WO2017043449A1 - Agglomérat d'oxyde de titane, procédé de production d'agglomérat d'oxyde de titane, poudre d'oxyde de titane, corps moulé d'oxyde de titane, catalyseur d'électrode de batterie, matériau conducteur d'électrode de batterie, et diélectrique à micro-ondes et ondes millimétriques - Google Patents

Agglomérat d'oxyde de titane, procédé de production d'agglomérat d'oxyde de titane, poudre d'oxyde de titane, corps moulé d'oxyde de titane, catalyseur d'électrode de batterie, matériau conducteur d'électrode de batterie, et diélectrique à micro-ondes et ondes millimétriques Download PDF

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Publication number
WO2017043449A1
WO2017043449A1 PCT/JP2016/076049 JP2016076049W WO2017043449A1 WO 2017043449 A1 WO2017043449 A1 WO 2017043449A1 JP 2016076049 W JP2016076049 W JP 2016076049W WO 2017043449 A1 WO2017043449 A1 WO 2017043449A1
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Prior art keywords
titanium oxide
oxide aggregate
battery electrode
microwave
aggregate according
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PCT/JP2016/076049
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English (en)
Japanese (ja)
Inventor
慎一 大越
裕子 所
義総 奈須
飛鳥 生井
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国立大学法人東京大学
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Publication of WO2017043449A1 publication Critical patent/WO2017043449A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a titanium oxide aggregate, a method for producing a titanium oxide aggregate, a titanium oxide powder body, a titanium oxide molded body, a battery electrode catalyst, a battery electrode conductive material, and a microwave / millimeter wave dielectric.
  • Ti 2 O 3 which is representative of an oxide containing Ti 3+ (hereinafter simply referred to as titanium oxide), is a phase transition material having various interesting physical properties, such as metal-insulator transition, It is known that a magnetic-antiferromagnetic transition occurs. Ti 2 O 3 is also known for infrared absorption, thermoelectric effect, magnetoelectric (ME) effect, etc. In addition, in recent years, magnetoresistance (MR) effect has also been found. Such various physical properties have been studied only in bulk bodies ( ⁇ m size) (see, for example, Non-Patent Document 1), and the mechanism is still unclear.
  • TiCl 4 has been synthesized as a bulk material by firing.
  • Ti 4 O 7 has attracted attention in addition to Ti 2 O 3 and Ti 3 O 5 as titanium oxide.
  • titanium oxide composed of Ti 4 O 7 will be applied to various technical fields. It is also possible to do. Therefore, in recent years, development of Ti 4 O 7 having a new particle structure that can be easily applied to various technical fields is also desired.
  • the present invention has been made in consideration of the above points, a titanium oxide aggregate composed of Ti 4 O 7 having a novel particle structure that has not been conventionally, a method for producing a titanium oxide aggregate, a titanium oxide powder body , And a titanium oxide molded body, and further, a battery electrode catalyst, a battery electrode conductive material, and a microwave / millimeter wave dielectric using the titanium oxide aggregate.
  • the titanium oxide aggregate according to the present invention is composed of particles composed of Ti 4 O 7 , and the particles are composed of particulate secondary particles in which a plurality of crystallites as primary particles are bonded. And a plurality of the secondary particles are aggregated, and the particle surface has an uneven porous structure.
  • the method for producing a titanium oxide aggregate according to the present invention includes a precursor powder composed of nano-sized TiO 2 particles fired in a hydrogen atmosphere, and an oxidation composed of Ti 4 O 7 in which the particle surface is formed in an uneven shape. It comprises a firing step for producing a titanium aggregate.
  • the titanium oxide powder according to the present invention is in the form of a powder and contains the titanium oxide aggregate according to any one of claims 1 to 4.
  • the titanium oxide molded body according to the present invention is characterized in that the titanium oxide powder body containing the titanium oxide aggregate according to any one of claims 1 to 4 is solidified.
  • the battery electrode catalyst according to the present invention is a battery electrode catalyst provided on an electrode in a battery, and the noble metal is supported on the titanium oxide aggregate according to any one of claims 1 to 4. It is characterized by that.
  • the conductive material for battery electrodes according to the present invention is a conductive material for battery electrodes contained in a positive electrode or a negative electrode of a battery, and comprises the titanium oxide aggregate according to any one of claims 1 to 4.
