CN109100343A - The preparation method of tungsten oxide film - Google Patents
The preparation method of tungsten oxide film Download PDFInfo
- Publication number
- CN109100343A CN109100343A CN201810707265.3A CN201810707265A CN109100343A CN 109100343 A CN109100343 A CN 109100343A CN 201810707265 A CN201810707265 A CN 201810707265A CN 109100343 A CN109100343 A CN 109100343A
- Authority
- CN
- China
- Prior art keywords
- tungsten oxide
- preparation
- oxide film
- solid
- substrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 34
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000000926 separation method Methods 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 239000007864 aqueous solution Substances 0.000 claims abstract description 23
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000013067 intermediate product Substances 0.000 claims abstract description 16
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 16
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims description 20
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000012212 insulator Substances 0.000 claims description 8
- 239000004020 conductor Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims 1
- AAWZNWVCESLFTD-UHFFFAOYSA-N tungsten;hydrate Chemical compound O.[W] AAWZNWVCESLFTD-UHFFFAOYSA-N 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 10
- 239000010409 thin film Substances 0.000 abstract description 7
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 15
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 9
- 238000004528 spin coating Methods 0.000 description 6
- 238000001069 Raman spectroscopy Methods 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- QRNATDQRFAUDKF-UHFFFAOYSA-N 2-carbamothioylsulfanylethyl carbamodithioate Chemical compound NC(=S)SCCSC(N)=S QRNATDQRFAUDKF-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000036244 malformation Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种氧化钨薄膜的制备方法。它先将钨酸铵粉末退火，得到三氧化钨粉末，再将三氧化钨粉末和水混合，得到三氧化钨水溶液，之后，先向三氧化钨水溶液中加入硼氢化钠后反应0.5‑5h，得到反应液，再对反应液依次进行固液分离、洗涤和干燥的处理，得到粉末状中间产物，最后，先将粉末状中间产物分散于乙醇中，得到分散液，再将分散液涂敷于衬底上，制得目的产物。它有着工艺简便、安全和所需设备价廉的特点，使制得的目的产物极易于广泛地商业化应用于对罗丹明6G和3,3’‑二乙基硫代三碳菁碘化物的快速痕量检测。
The invention discloses a preparation method of a tungsten oxide thin film. It first anneals the ammonium tungstate powder to obtain tungsten trioxide powder, then mixes the tungsten trioxide powder and water to obtain a tungsten trioxide aqueous solution, and then adds sodium borohydride to the tungsten trioxide aqueous solution and reacts for 0.5‑5h. The reaction solution is obtained, and then the reaction solution is sequentially subjected to solid-liquid separation, washing and drying to obtain a powdery intermediate product. Finally, the powdery intermediate product is first dispersed in ethanol to obtain a dispersion, and then the dispersion is coated on On the substrate, the target product was obtained. It has the characteristics of simple process, safety and low cost of required equipment, which makes the obtained target product very easy to be widely commercialized and applied to rhodamine 6G and 3,3'-diethylthiotricarbocyanine iodide rapid trace detection.
Description
Technical field
The present invention relates to a kind of preparation method of film, especially a kind of preparation method of tungsten oxide film.
Background technique
Surface enhanced Raman scattering (SERS) technology, which refers to, is adsorbed on the tables such as the coarse noble metal gold, silver of Nano grade, copper
Molecular Raman signal on face is obtained the phenomenon that greatly enlarging, because its have quickly, trace, lossless object is referred to
Line identification etc. advantages and become powerful surface analysis tool, be widely used in electrochemistry, Surface Science, catalysis, medicine detection,
The various fields such as biological food detection.Generally using noble metal nanometer material as Raman active substrate in SERS detection, preparation is high
The key of the active noble metal Raman substrate of SERS is accurately to regulate and control the structure of noble metal nanometer material, and constructs
There is the problems such as at high cost, time-consuming, complex process by the preparation process of structure-controllable SERS substrate.In addition, in actual inspection
It surveys in application, the biocompatibility of noble metal is bad, and catalytic activity is high, be easy to cause the malformation of measured target molecule.
