CN112299484B - Method for preparing cesium tungsten bronze material under normal pressure - Google Patents
Method for preparing cesium tungsten bronze material under normal pressure Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 67
- 229910000906 Bronze Inorganic materials 0.000 title claims abstract description 49
- OHUPZDRTZNMIJI-UHFFFAOYSA-N [Cs].[W] Chemical compound [Cs].[W] OHUPZDRTZNMIJI-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000010974 bronze Substances 0.000 title claims abstract description 49
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 99
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims abstract description 39
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims abstract description 39
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims abstract description 39
- 238000002834 transmittance Methods 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000002105 nanoparticle Substances 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 13
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 description 46
- 239000000843 powder Substances 0.000 description 30
- 238000005303 weighing Methods 0.000 description 30
- 229910052792 caesium Inorganic materials 0.000 description 17
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 17
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 17
- 239000010937 tungsten Substances 0.000 description 17
- 229910052721 tungsten Inorganic materials 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 230000004931 aggregating effect Effects 0.000 description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- 238000001514 detection method Methods 0.000 description 15
- 239000001301 oxygen Substances 0.000 description 15
- 229910052760 oxygen Inorganic materials 0.000 description 15
- 229910052710 silicon Inorganic materials 0.000 description 15
- 239000010703 silicon Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- 238000000584 ultraviolet--visible--near infrared spectrum Methods 0.000 description 15
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000005855 radiation Effects 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001089723 Metaphycus omega Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000001392 ultraviolet--visible--near infrared spectroscopy Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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Abstract
本发明提供了一种常压制备铯钨青铜材料的方法，包括如下步骤：在常压、40‑78℃下，将六氯化钨和氢氧化铯溶于乙醇，混合均匀后加入乙酸，得反应液；搅拌反应10‑30min，离心洗涤、沉淀、干燥，得铯钨青铜材料。该方法首次实现了在常压、低于80℃条件下，1小时内制备得到铯钨青铜材料。且该制备方法的设备简单，操作简易，尤其是制备时间短，可应用于规模生产。此外，由本发明提供的制备方法制备得到的铯钨青铜材料具有良好的红外光线吸收性能，在波长为800‑1100nm的范围内，近红外光的透光率由18％快速下降至10％，在波长为1100‑2000nm的范围内，近红外光的透光率基本维持在10％。
The invention provides a method for preparing cesium tungsten bronze material under normal pressure, comprising the following steps: dissolving tungsten hexachloride and cesium hydroxide in ethanol under normal pressure and 40-78°C, mixing them uniformly and adding acetic acid to obtain Reaction solution; stirred for 10-30min, centrifuged, washed, precipitated, and dried to obtain a cesium tungsten bronze material. For the first time, the method realizes the preparation of cesium tungsten bronze material under the condition of normal pressure and lower than 80°C within one hour. Moreover, the preparation method has simple equipment, easy operation, especially short preparation time, and can be applied to large-scale production. In addition, the cesium tungsten bronze material prepared by the preparation method provided by the present invention has good infrared light absorption performance. In the range of wavelength 800-1100nm, the transmittance of near-infrared light drops rapidly from 18% to 10%. In the wavelength range of 1100-2000nm, the transmittance of near-infrared light is basically maintained at 10%.
Description
Technical Field
The invention relates to the technical field of near-infrared absorption materials. And more particularly relates to a method for preparing a cesium tungsten bronze material under normal pressure.
Background
Solar radiation provides the energy supply for every life activity on earth. The bands of solar radiation mainly include ultraviolet band, visible band and near-infrared band, wherein the visible region and the near-infrared region are regions where solar radiation energy is concentrated. Ultraviolet rays having a wavelength ranging from 300 to 400nm account for about 5%; the visible light band with the wavelength range of 400-780 nm accounts for about 43 percent; the near infrared light band having a wavelength ranging from 780 to 2500nm accounts for about 52%. The near infrared light has obvious thermal effect, so that not only can the skin of a human body generate burning heat, but also the temperature in a room or a vehicle is easily increased through infrared radiation, and the energy consumption of an air conditioner is continuously increased. In order to meet the increasing requirements of energy conservation and emission reduction, the radiation energy of sunlight needs to be blocked by high blocking rate in a near infrared band. The research on novel near-infrared absorption materials has very wide application prospect in the fields of green energy-saving buildings and automobile glass heat insulation.
