WO2017086068A1 - Procédé de production de particules comprenant du dioxyde de vanadium, et procédé de production d'une dispersion de particules comprenant du dioxyde de vanadium - Google Patents

Procédé de production de particules comprenant du dioxyde de vanadium, et procédé de production d'une dispersion de particules comprenant du dioxyde de vanadium Download PDF

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WO2017086068A1
WO2017086068A1 PCT/JP2016/080571 JP2016080571W WO2017086068A1 WO 2017086068 A1 WO2017086068 A1 WO 2017086068A1 JP 2016080571 W JP2016080571 W JP 2016080571W WO 2017086068 A1 WO2017086068 A1 WO 2017086068A1
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vanadium dioxide
temperature
containing particles
hydrothermal reaction
producing
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PCT/JP2016/080571
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English (en)
Japanese (ja)
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孝 阪口
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コニカミノルタ株式会社
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Publication of WO2017086068A1 publication Critical patent/WO2017086068A1/fr

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    • 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 a method for producing a vanadium dioxide-containing particle dispersion.
  • the present invention relates to a method for producing vanadium dioxide-containing particles having a small average particle size and a small variation in particle size, and a method for producing a vanadium dioxide-containing particle dispersion using the production method.
  • Vanadium dioxide (VO 2 ) is attracting attention as a material exhibiting a thermochromic phenomenon in which optical characteristics such as light transmittance and light reflectance change reversibly with temperature change. Although many crystal structures exist in vanadium dioxide, only the rutile crystal phase (R phase) has thermochromic properties. In order to obtain good optical characteristics, it is desirable that the particle size of the vanadium dioxide-containing particles is on the order of nanometers, has no aggregation, and has a narrow particle size distribution. A hydrothermal synthesis method has been reported as a technique for producing such particles (see, for example, Patent Document 1).
  • vanadium dioxide-containing particles having thermochromic properties are relatively easily produced by hydrothermal reaction of a reaction solution containing water, a raw material containing vanadium (V), a reducing agent, and the like. be able to.
  • the particle size of the obtained vanadium dioxide-containing particles is not sufficiently small, and the variation in particle size is large.
  • the present invention has been made in view of the above-mentioned problems and situations, and the problem to be solved is a method for producing vanadium dioxide-containing particles having a small average particle size and a small variation in particle size, and a dioxide dioxide using the production method. It is to provide a method for producing a vanadium-containing particle dispersion.
  • a method for producing vanadium dioxide-containing particles containing vanadium dioxide having thermochromic properties A step of mixing at least water and a raw material containing vanadium (V) to prepare a reaction solution; Raising the temperature of the reaction solution from room temperature to a hydrothermal reaction temperature at a rate of temperature rise in the range of 5.8 to 15.0 ° C./min; And a step of hydrothermally reacting the reaction solution that has reached the hydrothermal reaction temperature.
  • a method for producing vanadium dioxide-containing particles comprising:
  • the temperature rise is stopped when the reaction solution reaches any temperature within the range of 100 to 200 ° C., 4.
  • a method for producing a vanadium dioxide-containing particle dispersion comprising a step of producing vanadium dioxide-containing particles by the method for producing vanadium dioxide-containing particles according to any one of items 1 to 4.
  • vanadium dioxide-containing particles having a small average particle diameter and small particle size variation can be produced, and a vanadium dioxide-containing particle dispersion containing the vanadium dioxide-containing particles can be produced.
  • the expression mechanism or action mechanism of the effect of the present invention is not clear, but is presumed as follows. It is considered that by increasing the heating rate immediately before the hydrothermal reaction to be within the predetermined range, a large number of nuclei are generated and the vanadium dioxide-containing particles are reduced in size. It is presumed that this is because the grain growth of crystal phases other than the R phase, such as the A phase, was suppressed.