To solve this problem, people have made some good tries and effort, as Chinese invention patent application CN106756853A in
A kind of tungsten oxide substrate and preparation method thereof with Surface enhanced Raman scattering function that on May 31st, 2017 announces.The hair
The tungsten oxide substrate recorded in bright patent application document is the thickness with hexagonal honeycomb shape nanostructure being overlying on substrate
For the tungsten oxide film of 30-100nm；The nano aluminum bowl that preparation method is obtained using secondary or multiple anodic oxidation as substrate,
Tungsten oxide nanometer thin film is prepared using magnetron sputtering method on substrate, then carries out oxygen content by making annealing treatment in hydrogen atmosphere
Regulation, obtain product.Though this method can get the tungsten oxide substrate with Surface enhanced Raman scattering function, there is also
Technical process is cumbersome, the equipment that uses is expensive, high-temperature hydrogen reduction method is uneconomical effectively and there is potential danger
It is insufficient.
Summary of the invention
The technical problem to be solved in the present invention place in order to overcome the shortcomings in the prior art, provides a kind of simple process, peace
Complete and the inexpensive tungsten oxide film of required equipment preparation method.
To solve technical problem of the invention, used technical solution is that the preparation method of tungsten oxide film includes liquid
Steps are as follows for phase reduction method, especially completion:
Step 1, ammonium tungstate powder is first placed at 300-500 DEG C the 1-4h that anneals, obtains tungsten trioxide powder, according still further to three
The weight ratio of tungsten oxide powder and water is that the ratio of 0.2-50:1-100 mixes the two, obtains tungstic acid aqueous solution；
Step 2, sodium borohydride first is added into tungstic acid aqueous solution, makes sodium borohydride in tungstic acid aqueous solution
Concentration remains 0.5-5mol/L, reacts 0.5-5h, obtains reaction solution, then reaction solution is successively separated by solid-liquid separation, wash and
Dry processing obtains powdered intermediate product；
Step 3, it first disperses powdered intermediate product in ethyl alcohol, obtains dispersion liquid, then by dispersed liquid coating in substrate
On, the tungsten oxide film that film thickness is 20-100 μm is made.
The further improvement of preparation method as tungsten oxide film:
Preferably, the partial size of ammonium tungstate powder is 0.1-10 μm.
Preferably, solid-liquid separation treatment is centrifuge separation, revolving speed 4000-6000r/min, time 5-10min.
Preferably, carrying out washing treatment is clear to solid progress 2-3 times isolated alternating using distilled water and ethyl alcohol
It washes, separation solid is centrifuge separation when cleaning.
Preferably, it is dried as the solid after cleaning is placed at 50-70 DEG C and dries 12-24h.
Preferably, it applies as dipping, or spraying or spin coating.
Preferably, substrate is conductor substrate or semiconductor substrate or insulator substrates.
Beneficial effect compared with the existing technology is:
First, being characterized respectively using X-ray diffractometer and scanning electron microscope to purpose product obtained, simultaneously by its result
In conjunction with preparation method it is found that purpose product is to be covered with tungsten oxide film on substrate；Wherein, the film thickness of tungsten oxide film is 20-100
μm。
Second, using purpose product obtained as SERS active-substrate, through respectively to rhodamine 6G (R6G) and 3,3 '-two
Ethylenebis dithiocarbamate tricarbocyanine iodide (DTTCI) carry out the test of multiple more batches under various concentration, when the concentration of measured object R6G
Down to 10-6The concentration of mol/L, DTTCI are down to 10-6It when mol/L, remains to be effectively detected out, and its detection is consistent
Property and repeatability in purpose product multiple spot and any point all very it is good.
Third, preparation method is simple, scientific, efficient.Purpose product has not only been made --- tungsten oxide film also makes its tool
There is the function of Surface enhanced Raman scattering, more there is that simple process, safe and required equipment are inexpensive；And then make obtained
Purpose product be extremely easy to widely commercial applications in rhodamine 6G and 3,3 '-diethyl sulfides for the quick of tricarbocyanine iodide
Trace detection.
Detailed description of the invention
Fig. 1 is one of the result for using X-ray diffraction (XRD) instrument to be characterized purpose product made from preparation method.
XRD spectra shows that the ingredient of purpose product is tungsten oxide.
Fig. 2 is to being attached with 10-6What the purpose product of the rhodamine 6G of mol/L was characterized using laser Raman spectrometer
One of as a result.
Fig. 3 is to being attached with 10-6The knot that the purpose product of the DTTCI of mol/L is characterized using laser Raman spectrometer
One of fruit.
