nanometer stick and preparation method thereof - Google Patents
A kind of tungsten oxide nanometer stick and preparation method thereof Download PDFInfo
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- CN106830086B CN106830086B CN201710084748.8A CN201710084748A CN106830086B CN 106830086 B CN106830086 B CN 106830086B CN 201710084748 A CN201710084748 A CN 201710084748A CN 106830086 B CN106830086 B CN 106830086B
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/00—Particle morphology
- 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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Abstract
A kind of tungsten oxide nanometer stick, the crystal form is in 2 θ of angle of diffraction at 15.32 °, 29.32 °, 30.68 °, 35.48 °, 38.76 °, 46.56 °, 50.92 °, 53.48 °, 59.80 °, 60.52 °, 63.46 °, 65.72 °, there is diffraction maximum at 71.32 °, Red Shift Phenomena occurs for tungsten oxide nanometer stick absorption peak of the present invention, radiation spectrum region expands, also there is certain absorption to the light of 400~450nm, preparation method simple possible, finished product purity is up to 98.7%, transferred product rate is up to 93.8% in terms of sodium tungstate, it easily realizes and produces in enormous quantities, it is simple and easy to get to prepare raw material, it is cheap, product size is uniform, ultra-violet absorption spectrum red shift, it is worth marketing application.
Description
Technical field
The present invention relates to a kind of tungsten oxide nanometer materials more particularly to a kind of tungsten oxide nanometer stick and preparation method thereof.
Background technology
Tungsten oxide is a kind of n-type semiconductor, due to its unique optics since finding its photochromism
Property shows huge applications foreground, the performance of these devices in information display devices, high sensitivity optical memory material etc.
Size, pattern and its nanostructure of assembling for depending greatly on tungsten oxide nanometer structural unit, just because of material
Decisive role of the structure of material in its performance.Current material scholar has prepared the different tungsten oxide nanometer of pattern
Material.
Currently, the UV-Vis DRS absorption spectrum of existing various pattern tungsten oxide nanometer materials, major absorbance peak is all
The energy of ultraviolet region for wavelength less than 350nm, only has the blue violet light of visible region faint absorption.
Invention content
Present invention aims at a kind of tungsten oxide nanometer stick novel crystal forms are provided, the tungsten oxide nanometer stick is in radiation spectrum region
With Red Shift Phenomena.
Another object of the present invention is to provide the preparation method of above-mentioned tungsten oxide nanometer stick crystal form.
The object of the invention is achieved through the following technical solutions：
A kind of tungsten oxide nanometer stick crystal form, it is characterised in that：The crystal form 2 θ of angle of diffraction 15.32 °, 29.32 °,
30.68°、35.48°、38.76°、46.56°、50.92°、53.48°、59.80°、60.52°、63.46°、65.72°、71.32°
There is diffraction maximum at place.
Specifically, above-mentioned tungsten oxide nanometer stick crystal form, it is characterised in that：It has X-ray powder as shown in Figure 1
Diffraction pattern.
The light of 400~450nm of tungsten oxide nanometer stick pair of the present invention has stronger absorption, the i.e. absorption peak of tungsten oxide nanometer stick
Red Shift Phenomena occurs, which has UV collection of illustrative plates as shown in Figure 2.
Tungsten oxide nanometer stick crystal form of the present invention, it is characterised in that：Its a diameter of 25~50nm or so, length 600~
800nm or so.
The preparation method of tungsten oxide nanometer stick of the present invention, which is characterized in that it is obtained as follows：
1. taking the sodium tungstate of 0.009~0.011mol and the cetyl trimethylammonium bromide of 0.01mol~0.1mol
(CTAB), it is dissolved in the distilled water of 20ml~50ml, stirs evenly, it is spare；
2. above-mentioned solution is instilled dropwise in the hydrochloric acid of a concentration of 3mol/L of 4~6mL, moves into water-bath device, be placed in
120 DEG C of stirring 2h are allowed to that the reaction was complete, and centrifugal sedimentation is washed 3~4 times repeatedly with distilled water, alcohol, spare；
3. the product after being washed in step 2 is placed in vacuum drying chamber, 60~80 DEG C of temperature of setting, vacuum degree 0.05~
0.08MPa takes out after 6~8 hours dry, is placed in Muffle furnace, and 280~350 DEG C of temperature is arranged, and 0.5~1.5h of calcination is obtained
Yellow powder to get.
