JP4392231B2 - Long fiber nano titanium oxide - Google Patents
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- JP4392231B2 JP4392231B2 JP2003407824A JP2003407824A JP4392231B2 JP 4392231 B2 JP4392231 B2 JP 4392231B2 JP 2003407824 A JP2003407824 A JP 2003407824A JP 2003407824 A JP2003407824 A JP 2003407824A JP 4392231 B2 JP4392231 B2 JP 4392231B2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 60
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 42
- 239000000835 fiber Substances 0.000 title claims description 33
- 239000013078 crystal Substances 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 32
- 239000000843 powder Substances 0.000 description 18
- 238000010335 hydrothermal treatment Methods 0.000 description 9
- 239000003513 alkali Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Description
本発明は、例えば活性の高い光触媒や、光電変換効率の高い色素増感太陽電池用電極材料などに利用できる長繊維状ナノ酸化チタンに関する。 The present invention is, for example, high or the photocatalytic active, available like high dye-sensitized solar cell electrode material photoelectric conversion efficiency relates to the filamentous nano titanium oxide emissions.
酸化チタンは、例えば光触媒の用途や色素増感太陽電池の用途などに使用されるが、この酸化チタンとしては、単位塗布面積当たりの反応量を増加させるために、できるだけ大きな比表面積を持った材料が要求されている。 Titanium oxide is used for photocatalyst applications and dye-sensitized solar cell applications, for example. This titanium oxide is a material having a specific surface area as large as possible in order to increase the amount of reaction per unit coating area. Is required.
そこで、従来では、大きな比表面積を得るために、粒状酸化チタン粉末の粒径を数十nmから数nmのサイズに小さくする方向で検討が進められていたが、実際に現在販売されているこれらの粒状粉末では、５０〜３００m2／g程度までの比表面積しか実現されていない。 Therefore, in the past, in order to obtain a large specific surface area, studies were made in the direction of reducing the particle size of granular titanium oxide powder from several tens of nanometers to several nanometers. In the granular powder, only a specific surface area of about 50 to 300 m 2 / g is realized.
これに対し、近年では、より大きな比表面積を得るために、各種の技術が開発されている（例えば特許文献１参照）。この技術とは、酸化チタン粉末を水酸化ナトリウムでアルカリ処理することにより、直径５〜８nm、長さ５０〜１５０nmのチューブ状酸化チタンを製造するというものである。
しかしながら、上述したチューブ状酸化チタンの製造方法では、２００〜４８０m2／g程度の比較的大きな比表面積を実現できると記述されているが、特性の再現性に問題があった。 However, although it has been described that the tube-shaped titanium oxide manufacturing method described above can achieve a relatively large specific surface area of about 200 to 480 m 2 / g, there is a problem in the reproducibility of characteristics.
つまり、前記公報の製造方法によってチューブ状酸化チタンを製造する場合には、常に大きな比表面積を有するチューブ状酸化チタンを実現できるとは限らず、特性の再現性に問題があり、一層の改善が望まれていた。 That is, when producing tubular titanium oxide by the production method of the above publication, it is not always possible to realize tubular titanium oxide having a large specific surface area, and there is a problem in the reproducibility of characteristics, and further improvement is achieved. It was desired.
本発明の目的は、大きな比表面積を有し、従来とは全く異なる長繊維状ナノ酸化チタンを提供することである。 This onset bright object has a large specific surface area, it is to provide a totally different lengths fibrous nano titanium oxide emissions from the traditional.
・かかる目的を達成するためになされた本発明は、 結晶形状が中実かつ長繊維状であり、その長繊維状結晶の組成が、（Ｋ、Ｈ） 2 Ｔｉ 2 Ｏ 5 であることを特徴とする長繊維状ナノ酸化チタンを要旨とする。
本発明の長繊維状ナノ酸化チタンは、いわゆるナノレベルの極めて細い繊維状（ワイヤー状）の酸化チタンである。つまり、酸化チタンの結晶形状が長繊維状である。この長繊維状ナノ酸化チタンは、従来の様な（中空の）チューブ状酸化チタンとは異なり、（中空では無く）中身の詰まった例えば毛髪の様な中実の繊維状の結晶である。
- according the present invention the objective has been made in order to achieve the Ri solid and long fibrous der crystal shape, the composition of the long-fiber crystals, that is 2 Ti 2 O 5 (K, H) The feature is a long-fiber nano-titanium oxide characterized.
