WO2017086376A1 - Procédé de production de particules contenant du dioxyde de vanadium - Google Patents

Procédé de production de particules contenant du dioxyde de vanadium Download PDF

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Publication number
WO2017086376A1
WO2017086376A1 PCT/JP2016/084062 JP2016084062W WO2017086376A1 WO 2017086376 A1 WO2017086376 A1 WO 2017086376A1 JP 2016084062 W JP2016084062 W JP 2016084062W WO 2017086376 A1 WO2017086376 A1 WO 2017086376A1
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Prior art keywords
vanadium dioxide
containing particles
particles
particle size
hydrothermal reaction
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PCT/JP2016/084062
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English (en)
Japanese (ja)
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貴志 鷲巣
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コニカミノルタ株式会社
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Priority to JP2017551918A priority Critical patent/JPWO2017086376A1/ja
Priority to CN201680066573.1A priority patent/CN108349745B/zh
Publication of WO2017086376A1 publication Critical patent/WO2017086376A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy

Definitions

  • the present invention relates to a method for producing vanadium dioxide-containing particles, and more particularly to a method for producing vanadium dioxide-containing particles having excellent thermochromic properties and storage stability.
  • Vanadium dioxide (VO 2 ) particles have attracted attention as a material exhibiting a thermochromic phenomenon in which optical characteristics such as light transmittance and light reflectance change reversibly with temperature changes.
  • rutile-type crystal phase In the crystal structure of vanadium dioxide particles, there are several polymorphs of crystal phases such as A phase, B phase, C phase and R phase (referred to as so-called “rutile-type crystal phase”).
  • the crystal structure showing the thermochromic phenomenon as described above is limited to the R phase. Since this R phase has a monoclinic structure below the transition temperature, it is also called an M phase.
  • the particle size is on the order of nanometers, there is no aggregation, and the particle size distribution is narrow.
  • a hydrothermal synthesis method has been reported as a technique for producing such particles (see, for example, Patent Document 1). According to the hydrothermal synthesis method, it is possible to produce particles having a particle size of the order of nanometers. However, when vanadium dioxide particles are used for window films or the like, the vanadium dioxide particles need to have a particle size of 40 nm or less in order to prevent the occurrence of haze, but such vanadium dioxide particles are produced only by the hydrothermal synthesis method. Is not enough. In addition, it is difficult to synthesize vanadium dioxide particles having a uniform particle size, and particles having a particle size of 40 nm or more are mixed. Filtration or the like can be considered as a means for removing particles having a large particle diameter mixed in this way. However, particles having a particle diameter of about 200 nm are clogged during filtration and are difficult to remove.
  • Patent Document 2 As a method for obtaining vanadium dioxide particles having a smaller particle diameter, it is conceivable to crush vanadium dioxide particles (for example, see Patent Document 2).
  • Patent Document 2 introduces a crushing method and conditions using a bead mill. However, when a large particle size is crushed, many defective sites are generated in the crystal structure, resulting in decreased thermochromic properties and storage stability. Resulting in.
  • the present invention has been made in view of the above-mentioned problems and situations, and the problem to be solved is to provide a method for producing vanadium dioxide-containing particles having excellent thermochromic properties and storage stability.
  • the present inventor has a process of forming vanadium dioxide-containing particles by hydrothermal reaction and a process of crushing vanadium dioxide-containing particles by a hydrothermal reaction.
  • the vanadium dioxide-containing particles having excellent thermochromic properties and storage stability can be provided by setting the particle size of the vanadium dioxide-containing particles of 80% by number or more to 50 nm or less.
  • the headline, the present invention has been reached.
  • a method for producing vanadium dioxide-containing particles having thermochromic properties Forming vanadium dioxide-containing particles by a hydrothermal reaction; Crushing the vanadium dioxide-containing particles; Have In the step of crushing the vanadium dioxide-containing particles, the particle size of the vanadium dioxide-containing particles of 80% by number or more is set to 50 nm or less.
