JP2001278627A - Method of producing titanium oxide - Google Patents
Method of producing titanium oxideInfo
- Publication number
- JP2001278627A JP2001278627A JP2000098705A JP2000098705A JP2001278627A JP 2001278627 A JP2001278627 A JP 2001278627A JP 2000098705 A JP2000098705 A JP 2000098705A JP 2000098705 A JP2000098705 A JP 2000098705A JP 2001278627 A JP2001278627 A JP 2001278627A
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- titanium
- ammonium
- producing titanium
- present
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 238000010304 firing Methods 0.000 claims abstract description 8
- ZWNZGTHTOBNSDL-UHFFFAOYSA-N N.[Ti+4] Chemical compound N.[Ti+4] ZWNZGTHTOBNSDL-UHFFFAOYSA-N 0.000 claims abstract description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001882 dioxygen Inorganic materials 0.000 claims abstract description 4
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 239000007983 Tris buffer Substances 0.000 abstract description 2
- 239000013522 chelant Substances 0.000 abstract description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 1
- 229910000348 titanium sulfate Inorganic materials 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 102100025490 Slit homolog 1 protein Human genes 0.000 description 2
- 101710123186 Slit homolog 1 protein Proteins 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 102100032566 Carbonic anhydrase-related protein 10 Human genes 0.000 description 1
- LLQPHQFNMLZJMP-UHFFFAOYSA-N Fentrazamide Chemical compound N1=NN(C=2C(=CC=CC=2)Cl)C(=O)N1C(=O)N(CC)C1CCCCC1 LLQPHQFNMLZJMP-UHFFFAOYSA-N 0.000 description 1
- 101000867836 Homo sapiens Carbonic anhydrase-related protein 10 Proteins 0.000 description 1
- -1 N-aminoethyl-aminoethyl Chemical group 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- VULAXXNFNMUCIP-UHFFFAOYSA-M [NH4+].[O-]S(=O)(=O)O[Ti] Chemical compound [NH4+].[O-]S(=O)(=O)O[Ti] VULAXXNFNMUCIP-UHFFFAOYSA-M 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は酸化チタンの製造方
法に関するものであり、詳しくは光触媒活性を示す酸化
チタンの製造方法に関するものである。The present invention relates to a method for producing titanium oxide, and more particularly, to a method for producing titanium oxide having photocatalytic activity.
【0002】[0002]
【従来の技術】光触媒に光を照射すると還元作用を持つ
電子と酸化作用を持つ正孔が生成し、有機物等を酸化還
元作用により分解することができ、例えば、大気中のＮ
Ｏｘの分解、居住空間や作業空間での悪臭物質やカビな
どの分解除去、あるいは水中の有機溶剤や農薬、界面活
性剤などの分解除去への適用が検討されている。2. Description of the Related Art When a photocatalyst is irradiated with light, electrons having a reducing action and holes having an oxidizing action are generated, and organic substances and the like can be decomposed by a redox action.
Application to decomposition of Ox, decomposition and removal of malodorous substances and molds in living and working spaces, and decomposition and removal of organic solvents, pesticides, surfactants, and the like in water are being studied.
【0003】以前は光触媒に活性を発現させるには、紫外線
を照射することが必要であると考えられていたが、最
近、可視光線を照射することによって触媒活性を示す酸
化チタンが発見され、この酸化チタンの製造方法が提案
されている。例えば、ＷＯ９８２３７４号公報には、酸
化チタンをマイクロ波低温プラズマ法により処理しその
表面に炭化チタンを形成することによって触媒活性を示
す酸化チタンを得る方法が記載されている。[0003] Previously, it was thought that it was necessary to irradiate ultraviolet light in order for the photocatalyst to exhibit activity. Recently, however, titanium oxide, which exhibits catalytic activity by irradiating visible light, was discovered. A method for producing titanium oxide has been proposed. For example, WO 982374 describes a method for obtaining titanium oxide having catalytic activity by treating titanium oxide by a microwave low-temperature plasma method and forming titanium carbide on the surface thereof.
【0004】しかし、ＷＯ９８２３７４号公報に記載された
方法では、酸化チタンを処理するためにマイクロ波低温
プラズマ発生装置等の真空容器を備えた特定の装置が必
要であり、操作が煩雑となる問題があった。[0004] However, the method described in WO982374 requires a specific apparatus equipped with a vacuum vessel such as a microwave low-temperature plasma generator for treating titanium oxide, and the operation becomes complicated. there were.
