JP2007210802A - Method for forming finely acicular titanium dioxide group and method for measuring actual reaction area on surface of sheet - Google Patents

Method for forming finely acicular titanium dioxide group and method for measuring actual reaction area on surface of sheet Download PDF

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JP2007210802A
JP2007210802A JP2005317981A JP2005317981A JP2007210802A JP 2007210802 A JP2007210802 A JP 2007210802A JP 2005317981 A JP2005317981 A JP 2005317981A JP 2005317981 A JP2005317981 A JP 2005317981A JP 2007210802 A JP2007210802 A JP 2007210802A
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titanium dioxide
reaction area
dioxide group
group
area
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Masato Shinada
正人 品田
Keisuke Kasahara
敬介 笠原
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ITAGAKI KINZOKU KK
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ITAGAKI KINZOKU KK
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for forming a finely acicular titanium dioxide group by irradiating the surface of titanium or a titanium alloy with a low-energy-density laser to form a group of finely acicular titanium dioxide protrusions on the surface to thereby form a surface with a large actual reaction area thereon and to provide a method for measuring the actual reaction area on the surface of the sheet by determining a titanium dioxide group of a desired actual reaction area on the basis of the color developed on the surface of the sheet by the laser processing. <P>SOLUTION: A titanium sheet 3 is irradiated with a low-energy-density laser 6 at varied irradiation pitches and varied tracking counts by using a laser processing machine 4 using e.g., YVO4 to form a titanium dioxide group 1 comprising finely acicular protrusions 2. The titanium dioxide group 1 has an actual reaction area several times larger than that of the initial area (A) and variously develops colors. Therefore, it is possible to determine the actual reaction area (Ar) on the basis of the color developed. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

光触媒反応効果のある二酸化チタン群を板表面に形成し、かつその形成される実質的反応面積に対応する光触媒反応効果の高い板材を形成するための微細針状二酸化チタン群生成方法及び板表面の実質的反応面積測定方法に関する。   A method of generating fine acicular titanium dioxide groups for forming a titanium dioxide group having a photocatalytic reaction effect on the plate surface and forming a plate material having a high photocatalytic reaction effect corresponding to the formed substantial reaction area, and the plate surface The present invention relates to a method for measuring a substantial reaction area.

二酸化チタンは光触媒効果に優れ、有機物分解特性、殺菌特性、超親水性、電気分解効果等の様々な有効な特性を有する。以上の二酸化チタンの諸特性を最大限に引き出すには、反応に必要な紫外線を出来るだけ多く確保する必要があると共に、二酸化チタンの形成される反応面積を出来るだけ大きくすることが必要である。この反応面積を大きくするにはそれに対応して装置も大きくなり、高価なものとなると共に省スペースやコンパク化等の最近必要とされている志向に反する結果を招く。
なお、従来においても二酸化チタンを形成する各種の方法が開示されており、その一例として「特許文献1」が挙げられる。
特開2002−302760号(請求項1)
Titanium dioxide has an excellent photocatalytic effect, and has various effective properties such as organic matter decomposition properties, bactericidal properties, super hydrophilicity, and electrolysis effects. In order to maximize the various characteristics of titanium dioxide, it is necessary to secure as much ultraviolet rays as necessary for the reaction and to increase the reaction area where titanium dioxide is formed as much as possible. In order to increase the reaction area, the apparatus becomes correspondingly large, which is expensive and results in contrary to the recently required orientation such as space saving and compactness.
Conventionally, various methods for forming titanium dioxide have been disclosed, and an example thereof is “Patent Document 1”.
JP-A-2002-302760 (Claim 1)