  • the vanadium dioxide-containing particles according to claim 1 wherein the vanadium dioxide-containing particles having a particle diameter of 100 nm or less are formed by hydrothermal reaction to form 70% by number or more. Production method.
  • the hydrothermal reaction is performed at 230 ° C. or higher, and the time until the reaction system reaches from 25 ° C. to 200 ° C. is within one hour.
  • the above-mentioned means of the present invention can provide a method for producing vanadium dioxide-containing particles having excellent thermochromic properties and storage stability.
  • the method for producing vanadium dioxide-containing particles according to the present invention is characterized in that after the vanadium dioxide-containing particles are formed by a hydrothermal reaction, the particle size of the vanadium dioxide-containing particles of 80% by number or more is crushed so as to be 50 nm or less. Yes.
  • particles having a large particle size are mixed, but as described above, by crushing the particles synthesized by the hydrothermal reaction, the target particles are minimized while minimizing the defect site. Particles containing vanadium dioxide having a diameter can be obtained.
  • particles synthesized by hydrothermal reaction are slightly lower in crystallinity than particles produced by a baking method, etc., and are easily crushed. It is done.
  • the vanadium dioxide-containing particles produced by the method for producing vanadium dioxide-containing particles of the present invention have a particle size of 80% by number or more and 50 nm or less.
  • the haze value is small and the defect site is kept to a minimum, it is presumed that the thermochromic property and the storage stability of the thermochromic property can be maintained.
  • thermochromic vanadium dioxide-containing particles of the present invention comprises a step of forming vanadium dioxide-containing particles by a hydrothermal reaction, and a step of crushing vanadium dioxide-containing particles, and the vanadium dioxide-containing particles In the step of crushing, the particle size of the vanadium dioxide-containing particles of 80% by number or more is 50 nm or less. This feature is a technical feature common to the claimed invention.
  • part can be minimized more and thermochromic property and its storage stability can be maintained.
  • vanadium dioxide-containing particles that exhibit thermochromic properties
  • at least the vanadium compound, the reducing agent, and water are mixed and hydrothermally reacted in the step of forming the vanadium dioxide-containing particles.
  • the reducing agent is oxalic acid, formic acid, hydrazine, or a hydrate thereof from the viewpoint that 70% by number or more of vanadium dioxide-containing particles having a particle size of 100 nm or less can be stably produced. It is preferable that the hydrothermal reaction is performed at 230 ° C. or higher and the time until the reaction system reaches from 25 ° C. to 200 ° C. is within 1 hour.
  • ⁇ representing a numerical range is used in the sense that numerical values described before and after the numerical value range are included as a lower limit value and an upper limit value.
  • the method for producing thermochromic vanadium dioxide-containing particles of the present invention comprises a step of forming vanadium dioxide-containing particles by a hydrothermal reaction, and a step of crushing vanadium dioxide-containing particles, and the vanadium dioxide-containing particles In the step of crushing, the particle size of the vanadium dioxide-containing particles of 80% by number or more is 50 nm or less.
  • the particle size of the vanadium dioxide-containing particles is measured with a laser diffraction particle size distribution meter, and for example, a laser diffraction particle size distribution measuring device manufactured by Shimadzu Corporation can be used. Since the appropriate concentration range of the measurement object (sample) varies depending on each device, it is appropriately concentrated and diluted for use.
  • ⁇ Hydrothermal reaction> it is preferable to synthesize vanadium dioxide-containing particles by mixing at least a vanadium compound, a reducing agent, and water and causing a hydrothermal reaction.
  • vanadium dioxide-containing particles having a rutile-type crystal structure R phase (M layer)
  • the hydrothermal reaction means a chemical reaction in which temperature and pressure are lower than the critical point of water (374 ° C., 22 MPa) and proceed in hot water (subcritical water) at 100 ° C. or higher.
  • the hydrothermal reaction is performed, for example, in a closed container such as an autoclave apparatus. At this time, hydrogen peroxide may be mixed.
  • the conditions of the hydrothermal reaction treatment are set as appropriate, but the liquid temperature of the hydrothermal reaction is, for example, in the range of 200 to 350 ° C. Is preferable, more preferably in the range of 200 to 300 ° C., and particularly preferably in the range of 230 to 300 ° C. If the liquid temperature is 200 ° C. or higher, a sufficient reaction rate can be obtained.