【0005】[0005]
【発明が解決しようとする課題】そこで、本発明の目的
は、可視光線を照射することによって触媒活性を示す酸
化チタンを真空容器を備えた特定の装置を用いることな
く簡易に製造する方法を提供することにある。Accordingly, an object of the present invention is to provide a method for easily producing titanium oxide having catalytic activity by irradiating visible light without using a specific apparatus equipped with a vacuum vessel. Is to do.
【0006】[0006]
【課題を解決するための手段】本発明者等は光触媒活性
を示す酸化チタンの簡易な製造方法について検討を行っ
た結果、本発明を完成するに至った。Means for Solving the Problems The present inventors have studied a simple method for producing titanium oxide having photocatalytic activity, and have completed the present invention.
【0007】すなわち、本発明は窒素とチタンとを含有する
化合物を分子状酸素存在下で焼成することを特徴とする
酸化チタンの製造方法を提供するものである。That is, the present invention provides a method for producing titanium oxide, which comprises firing a compound containing nitrogen and titanium in the presence of molecular oxygen.
【0008】[0008]
【発明の実施の形態】以下、本発明を詳細に説明する。
本発明に用いられる窒素とチタンとを含有する化合物
（以下、チタン含有化合物という。）は、例えば、オキ
シ蓚酸チタンアンモニウム（(ＮＨ4)2・ＴｉＯ（Ｃ
2Ｏ4）2）、硫酸チタンアンモニウム（(ＮＨ4)2ＳＯ4・
３Ｔｉ2（ＳＯ4）3）等のアンモニウム塩とその水和
物、又はイソプロピルトリス（Ｎ−アミノエチル−アミ
ノエチル）チタネート等のチタンキレート化合物が挙げ
られる。中でも、オキシ蓚酸チタンアンモニウムを用い
ることが好ましい。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
The compound containing nitrogen and titanium (hereinafter, referred to as a titanium-containing compound) used in the present invention is, for example, titanium ammonium oxyoxalate ((NH 4 ) 2 .TiO. (C
2 O 4 ) 2 ), titanium ammonium sulfate ((NH 4 ) 2 SO 4.
Examples thereof include ammonium salts such as 3Ti 2 (SO 4 ) 3 ) and hydrates thereof, and titanium chelate compounds such as isopropyl tris (N-aminoethyl-aminoethyl) titanate. Among them, it is preferable to use titanium ammonium oxyoxalate.
【0009】本発明では、このチタン含有化合物を原料の主
成分として用い、これを分子状酸素存在下で焼成する。
焼成温度は３００℃以上が好ましく、また５００℃未満
が適当である。焼成は酸素分子を含む気体中で行えばよ
く、例えば、チタン含有化合物をルツボに入れ、そのル
ツボを雰囲気焼成炉内に置き、雰囲気の酸素濃度を調整
しながら雰囲気を昇温する方法、チタン含有化合物をそ
のまま若しくは造粒した後、流通式焼成炉内に層状に置
き、酸素濃度を調節し昇温した気体を流通式焼成炉に通
じる方法、又はチタン含有化合物をセラミックス製容器
に入れ、その容器を電気炉内に置き、酸素を一定濃度含
む気体を導入しながら電気炉内を昇温する方法で行えば
よい。In the present invention, this titanium-containing compound is used as a main component of a raw material, and is fired in the presence of molecular oxygen.
The firing temperature is preferably 300 ° C. or higher, and suitably lower than 500 ° C. The sintering may be performed in a gas containing oxygen molecules.For example, a method in which a titanium-containing compound is placed in a crucible, the crucible is placed in an atmosphere sintering furnace, and the temperature of the atmosphere is increased while adjusting the oxygen concentration of the atmosphere, After the compound as it is or after granulation, it is placed in a layered form in a flow-type firing furnace, the oxygen concentration is adjusted and the temperature-raised gas is passed through the flow-type firing furnace, or the titanium-containing compound is placed in a ceramic container, and the container is May be placed in an electric furnace, and the temperature inside the electric furnace may be raised while introducing a gas containing a certain concentration of oxygen.
【0010】本発明で得られる酸化チタンは通常、粒子状で
あって結晶構造がアナターゼ型である。この酸化チタン
は波長が４３０ｎｍ以上である可視光線の照射によって
光触媒活性を示すので、これをそのまま又は成形加工し
て用いることにより、居住空間や作業空間での悪臭物質
やカビなどの分解除去、あるいは水中の有機溶剤や農
薬、界面活性剤などの分解除去に適用できる光触媒とす
ることができる。[0010] The titanium oxide obtained in the present invention is usually in the form of particles and has a crystal structure of an anatase type. This titanium oxide exhibits photocatalytic activity when irradiated with visible light having a wavelength of 430 nm or more. By using this titanium oxide as it is or by molding, it can be used to decompose and remove malodorous substances and mold in living and working spaces, or The photocatalyst can be used for decomposing and removing organic solvents, pesticides, surfactants and the like in water.