前記「特許文献1」は金属板上に光触媒性の高い二酸化チタンを作製する方法に関するものであるが、成膜法を用いるものであり、本発明のように直接レーザを板表面に照射し、その照射条件によって室質的反応面積の広大を図り、かつその実質的反応面積を計測し得るものではない。
一定の面積Aの表面に二酸化チタンを形成する場合、前記のようにこの面積Aを大きくすればよいが、面積Aのままで実質的の面積を大きくすることができれば、省スペース化がコンパクト化の志向に相反することなく光触媒効果を上げることができる。
出願人の研究によれば、微小出力がコントロール可能なレーザ加工機(例えば、YVO4レーザ(6.5w、Q−switch)で弱いエネルギー密度の熱エネルギーをチタン等の板材の表面に(ガルバノ)等によって所定の照射ピッチで集中的に繰返し照射することによりその照射エリアに微細針状突起ができ、実質的反応面積の広い二酸化チタン群を形成することができることがわかった。
The above-mentioned “Patent Document 1” relates to a method of producing titanium dioxide having high photocatalytic property on a metal plate, but uses a film forming method, and directly irradiates the plate surface with a laser as in the present invention, Depending on the irradiation conditions, the roomy reaction area cannot be expanded and the substantial reaction area cannot be measured.
When titanium dioxide is formed on the surface of a certain area A, the area A may be increased as described above. However, if the substantial area can be increased while the area A is maintained, the space saving is reduced. The photocatalytic effect can be increased without contradicting the orientation of the.
According to the applicant's research, a laser machine capable of controlling a minute output (for example, YVO4 laser (6.5 w, Q-switch)) is used to apply heat energy of weak energy density to the surface of a plate material such as titanium (galvano), etc. Thus, it was found that fine acicular protrusions can be formed in the irradiated area by intensive and repeated irradiation at a predetermined irradiation pitch, and a titanium dioxide group having a substantially large reaction area can be formed.

本発明は、以上の事情に鑑みて発明されたものであり、チタン等の板の表面に微弱なエネルギー密度のレーザを照射ピッチや繰返し回数(トラッキング回数)を決めて照射し、数十ナノメートルから数面ナノメートルの微細針状突起からなる二酸化チタン群を形成する方法と、微細針状突起の突起高さに対応して変化する発色を照射ピッチに対応させて求め、発色によって実質的反応面積を求めるようにした微細針状二酸化チタン群生成方法及び板表面の実質的反応面積測定方法を提供することを目的とする。   The present invention has been invented in view of the above circumstances, and irradiates the surface of a plate of titanium or the like with a weak energy density laser with an irradiation pitch and repetition number (tracking number) determined, and several tens of nanometers. The method of forming titanium dioxide groups consisting of fine needle-like protrusions of several nanometers from the surface, and the color change that changes according to the protrusion height of the fine needle-like protrusions is determined according to the irradiation pitch. It is an object of the present invention to provide a method for producing fine acicular titanium dioxide groups and a method for measuring a substantial reaction area on the surface of a plate in which the area is obtained.

本発明は、以上の目的を達成するために、請求項1の発明は、チタン又はチタン合金又はステンレス,アルミ,アルミナ,ニッケル等の金属板の板表面(面積A)に微弱エネルギー密度にコントロールされたレーザを照射し、前記表面に微細針状突起(突起高さd)の二酸化チタン群を形成することを特徴とする。   In order to achieve the above object, the present invention is controlled to have a weak energy density on the plate surface (area A) of a metal plate such as titanium, a titanium alloy, stainless steel, aluminum, alumina, or nickel. Then, a laser beam is irradiated to form a group of titanium dioxide having fine needle-like projections (projection height d) on the surface.

また、請求項2の発明は、前記二酸化チタン群は、前記微細針状突起の突起高さdに対応して色彩を変化させるものからなり、突起高さdの増加に対応して色彩が濃色になることを特徴とする。   According to a second aspect of the present invention, the titanium dioxide group has a color that changes in accordance with the protrusion height d of the fine needle-like protrusion, and the color is darker in response to an increase in the protrusion height d. It is characterized by becoming a color.

また、請求項3の発明は、前記微細針状突起の突起高さdが、数十ナノメートルから数百ナノメートルのものからなることを特徴とする。   The invention of claim 3 is characterized in that the projection height d of the fine needle-like projections is from several tens of nanometers to several hundreds of nanometers.

また、請求項4の発明は、前記二酸化チタン群は、照射ピッチ及び照射繰返し回数(トラッキング回数という)に対応して前記面積Aよりも広い実質的反応面積(Ar)を形成するものからなることを特徴とする。   According to a fourth aspect of the present invention, the titanium dioxide group comprises a substantial reaction area (Ar) larger than the area A corresponding to the irradiation pitch and the number of repetitions of irradiation (referred to as the number of tracking times). It is characterized by.