Specific embodiment
Preferred embodiment of the invention is described in further detail with reference to the accompanying drawing.
It buys from market or is voluntarily made first:
Ammonium tungstate powder；
Sodium borohydride；
Distilled water；
Ethyl alcohol；
Conductor substrate, semiconductor substrate and insulator substrates as substrate.
Then:
Embodiment 1
The specific steps of preparation are as follows:
Step 1, ammonium tungstate powder is first placed at 300 DEG C the 4h that anneals；Wherein, the partial size of ammonium tungstate powder is 0.1 μm, is obtained
To tungsten trioxide powder.The two is mixed according still further to the ratio that the weight ratio of tungsten trioxide powder and water is 0.2:100, obtains three
Tungsten oxide aqueous solution.
Step 2, sodium borohydride first is added into tungstic acid aqueous solution, makes sodium borohydride in tungstic acid aqueous solution
Concentration remains 0.5mol/L, reacts 5h, obtains reaction solution.Reaction solution is successively separated by solid-liquid separation, is washed and is dried again
Processing；Wherein, solid-liquid separation treatment is centrifuge separation, and revolving speed 4000r/min, time 10min, carrying out washing treatment is to use
The alternating that distilled water and ethyl alcohol carry out 2 times to isolated solid is cleaned, and separation solid is centrifuge separation when cleaning, is done
Dry processing is dried for 24 hours for the solid after cleaning to be placed at 50 DEG C, obtains powdered intermediate product.
Step 3, it first disperses powdered intermediate product in ethyl alcohol, obtains dispersion liquid.Again by dispersed liquid coating in substrate
On；Wherein, it applies as spin coating, substrate is insulator substrates.It is made as shown in Figure 1, Figure 2 and tungsten oxide shown in the curve in Fig. 3 is thin
Film.
Embodiment 2
The specific steps of preparation are as follows:
Step 1, ammonium tungstate powder is first placed at 350 DEG C the 3h that anneals；Wherein, the partial size of ammonium tungstate powder is 0.5 μm, is obtained
To tungsten trioxide powder.The two is mixed according still further to the ratio that the weight ratio of tungsten trioxide powder and water is 1:75, obtains three oxygen
Change tungsten aqueous solution.
Step 2, sodium borohydride first is added into tungstic acid aqueous solution, makes sodium borohydride in tungstic acid aqueous solution
Concentration remains 1mol/L, reacts 3.5h, obtains reaction solution.Reaction solution is successively separated by solid-liquid separation, is washed and is dried again
Processing；Wherein, solid-liquid separation treatment is centrifuge separation, and revolving speed 4500r/min, time 8.75min, carrying out washing treatment is to make
Clean with the alternating that distilled water and ethyl alcohol carry out 2 times to isolated solid, separation solid is to be centrifugated when cleaning,
It is dried as the solid after cleaning is placed at 55 DEG C and dries 21h, obtains powdered intermediate product.
Step 3, it first disperses powdered intermediate product in ethyl alcohol, obtains dispersion liquid.Again by dispersed liquid coating in substrate
On；Wherein, it applies as spin coating, substrate is insulator substrates.It is made as shown in Figure 1, Figure 2 and tungsten oxide shown in the curve in Fig. 3 is thin
Film.
Embodiment 3
The specific steps of preparation are as follows:
Step 1, ammonium tungstate powder is first placed at 400 DEG C the 3h that anneals；Wherein, the partial size of ammonium tungstate powder is 1 μm, is obtained
Tungsten trioxide powder.The two is mixed according still further to the ratio that the weight ratio of tungsten trioxide powder and water is 17:50, obtains three oxidations
Tungsten aqueous solution.
Step 2, sodium borohydride first is added into tungstic acid aqueous solution, makes sodium borohydride in tungstic acid aqueous solution
Concentration remains 2.5mol/L, reacts 2.5h, obtains reaction solution.Reaction solution is successively separated by solid-liquid separation, is washed and is dried again
Processing；Wherein, solid-liquid separation treatment is to be centrifugated, revolving speed 5000r/min, time 7.5min, and carrying out washing treatment is
It is cleaned using the alternating that distilled water and ethyl alcohol carry out 3 times to isolated solid, separation solid is centrifugation point when cleaning
From being dried as the solid after cleaning to be placed at 60 DEG C and dries 18h, obtain powdered intermediate product.