  • the method for producing vanadium dioxide-containing particles of the present invention is a method for producing vanadium dioxide-containing particles containing vanadium dioxide having thermochromic properties, wherein at least water and a raw material containing vanadium (V) are mixed. Preparing the reaction solution, raising the temperature of the reaction solution from room temperature to the hydrothermal reaction temperature at a temperature rise rate in the range of 5.8 to 15.0 ° C./min, and adjusting the hydrothermal reaction temperature to And a hydrothermal reaction of the reached reaction liquid.
  • the hydrothermal reaction temperature is preferably in the range of 200 to 350 ° C.
  • the reaction solution in the hydrothermal reaction step, is preferably hydrothermally reacted for 0.1 to 24 hours. Thereby, it is easy to control the average particle diameter of the obtained vanadium dioxide-containing particles, and it is possible to suppress an excessive increase in energy consumption.
  • the reaction solution in the step of raising the temperature, the reaction solution reaches any temperature within a range of 100 to 200 ° C. before the reaction solution reaches the hydrothermal reaction temperature. It is sometimes preferable to stop the temperature rise and hold the temperature for 0.5 to 5 hours. Thus, it is considered that all the materials can be dissolved by temporarily stopping the temperature increase, and uniform particles can be formed by the subsequent temperature increase.
  • the method for producing a vanadium dioxide-containing particle dispersion of the present invention is characterized by having a step of producing vanadium dioxide-containing particles by the method for producing vanadium dioxide-containing particles.
  • a vanadium dioxide-containing particle dispersion containing vanadium dioxide-containing particles having a small particle diameter and a small variation in particle diameter can be produced.
  • ⁇ is used to mean that the numerical values described before and after it are included as a lower limit value and an upper limit value.
  • the method for producing vanadium dioxide-containing particles of the present invention is a method for producing vanadium dioxide-containing particles containing vanadium dioxide having thermochromic properties, wherein at least water and a raw material containing vanadium (V) are mixed.
  • a reaction solution reaction solution preparation step
  • a step (hydrothermal reaction step) of hydrothermal reaction of the reaction solution that has reached the hydrothermal reaction temperature Preparing a reaction solution (reaction solution preparation step), and a step of raising the reaction solution from normal temperature to a hydrothermal reaction temperature at a temperature increase rate in the range of 5.8 to 15.0 ° C./min (temperature increase).
  • a step hydrothermal reaction of the reaction solution that has reached the hydrothermal reaction temperature.
  • reaction liquid preparation step In the reaction liquid preparation step, at least water and a raw material containing vanadium (V) are mixed to prepare a reaction liquid.
  • This reaction solution may be an aqueous solution in which the raw material is dissolved in water, or may be a suspension in which the raw material is dispersed in water.
  • the raw material containing vanadium (V) refers to a vanadium compound containing vanadium (V) or a mixture of the vanadium compound and other compounds.
  • a material dissolved in a solvent may be used, or a material dispersed in a dispersion medium may be used.
  • the vanadium compound contained in the raw material is not particularly limited as long as it is a pentavalent vanadium (V) compound.
  • V pentavalent vanadium
  • VOCl 3 Vanadium trichloride oxide
  • NaVO 3 sodium metavanadate
  • a compound selected from is preferred.
  • as a vanadium compound contained in a raw material only 1 type may be sufficient and 2 or more types may be sufficient.
  • the above-described raw material may be pretreated in the presence of hydrogen peroxide before performing the hydrothermal reaction step described later.
  • the reaction solution becomes a sol even when a nonionic vanadium compound such as divanadium pentoxide is contained, Hydrothermal reaction can proceed uniformly.
  • 0.5 to 10 mol of hydrogen peroxide is added to the reaction solution with respect to 1 mol of the vanadium compound, and the mixture is stirred at 20 to 40 ° C. for about 0.5 to 10 hours as necessary. What is necessary is just to make it react.
  • water Although the water which concerns on this invention is not specifically limited, The highly purified thing with few impurities is preferable, Specifically, purified water, such as ion-exchange water and distilled water, can be used.
  • the reaction solution according to the present invention preferably contains a reducing agent.
  • the reducing agent has a property of easily dissolving in water, and may function as a reducing agent for a raw material containing vanadium (V).
  • V vanadium
  • a reducing agent it may be used individually by 1 type and may be used in combination of 2 or more type.