また、請求項5の発明は、二酸化チタン群によって形成される反応面積の測定方法であって、該方法は、前記請求項1乃至4の微細針状二酸化チタン群生成方法によって形成される二酸化チタン群の色彩を基にして前記実質的反応面積Arを求めることを特徴とする。   The invention of claim 5 is a method for measuring the reaction area formed by the titanium dioxide group, which method comprises the titanium dioxide formed by the fine needle-like titanium dioxide group generation method of the first to fourth aspects. The substantial reaction area Ar is obtained based on the color of the group.

本発明の請求項1の微細針状二酸化チタン群生成方法によれば、チタン等の板材の表面に弱エネルギー密度にコントロールされたレーザを照射することにより微細針状突起ができ、これによる二酸化チタン群を容易に生成することができる。この二酸化チタン群は突起群からなり実質的な面積の拡大化が図れる。   According to the fine needle-like titanium dioxide group generation method of claim 1 of the present invention, fine needle-like protrusions can be formed by irradiating the surface of a plate material such as titanium with a laser controlled to a weak energy density. Groups can be generated easily. This titanium dioxide group consists of projection groups, and can substantially expand the area.

また、請求項2の微細針状二酸化チタン群生成方法によれば、突起高さによって表面に生ずる色彩が相異し、この発色は照射ピッチによって異なり、照射ピッチと発色との関係を求めることができる。   Further, according to the fine acicular titanium dioxide group generation method of claim 2, the color generated on the surface varies depending on the height of the protrusion, and this color development varies depending on the irradiation pitch, and the relationship between the irradiation pitch and the color development can be obtained. it can.

また、請求項3の微細針状二酸化チタン群生成方法によれば、突起高さdを数十ナノメートル乃至数百ナノメートルにすることにより異なる発色の二酸化チタン群を形成することができる。   According to the fine acicular titanium dioxide group generation method of claim 3, different colored titanium dioxide groups can be formed by setting the protrusion height d to several tens of nanometers to several hundreds of nanometers.

また、請求項4の微細針状二酸化チタン群生成方法によれば、実質的反応面積(Ar)は照射ピッチとトラッキング回数により異なるため、所望の広面積の二酸化チタン群をこれ等の条件を基にして形成することができる。   Further, according to the method for generating fine acicular titanium dioxide groups of claim 4, since the substantial reaction area (Ar) varies depending on the irradiation pitch and the number of tracking times, a desired wide area titanium dioxide group is determined based on these conditions. Can be formed.

また、請求項5の微細針状二酸化チタン群による板表面の実質的反応面積の測定方法によれば、照射ピッチを基にして板表面に形成される発光の色彩によって元の照射面積Aの数倍の所望の実質的反応面積(Ar)の二酸化チタン群を形成することができる。即ち、発色を基にして実質的反応面積(Ar)を求めることができる。   According to the method for measuring the substantial reaction area of the plate surface by the fine acicular titanium dioxide group according to claim 5, the number of the original irradiation areas A depending on the color of light emission formed on the plate surface based on the irradiation pitch. Double the desired substantial reaction area (Ar) of titanium dioxide groups can be formed. That is, the substantial reaction area (Ar) can be obtained based on the color development.

以下、本発明の微細針状二酸化チタン群生成方法及び板表面の実質的反応面積測定方法の実施の形態を図面や表に基づいて詳述する。
まず、レーザが加工機4としては一例としてYVO4レーザ(6.5w,Q−switch)を用い、そのガルバノ5のコントロールにより照射ピッチやトラッキング回数をコントロールして微弱エネルギー密度のレーザ6を照射するようにする。なお、レーザ加工機き前記のものに限定するものではないことは勿論である。また、レーザ6を照射するための板材としてはチタンやチタン合金、ステンレス、アルミ、アルミナ及びニッケル等の金属が適用されるが、チタン又はチタン合金が最も望ましい。
Hereinafter, embodiments of the method for producing fine acicular titanium dioxide groups and the method for measuring the substantial reaction area of the plate surface of the present invention will be described in detail with reference to the drawings and tables.
First, as a processing machine 4, a laser uses a YVO 4 laser (6.5 w, Q-switch) as an example, and the irradiation pitch and tracking frequency are controlled by controlling the galvano 5 so as to irradiate the laser 6 with weak energy density. To. Of course, the laser processing machine is not limited to the above-described one. Further, as the plate material for irradiating the laser 6, metals such as titanium, titanium alloy, stainless steel, aluminum, alumina and nickel are applied, but titanium or titanium alloy is most desirable.