Step 3, it first disperses powdered intermediate product in ethyl alcohol, obtains dispersion liquid.Again by dispersed liquid coating in substrate
On；Wherein, it applies as spin coating, substrate is insulator substrates.It is made as shown in Figure 1, Figure 2 and tungsten oxide shown in the curve in Fig. 3 is thin
Film.
Embodiment 4
The specific steps of preparation are as follows:
Step 1, ammonium tungstate powder is first placed at 450 DEG C the 2h that anneals；Wherein, the partial size of ammonium tungstate powder is 5 μm, is obtained
Tungsten trioxide powder.The two is mixed according still further to the ratio that the weight ratio of tungsten trioxide powder and water is 33:25, obtains three oxidations
Tungsten aqueous solution.
Step 2, sodium borohydride first is added into tungstic acid aqueous solution, makes sodium borohydride in tungstic acid aqueous solution
Concentration remains 3.5mol/L, reacts 1h, obtains reaction solution.Reaction solution is successively separated by solid-liquid separation, is washed and is dried again
Processing；Wherein, solid-liquid separation treatment is centrifuge separation, and revolving speed 5500r/min, time 6.25min, carrying out washing treatment is to make
Clean with the alternating that distilled water and ethyl alcohol carry out 3 times to isolated solid, separation solid is to be centrifugated when cleaning,
It is dried as the solid after cleaning is placed at 65 DEG C and dries 15h, obtains powdered intermediate product.
Step 3, it first disperses powdered intermediate product in ethyl alcohol, obtains dispersion liquid.Again by dispersed liquid coating in substrate
On；Wherein, it applies as spin coating, substrate is insulator substrates.It is made as shown in Figure 1, Figure 2 and tungsten oxide shown in the curve in Fig. 3 is thin
Film.
Embodiment 5
The specific steps of preparation are as follows:
Step 1, ammonium tungstate powder is first placed at 500 DEG C the 1h that anneals；Wherein, the partial size of ammonium tungstate powder is 10 μm, is obtained
To tungsten trioxide powder.The two is mixed according still further to the ratio that the weight ratio of tungsten trioxide powder and water is 50:1, obtains three oxygen
Change tungsten aqueous solution.
Step 2, sodium borohydride first is added into tungstic acid aqueous solution, makes sodium borohydride in tungstic acid aqueous solution
Concentration remains 5mol/L, reacts 0.5h, obtains reaction solution.Reaction solution is successively separated by solid-liquid separation, is washed and is dried again
Processing；Wherein, solid-liquid separation treatment is centrifuge separation, and revolving speed 6000r/min, time 5min, carrying out washing treatment is to use
The alternating that distilled water and ethyl alcohol carry out 3 times to isolated solid is cleaned, and separation solid is centrifuge separation when cleaning, is done
Dry processing dries 12h for the solid after cleaning to be placed at 70 DEG C, obtains powdered intermediate product.
Step 3, it first disperses powdered intermediate product in ethyl alcohol, obtains dispersion liquid.Again by dispersed liquid coating in substrate
On；Wherein, it applies as spin coating, substrate is insulator substrates.It is made as shown in Figure 1, Figure 2 and tungsten oxide shown in the curve in Fig. 3 is thin
Film.
It selects dipping or the spraying in coating respectively again, and selects the conductor substrate or semiconductor as substrate respectively
Substrate, repeat above-described embodiment 1-5, be equally made as shown in Figure 1, Figure 2 and Fig. 3 in curve shown in tungsten oxide film.
Obviously, those skilled in the art can to the preparation method of tungsten oxide film of the invention carry out it is various change and
Modification is without departing from the spirit and scope of the present invention.If in this way, belonging to power of the present invention to these modifications and changes of the present invention
Within the scope of benefit requirement and its equivalent technologies, then the present invention is also intended to include these modifications and variations.