  • the hydrothermal reaction is carried out at 230 ° C. or higher, and the time until the reaction system reaches from 25 ° C. to 200 ° C. is preferably within 2 hours, more preferably within 1 hour. Thereby, the vanadium dioxide containing particle produced can be reduced in particle size.
  • the hydrothermal reaction time is, for example, 1 hour to 7 days. By increasing the time, it is possible to control the average particle size and the like of the obtained vanadium dioxide-containing particles, and when it is within 7 days, it is possible to suppress an excessive increase in energy consumption.
  • the hydrothermal reaction is performed with stirring because the particle diameter of the vanadium dioxide-containing particles can be made more uniform.
  • the hydrothermal reaction may be performed by either a batch method or a continuous method.
  • the hydrothermal reaction it is preferable to form 70% by number or more of vanadium dioxide-containing particles having a particle size of 100 nm or less.
  • the method for controlling the particle size of the vanadium dioxide-containing particles produced by the hydrothermal reaction can be controlled by appropriately selecting the temperature during the hydrothermal reaction, the temperature rising rate, and the like.
  • the particle size is greatly influenced by the temperature rising rate, and the temperature rising rate up to 200 ° C. can be controlled within 1 hour to control the desired particle size.
  • the reaction After completion of the reaction, it is preferable to quickly cool to 150 ° C. or lower. More preferably, it cools to 150 degrees C or less within 30 minutes. Further, the solvent may be replaced by using ultrafiltration to perform washing.
  • the vanadium dioxide-containing particles may be dispersed in a predetermined solvent (dispersion medium) to form a dispersion.
  • the dispersion medium is not particularly limited, and a known medium can be used.
  • Ultrafiltration As the ultrafiltration, for example, using Vivaflow 50 (effective filtration area 50 cm 2 , molecular weight cut-off 5000) manufactured by Sartorius steady, flow rate 300 mL / min, liquid pressure 1 bar (0.1 MPa), normal temperature (20-30) Filtration).
  • the particle size of the vanadium dioxide-containing particles of 80% by number or more is 50 nm or less.
  • the method for crushing the vanadium dioxide-containing particles is not particularly limited, and can be performed using a device such as a high-speed stirrer, a high-pressure homogenizer, a bead mill, and a shaker. Among them, it is preferable to crush using a high-pressure homogenizer or a bead mill from the viewpoint of particle miniaturization.
  • a high-pressure homogenizer is a commercially available device that grinds by shearing force due to accelerated high flow velocity, rapid pressure drop (cavitation), and impact force caused by high-velocity particles colliding face-to-face within a fine orifice.
  • a nanomizer manufactured by Nanomizer Co., Ltd.
  • a microfluidizer manufactured by Microfluidics
  • the degree of crushing by the high-pressure homogenizer depends on the pressure fed to the high-pressure homogenizer and the number of passes through the high-pressure homogenizer (number of passes).
  • the bead mill has a step of filling a container with beads as a medium, pouring a slurry of particles and medium into the stirred beads, and crushing and pulverizing and dispersing the aggregated particles by stirring together with the beads in the medium.
  • Device There is also an apparatus that uses centrifugal separation to separate the slurry and beads.
  • Such a bead mill include Star Mill ZRS (manufactured by Ashizawa Finetech Co., Ltd.), Ultra Apex Mill (manufactured by Kotobuki Kogyo Co., Ltd.), and MSC-MILL (Mitsui Mining Co., Ltd.).
  • the beads used in the bead mill are not particularly limited, and examples thereof include metals and ceramics.
  • zirconia beads and alumina beads can be used.
  • the size of the beads is selected according to the purpose.
  • the particle size of the beads to be applied is preferably about 0.03 to 0.3 mm.
  • the crushing using a bead mill is preferably used such that the beads are in the range of 10 to 80% by volume in the container.