  • the content of the reducing agent in the reaction solution is not particularly limited, but is, for example, 0.01 to 2 mol with respect to 1 mol of the vanadium compound.
  • the reaction liquid when the above-mentioned reducing agent is contained in the reaction liquid, it is possible to perform an oxidation-reduction reaction before the hydrothermal reaction step described later.
  • the reaction solution containing the reducing agent may be reacted at 20 to 40 ° C. for about 0.5 to 10 hours with stirring as necessary.
  • a plurality of reducing agents When a plurality of reducing agents are employed, a plurality of reducing agents can be added simultaneously or sequentially to cause the redox reaction.
  • the oxidation-reduction reaction with the reducing agent may be performed simultaneously with the above-described pretreatment of the raw material with hydrogen peroxide (that is, the pretreatment is performed using a reaction solution containing hydrogen peroxide and a reducing agent), or You may carry out sequentially separately from the pre-processing by hydrogen peroxide.
  • the oxidation-reduction reaction before the hydrothermal reaction step vanadium dioxide can be easily generated.
  • the reaction solution according to the present invention includes, for example, tungsten (W), molybdenum (Mo), niobium (Nb), tantalum (Ta), tin (Sn), rhenium (Re), iridium (Ir), and osmium (Os). ), Ruthenium (Ru), germanium (Ge), chromium (Cr), iron (Fe), gallium (Ga), aluminum (Al), fluorine (F), phosphorus (P) and titanium (Ti).
  • a selected compound containing at least one atom may be contained.
  • thermochromic properties (particularly the transition temperature) of the finally obtained vanadium dioxide-containing particles can be controlled.
  • reaction liquid according to the present invention may further contain a substance having oxidizing property or reducing property.
  • a substance having oxidizing property or reducing property include, for example, hydrogen peroxide (H 2 O 2 ).
  • H 2 O 2 hydrogen peroxide
  • reaction solution according to the present invention may contain an organic or inorganic acid or alkali such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, ammonium hydroxide, or ammonia as a pH regulator.
  • the pH of the reaction solution is, for example, 4 to 7 from the viewpoint of the particle size and thermochromic properties of the vanadium dioxide-containing particles.
  • the temperature of the reaction solution prepared in the reaction solution preparation step is raised from room temperature to the hydrothermal reaction temperature at a temperature rising rate in the range of 5.8 to 15.0 ° C./min.
  • the prepared reaction solution is housed in a sealed container such as an autoclave apparatus used for hydrothermal reaction treatment, and heated in a sealed space to a range of 5.8 to 15.0 ° C./min.
  • the temperature is raised from normal temperature (for example, 25 ° C.) to the hydrothermal reaction temperature at the temperature rising rate.
  • the rate of temperature rise is less than 5.8 ° C./min, the average particle size and variation in particle size of the obtained vanadium dioxide-containing particles cannot be reduced.
  • the hydrothermal reaction temperature refers to the liquid temperature of the reaction liquid when performing the hydrothermal reaction process described later, and the hydrothermal reaction process is performed after the reaction liquid is heated to reach the hydrothermal reaction temperature.
  • the hydrothermal reaction temperature is, for example, in the range of 200 to 350 ° C., preferably in the range of 200 to 300 ° C., more preferably in the range of 230 to 300 ° C.
  • the rate of temperature increase in the temperature increasing step may be constant at any one value within the range of 5.8 to 15.0 ° C./min during the temperature increasing period from room temperature to the hydrothermal reaction temperature.
  • the rate of temperature rise may vary with time within a range of 5.8 to 15.0 ° C./min.
  • the temperature rise is stopped before the reaction solution reaches the hydrothermal reaction temperature, and when the reaction solution reaches a holding temperature that is in the range of 100 to 200 ° C.,
  • the holding temperature is preferably held for 0.5 to 5 hours. It is considered that all the materials can be dissolved by temporarily stopping the temperature increase in this way, and uniform particles can be formed by the subsequent temperature increase.