以上のレーザ加工機4からのレーザ6を図1に示すようにチタン板3の面積Aの部分に照射するとその面積Aの部分には突起高さdの微細針状突起2が形成され、これが二酸化チタン群1が形成される。この場合、照射ピッチ及びトラッキング回数を変えると例えば「表1」が求められる。また、形成される突起高さdは数ナノメートル及び数百ナノメートルであるが、これに限定するものではない。   As shown in FIG. 1, when the area A of the titanium plate 3 is irradiated with the laser 6 from the laser processing machine 4 described above, fine needle-like protrusions 2 having a protrusion height d are formed on the area A, Titanium dioxide group 1 is formed. In this case, for example, “Table 1” is obtained by changing the irradiation pitch and the number of tracking times. Moreover, although the protrusion height d to be formed is several nanometers and several hundred nanometers, it is not limited to this.

Figure 2007210802
Figure 2007210802

表1に示すように、照射ピッチとトラッキング回数を変化させると実質的反応面積(Ar)が大きく変化する。なお、表1に示すように照射ピッチが小さくトラッキング回数が大きい場合に実質的反応面積(Ar)は大きくなり、例えば、照射ピッチ0.01mmでトラッキング回数が20回の場合はAr/A=4.55となり、面積Aの4.55倍となる。よってレーザ加工機6によるレーザ密度を決めて、照射ピッチやトラッキング回数を変化させることにより所望の実質的反応面積(Ar)を求めることができる。   As shown in Table 1, when the irradiation pitch and the number of tracking times are changed, the substantial reaction area (Ar) changes greatly. As shown in Table 1, when the irradiation pitch is small and the number of tracking times is large, the substantial reaction area (Ar) becomes large. For example, when the irradiation pitch is 0.01 mm and the number of tracking times is 20, Ar / A = 4. .55, which is 4.55 times the area A. Therefore, the desired substantial reaction area (Ar) can be obtained by determining the laser density by the laser processing machine 6 and changing the irradiation pitch and the number of tracking times.

以上のように、レーザ照射によりチタン板3に所望の実質的反応面積(Ar)の二酸化チタン群1を形成することができるが、この場合、照射されるレーザの照射条件により突起高さdが相異し、この突起高さdの値により発色が異なる。この突起高さdと発色との関係は照射ピッチごとに予め求められるが、突起高さdが大きくなるに従って発色は濃くなる結果となる。「表2」はその状態を示す模式図である。   As described above, the titanium dioxide group 1 having a desired substantial reaction area (Ar) can be formed on the titanium plate 3 by laser irradiation. In this case, the projection height d depends on the irradiation condition of the irradiated laser. The color development differs depending on the value of the protrusion height d. The relationship between the projection height d and the color development is obtained in advance for each irradiation pitch, but the color development becomes deeper as the projection height d increases. “Table 2” is a schematic diagram showing the state.

Figure 2007210802
Figure 2007210802

次に、「表1」や「表2」を基にして所望の実質的反応面積(Ar)の二酸化チタン群1を生成する方法と、実質的反応面積(Ar)の求め方について説明する。
まず、レーザ加工機4を選定し、微弱エネルギー密度をコントロールし、微細針状突起の突起高さdが数十ナノメートル乃至数百ナノメートルになるようにレーザ6をチタン板3等の表面に照射する。以上から照射ピッチ及びトラッキング回数を決めることにより「表1」のように所望の実質的反応面積(Ar)を容易に求めることができる。
Next, a method for generating the titanium dioxide group 1 having a desired substantial reaction area (Ar) based on “Table 1” and “Table 2” and a method for obtaining the substantial reaction area (Ar) will be described.
First, the laser processing machine 4 is selected, the weak energy density is controlled, and the laser 6 is placed on the surface of the titanium plate 3 or the like so that the protrusion height d of the fine needle-like protrusions is several tens to several hundreds of nanometers. Irradiate. From the above, by determining the irradiation pitch and the number of tracking times, the desired substantial reaction area (Ar) can be easily obtained as shown in Table 1.