Cesium tungsten bronze (Cs) x WO 3 ，0<x<1) The material is a non-stoichiometric narrow-band-gap semiconductor material, can generate strong absorption for light with the wavelength of more than 1100nm, and is an excellent near infrared absorption material. At present, the preparation method of cesium tungsten bronze generally needs higher reaction temperature and pressure, the preparation conditions are harsh, and the requirement on equipment is high. The high-temperature reduction method requires introducing hydrogen in the high-temperature heating (800 ℃), and has the disadvantages of complicated preparation process, low raw material utilization rate and certain dangerousness (H.Takeda, K.Adachi, J.Am.Ceramic Soc.,2007,90 (12), 4059-4061). Solvothermal or hydrothermal reactions also require high reaction temperatures (typically above 200 ℃), long preparation times, tens of hours or even days (c.guo, s.yin, m.yan, t.sato, j.mater.chem.,2011,21 (13), 5099).
Therefore, it is required to provide a method for preparing a cesium tungsten bronze material at normal pressure and at a relatively low temperature.
Disclosure of Invention
The invention aims to provide a method for preparing a cesium tungsten bronze material under normal pressure, which is used for preparing the cesium tungsten bronze material within 1 hour by taking tungsten hexachloride as a tungsten source and cesium hydroxide as a cesium source at 40-78 ℃ under normal pressure for the first time.
The invention also provides a cesium tungsten bronze material prepared by the method.
In order to achieve an object of the invention, the invention adopts the following technical scheme:
a method for preparing a cesium tungsten bronze material under normal pressure comprises the following steps:
dissolving tungsten hexachloride and cesium hydroxide in ethanol at normal pressure and 40-78 ℃, uniformly mixing, and adding acetic acid to obtain a reaction solution; stirring and reacting for 10-30min, centrifuging, washing, precipitating and drying to obtain the cesium tungsten bronze material.
In a specific implementation process, the preparation process of the reaction solution comprises the following steps:
dissolving tungsten hexachloride in ethanol at 40-78 deg.C under normal pressure, stirring to obtain yellow solution, stirring for 2-10min, adding cesium hydroxide, stirring for 2-5min, adding acetic acid, and stirring to obtain reaction solution.
The purity of tungsten hexachloride used in the present invention was 99%, the purity of cesium hydroxide was 99.9%, and the cesium tungsten bronze material prepared was a deep blue powder.
Preferably, the concentration of the tungsten hexachloride in the reaction liquid is 2-15mg/mL; the concentration of the cesium hydroxide is 0.7-2.5mg/mL.
Preferably, the volume ratio of ethanol to acetic acid in the reaction solution is 4:1-12.
Preferably, the purity of the ethanol is analytically pure and the purity of the acetic acid is analytically pure.
Preferably, the centrifugal washing comprises an alcohol washing and a water washing process. The water used was ultrapure water having a resistivity of 18.2 M.OMEGA.cm.
Preferably, the drying is in air at 30-50 ℃ for 24h.
It should be noted that the preparation process of the cesium tungsten bronze material provided by the invention is carried out under normal pressure, the whole reaction and drying temperature does not exceed 80 ℃, and the whole preparation process can be completed within 1h, compared with the reaction temperature of 800 ℃ in the traditional high-temperature reduction method and the reaction time of dozens of hours at 200 ℃ in the hydrothermal method, the reaction temperature is reduced, the reaction time is greatly shortened, the reaction conditions are greatly simplified, the production efficiency is improved, and the resources are saved.
In order to realize the second purpose of the invention, the following technical scheme is adopted:
the cesium tungsten bronze material prepared by the preparation method.
Preferably, the cesium tungsten bronze material is a nanoparticle aggregate of 10-20 nm.
Preferably, the cesium tungsten bronze material has a light transmittance of near infrared light of 10% in the range of 1100-2000 nm.