  • the temperature of the reaction solution is restarted and raised to the hydrothermal reaction temperature.
  • the rate of temperature rise may be different before the temperature rise is stopped and after the temperature rise is resumed.
  • the temperature rise is stopped when the reaction solution reaches a temperature within the temperature range of 100 to 200 ° C. and higher than the holding temperature, and is held at the temperature for 0.5 to 5 hours. It is also good. Moreover, it is good also as what repeats such temperature rising stop, temperature holding
  • hydrothermal reaction step In the hydrothermal reaction step, a hydrothermal reaction process is performed using the reaction liquid heated to the hydrothermal reaction temperature in the temperature raising step.
  • “hydrothermal reaction” means a chemical reaction that occurs in hot water (subcritical water) having a temperature and pressure lower than the critical point of water (374 ° C., 22 MPa) and at 100 ° C. or higher.
  • a hydrothermal reaction process is implemented in airtight containers, such as an autoclave apparatus, for example. By carrying out a hydrothermal reaction treatment on the reaction solution heated in the temperature raising step, vanadium dioxide crystal grows to obtain vanadium dioxide-containing particles.
  • the conditions of the hydrothermal reaction treatment are appropriately set, but the hydrothermal reaction temperature is, for example, within the range of 200 to 350 ° C. as described above. Yes, preferably in the range of 200 to 300 ° C, more preferably in the range of 230 to 300 ° C.
  • the hydrothermal reaction temperature is, for example, within the range of 200 to 350 ° C. as described above. Yes, preferably in the range of 200 to 300 ° C, more preferably in the range of 230 to 300 ° C.
  • the hydrothermal reaction treatment time is, for example, in the range of 0.1 hour to 7 days, and preferably in the range of 0.1 to 24 hours. 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 time for the hydrothermal reaction treatment does not include the time for the temperature raising step.
  • the pressure of the hydrothermal reaction treatment is not particularly limited, but is, for example, the saturated water vapor pressure during the hydrothermal reaction, and more specifically, for example, within a range of 5 to 7 MPa.
  • the hydrothermal reaction is performed with stirring because the particle diameter of the vanadium dioxide-containing particles can be made more uniform.
  • hydrothermal reaction treatment may be performed in a batch method or a continuous method.
  • the temperature of the reaction solution After completion of the hydrothermal reaction treatment, it is preferable to quickly cool the temperature of the reaction solution to 150 ° C. or less. More preferably, it cools to 150 degrees C or less within 30 minutes.
  • a suspension containing vanadium dioxide-containing particles having thermochromic properties is obtained.
  • the suspension may be replaced with a dispersion medium or a solvent by filtering (for example, ultrafiltration) or centrifuging, and the vanadium dioxide-containing particles may be washed with water or alcohol.
  • the obtained vanadium dioxide-containing particles may be dried by any means. Thereby, the vanadium dioxide containing particle
  • the vanadium dioxide-containing particles produced by the method for producing vanadium dioxide-containing particles of the present invention contain at least vanadium dioxide (VO 2 ) and have thermochromic properties.
  • the average particle diameter of the vanadium dioxide-containing particles is preferably in the range of 1 to 100 nm.
  • An optical film can be produced by providing the vanadium dioxide-containing particles produced by the production method of the present invention on a substrate, for example, in a state dispersed in a binder resin.
  • the vanadium dioxide-containing particles according to the present invention have thermochromic properties and transparency. The higher the visible light transmittance of the vanadium dioxide-containing particles according to the present invention, the better, but 70% or more is preferable.
  • thermochromic property of the vanadium dioxide-containing particles is not particularly limited as long as optical properties such as light transmittance and light reflectance are reversibly changed by temperature change.
  • the difference in light transmittance at 25 ° C./50% RH and 85 ° C./85% RH is preferably 30% or more.
  • the light transmittance of the vanadium dioxide-containing particles can be measured as the light transmittance at a wavelength of 2000 nm using, for example, a spectrophotometer V-670 (manufactured by JASCO Corporation).