  • the microwave / millimeter-wave dielectric according to the present invention is a microwave / millimeter-wave dielectric provided in a microwave / millimeter-wave electromagnetic wave absorber, according to any one of claims 1 to 4. It consists of the described titanium oxide aggregate.
  • the titanium oxide aggregate consisting of Ti 4 O 7 having a novel particle structure unprecedented method for producing titanium oxide aggregates, titanium oxide powder material, and titanium oxide molded bodies can be provided.
  • FIG. 3A is a photograph showing a precursor powder before firing
  • FIG. 3B is a photograph showing a titanium oxide powder body obtained after firing.
  • surface which shows the dielectric constant of the titanium oxide powder body after sintering.
  • 1 represents the titanium oxide aggregate of the present invention, and this titanium oxide aggregate 1 is composed of granules 2 made of Ti 4 O 7. It consists of a porous structure whose surface is uneven.
  • the titanium oxide aggregate 1 is formed so that the particle size of the granule 2 obtained through the firing step described below is 1000 [nm] or less (hereinafter referred to as nano-size), and the primary particles and A plurality of crystallites are combined to form particulate secondary particles 3.
  • the granule 2 that becomes the titanium oxide aggregate 1 is formed into particles by agglomerating a plurality of secondary particles 3 into one lump.
  • a plurality of secondary particles 3 having an irregular shape or size in a spherical shape, a semispherical shape, a semi-elliptical shape, a spherical crown shape, or a droplet shape are densely formed on the particle surface of the particle body 2.
  • a flake-like uneven shape or a coral reef-like uneven shape is formed.
  • the secondary particles 3 on the particle surface have no sharp corners, and are a plurality of secondary particles 3 having a smooth curved surface. It is configured.
  • the secondary particles 3 having irregular sizes, shapes, and formation positions are densely aggregated on the surface of the granules, the granules 2 are added to the secondary particles 3 formed in a convex shape. Irregularly sized recesses are also formed in which the inside is uneven.
  • the crystallites that are the primary particles forming the secondary particles 3 are Ti 4 O 7 crystallites having an average particle diameter of 26 ⁇ 23 [nm] and a nanostructure.
  • the size of the crystallite is confirmed by the TEM image of the titanium oxide aggregate 1 shown in the SEM images of FIGS. 1 and 2.
  • the average grain size of the crystallites was measured by visually checking the change in crystal orientation that appeared in the TEM image, considering the region where the crystal orientation did not change as one crystallite, and selecting it randomly. It means the average value of the size of a plurality of crystallites.
  • the titanium oxide aggregate 1 having such a configuration can be adjusted to a predetermined particle size through a pulverization step described later. That is, the titanium oxide aggregate 1 shown in FIG. 1 and FIG. 2 is pulverized according to the intended use, and the particle size of the granule 2 can be formed to 500 [nm] or less, preferably 10 to 100 [nm]. .
  • a titanium oxide aggregate 1 is produced by the production method described in “(2) Method for producing titanium oxide aggregate”, which will be described later. The obtained titanium oxide powder can be obtained.
  • the titanium oxide powder body preferably contains 95% or more of the titanium oxide aggregate 1 and can be formed into a predetermined shape by compression or solidification with a solidifying material (for example, polyvinyl alcohol).
  • a solidifying material for example, polyvinyl alcohol.
  • the intrinsic electric conductivity of Ti 4 O 7 is 10 3 to 10 4 [S cm ⁇ 1 ]
  • the titanium oxide aggregate of the present invention comprising Ti 4 O 7 is a battery. It can be used as a battery electrode catalyst provided in the inner electrode or a battery electrode conductive material contained in the positive electrode or negative electrode of the battery.
  • this titanium oxide molded body has a dielectric constant of 20 or more at a frequency of 75 [GHz] or more and a dielectric loss tangent of 0.10 or more. More specifically, the dielectric constant can be 23 to 33 and the dielectric loss tangent can be 0.15 to 0.19 at a frequency of 75 to 90 [GHz].
  • a method for producing such a titanium oxide aggregate 1 will be described below.
  • a predetermined amount of precursor powder made of nano-sized TiO 2 particles is prepared.
  • the TiO 2 particles constituting the precursor powder an anatase type or a rutile type can be used, and the particle size is preferably 500 [nm] or less.
  • the precursor powder composed of these TiO 2 particles is fired in a hydrogen atmosphere of 0.05 to 0.5 [L / min], preferably 0.3 ⁇ 0.2 [L / min].
  • firing is preferably performed at a temperature of 900 to 1200 [° C.], preferably 1000 to 1200 [° C.].
  • the time for maintaining the predetermined firing temperature is 0 to 10 hours, preferably 5 ⁇ 2 hours.