The long-fiber nano-titanium oxide of the present invention is a so-called nano-level very thin fibrous (wire-like) titanium oxide. That is, the crystal shape of titanium oxide is long fiber. Unlike the conventional (hollow) tube-like titanium oxide, the long-fiber nano titanium oxide is a solid fibrous crystal such as hair that is packed (not hollow).
この長繊維状ナノ酸化チタンは、ナノレベルの非常に細い結晶構造を有しているので、比表面積が大きく、例えば光触媒の用途及び色素増感太陽電池の用途に使用される場合には、その単位塗布面積当たりの反応量を大きく増加させることができ、好適である。
なお、後述する様に、本発明者らの研究により、この長繊維状結晶の組成が確認されている。
The long fibrous nano-titanium oxide has a very thin crystal structure at the nano level, and therefore has a large specific surface area. For example, when used in photocatalyst applications and dye-sensitized solar cell applications, The reaction amount per unit coating area can be greatly increased, which is preferable.
As will be described later, the composition of the long fibrous crystals has been confirmed by the study of the present inventors.
・前記長繊維状ナノ酸化チタンは、前記長繊維状結晶の直径が、２〜８０nmであることを特徴とするように構成することができる。
本発明は、長繊維状ナノ酸化チタンの長繊維状結晶の直径を例示したものである。本発明では、長繊維状結晶の直径が、２〜８０nm（例えば主として５〜３０nm）と十分に細いので、大きな比表面積を有する。
The long-fiber nano titanium oxide can be configured such that the long-fiber crystal has a diameter of 2 to 80 nm.
The present invention exemplifies the diameter of the long fibrous crystal of the long fibrous nano titanium oxide. In the present invention, since the diameter of the long fibrous crystal is sufficiently thin as 2 to 80 nm (for example, mainly 5 to 30 nm), it has a large specific surface area.
尚、長繊維状ナノ酸化チタンは細長い結晶（即ち繊維が伸びる方向と径方向とのアスペクト比の大きな結晶）であるので、長繊維状結晶の直径とは、その細長い結晶の各位置における直径の平均値を意味している。 Since the long fibrous nano-titanium oxide is an elongated crystal (that is, a crystal having a large aspect ratio between the direction in which the fiber extends and the radial direction), the diameter of the long fibrous crystal is the diameter at each position of the elongated crystal. Mean value.
・前記長繊維状ナノ酸化チタンは、前記長繊維状結晶の長さが、１００nm以上であることを特徴とするように構成することができる。
本発明は、長繊維状ナノ酸化チタンの長繊維状結晶の長さを例示したものである。本発明では、長繊維状結晶の長さが、１００nm以上と長いので、その長繊維状結晶が集合した集合体は、例えば不織布の繊維が絡みあったような構造となる。
The long fibrous nano-titanium oxide can be configured such that the length of the long fibrous crystal is 100 nm or more.
The present invention illustrates the length of long fibrous crystals of long fibrous nano-titanium oxide. In the present invention, since the length of the long fibrous crystals is as long as 100 nm or more, the aggregate in which the long fibrous crystals are assembled has a structure in which, for example, the fibers of the nonwoven fabric are entangled.
・前記長繊維状ナノ酸化チタンは、比表面積が、３００〜４５０ｍ2／ｇであることを特徴とするように構成することができる。
本発明は、長繊維状ナノ酸化チタンの比表面積を例示したものである。本発明では、比表面積が３００〜４５０ｍ2／ｇ（例えば主として３５０〜４００ｍ2／ｇ）と大きいので、例えば光触媒の用途及び色素増感太陽電池の用途に使用される場合には、その単位塗布面積当たりの反応量を大きく増加させることができ、好適である。
The long fibrous nano-titanium oxide may have a specific surface area of 300 to 450 m 2 / g.