  • vanadium dioxide-containing particles other than vanadium dioxide (VO 2 ), tungsten (W), molybdenum (Mo), niobium (Nb), tantalum (Ta), tin (Sn), Rhenium (Re), iridium (Ir), osmium (Os), ruthenium (Ru), germanium (Ge), chromium (Cr), iron (Fe), gallium (Ga), aluminum (Al), fluorine (F), It may contain at least one kind of atom selected from the group consisting of phosphorus (P) and titanium (Ti).
  • the total amount of these atoms added to the finally obtained vanadium dioxide-containing particles is sufficient to be about 0.1 to 5.0 atomic% with respect to the vanadium (V) atom. %.
  • the total amount added is 5.0 atomic% or less, sufficient thermochromic properties (for example, a difference in light transmittance before and after dimming) can be ensured.
  • the average particle size of the vanadium dioxide-containing particles can be measured, for example, by the following method. First, vanadium dioxide-containing particles are mixed with water at a concentration of 1% by mass, and dispersed with ultrasonic waves for 15 minutes to prepare a measurement sample. Next, the particle size D50 of the vanadium dioxide-containing particles is measured for the produced measurement sample using a laser diffraction particle size distribution measuring device manufactured by Shimadzu Corporation. The number reference value can be adopted as the measurement value.
  • the method for producing a vanadium dioxide-containing particle dispersion of the present invention includes a step of producing vanadium dioxide-containing particles by the above-described method for producing vanadium dioxide-containing particles.
  • the reaction liquid after the hydrothermal reaction step may be used as it is to obtain a vanadium dioxide-containing particle dispersion, or the vanadium dioxide obtained after the hydrothermal reaction step.
  • a step of dispersing the contained particles in a dispersion medium may be further included.
  • the dispersion medium is not particularly limited, and an organic solvent such as alcohol or an inorganic solvent such as water can be used.
  • the dispersion medium may be composed of water alone, for example, in addition to water, an organic solvent of about 0.1 to 10% by mass (in the dispersion), such as methanol, Alcohols such as ethanol, isopropanol and butanol, and ketones such as acetone may also be included.
  • buffer solutions such as a phosphate buffer and an acetate buffer, can also be used as phosphate buffer and an acetate buffer.
  • the vanadium dioxide-containing particle dispersion may contain, for example, an organic or inorganic acid such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, ammonium hydroxide, ammonia, or a pH adjuster such as alkali. You may adjust to pH of this.
  • the pH is preferably 4 to 7.
  • a film can be produced by applying a vanadium dioxide-containing particle dispersion produced as described above onto a substrate.
  • the prepared reaction solution was put into a commercially available autoclave for hydrothermal reaction treatment (OMJ Lab Tech Co., Ltd., MMJ-100), the heating rate was set to 5.8 ° C./min, and the temperature was increased from 25 ° C. (normal temperature) to 270 ° C. The temperature was raised to ° C (hydrothermal reaction temperature). After the temperature increase, a hydrothermal reaction was performed at 270 ° C. for 24 hours. After the hydrothermal reaction, the obtained reaction product was cooled to room temperature, ultrafiltered, and washed with water and ethanol. Furthermore, this reaction product was dried at 60 ° C. for 10 hours using a constant temperature dryer. Thereby, vanadium dioxide containing particles 101 were obtained.
  • vanadium dioxide-containing particles 102 were prepared in the same manner except that the temperature rising rate was set to 10.0 ° C./min.
  • vanadium dioxide-containing particles 103 were prepared in the same manner except that the temperature rising rate was set to 15.0 ° C./min.
  • the prepared reaction liquid was put into a commercially available autoclave for hydrothermal reaction treatment (OMJ Lab Tech Co., Ltd., MMJ-100), the temperature rising rate was set to 10.0 ° C./min, and the temperature was increased from 25 ° C. (normal temperature) to 270. The temperature was raised to ° C (hydrothermal reaction temperature). After the temperature increase, a hydrothermal reaction was performed at 270 ° C. for 24 hours. After the hydrothermal reaction, the obtained reaction product was cooled to room temperature, ultrafiltered, and washed with water and ethanol. Furthermore, this reaction product was dried at 60 ° C. for 10 hours using a constant temperature dryer. Thereby, vanadium dioxide containing particles 105 were obtained.