  • the treatment time in the bead mill is preferably about 10 minutes to 24 hours, and if the treatment is further performed, contamination from the beads may be mixed.
  • a dispersing agent can be added as needed during crushing.
  • Commercially available anionic surfactants, cationic surfactants, nonionic surfactants, metal alkoxides and the like can be preferably used.
  • the addition amount of the dispersant is preferably 40% by mass or less of the particle mass.
  • the vanadium dioxide-containing particles according to the present invention are configured to include at least vanadium dioxide, and thereby can exhibit thermochromic properties.
  • the thermochromic property of the vanadium dioxide-containing particles is not particularly limited as long as optical properties such as light transmittance and light reflectance change reversibly with temperature.
  • the light transmittance of the film to which the vanadium dioxide-containing particles are added can be measured as the light transmittance at a wavelength of 2000 nm using, for example, a spectrophotometer V-670 (manufactured by JASCO Corporation).
  • the light transmittance of the film to which the vanadium dioxide-containing particles are added is preferably as high as possible, but is preferably 70% or more.
  • the vanadium dioxide-containing particles according to the present invention are characterized in that a particle size of 80% by number or more is 50 nm or less. For this reason, even when the vanadium dioxide-containing particles according to the present invention are used mixed with a window film, the haze value is small, and since the defect site is minimized, the thermochromic property and its storage stability Sex can be maintained.
  • the vanadium compound according to the present invention is not particularly limited, but is preferably divanadium pentoxide (V 2 O 5 ), ammonium vanadate or vanadium trichloride oxide.
  • ⁇ Reducing agent Although it does not specifically limit as a reducing agent which concerns on this invention, It is preferable that they are oxalic acid, formic acid, hydrazine, or those hydrates.
  • the particle size distribution of the produced particles was measured using a laser diffraction particle size distribution meter. Specifically, the particles were mixed with water so as to have a concentration of 1% by mass, dispersed with ultrasonic waves for 15 minutes to prepare a sample, and measured using a laser diffraction particle size distribution analyzer manufactured by Shimadzu Corporation. .
  • Vanadium dioxide particles were prepared with reference to Example 1 of Japanese Patent No. 5625172.
  • the vanadium dioxide particles contained 32% by number of particles having a particle size of 100 nm or less.
  • the produced particles were subjected to bead milling to crush the particles.
  • particles and water were mixed to make 500 mL of a 10% by mass dispersion.
  • 200 g of zirconia beads having a particle diameter of 0.1 mm was mixed, and crushed for 20 minutes using an Ultra Apex Mill (manufactured by Kotobuki Industries Co., Ltd.) to prepare Sample 101.
  • the particle diameter of 81% by number of vanadium dioxide-containing particles was 50 nm or less.
  • the prepared liquid mixture is put in a high-pressure reaction decomposition container stationary HU 50 ml set (pressure-resistant stainless steel outer tube, PTFE sample container HUTc-50: manufactured by Sanai Kagaku Co., Ltd.), and subjected to a hydrothermal reaction at 260 ° C. for 48 hours. went. At this time, the temperature raising time from 25 ° C. to 200 ° C. was 3 hours.
  • the vanadium dioxide-containing particles contained 31% by number of particles having a particle size of 100 nm or less.
  • the obtained product was washed using ultrafiltration to prepare an aqueous dispersion of vanadium dioxide-containing particles.
  • the prepared dispersion was subjected to bead milling to crush the particles.
  • the dispersion was concentrated to 500 mL of a 10% by mass dispersion.
  • 200 g of zirconia beads having a particle size of 0.1 mm was mixed with this dispersion, and crushing was performed for 15 minutes using an Ultra Apex Mill (manufactured by Kotobuki Industries Co., Ltd.) to produce Sample 102.
  • the particle diameter of 73% by number of vanadium dioxide-containing particles was 50 nm or less.
  • Sample 103 was prepared in the same manner as in the preparation of sample 102, except that the crushing time by the bead mill was 20 minutes. In the sample 103 after crushing, the particle size of 82% by number of vanadium dioxide-containing particles was 50 nm or less.