【0011】[0011]
【実施例】以下、実施例により本発明をさらに詳細に説
明するが本発明はこれら実施例に限定されるものではな
い。EXAMPLES The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples.
【0012】実施例１ オキシ蓚酸チタンアンモニウム（アルドリッチ製）５．
１ｇをアルミナ製ルツボに入れ、そのルツボを箱型電気
炉内に設置した後、空気を導入しながら電気炉内を４５
０℃まで昇温しそのまま１時間保持して焼成した。この
時の昇温速度は２００℃／時間とした。得られた酸化チ
タンは粒子状であった。また、この酸化チタンにつき、
Ｘ線回折装置（商品名：ＲＡＤ−ＩＩＡ、理学電機工業
製）を用いて、Ｘ線管球Ｃｕ、管電圧４０ｋＶ、管電流
３５ｍＡ、発散スリット１度、散乱スリット１度、受光
スリット０．３０ｍｍ、サンプリング幅０．０２０度、
走査速度２．００度／分、測定積算回数１回の条件でＸ
線回折スペクトル測定し、その結晶構造を同定した結
果、アナターゼ型であった。Example 1 Titanium ammonium oxyoxalate (manufactured by Aldrich) 5.
1 g was placed in an alumina crucible, and the crucible was placed in a box-type electric furnace.
The temperature was raised to 0 ° C., and it was kept for 1 hour and calcined. The heating rate at this time was 200 ° C./hour. The obtained titanium oxide was in the form of particles. Also, for this titanium oxide,
Using an X-ray diffractometer (trade name: RAD-IIA, manufactured by Rigaku Corporation), X-ray tube Cu, tube voltage 40 kV, tube current 35 mA, divergence slit 1 degree, scattering slit 1 degree, light receiving slit 0.30 mm , Sampling width 0.020 degrees,
X at a scanning speed of 2.00 degrees / minute and one measurement integration
X-ray diffraction spectrum was measured and the crystal structure was identified.
【0013】密閉式のパイレックス（登録商標）製反応容器
（直径８ｃｍ×高さ１０ｃｍ、容量約０．５リットル）
内に、直径５ｃｍのガラス製シャーレを設置し、そのシ
ャーレ上に、上で得られた酸化チタンを置いた。反応容
器内を混合ガス（酸素と窒素との体積比が１：４であ
る。）で満たし、アセトアルデヒドを１３．４μｍｏｌ
封入した後、反応容器の外から可視光線を照射した。可
視光線の照射には、５００Ｗキセノンランプ（ウシオ電
機製、商品名：オプティカルモジュレックスＳＸ−ＵＩ
５００ＸＱ、ランプＵＸＬ−５００ＳＸ）に、波長約４
３０ｎｍ以下の紫外線をカットするフィルター（東芝硝
子製、商品名：Ｙ−４５）と波長約８３０ｎｍ以上の赤
外線をカットするフィルター（ウシオ電機製、商品名：
スーパーコールドフィルター）とを装着したものを光源
として用いた。可視光線の照射によりアセトアルデヒド
が分解すると、二酸化炭素が発生するので二酸化炭素の
濃度を光音響マルチガスモニタ（ＩＮＮＯＶＡ製、１３
１２型）で経時的に測定し、濃度変化より算出した二酸
化炭素の生成速度により、酸化チタンのアセトアルデヒ
ドに対する光分解作用を評価した。この例における二酸
化炭素の生成速度は、酸化チタン１ｇあたり３．０μｍ
ｏｌ／ｈであった。A closed Pyrex (registered trademark) reaction vessel (diameter 8 cm × height 10 cm, capacity about 0.5 liter)
A glass petri dish having a diameter of 5 cm was placed therein, and the titanium oxide obtained above was placed on the petri dish. The reaction vessel was filled with a mixed gas (volume ratio of oxygen and nitrogen was 1: 4), and acetaldehyde was added at 13.4 μmol.
After sealing, visible light was irradiated from outside the reaction vessel. For irradiation with visible light, use a 500 W xenon lamp (made by Ushio Inc., trade name: Optical Modlex SX-UI)
500XQ, lamp UXL-500SX)
A filter that cuts ultraviolet light of 30 nm or less (product name: Y-45, manufactured by Toshiba Glass) and a filter that cuts infrared light having a wavelength of about 830 nm or more (product name: manufactured by Ushio Inc.)