  • vanadium dioxide-containing particles 106 were prepared in the same manner except that the hydrothermal reaction time was changed to 10 hours.
  • vanadium Dioxide-Containing Particles 108 In the preparation of the vanadium dioxide-containing particles 101, vanadium dioxide-containing particles 108 were prepared in the same manner except that the temperature rising rate was set to 2.2 ° C./min.
  • Vanadium Dioxide-Containing Particles 109 In the preparation of the vanadium dioxide-containing particles 101, vanadium dioxide-containing particles 109 were prepared in the same manner except that the temperature rising rate was set to 3.5 ° C./min.
  • the average particle diameter and CV value of vanadium dioxide-containing particles were evaluated by a scanning electron microscope (FE-SEM) using the obtained particles.
  • the particle diameter of each particle was a so-called area circle equivalent diameter, the area of each particle was measured in an SEM photograph, and the diameter of a circle having the same area was defined as the particle diameter of each particle. Further, in the SEM photograph, 10 particles having the most universal size and shape were selected, and the average particle size and coefficient of variation (CV value) of the 10 particles were calculated.
  • thermochromic properties Pure water is added to vanadium dioxide-containing particles so that the solid content is 0.0001% by mass, and ultrasonic dispersion treatment is performed for 5 minutes with an ultrasonic disperser (UH-300 manufactured by SMT). And redispersed to prepare a measurement sample.
  • the sample was placed in a commercially available quartz cell with a plug (double-sided translucent type 45 mm ⁇ 12.5 mm ⁇ 10 mm), and a spectrophotometer (V-670, manufactured by JASCO Corporation, 190-2500 nm) capable of adjusting the temperature was 25
  • the light transmittance of the sample at a wavelength of 1300 nm at 80 ° C. and 80 ° C. was measured.
  • the difference was calculated and evaluated by subtracting the light transmittance at a wavelength of 1300 nm at 80 ° C. from the light transmittance at a wavelength of 1300 nm at 25 ° C. In addition, it shows that it is excellent in thermochromic property, so that a difference is large.
  • the vanadium dioxide-containing particles according to the present invention have a smaller average particle size and CV value than the vanadium dioxide-containing particles of the comparative example. Therefore, according to the method for producing vanadium dioxide-containing particles of the present invention, it can be said that vanadium dioxide-containing particles having a small average particle size and a small variation in particle size can be produced. Furthermore, it turns out that the vanadium dioxide containing particle
  • the present invention provides a method for producing vanadium dioxide-containing particles having a small average particle size and small variation in particle size, and a method for producing a vanadium dioxide-containing particle dispersion using the production method. Is suitable.

Abstract

La présente invention vise à fournir un procédé de production de particules comprenant du dioxyde de vanadium ayant un petit diamètre moyen de particule et une faible irrégularité de diamètre de particule. Le procédé de production des particules comprenant du dioxyde de vanadium est destiné à produire des particules comprenant du dioxyde de vanadium présentant des propriétés thermochromiques, et est caractérisé en ce qu'il comprend : une étape durant laquelle au moins de l'eau et une matière première contenant du vanadium (V) sont mélangées pour préparer un mélange réactionnel liquide; une étape durant laquelle le mélange réactionnel liquide est chauffé de la température ordinaire jusqu'à une température de réaction hydrothermique à une vitesse de chauffage comprise entre 5,8 et 15,0 °C/min.; et une étape durant laquelle le mélange réactionnel liquide chauffé à la température de réaction hydrothermique est amené à subir une réaction hydrothermique.