The present invention exemplifies the specific surface area of long fibrous nano-titanium oxide. In the present invention, since the specific surface area is as large as 300 to 450 m 2 / g (for example, mainly 350 to 400 m 2 / g), for example, when used for a photocatalyst and a dye-sensitized solar cell, the unit coating is performed. The reaction amount per area can be greatly increased, which is preferable.
・また、本発明の長繊維状ナノ酸化チタンは、酸化チタン及び酸化チタン塩の少なくとも１種を主成分とする材料を用いて製造することができる。 It also filamentous nano titanium oxide of the present invention can be produced using a material containing as a main component at least one of titanium oxide and titanium salt.
さらに、本発明の長繊維状ナノ酸化チタンは、酸化チタン及び酸化チタン塩の少なくとも１種を主成分とする材料（例えば酸化チタン、酸化チタン塩、又は、酸化チタン及び酸化チタン塩からなる材料）を、水酸化カリウムで水熱処理（アルカリ処理）する工程を利用して製造することができる。 Furthermore, the long fibrous nano-titanium oxide of the present invention is a material mainly comprising at least one of titanium oxide and titanium oxide salt (for example, titanium oxide, titanium oxide salt, or material comprising titanium oxide and titanium oxide salt). Can be produced by utilizing a hydrothermal treatment (alkali treatment) with potassium hydroxide .
なお、前記水熱処理（アルカリ処理）の条件としては、水酸化カリウム濃度１０〜２５mol／kg、温度７０〜１５０℃の条件を採用できる。 In addition, as the conditions for the hydrothermal treatment (alkali treatment), a potassium hydroxide concentration of 10 to 25 mol / kg and a temperature of 70 to 150 ° C. can be adopted .
ここで、水酸化カリウム濃度が１０mol／kgを下回るか２５mol／kgを上回ると、比表面積が小さくなる傾向があるので、この濃度範囲が好ましい。また、処理温度が７０℃を下回るか１５０℃を上回る場合には、比表面積が小さくなる傾向があるので、この温度範囲が好ましい。尚、より好ましい範囲は、水酸化カリウム濃度１５〜２０mol／kg、温度１００〜１３０℃である。 Here, when the potassium hydroxide concentration is less than 10 mol / kg or more than 25 mol / kg, the specific surface area tends to decrease, so this concentration range is preferable. Further, when the processing temperature is lower than 70 ° C. or higher than 150 ° C., the specific surface area tends to be small, so this temperature range is preferable. A more preferable range is a potassium hydroxide concentration of 15 to 20 mol / kg and a temperature of 100 to 130 ° C.
次に、本発明の最良の形態の例（実施例）について説明する。 Next, an example (example) of the best mode of the present invention will be described.
ａ）まず、本実施例の長繊維状ナノ酸化チタンの構造について説明する。
図１に破断して模式的に示す様に、本実施例の長繊維状ナノ酸化チタン１は、ナノレベルの極細の酸化チタンの結晶であり、その結晶形状は、（中身の詰まった）中実の長繊維状（ワイヤー状）である。
a) First, the structure of the long fibrous nano-titanium oxide of this example will be described.
As shown schematically in FIG. 1, the long-fiber nano-titanium oxide 1 of this example is a nano-level ultra-fine titanium oxide crystal, and its crystal shape is medium (filled) Real long fiber shape (wire shape).
この長繊維状ナノ酸化チタン１の直径（平均値）は、約２〜８０nmと極めて細く、その長さは、約１００nm以上であり、しかも、その比表面積は、約３００〜４５０ｍ2／ｇと非常に大きなものである。 The long fibrous nano-titanium oxide 1 has a very thin diameter (average value) of about 2 to 80 nm, a length of about 100 nm or more, and a specific surface area of about 300 to 450 m 2 / g. It is very big.