Further, the preparation method of above-mentioned tungsten oxide nanometer stick, which is characterized in that it is obtained as follows：
1. taking the sodium tungstate of 0.01mol and the cetyl trimethylammonium bromide of 0.01mol, it is dissolved in 30mL distilled water,
It stirs evenly, it is spare；
2. above-mentioned solution is instilled dropwise in the hydrochloric acid of a concentration of 3mol/L of 5mL, moves into water-bath device, be placed in 120
DEG C stirring 2h is allowed to that the reaction was complete, and centrifugal sedimentation is washed 4 times repeatedly with distilled water, alcohol, spare；
3. the product after being washed in step 2 is taken to be placed in vacuum drying chamber, it is arranged 80 DEG C, vacuum degree 0.07MPa dries 7h
After take out, be placed in Muffle furnace, be arranged 300 DEG C of calcination 1h of temperature, obtain yellow powder to get.The present invention has with following
Beneficial effect：
Red Shift Phenomena occurs for tungsten oxide nanometer stick absorption peak of the present invention, and radiation spectrum region expands, to 400~450nm's
Light has certain absorption, preparation method simple possible, finished product purity to be up to 98.7%, and transferred product rate is up in terms of sodium tungstate
93.8%, it easily realizes and produces in enormous quantities, it is simple and easy to get to prepare raw material, cheap, products obtained therefrom size uniform, UV absorption
It has excellent performance, is worth marketing application.
Description of the drawings
Fig. 1 is tungsten oxide nanometer stick X-ray diffractogram of the present invention；
Fig. 2 is the UV scanning figures of tungsten oxide nanometer stick of the present invention；
Fig. 3 is tungsten oxide nanometer stick scanning electron microscope (SEM) photograph of the present invention.
Specific implementation mode
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is only used
In invention is further explained, it should not be understood as limiting the scope of the invention, person skilled in art can
To make some nonessential modifications and adaptations to the present invention according to aforementioned present invention content.
Embodiment 1
The sodium tungstate of 0.01mol and the cetyl trimethylammonium bromide of 0.01mol are taken, is dissolved in 30mL distilled water, stirs
It mixes uniformly, it is spare；Above-mentioned solution is instilled dropwise in the hydrochloric acid of a concentration of 3mol/L of 5mL, moves into water-bath device, be placed in
120 DEG C of stirring 2h are allowed to that the reaction was complete, and centrifugal sedimentation is washed 4 times repeatedly with distilled water, alcohol, spare；It takes in step 2 and washs
Product afterwards is placed in vacuum drying chamber, is arranged 80 DEG C, is taken out after vacuum degree 0.07MPa dryings 7h, be placed in Muffle furnace, be arranged
300 DEG C of calcination 1h of temperature, obtain yellow powder to get.After testing, tungsten oxide nanometer stick purity is 98.7%, transferred product rate
It is calculated as 93.8% with sodium tungstate.
Embodiment 2
By the tungsten oxide nanometer stick obtained by embodiment 1, XRD tests are done：
Using D/Max-1200 type X-ray diffractometers, radiation source is Cu targets,Scanning angle is 10 °
~80 °, voltage 40kV, electric current 30mA, sweep speed is 2 °/min.Its X-ray powder diffraction figure is as shown in Figure 1.
The tungsten oxide nanometer stick 2 θ of angle of diffraction 15.32 °, 29.32 °, 30.68 °, 35.48 °, 38.76 °,
There is diffraction maximum at 46.56 °, 50.92 °, 53.48 °, 59.80 °, 60.52 °, 63.46 °, 65.72 °, 71.32 °.
As shown in Fig. 2, as seen from the figure, the light of 400~450nm of this product pair has certain for the UV scanning figures of tungsten oxide nanometer stick
It absorbs, that is, Red Shift Phenomena occurs.