  • a titanium oxide aggregate made of Ti 4 O 7 (Ti 3+ Ti 4+ O 7 ), which is an oxide containing Ti 3+, is obtained by a reduction reaction of TiO 2 particles. 1 can be manufactured.
  • a titanium oxide powder body in the form of a black powder is obtained by firing the precursor powder composed of TiO 2 particles, and the titanium oxide aggregate of the present invention is obtained on the titanium oxide powder body. 1 is contained.
  • the hydrogen atmosphere is 0.05 [L / min.
  • the firing temperature may be 1000 to 1200 [° C.] and the firing time may be 3 hours or more.
  • the titanium oxide aggregate 1 obtained in the above-described firing step is used.
  • a pulverization step is performed to pulverize.
  • the pulverization step has a desired particle size by pulverizing the titanium oxide aggregate 1 obtained in the firing step by various other pulverization processes such as a ball mill method, a rod mill method, and a pulverization method by pressing pulverization.
  • a titanium oxide aggregate can be obtained.
  • a titanium oxide powder body made of a titanium oxide aggregate obtained in a firing step, a plurality of hard balls, and water are placed in a container of a pulverizer, and the container is rotated to thereby form titanium oxide.
  • the aggregate can be pulverized with a hard ball to produce a titanium oxide aggregate having a desired particle size.
  • the titanium oxide aggregate 1 can be formed to an optimum particle size according to the usage form of the titanium oxide aggregate.
  • the titanium oxide powder body obtained in the above-mentioned firing step and the titanium oxide powder body obtained through the pulverization step are filled in a molding machine of a predetermined shape and compressed, or, for example, polyvinyl alcohol or the like It can be solidified by adding a solidifying agent, and a titanium oxide molded body having a predetermined shape can be produced.
  • the titanium oxide aggregate was actually manufactured according to the manufacturing method described above, and various verification tests were performed.
  • FIG. 3A for example, about 2.9 [g] of a powder body made of anatase-type TiO 2 particles having a particle diameter of about 7 [nm] was prepared.
  • the precursor powder 6 was fired at 1000 [° C.] for about 5 hours under a hydrogen atmosphere of 0.3 [L / min]
  • about 2.3 [g] of a black powder body 10 as shown in FIG. 3B was obtained. .
  • FIG. 4 the horizontal axis indicates the diffraction angle, and the vertical axis indicates the diffraction X-ray intensity.
  • the actual measurement value is indicated by +
  • the measurement value is indicated by a solid line a
  • the error is indicated by a solid line b
  • the background intensity (bkg) is indicated by a solid line c.
  • a plurality of peaks appeared, and it was confirmed from these peaks that Ti 4 O 7 was generated in the powder body 10.
  • 98.6 (6)% Ti 4 O 7 was produced and 1.4 (5)% Ti 3 O 5 was produced.
  • particulate titanium oxide aggregates 1 as shown in FIGS. 1 and 2 were confirmed. From this, it was confirmed that the obtained powder body 10 was a titanium oxide powder body in which the titanium oxide aggregates 1 were collected. Next, the titanium oxide aggregate 1 contained in the titanium oxide powder was confirmed with an SEM image, and when the particle size of the titanium oxide aggregate 1 was measured visually, the particle size was 100 to 1000 [nm]. It was confirmed that the average particle size of the 500 selected titanium oxide aggregates 1 randomly selected was 451 ⁇ 191 [nm].
  • this titanium oxide powder was pulverized by a ball mill method. Specifically, 200 [mL] water, 191.01 [g] ZrO 2 balls ( ⁇ 2 [mm]), 1000.5 [mg] titanium oxide powder (sample) in a 300 [mL] container The container was continuously rotated at a rotational speed of 70 [rpm] for 3 days by a pulverizer, and the titanium oxide powder was pulverized in the container.
  • the solution in the container was transferred to a petri dish and dried at 60 [° C.], and the residue was collected as a sample.
  • the XRD pattern of the sample thus obtained was analyzed, an analysis result as shown in FIG. 5 was obtained.
  • the horizontal axis represents the diffraction angle
  • the vertical axis represents the diffraction X-ray intensity.
  • the actual measurement value is indicated by a solid line d
  • the measurement value is indicated by a solid line e
  • the error is indicated by a solid line f
  • the background intensity (bkg) is indicated by a solid line g.
  • the titanium oxide aggregates contained in the pulverized titanium oxide powder were confirmed by SEM images, and the particle size of the titanium oxide aggregates was visually measured.
  • the particle size was 50 to 500 [nm]. It was confirmed that the average particle diameter of the 500 selected titanium oxide aggregates selected at random was 185 ⁇ 70 [nm]. From this, it was confirmed that the particle diameter of the titanium oxide aggregate was reliably reduced by the ball mill method.