詳しくは、後述する製造方法にて得られる長繊維状ナノ酸化チタン１は、その多くが、５〜３０nmの直径を有するとともに、１００nm以上の長さを有しており、長いものでは２〜３μｍ以上のものがある。つまり、後述する図２〜図４に示す様に、長繊維状ナノ酸化チタン１は、非常に細長い繊維状の結晶である。 Specifically, many of the long fibrous nano-titanium oxides 1 obtained by the manufacturing method described later have a diameter of 5 to 30 nm and a length of 100 nm or more. There are more. That is, as shown in FIGS. 2 to 4 to be described later, the long fibrous nano-titanium oxide 1 is a very elongated fibrous crystal.
ｂ）次に、本実施例の長繊維状ナノ酸化チタン１の製造方法の要部について説明する。
本実施例では、以下に述べる様に、チタニア（ＴｉＯ2）粉末を水酸化カリウム（ＫＯＨ）の水溶液を用いて水熱処理することにより、長繊維状ナノ酸化チタン１を製造する。
b) Next, the principal part of the manufacturing method of the long-fiber nano titanium oxide 1 of a present Example is demonstrated.
In the present embodiment, as described below, long-fiber nano titanium oxide 1 is manufactured by hydrothermally treating titania (TiO 2 ) powder using an aqueous solution of potassium hydroxide (KOH).
(1)原料粉末
原料粉末としては、例えば粒径約３０nmのアナターゼ型のチタニア粉末を用いる。
(1) Raw material powder As the raw material powder, for example , anatase-type titania powder having a particle size of about 30 nm is used.
(2)水熱処理（アルカリ処理）
濃度１０〜２５mol／kgの水酸化カリウムの水溶液に前記チタニア粉末を加え、よく攪拌する。その後、温度７０〜１５０℃の条件で、５〜４０時間加熱して、水熱処理を行う。
(2) Hydrothermal treatment (alkali treatment)
The titania powder is added to an aqueous solution of potassium hydroxide having a concentration of 10 to 25 mol / kg and stirred well. Thereafter, hydrothermal treatment is performed by heating at a temperature of 70 to 150 ° C. for 5 to 40 hours.
(3)中和処理
前記水熱処理の後に、イオン交換水等を用いて洗浄し、希塩酸等の無機酸を用いて中和処理を行い、余剰のアルカリ分を取り除く。
(3) Neutralization treatment After the hydrothermal treatment, washing is performed using ion exchange water or the like, and neutralization treatment is performed using an inorganic acid such as dilute hydrochloric acid to remove excess alkali.
(4)乾燥処理
前記中和処理後に、遠心分離し、遠心分離した固定分を凍結乾燥器で乾燥して、長繊維状ナノ酸化チタン１が集合した集合体（粉末）を得る。
(4) Drying treatment After the neutralization treatment, the mixture is centrifuged, and the centrifuged fixed portion is dried with a freeze dryer to obtain an aggregate (powder) in which the long fibrous nano-titanium oxide 1 is assembled.
ｃ）この様にして得られた長繊維状ナノ酸化チタン１は、その直径がナノレベルの非常に細い長繊維状であるので、比表面積も十分に大きなものである。
従って、この長繊維状ナノ酸化チタン１を、例えば光触媒の用途及び色素増感太陽電池の用途に使用した場合には、単位塗布面積当たりの反応量を大きく増加させることができるので、その性能が向上することが期待できる。
c) The long-fiber nano-titanium oxide 1 obtained in this way is a very thin long-fiber having a nanometer diameter, and therefore has a sufficiently large specific surface area.
Accordingly, when this long-fiber nano titanium oxide 1 is used for, for example, a photocatalyst and a dye-sensitized solar cell, the reaction amount per unit coating area can be greatly increased. It can be expected to improve.