  • Sample 104 was prepared in the same manner as in the preparation of Sample 103 except that the temperature raising time from 25 ° C. to 200 ° C. was set to 1 hour.
  • the vanadium dioxide-containing particles immediately after the hydrothermal reaction contained 72% by number of particles having a particle size of 100 nm or less. Further, in the sample 104 after crushing, the particle size of 81% by number of vanadium dioxide-containing particles was 50 nm or less.
  • Sample 105 was prepared in the same manner as in the preparation of sample 104 except that the crushing time by the bead mill was 45 minutes. In the sample 105 after crushing, the particle size of 92% by number of vanadium dioxide-containing particles was 50 nm or less.
  • Sample 106 was produced in the same manner as in the production of sample 105 except that the temperature raising time from 25 ° C. to 200 ° C. was changed to 45 minutes.
  • the vanadium dioxide-containing particles immediately after the hydrothermal reaction contained 81% by number of particles having a particle size of 100 nm or less.
  • the particle size of 91% by number of vanadium dioxide-containing particles was 50 nm or less.
  • Sample 107 was produced in the same manner as in the production of sample 105 except that the hydrothermal reaction was performed as follows.
  • V divanadium pentoxide
  • V 2 O 5 special grade, Wako Pure Chemical Industries
  • aqueous solution obtained by mixing 2 mL of 35% by mass of hydrogen peroxide (manufactured by Wako Pure Chemical Industries, Ltd.) and 20 mL of pure water.
  • the prepared liquid mixture is put in a high-pressure reaction decomposition container stationary HU 50 ml set (pressure-resistant stainless steel outer tube, PTFE sample container HUTc-50: manufactured by Sanai Kagaku Co., Ltd.), and subjected to a hydrothermal reaction at 260 ° C. for 48 hours. went. At this time, the temperature raising time from 25 ° C. to 200 ° C. was set to 1 hour.
  • the vanadium dioxide-containing particles immediately after the hydrothermal reaction contained 71% by number of particles having a particle size of 100 nm or less. Further, in the sample 107 after crushing, the particle size of 91% by number of vanadium dioxide-containing particles was 50 nm or less.
  • Sample 108 was produced in the same manner as in the production of sample 105 except that the hydrothermal reaction was performed as follows.
  • V divanadium pentoxide
  • HCOOH formic acid
  • the prepared liquid mixture is put in a high-pressure reaction decomposition container stationary HU 50 ml set (pressure-resistant stainless steel outer tube, PTFE sample container HUTc-50: manufactured by Sanai Kagaku Co., Ltd.), and subjected to a hydrothermal reaction at 260 ° C. for 48 hours. went. At this time, the temperature raising time from 25 ° C. to 200 ° C. was set to 1 hour.
  • the vanadium dioxide-containing particles immediately after the hydrothermal reaction contained 72% by number of particles having a particle size of 100 nm or less.
  • the particle size of 92% by number of vanadium dioxide-containing particles was 50 nm or less.
  • thermochromic storage stability The light transmittance difference ( ⁇ T (%)) after storing each measurement film prepared above at 60 ° C./90% RH for 1000 hours was calculated in the same manner as the thermochromic evaluation, before and after storage.
  • Retention rate (%) ( ⁇ T (%) after storage) / ( ⁇ T (%) before storage) ⁇ 100
  • the samples 103 to 108 produced by the method for producing vanadium dioxide-containing particles of the present invention are superior in thermochromic properties and their storage stability compared to the samples 101 and 102 of the comparative examples. It is shown that.
  • sample 101 vanadium dioxide-containing particles before crushing are produced by firing instead of the hydrothermal method. Therefore, particle deterioration (defect site) due to crushing is large, and as a result, thermochromic properties and storage stability thereof are improved. It is falling.
  • the sample 102 shortens the crushing time, the deterioration due to crushing is small and the same storage stability as that of the sample 103 is obtained.
  • the step of crushing vanadium dioxide-containing particles contains 80% or more vanadium dioxide. It can be seen that the method for producing vanadium dioxide-containing particles having a particle size of 50 nm or less is useful for providing vanadium dioxide-containing particles having excellent thermochromic properties and storage stability.