Claims (7)
1. a kind of preparation method of tungsten oxide film, including liquid phase reduction, it is characterised in that steps are as follows for completion:
Step 1, ammonium tungstate powder is first placed at 300-500 DEG C the 1-4h that anneals, obtains tungsten trioxide powder, according still further to three oxidations
The weight ratio of tungsten powder and water is that the ratio of 0.2-50:1-100 mixes the two, obtains tungstic acid aqueous solution；
Step 2, sodium borohydride first is added into tungstic acid aqueous solution, makes concentration of the sodium borohydride in tungstic acid aqueous solution
0.5-5mol/L is remained, 0.5-5h is reacted, obtains reaction solution, then reaction solution is successively separated by solid-liquid separation, is washed and is dried
Processing, obtain powdered intermediate product；
Step 3, it first disperses powdered intermediate product in ethyl alcohol, obtains dispersion liquid, then dispersed liquid coating is made on substrate
Obtain the tungsten oxide film that film thickness is 20-100 μm.
2. the preparation method of tungsten oxide film according to claim 1, it is characterized in that the partial size of ammonium tungstate powder is 0.1-
10μm。
3. the preparation method of tungsten oxide film according to claim 1, it is characterized in that solid-liquid separation treatment is centrifuge separation,
Its revolving speed is 4000-6000r/min, time 5-10min.
4. the preparation method of tungsten oxide film according to claim 1, it is characterized in that carrying out washing treatment be using distilled water and
The alternating that ethyl alcohol carries out 2-3 time to isolated solid is cleaned, and separation solid is to be centrifugated when cleaning.
5. the preparation method of tungsten oxide film according to claim 1, it is characterized in that being dried is consolidating after cleaning
State object, which is placed at 50-70 DEG C, dries 12-24h.
6. the preparation method of tungsten oxide film according to claim 1, it is characterized in that coating is dipping, or spraying, or rotation
It applies.
7. the preparation method of tungsten oxide film according to claim 1, it is characterized in that substrate is conductor substrate or semiconductor
Substrate or insulator substrates.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810707265.3A CN109100343A (en) | 2018-07-02 | 2018-07-02 | The preparation method of tungsten oxide film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810707265.3A CN109100343A (en) | 2018-07-02 | 2018-07-02 | The preparation method of tungsten oxide film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109100343A true CN109100343A (en) | 2018-12-28 |
Family
ID=64845254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810707265.3A Pending CN109100343A (en) | 2018-07-02 | 2018-07-02 | The preparation method of tungsten oxide film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109100343A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613777A (en) * | 2004-11-11 | 2005-05-11 | 北京科技大学 | Preparation for nanometer anhydrous wolframic acid powder |
| CN1745149A (en) * | 2003-10-20 | 2006-03-08 | 住友金属矿山株式会社 | Infrared shielding material microparticle dispersion, infrared shield, process for producing infrared shielding material microparticle, and infrared shielding material microparticle |
| CN101261905A (en) * | 2008-01-30 | 2008-09-10 | 西安理工大学 | A method for making WCu-CeO2 contact header material |
| CN101381106A (en) * | 2007-09-05 | 2009-03-11 | 西南交通大学 | Method for preparing nanometer tungsten trioxide powder |
| US20110155974A1 (en) * | 2009-12-29 | 2011-06-30 | Taiwan Textile Research Institute | Near Infrared Absorbing Agent and Near Infrared Absorbing Film |
| CN102211789A (en) * | 2010-04-08 | 2011-10-12 | 中国科学院合肥物质科学研究院 | Method for preparing tungsten trioxide nano material |
| CN106739597A (en) * | 2016-12-31 | 2017-05-31 | 武汉理工大学 | A kind of all print multifunctional transparent film and preparation method thereof |
| CN107200357A (en) * | 2016-03-18 | 2017-09-26 | 纳琳威纳米科技（上海）有限公司 | A kind of heat insulation nano powder and its production and use |
| US10584202B2 (en) * | 2014-04-14 | 2020-03-10 | Toray Industries, Inc | Photovoltaic element |
-
2018
- 2018-07-02 CN CN201810707265.3A patent/CN109100343A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1745149A (en) * | 2003-10-20 | 2006-03-08 | 住友金属矿山株式会社 | Infrared shielding material microparticle dispersion, infrared shield, process for producing infrared shielding material microparticle, and infrared shielding material microparticle |