PCT/JP2016/080571 2015-11-18 2016-10-14 Procédé de production de particules comprenant du dioxyde de vanadium, et procédé de production d'une dispersion de particules comprenant du dioxyde de vanadium WO2017086068A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019006624A (ja) * 2017-06-23 2019-01-17 国立研究開発法人産業技術総合研究所 フッ素ドープ型酸化チタンバナジウムのナノ粒子及びその製造方法、並びに該ナノ粒子を含む分散液、塗料、透明樹脂成形体及び積層体
JP2020138871A (ja) * 2019-02-26 2020-09-03 国立研究開発法人産業技術総合研究所 二酸化バナジウム粒子の製造方法

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08229386A (ja) * 1995-02-28 1996-09-10 Mazda Motor Corp 炭化水素吸着剤及びその製造方法並びに排気ガス浄化触媒
JPH09298324A (ja) * 1996-03-06 1997-11-18 Seiko Epson Corp 圧電体薄膜素子及びその製造方法、並びにこれを用いたインクジェット式記録ヘッド
JPH11263623A (ja) * 1998-03-18 1999-09-28 Nittetsu Mining Co Ltd 磁性粉体の製造方法
JP2001180930A (ja) * 1999-12-28 2001-07-03 Ykk Corp 薄片状ベーマイト粒子及びその製造方法
JP2010069474A (ja) * 2008-08-22 2010-04-02 National Institute Of Advanced Industrial Science & Technology 流通式超臨界水熱合成によるナノ粒子の合成方法及びその装置
JP2010083708A (ja) * 2008-09-30 2010-04-15 Tdk Corp チタン酸バリウム微粒子の製造方法および電子部品の製造方法
JP2011178825A (ja) * 2010-02-26 2011-09-15 National Institute Of Advanced Industrial Science & Technology 単結晶微粒子、その製造方法、及びその用途
JP2014040331A (ja) * 2012-08-21 2014-03-06 Fujifilm Corp 亜鉛錫酸化物の製造方法
WO2016158432A1 (fr) * 2015-03-31 2016-10-06 コニカミノルタ株式会社 Particules contenant du dioxyde de vanadium présentant des propriétés thermochromiques et leur procédé de fabrication

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08229386A (ja) * 1995-02-28 1996-09-10 Mazda Motor Corp 炭化水素吸着剤及びその製造方法並びに排気ガス浄化触媒
JPH09298324A (ja) * 1996-03-06 1997-11-18 Seiko Epson Corp 圧電体薄膜素子及びその製造方法、並びにこれを用いたインクジェット式記録ヘッド
JPH11263623A (ja) * 1998-03-18 1999-09-28 Nittetsu Mining Co Ltd 磁性粉体の製造方法
JP2001180930A (ja) * 1999-12-28 2001-07-03 Ykk Corp 薄片状ベーマイト粒子及びその製造方法
JP2010069474A (ja) * 2008-08-22 2010-04-02 National Institute Of Advanced Industrial Science & Technology 流通式超臨界水熱合成によるナノ粒子の合成方法及びその装置
JP2010083708A (ja) * 2008-09-30 2010-04-15 Tdk Corp チタン酸バリウム微粒子の製造方法および電子部品の製造方法
JP2011178825A (ja) * 2010-02-26 2011-09-15 National Institute Of Advanced Industrial Science & Technology 単結晶微粒子、その製造方法、及びその用途
JP2014040331A (ja) * 2012-08-21 2014-03-06 Fujifilm Corp 亜鉛錫酸化物の製造方法
WO2016158432A1 (fr) * 2015-03-31 2016-10-06 コニカミノルタ株式会社 Particules contenant du dioxyde de vanadium présentant des propriétés thermochromiques et leur procédé de fabrication

Cited By (3)

* Cited by examiner, † Cited by third party
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JP2019006624A (ja) * 2017-06-23 2019-01-17 国立研究開発法人産業技術総合研究所 フッ素ドープ型酸化チタンバナジウムのナノ粒子及びその製造方法、並びに該ナノ粒子を含む分散液、塗料、透明樹脂成形体及び積層体
JP2020138871A (ja) * 2019-02-26 2020-09-03 国立研究開発法人産業技術総合研究所 二酸化バナジウム粒子の製造方法
JP7145506B2 (ja) 2019-02-26 2022-10-03 国立研究開発法人産業技術総合研究所 二酸化バナジウム粒子の製造方法

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