  • the dielectric constant at a frequency of 75 to 90 [GHz] and the dielectric loss tangents were examined the results shown in FIG. 6 were obtained.
  • the real part ⁇ ′ and the imaginary part ⁇ ′′ of the dielectric constant of a titanium oxide molded body made of flaky Ti 4 O 7 are measured by the free space method, and the dielectric constant
  • the flaky Ti 4 O 7 according to the present invention had a dielectric constant of 20 or more at a frequency of 75 to 90 [GHz] and a dielectric loss tangent of 0.10 or more. From this, it can be confirmed that the flaky Ti 4 O 7 according to the present invention can be used as a dielectric for microwaves and millimeter waves to be blended with a microwave and millimeter wave absorber. It was.
  • the titanium oxide aggregate 1 according to the present invention can conduct electricity when it is formed into a titanium oxide molded body, so that it has been conventionally used as a battery electrode catalyst in a fuel cell. It can be used as an alternative to carbon.
  • a battery electrode catalyst may have a configuration in which a noble metal such as platinum, a platinum alloy, or palladium is supported on the surface of the titanium oxide aggregate 1.
  • the particle size of the titanium oxide aggregate 1 used as a battery electrode catalyst is preferably 10 to 100 [nm]. By forming the particle size by a pulverization step or the like, the particle size of the titanium oxide aggregate 1 can be reduced. It can be used as an alternative to the conventional carbon used.
  • the titanium oxide aggregate 1 of the present invention can be used as a battery electrode conductive material to be blended with a positive electrode or a negative electrode used in a secondary battery such as a lithium ion battery, in addition to being used as a battery electrode catalyst.
  • the positive electrode or the negative electrode contains the titanium oxide aggregate 1 of the present invention as a battery electrode conductive material together with an active material.
  • the dielectric constant is 20 or more at a frequency of 75 to 90 [GHz]
  • the dielectric loss tangent is 0.10 or more. Therefore, it can be used as a microwave / millimeter wave dielectric provided in a microwave / millimeter wave electromagnetic wave absorber used at a frequency of 75 to 90 [GHz].
  • the microwave / millimeter wave dielectric made of the titanium oxide aggregate 1 may be formed in a layered manner on the substrate surface.
  • the titanium oxide aggregate 1 made of Ti 4 O 7 was produced by firing the precursor powder made of nano-sized TiO 2 particles in a hydrogen atmosphere. .
  • the particulate secondary particles 3 in which a plurality of crystallites serving as primary particles are combined are formed, and the plurality of secondary particles 3 are aggregated to form an irregular surface on the particle surface.
  • a titanium oxide aggregate 1 having a porous structure can be produced.
  • this titanium oxide aggregate 1 has an average particle size of 26 ⁇ 23 [nm] of crystallites forming the secondary particles 3, and a particle size of the aggregates of the secondary particles 3 of 1000 [nm]. Since it can be formed into the following nanoparticulate form, Ti 4 O 7 that can be applied to new technical fields can be provided by expanding processing methods and forms of use.
  • this titanium oxide aggregate 1 conducts electricity, it can be used as an alternative to carbon conventionally used as a battery electrode catalyst in fuel cells.
  • this titanium oxide aggregate 1 has a dielectric constant of 20 or more at a frequency of 75 to 90 [GHz] and a dielectric loss tangent of 0.10 or more, the microwave provided in the microwave / millimeter wave wave absorber is provided. -It can also be used as a millimeter wave dielectric.
  • the present invention is not limited to the above-described embodiments, and various modifications can be made within the scope of the gist of the present invention.
  • the battery electrode catalyst used in, for example, a fuel cell is described as the battery electrode catalyst in which the noble metal is supported on the titanium oxide aggregate 1.
  • the present invention is not limited thereto, and the titanium oxide aggregate is not limited thereto.
  • the battery electrode catalyst in which the aggregate 1 supports a noble metal may be applied to battery electrode catalysts for various batteries.
  • the battery electrode conductive material included in the positive electrode or the negative electrode of the lithium ion battery has been described as the battery electrode conductive material comprising the titanium oxide aggregate 1.
  • the present invention is not limited thereto.
  • the battery electrode conductive material made of the titanium oxide aggregate 1 may be applied to various other batteries such as a primary battery and a secondary battery.
  • Titanium oxide aggregate 2 Granule 3 Secondary particle 6 Precursor powder 10 Powder body (Titanium oxide powder body)