また、後述する実験例に示される様に、上述した製造方法により、再現性良く本実施例の長繊維状ナノ酸化チタン１を製造することができる。
（実験例）
次に、本発明の効果を確認するために行った具体的な実験例について説明する。
Further, as shown in the experimental examples described later, the long-fiber nano titanium oxide 1 of this example can be manufactured with good reproducibility by the above-described manufacturing method.
(Experimental example)
Next, a specific experimental example performed for confirming the effect of the present invention will be described.
ａ）まず、テフロン（登録商標）容器にて、１０ｍＬの純水に１１．２ｇの水酸化カリウム（純度８５％）を混入し、良く攪拌して、濃度（純水１ｋｇに対するＫＯＨのモル数）１７．０mol／kgの水酸化カリウム水溶液を調製した。 a) First, in a Teflon (registered trademark) container, 11.2 g of potassium hydroxide (purity 85%) was mixed in 10 mL of pure water, and stirred well to obtain a concentration (number of moles of KOH relative to 1 kg of pure water). A 17.0 mol / kg aqueous potassium hydroxide solution was prepared.
次に、前記容器内に、粒径約３０nmの酸化チタンの微粒子（チタニア粉末）を０．２１ｇ混入し、良く攪拌した。
次に、前記容器を密閉し、その容器を乾燥機内に配置して、１１０℃で２０時間加熱し、水熱処理（アルカリ処理）を行った。
Next, 0.21 g of titanium oxide fine particles (titania powder) having a particle size of about 30 nm were mixed in the container and stirred well.
Next, the said container was sealed, the container was arrange | positioned in dryer, and it heated at 110 degreeC for 20 hours, and performed the hydrothermal treatment (alkali treatment).
次に、水熱処理によって生成した生成物を、イオン交換水で水洗いし、希塩酸で中和して、余剰のアルカリ分を除去した。
次に、生成物を遠心分離し、その固定分を凍結乾燥器で乾燥して、長繊維状ナノ酸化チタンが集合した集合体（粉末）を得た。
Next, the product produced by the hydrothermal treatment was washed with ion-exchanged water and neutralized with dilute hydrochloric acid to remove excess alkali.
Next, the product was centrifuged, and the fixed part was dried with a freeze dryer to obtain an aggregate (powder) in which long fibrous nano-titanium oxide was aggregated.
ｂ）そして、上述した製造方法で得られた粉末を、走査型電子顕微鏡（ＳＥＭ）にて観察したところ、図２（１０，０００倍のＳＥＭ写真）、図３（２５，０００倍のＳＥＭ写真）、及び図４（１００，０００倍のＳＥＭ写真）に示す様に、細長い繊維が不織布の様に密集した構造が観察された。尚、各長繊維状の物質がそれぞれ長繊維状ナノ酸化チタンである。 b) Then, when the powder obtained by the above-described manufacturing method was observed with a scanning electron microscope (SEM), FIG. 2 (10,000 times SEM photograph) and FIG. 3 (25,000 times SEM photograph). ) And FIG. 4 (100,000 times SEM photograph), a structure in which elongated fibers are densely packed like a nonwoven fabric was observed. Each long fibrous substance is long fibrous nano-titanium oxide.
また、前記粉末を、透過型電子顕微鏡（ＴＥＭ）にて観察したところ、図５（１５０，０００倍のＴＥＭ写真）に示す様に、長繊維状ナノ酸化チタンが、空洞の無い中実の長繊維状であることが確認できた。 Further, when the powder was observed with a transmission electron microscope (TEM), as shown in FIG. 5 (150,000 times TEM photograph), the long fibrous nano-titanium oxide had a solid length without a cavity. It was confirmed to be fibrous.
更に、前記粉末を構成する長繊維状ナノ酸化チタンの組成を、電子線回折により測定したところ、（Ｋ、Ｈ）2Ｔｉ2Ｏ5であることが確認された。
その上、前記粉末（従って長繊維状ナノ酸化チタン）の比表面積（生成物のＢＥＴ 比表面積）を、QUANTACHROME NOVA-1000-TSを用いて測定したところ、３９６．３１ｍ2／ｇと非常に大きな比表面積であることが確認できた。
Further, the composition of the long fibrous nano-titanium oxide constituting the powder was measured by electron diffraction, and it was confirmed that it was (K, H) 2 Ti 2 O 5 .