  • the present invention can be particularly suitably used for providing a method for producing vanadium dioxide-containing particles having excellent thermochromic properties and storage stability.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

La présente invention aborde le problème consistant à proposer un procédé de production de particules contenant du dioxyde de vanadium qui présentent d'excellentes propriétés thermochromiques et une grande stabilité au stockage. Ce procédé de production de particules contenant du dioxyde de vanadium est caractérisé en ce qu'il comprend une étape de formation de particules contenant du dioxyde de vanadium par réaction hydrothermique; et une étape de fracturation des particules contenant du dioxyde de vanadium, dans laquelle la taille de particule d'au moins 80 % des particules contenant du dioxyde de vanadium est égale ou inférieure à 50 nm.
PCT/JP2016/084062 2015-11-20 2016-11-17 Procédé de production de particules contenant du dioxyde de vanadium WO2017086376A1 (fr)

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JP2017551918A JPWO2017086376A1 (ja) 2015-11-20 2016-11-17 二酸化バナジウム含有粒子の製造方法
CN201680066573.1A CN108349745B (zh) 2015-11-20 2016-11-17 含有二氧化钒的粒子的制造方法

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JP2015-227185 2015-11-20

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010031235A (ja) * 2008-06-30 2010-02-12 National Institute Of Advanced Industrial & Technology サーモクロミック微粒子、その分散液、その製造方法、ならびに調光性塗料、調光性フィルムおよび調光性インク
JP2011136873A (ja) * 2009-12-28 2011-07-14 Tsurumi Soda Co Ltd 二酸化バナジウム微粒子、その製造方法、及びサーモクロミックフィルム
JP2014080350A (ja) * 2012-09-28 2014-05-08 Sekisui Chem Co Ltd 酸化バナジウム粒子
JP2014094881A (ja) * 2012-10-11 2014-05-22 Sekisui Chem Co Ltd 二酸化バナジウム粒子の製造方法
JP2015063455A (ja) * 2013-08-30 2015-04-09 積水化学工業株式会社 サーモクロミック性を有する二酸化バナジウム微粒子の製造方法

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5989514A (en) * 1997-07-21 1999-11-23 Nanogram Corporation Processing of vanadium oxide particles with heat
WO2005060610A2 (fr) * 2003-12-11 2005-07-07 The Trustees Of Columbia University In The City Ofnew York Particules a taille nanometrique, leurs procedes d'obtention, compositions et leurs utilisations
JP5548479B2 (ja) * 2010-02-26 2014-07-16 独立行政法人産業技術総合研究所 単結晶微粒子の製造方法
JP5781837B2 (ja) * 2011-06-03 2015-09-24 積水化学工業株式会社 サーモクロミック性フィルム、合わせガラス用中間膜、合わせガラス及び貼り付け用フィルム
CN103157480B (zh) * 2013-02-04 2015-02-18 合肥工业大学 一种氧化钒/铁氧化物脱硝催化剂及其制备方法和应用
CN104261693B (zh) * 2014-08-28 2016-08-17 中国科学院上海硅酸盐研究所 一种二氧化钒基热致变色复合粉体及其制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010031235A (ja) * 2008-06-30 2010-02-12 National Institute Of Advanced Industrial & Technology サーモクロミック微粒子、その分散液、その製造方法、ならびに調光性塗料、調光性フィルムおよび調光性インク
JP2011136873A (ja) * 2009-12-28 2011-07-14 Tsurumi Soda Co Ltd 二酸化バナジウム微粒子、その製造方法、及びサーモクロミックフィルム
JP2014080350A (ja) * 2012-09-28 2014-05-08 Sekisui Chem Co Ltd 酸化バナジウム粒子
JP2014094881A (ja) * 2012-10-11 2014-05-22 Sekisui Chem Co Ltd 二酸化バナジウム粒子の製造方法
JP2015063455A (ja) * 2013-08-30 2015-04-09 積水化学工業株式会社 サーモクロミック性を有する二酸化バナジウム微粒子の製造方法

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