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Abstract

La présente invention produit un agglomérat d'oxyde de titane 1, comprenant du Ti4O7 par cuisson d'une poudre de précurseur comprenant des particules de TiO2 de taille nanométrique dans une atmosphère d'hydrogène. En conséquence, la présente invention est apte à produire l'agglomérat d'oxyde de titane 1, qui présente une structure poreuse dans laquelle des particules secondaires particulaires 3 sont formées dans lesquelles une pluralité de cristallites, qui sont des particules primaires, sont liées, et dans laquelle la pluralité de particules secondaires 3 sont agrégées pour former une surface granulaire irrégulière. Ainsi, la présente invention est apte à fournir l'agglomérat d'oxyde de titane 1, comprenant du Ti4O7 présentant une nouvelle structure de particules non conventionnelle.
PCT/JP2016/076049 2015-09-07 2016-09-05 Agglomérat d'oxyde de titane, procédé de production d'agglomérat d'oxyde de titane, poudre d'oxyde de titane, corps moulé d'oxyde de titane, catalyseur d'électrode de batterie, matériau conducteur d'électrode de batterie, et diélectrique à micro-ondes et ondes millimétriques WO2017043449A1 (fr)

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JP2015175989A JP2017052659A (ja) 2015-09-07 2015-09-07 酸化チタン凝集体、酸化チタン凝集体の製造方法、酸化チタン粉末体、酸化チタン成形体、電池電極用触媒、電池電極用導電材及びマイクロ波・ミリ波用誘電体

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CN107742730A (zh) * 2017-09-08 2018-02-27 西安电子科技大学 Ag/Ti4O7锌‑空气电池阴极催化剂的制备方法
JP2018177553A (ja) * 2017-04-04 2018-11-15 東京印刷機材トレーディング株式会社 亜酸化チタン粒子を製造する方法及び亜酸化チタン粒子
WO2019004104A1 (fr) * 2017-06-30 2019-01-03 国立大学法人東京大学 Absorbeur d'ondes radioélectriques
CN112678867A (zh) * 2020-12-25 2021-04-20 苏州锦艺新材料科技有限公司 一种金红石型二氧化钛及其制备方法和应用
CN113416070A (zh) * 2021-06-10 2021-09-21 大连工业大学 一种Ti4O7陶瓷电极的制备方法
CN113423255A (zh) * 2021-06-09 2021-09-21 西北工业大学 核壳结构Ti4O7/磁性金属复合吸收剂及其制备方法
WO2022014402A1 (fr) * 2020-07-16 2022-01-20 堺化学工業株式会社 Matériau d'absorption et décharge d'énergie
CN115947614A (zh) * 2022-06-09 2023-04-11 松山湖材料实验室 亚氧化钛陶瓷电极及其制备方法、应用和电设备

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CN108383154B (zh) * 2018-04-03 2020-02-21 陕西师范大学 一种具有大比表面积的空心介孔Ti4O7@C纳米球的制备方法
WO2022092137A1 (fr) * 2020-10-27 2022-05-05 パナソニック株式会社 Feuille d'absorption d'ondes électromagnétiques

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JP6994684B2 (ja) 2017-04-04 2022-01-14 東京印刷機材トレーディング株式会社 亜酸化チタン粒子を製造する方法及び亜酸化チタン粒子
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JP2019012799A (ja) * 2017-06-30 2019-01-24 国立大学法人 東京大学 電波吸収体
CN110771276A (zh) * 2017-06-30 2020-02-07 国立大学法人东京大学 无线电波吸收体
CN110771276B (zh) * 2017-06-30 2020-12-08 国立大学法人东京大学 无线电波吸收体
JP7216360B2 (ja) 2017-06-30 2023-02-01 国立大学法人 東京大学 電波吸収体
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CN115947614B (zh) * 2022-06-09 2024-05-03 松山湖材料实验室 亚氧化钛陶瓷电极及其制备方法、应用和电设备

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