In addition, the specific surface area (the BET specific surface area of the product) of the powder (and thus the long fibrous nano-titanium oxide) was measured using a QUANTACHROME NOVA-1000-TS, which was as large as 396.31 m 2 / g. The specific surface area was confirmed.
ｃ）次に、前記実験の条件のうち、水酸化カリウムの濃度と水熱処理の温度を変更した各実験を行って、各試料の比表面積［ｍ2／ｇ］を測定した。その結果を、合わせて下記表１に記す。 c) Next, among the experimental conditions, each experiment was performed by changing the concentration of potassium hydroxide and the hydrothermal treatment temperature, and the specific surface area [m 2 / g] of each sample was measured. The results are shown in Table 1 below.
この表１から明らかな様に、粒径約３０nmの酸化チタンの微粒を用いた場合には、濃度１０〜２５mol／kgの水酸化カリウム水溶液を用いて、温度７０〜１５０℃で水熱処理することにより、最大で約４００ｍ2／ｇ程度に達する様な大きな比表面積を有する粉末（従って長繊維状ナノ酸化チタン）が得られることが分かる。 As is apparent from Table 1 , when titanium oxide fine particles having a particle diameter of about 30 nm are used, hydrothermal treatment is performed at a temperature of 70 to 150 ° C. using a potassium hydroxide aqueous solution having a concentration of 10 to 25 mol / kg. Thus, it can be seen that a powder having a large specific surface area of about 400 m 2 / g at the maximum (thus, long-fiber nano titanium oxide) can be obtained.
また、前記表１における各試料（粉末）のＳＥＭ写真から、全試料の長繊維状ナノ酸化チタンの直径及び長さを測定したところ、長繊維状ナノ酸化チタンの直径は、平均で約２〜８０nm（多くは５〜３０nm）で、その平均長さは、約１００nm以上の非常に細長い繊維であることが確認できた。 Moreover, from the SEM photograph of each sample (powder) in Table 1, the diameter and length of the long fibrous nano-titanium oxide of all the samples were measured. It was confirmed that the average length was 80 nm (many 5 to 30 nm), and the fibers were very long fibers having an average length of about 100 nm or more.
更に、前記表１における各試料（粉末）のＴＥＭ写真から、全試料の長繊維状ナノ酸化チタンが中実の長繊維状であることが確認できた。
つまり、上述した実験例から、本発明の長繊維状ナノ酸化チタンは、ナノレベルの極細の非常に長い繊維であり、しかも、比表面積が大きなものであることが分かる。
Furthermore, from the TEM photograph of each sample (powder) in Table 1, it was confirmed that the long fibrous nano-titanium oxide of all the samples was a solid long fiber.
That is, it can be seen from the above-described experimental example that the long-fiber nanotitanium oxide of the present invention is a nano-sized ultra-fine and extremely long fiber and has a large specific surface area.
尚、本発明は前記実施例になんら限定されるものではなく、本発明の要旨を逸脱しない範囲において種々の態様で実施しうることはいうまでもない。
例えば、処理温度、処理時間、水酸化カリウム濃度を調節する等により、長繊維状ナノ酸化チタンの直径、長さ、比表面積などを調整することが可能である。例えば処理時間を適度に長くすることにより、比表面積を大きくする等の調整を行うことが可能である。
In addition, this invention is not limited to the said Example at all, and it cannot be overemphasized that it can implement with a various aspect in the range which does not deviate from the summary of this invention.
For example, it is possible to adjust the diameter, length, specific surface area, and the like of the long fibrous nano-titanium oxide by adjusting the treatment temperature, treatment time, potassium hydroxide concentration, and the like. For example, it is possible to make adjustments such as increasing the specific surface area by appropriately increasing the treatment time.
１…長繊維状ナノ酸化チタン 1 ... long fiber nano titanium oxide
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