The cesium tungsten bronze material prepared by the method has good infrared ray absorption performance, the light transmittance of near infrared light is rapidly reduced to 10% from 18% in the wavelength range of 800-1100nm, and the light transmittance of near infrared light is basically maintained at 10% in the wavelength range of 1100-2000 nm.
The invention has the following beneficial effects:
the invention provides a preparation method of a cesium tungsten bronze material, which takes tungsten hexachloride as a tungsten source, cesium hydroxide as a cesium source, ethanol as a solvent and acetic acid as a reactant and can be completed within 1 hour under the conditions of normal pressure and the temperature lower than 80 ℃. The preparation equipment is simple, the operation is simple, the preparation time is short, and the method can be applied to large-scale production.
In addition, the cesium tungsten bronze material prepared by the preparation method provided by the invention has good infrared ray absorption performance, the light transmittance of near infrared light is rapidly reduced from 18% to 10% in the wavelength range of 800-1100nm, and the light transmittance of near infrared light is basically maintained at 10% in the wavelength range of 1100-2000 nm.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 shows an XRD spectrum of a sample of cesium tungsten bronze material prepared in example 2 of the present invention.
Fig. 2 shows a scanning electron micrograph of a cesium tungsten bronze material sample prepared in example 5 of the present invention.
FIG. 3 shows a scanning electron micrograph and a spectrum of a cesium tungsten bronze material sample prepared in example 5 of the present invention (the spectrum of the lower sample in FIG. 3 is a spectrum obtained by taking a sample of a square area in the upper scanning electron micrograph).
Fig. 4 shows a uv-vis-nir transmission spectrum of a sample of cesium tungsten bronze material prepared in example 6 of the present invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
In the present invention, the preparation methods are all conventional methods unless otherwise specified. The starting materials used are available from published commercial sources unless otherwise specified, and the percentages are by mass unless otherwise specified.
Example 1
Weighing 0.2-0.4 g of tungsten hexachloride, dissolving the tungsten hexachloride in 40-60 mL of ethanol, stirring for 2-10min under the condition of constant-temperature water bath at 40 ℃, weighing 0.05-0.07 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. And measuring 5mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 20min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is basically consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to perform ultraviolet visible near infrared spectrum test, and under an integrating sphere mode, measuring that the light transmittance of near infrared light of the sample is below 18% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 2
Weighing 0.2-0.4 g of tungsten hexachloride, dissolving the tungsten hexachloride in 40-60 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 60 ℃, weighing 0.05-0.07 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. 10mL of acetic acid is measured and quickly added into the reaction solution, and after the stirring is continued for 10min, the mixture is centrifugally washed and dried to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection, obtaining a spectrogram as shown in figure 1, and showing that the spectrogram is basically consistent with a standard spectrogram (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to perform ultraviolet visible near infrared spectrum test, and under an integrating sphere mode, measuring that the light transmittance of near infrared light of the sample is below 18% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 3
Weighing 0.4-0.6 g of tungsten hexachloride, dissolving the tungsten hexachloride in 40-60 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 50 ℃, weighing 0.07-0.09 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. And measuring 5mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 10min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein the light transmittance of the near infrared light of the tested sample is below 18% at the wavelength of 800-1100nm and is basically maintained at 10% at the wavelength of 1100-2000nm in an integrating sphere mode.
Example 4
Weighing 0.4-0.6 g of tungsten hexachloride, dissolving the tungsten hexachloride in 60-80 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 50 ℃, weighing 0.07-0.09 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. 10mL of acetic acid is measured and quickly added into the reaction solution, and after the stirring is continued for 20min, the mixture is centrifugally washed and dried to obtain a dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 5
Weighing 0.4-0.6 g of tungsten hexachloride, dissolving the tungsten hexachloride in 60-80 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 60 ℃, weighing 0.09-0.12 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. And measuring 10mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 10min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is basically consistent with a standard spectrum (JCPDS 83-1334). Another small amount of dried sample is re-dispersed in pure water (resistivity 18.2M Ω · cm), and spotted on a silicon wafer for scanning electron microscope observation, and then the sample is observed by a scanning electron microscope, and the obtained sample is formed by aggregating nano particles with the particle size of 10-20nm, as shown in fig. 2. As shown in fig. 3, the material was confirmed to contain cesium, tungsten, and oxygen components by energy spectroscopy (EDS). And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 6
Weighing 0.4-0.6 g of tungsten hexachloride, dissolving the tungsten hexachloride in 80-100 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 60 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. 10mL of acetic acid is measured and quickly added into the reaction solution, and after the stirring is continued for 20min, the mixture is centrifugally washed and dried to obtain a dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. A proper amount of powder samples are taken to carry out ultraviolet visible near infrared spectrum test, under the mode of an integrating sphere, the light transmittance of near infrared light of the tested samples is rapidly reduced from 18 percent to 10 percent when the wavelength is 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10 percent when the wavelength is 1100-2000nm, as shown in figure 4.