A super cold filter) was used as a light source. When acetaldehyde is decomposed by irradiation with visible light, carbon dioxide is generated. Therefore, the concentration of carbon dioxide is measured using a photoacoustic multigas monitor (manufactured by INNOVA, 13
12), and the photodecomposition effect of titanium oxide on acetaldehyde was evaluated based on the carbon dioxide generation rate calculated from the concentration change. The production rate of carbon dioxide in this example was 3.0 μm / g of titanium oxide.
ol / h.
【0014】実施例２ 焼成温度を３２０℃、焼成時間を５時間とした以外は実
施例１と同様にして酸化チタンを製造した。得られた酸
化チタンは粒子状で、結晶構造がアナターゼ型であっ
た。次いで、実施例１と同様にしてアセトアルデヒドに
対する光分解作用を評価した。二酸化炭素の生成速度は
酸化チタン１ｇあたり２．７μｍｏｌ／ｈであった。Example 2 Titanium oxide was produced in the same manner as in Example 1 except that the firing temperature was 320 ° C. and the firing time was 5 hours. The obtained titanium oxide was particulate and had a crystal structure of the anatase type. Next, the photodegradation effect on acetaldehyde was evaluated in the same manner as in Example 1. The generation rate of carbon dioxide was 2.7 μmol / h per 1 g of titanium oxide.
【0015】[0015]
【発明の効果】以上説明した様に、本発明によれば、波
長が４３０ｎｍ以上である可視光線を照射することによ
って光触媒活性を示す酸化チタンを簡易に製造すること
ができる。As described above, according to the present invention, it is possible to easily produce titanium oxide having photocatalytic activity by irradiating visible light having a wavelength of 430 nm or more.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 小池 宏信 愛媛県新居浜市惣開町５番１号 住友化学 工業株式会社内 Ｆターム(参考） 4G047 CA02 CB04 CC03 CD03 4G069 AA02 AA08 AA09 BA04A BA04B BA21C BA48A BC50C BE17C CA10 CA17 EA02Y EC22Y FA01 FB40 FC02 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Hironobu Koike 5-1 Sokai-cho, Niihama-shi, Ehime Sumitomo Chemical Co., Ltd. F-term (reference) 4G047 CA02 CB04 CC03 CD03 4G069 AA02 AA08 AA09 BA04A BA04B BA21C BA48A BC50C BE17C CA10 CA17 EA02Y EC22Y FA01 FB40 FC02
Claims (3)
状酸素存在下で焼成することを特徴とする酸化チタンの
製造方法。1. A method for producing titanium oxide, comprising firing a compound containing nitrogen and titanium in the presence of molecular oxygen.
ンを含むアンモニウム塩である請求項１記載の方法。2. The method according to claim 1, wherein the compound containing nitrogen and titanium is an ammonium salt containing titanium.
シ蓚酸チタンアンモニウムである請求項２記載の方法。3. The method according to claim 2, wherein the compound containing nitrogen and titanium is titanium ammonium oxyoxalate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000098705A JP2001278627A (en) | 2000-03-31 | 2000-03-31 | Method of producing titanium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000098705A JP2001278627A (en) | 2000-03-31 | 2000-03-31 | Method of producing titanium oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001278627A true JP2001278627A (en) | 2001-10-10 |
Family
ID=18613162
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000098705A Pending JP2001278627A (en) | 2000-03-31 | 2000-03-31 | Method of producing titanium oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001278627A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1338564A2 (en) | 2002-02-25 | 2003-08-27 | Sumitomo Chemical Co.,Ltd. | Titanium oxide precursor and production method thereof, and production method of titanium oxide using the precursor |
| JP2004292225A (en) * | 2003-03-26 | 2004-10-21 | Sumitomo Chem Co Ltd | Titanium oxide, photocatalyst body, coating agent for photocatalyst body and producing method of titanium oxide |
| US6884753B2 (en) | 2002-05-27 | 2005-04-26 | Sumitomo Chemical Company, Limited | Method for producing ceramic dispersion composition |
| US6974611B2 (en) | 2002-06-25 | 2005-12-13 | Sumitomo Chemical Company, Limited | Titanium oxide dispersion composition, and method and container for preserving the same |
| US7045005B2 (en) | 2001-07-19 | 2006-05-16 | Sumitomo Chemical Company, Limited | Ceramics dispersion liquid, method for producing the same, and hydrophilic coating agent using the same |
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| WO2007105707A1 (en) * | 2006-03-13 | 2007-09-20 | Nikon Corporation | Process for production of carbon nanotube aggregates, carbon nanotube aggregates, catalyst particle dispersion membrane, electron emitters, and field emission displays |
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