Embodiment 3
A kind of preparation method of tungsten oxide nanometer stick, using following steps：
The sodium tungstate of 0.009mol and the cetyl trimethylammonium bromide of 0.01mol are taken, is dissolved in the distilled water of 20ml,
It stirs evenly, it is spare；Above-mentioned solution is instilled dropwise in the hydrochloric acid of a concentration of 3mol/L of 4mL, moves into water-bath device, be placed in
120 DEG C of stirring 2h are allowed to that the reaction was complete, and centrifugal sedimentation is washed 3 times repeatedly with distilled water, alcohol, spare；By the product after washing
It is placed in vacuum drying chamber, temperature 60 C is set, vacuum degree 0.05MPa takes out after 8 hours dry, is placed in Muffle furnace, is arranged
280 DEG C, calcination 1.5h of temperature, obtain yellow powder to get.After testing, tungsten oxide nanometer stick purity is 97.2%, transferred product
Rate is calculated as 91.7% with sodium tungstate.It is identified with the method for embodiment 2, is tungsten oxide nanometer stick of the present invention.
Embodiment 4
A kind of preparation method of tungsten oxide nanometer stick, using following steps：
The sodium tungstate of 0.011mol and the cetyl trimethylammonium bromide of 0.1mol are taken, is dissolved in the distilled water of 50ml,
It stirs evenly, it is spare；
2. above-mentioned solution is instilled dropwise in the hydrochloric acid of a concentration of 3mol/L of 6mL, moves into water-bath device, be placed in 120
DEG C stirring 2h is allowed to that the reaction was complete, and centrifugal sedimentation is washed 4 times repeatedly with distilled water, alcohol, spare；
3. the product after being washed in step 2 is placed in vacuum drying chamber, 80 DEG C, vacuum degree 0.08MPa of temperature is set, is done
Take out, be placed in Muffle furnace after dry 6 hours, be arranged 350 DEG C, calcination 0.5h of temperature, obtain yellow powder to get.After testing, oxygen
It is 98.3% to change tungsten nanometer rods purity, and transferred product rate is calculated as 92.5% with sodium tungstate.It is identified with the method for embodiment 2, for this
Invention tungsten oxide nanometer stick.
Claims (2)
1. a kind of preparation method of tungsten oxide nanometer stick, which is characterized in that it is obtained as follows：
A. the sodium tungstate of 0.009~0.011mol and the cetyl trimethylammonium bromide of 0.01mol~0.1mol are taken, is dissolved in
In the distilled water of 20ml~50ml, stir evenly, it is spare；
B. above-mentioned solution is instilled dropwise in the hydrochloric acid of a concentration of 3mol/L of 4~6mL, moves into water-bath device, is placed in 120 DEG C
Stirring 2h is allowed to that the reaction was complete, and centrifugal sedimentation is washed 3~4 times repeatedly with distilled water, alcohol, spare；
C. the product after being washed in step B is placed in vacuum drying chamber, 60~80 DEG C of temperature of setting, vacuum degree 0.05~
0.08MPa takes out after 6~8 hours dry, is placed in Muffle furnace, 280~350 DEG C of temperature is arranged, 0.5~1.5h of calcination to obtain the final product；
The obtained tungsten oxide nanometer stick crystal form 2 θ of angle of diffraction 15.32 °, 29.32 °, 30.68 °, 35.48 °, 38.76 °,
There are diffraction maximum, the tungsten oxide at 46.56 °, 50.92 °, 53.48 °, 59.80 °, 60.52 °, 63.46 °, 65.72 °, 71.32 °
Nanorod diameter is 25~50nm, and length is in 600~800nm.
2. the preparation method of tungsten oxide nanometer stick as described in claim 1, which is characterized in that it is obtained as follows
's：
A. the sodium tungstate of 0.01mol and the cetyl trimethylammonium bromide of 0.01mol are taken, is dissolved in 30mL distilled water, is stirred
Uniformly, spare；
B. above-mentioned solution is instilled dropwise in the hydrochloric acid of a concentration of 3mol/L of 5mL, moves into water-bath device, is placed in 120 DEG C and stirs
It mixes 2h and is allowed to that the reaction was complete, centrifugal sedimentation is washed 4 times repeatedly with distilled water, alcohol, spare；
C. it takes the product after being washed in step B to be placed in vacuum drying chamber, is arranged 80 DEG C, is taken after vacuum degree 0.07MPa dryings 7h
Go out, be placed in Muffle furnace, be arranged 300 DEG C of calcination 1h of temperature, obtain yellow powder to get.
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