Example 7
Weighing 0.4-0.6 g of tungsten hexachloride, dissolving the tungsten hexachloride in 80-100 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 78 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. 10mL of acetic acid is measured and quickly added into the reaction solution, and after the stirring is continued for 20min, the mixture is centrifugally washed and dried to obtain a dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 8
Weighing 0.6-0.8 g of tungsten hexachloride, dissolving the tungsten hexachloride in 60-80 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 50 ℃, weighing 0.07-0.09 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. Measuring 15mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 30min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And dispersing a small amount of dried sample in pure water again (the resistivity is 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain the sample which is formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 9
Weighing 0.6-0.8 g of tungsten hexachloride, dissolving the tungsten hexachloride in 60-80 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 50 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. And measuring 10mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 20min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 10
Weighing 0.8-1.0 g of tungsten hexachloride, dissolving the tungsten hexachloride in 60-80 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 60 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. Measuring 15mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 30min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 11
Weighing 0.8-1.0 g of tungsten hexachloride, dissolving the tungsten hexachloride in 60-80 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 78 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. Measuring 15mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 30min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 12
Weighing 0.8-1.0 g of tungsten hexachloride, dissolving the tungsten hexachloride in 80-100 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 70 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. 10mL of acetic acid is measured and quickly added into the reaction solution, and after the stirring is continued for 20min, the mixture is centrifugally washed and dried to obtain a dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is basically consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 13
Weighing 0.8-1.0 g of tungsten hexachloride, dissolving the tungsten hexachloride in 80-100 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 60 ℃, weighing 0.09-0.12 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. Measuring 15mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 30min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 14
Weighing 0.8-1.0 g of tungsten hexachloride, dissolving the tungsten hexachloride in 80-100 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 70 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. Measuring 15mL of acetic acid, quickly adding the acetic acid into the reaction solution, continuously stirring for 20min, centrifuging, washing and drying to obtain the dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
Example 15
Weighing 0.8-1.0 g of tungsten hexachloride, dissolving the tungsten hexachloride in 80-100 mL of ethanol, stirring for 2-10min under the condition of a constant-temperature water bath at 78 ℃, weighing 0.12-0.15 g of cesium hydroxide, dissolving the cesium hydroxide in the solution, and continuously stirring for 2-5 min. 10mL of acetic acid is measured and quickly added into the reaction solution, and after the stirring is continued for 20min, the mixture is centrifugally washed and dried to obtain a dark blue cesium tungsten bronze material. Taking a proper amount of powder sample for XRD detection. The obtained spectrum is substantially consistent with a standard spectrum (JCPDS 83-1334). And re-dispersing a small amount of dried sample in pure water (with the resistivity of 18.2M omega cm), spotting on a silicon wafer for scanning electron microscope observation, and observing by using a scanning electron microscope to obtain a sample formed by aggregating nano particles with the particle size of 10-20 nm. The energy spectrum (EDS) proves that the material contains cesium, tungsten and oxygen components. And (3) taking a proper amount of powder sample to carry out ultraviolet visible near infrared spectrum test, wherein in an integrating sphere mode, the light transmittance of the near infrared light of the tested sample is rapidly reduced from 18% to 10% at the wavelength of 800-1100nm, and the light transmittance of the near infrared light is basically maintained at 10% at the wavelength of 1100-2000 nm.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications belonging to the technical solutions of the present invention are within the scope of the present invention.
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