| CN1613777A (en) * | 2004-11-11 | 2005-05-11 | 北京科技大学 | Preparation for nanometer anhydrous wolframic acid powder |
| CN101381106A (en) * | 2007-09-05 | 2009-03-11 | 西南交通大学 | Method for preparing nanometer tungsten trioxide powder |
| CN101261905A (en) * | 2008-01-30 | 2008-09-10 | 西安理工大学 | A method for making WCu-CeO2 contact header material |
| US20110155974A1 (en) * | 2009-12-29 | 2011-06-30 | Taiwan Textile Research Institute | Near Infrared Absorbing Agent and Near Infrared Absorbing Film |
| CN102211789A (en) * | 2010-04-08 | 2011-10-12 | 中国科学院合肥物质科学研究院 | Method for preparing tungsten trioxide nano material |
| US10584202B2 (en) * | 2014-04-14 | 2020-03-10 | Toray Industries, Inc | Photovoltaic element |
| CN107200357A (en) * | 2016-03-18 | 2017-09-26 | 纳琳威纳米科技（上海）有限公司 | A kind of heat insulation nano powder and its production and use |
| CN106739597A (en) * | 2016-12-31 | 2017-05-31 | 武汉理工大学 | A kind of all print multifunctional transparent film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gopalakrishnan et al. | Disposable, efficient and highly selective electrochemical sensor based on Cadmium oxide nanoparticles decorated screen-printed carbon electrode for ascorbic acid determination in fruit juices | |
| CN107966485A (en) | A kind of electrochemical heavy metals detector and its detection method based on graphene test paper electrode structure | |
| Bao et al. | In situ SERS monitoring of photocatalytic organic decomposition using recyclable TiO2-coated Ag nanowire arrays | |
| Safardoust-Hojaghan et al. | Synthesis of micro sphere-like bismuth nanoparticles by microwave assisted polyol method; designing a novel electrochemical nanosensor for ultra-trace measurement of Pb 2+ ions | |
| Taniselass et al. | Current state of green reduction strategies: Solution-processed reduced graphene oxide for healthcare biodetection | |
| Vinothkumar et al. | Voltammetric determination of Sudan I by using Bi2WO6 nanosheets modified glassy carbon electrode | |
| CN106623973B (en) | A kind of controllable synthesis method of nickel platinum alloy nano particle | |
| CN109580583A (en) | A kind of dense form Raman spectrum base and the preparation method and application thereof | |
| CN107921418A (en) | Ternary intermetallic compounds X2YZ composite catalysts | |
| CN102975454B (en) | Silver nanometer square block-sodium polyacrylate composite film as well as preparation method and application thereof | |
| CN110907428B (en) | Method for preparing reusable porous SERS metal substrate by reduction induction method and application thereof | |
| CN102033088A (en) | Preparation method of gold nano-particle/carbon nano tube composite material and application thereof | |
| Jiang et al. | A sensitive SERS substrate based on Au/TiO2/Au nanosheets | |
| CN110747435B (en) | A kind of preparation method of nano-gold thin film SERS substrate based on electrochemical roughening | |
| CN109187679A (en) | A kind of electrochemical sensor and its preparation method and application | |
| Barveen et al. | Flexible SERS sensor based on the photodecoration of Au-NPs on Co3O4 NWs/carbon fiber cloth for the ultrasensitive detection of methylene blue in the curved fish surfaces | |
| CN103409734A (en) | Precious metal nanometer particle assembly for SERS base and application of prepared product in detection | |
| CN103691438A (en) | Controllable preparation method of Ag-manganese monoxide nanorods | |
| Chen et al. | An electrochemical sensor for selective detection of Cu2+ by using a self-assembled Cu coordinated β-cyclodextrin-nitrogen-doped carbon quantum dots composite | |
| CN109100343A (en) | The preparation method of tungsten oxide film | |
| CN113866151B (en) | A triple amplified SERS signal substrate, preparation method and application based on spiny nano-gold@silver | |
| Bhanjana et al. | Probing of silver oxide nanoblades for 4-hydroxybenzoic acid quantification: a tool for food and water safety assessment | |
| Kothandan et al. | Ultrasonic-assisted synthesis of nickel tungstate nanoparticles on poly (3, 4-ethylene dioxythiophene): poly (4-styrene sulfonate) for the effective electrochemical detection of caffeic acid | |
| CN107056667B (en) | A kind of mercury ion probe and its preparation method and application | |
| CN113777093A (en) | A fluorine-free preparation method of titanium carbide Mxene surface-enhanced Raman scattering base material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181228 |