一方、逆にレーザ照射されたチタン板3の発色状態を光の干渉によるホログラフィー効果によって求める(観察)ことができ、この場合の発色に対応した微細針状突起2を求め、これを発生させている照射ピッチを求めることができ、この場合のトラッキング回数を求めることにより実質的反応面積(Ar)を求めることができる。   On the other hand, the color development state of the titanium plate 3 irradiated with the laser can be obtained (observed) by the holographic effect due to the interference of light, and the fine needle-like protrusions 2 corresponding to the color development in this case are obtained and generated. The effective reaction area (Ar) can be determined by determining the number of times of tracking in this case.

本発明は、所望の光触媒効果を生じさせるためにチタン等の板材の表面に広い実質的反応面積を形成するものであり、二酸化チタン群を形成した広面積の板材は各種の場所に適用され、その利用範囲は極めて広い。また、省スペース、コンパクト化が図れ、環境保全への貢献も高い。   The present invention forms a wide substantial reaction area on the surface of a plate material such as titanium in order to produce a desired photocatalytic effect, and the wide area plate material formed with the titanium dioxide group is applied to various places, Its range of use is extremely wide. In addition, space saving and compactness can be achieved, and the contribution to environmental conservation is also high.

本発明の突起高さdの二酸化チタン群を示す模式図。The schematic diagram which shows the titanium dioxide group of the protrusion height d of this invention.

符号の説明Explanation of symbols

1 二酸化チタン群
2 微細針状突起
3 チタン板
4 レーザ加工機
5 ガルバノ
6 レーザ
DESCRIPTION OF SYMBOLS 1 Titanium dioxide group 2 Fine needle-like protrusion 3 Titanium plate 4 Laser processing machine 5 Galvano 6 Laser

Claims (5)

チタン又はチタン合金又はステンレス,アルミ,アルミナ,ニッケル等の金属板の板表面(面積A)に微弱エネルギー密度にコントロールされたレーザを照射し、前記表面に微細針状突起(突起高さd)の二酸化チタン群を形成することを特徴とする微細針状二酸化チタン群生成方法。   The surface (area A) of a metal plate such as titanium, titanium alloy, stainless steel, aluminum, alumina, or nickel is irradiated with a laser controlled to a weak energy density, and fine acicular protrusions (projection height d) are formed on the surface. A method for producing fine acicular titanium dioxide groups, comprising forming titanium dioxide groups. 前記二酸化チタン群は、前記微細針状突起の突起高さdに対応して色彩を変化させるものからなり、突起高さdの増加に対応して色彩が濃色になることを特徴とする請求項1に記載の微細針状二酸化チタン群生成方法。   The titanium dioxide group is made of a material that changes color according to the protrusion height d of the fine needle-like protrusions, and the color becomes dark as the protrusion height d increases. Item 2. The method for producing fine acicular titanium dioxide groups according to Item 1. 前記微細針状突起の突起高さdが、数十ナノメートルから数百ナノメートルのものからなることを特徴とする請求項1又は2にいずれかに記載の微細針状二酸化チタン群生成方法。   The method for generating fine acicular titanium dioxide groups according to claim 1 or 2, wherein the projection height d of the fine acicular projections is from several tens of nanometers to several hundreds of nanometers. 前記二酸化チタン群は、照射ピッチ及び照射繰返し回数(トラッキング回数という)に対応して前記面積Aよりも広い実質的反応面積(Ar)を形成するものからなることを特徴とする請求項1乃至3のいずれかに記載の微細針状二酸化チタン群生成方法。   The titanium dioxide group is formed of a material that forms a substantial reaction area (Ar) larger than the area A corresponding to the irradiation pitch and the number of irradiation repetitions (referred to as tracking number). The fine acicular titanium dioxide group production | generation method in any one of. 前記二酸化チタン群によって形成される反応面積の測定方法であって、該方法は、請求項1乃至4の微細針状二酸化チタン群生成方法によって形成される二酸化チタン群の色彩を基にして前記実質的反応面積Arを求めることを特徴とする微細針状二酸化チタン群による板表面の実質的反応面積測定方法。
A method for measuring a reaction area formed by the titanium dioxide group, wherein the method is based on the color of the titanium dioxide group formed by the fine acicular titanium dioxide group generation method according to claim 1. A method for measuring a substantial reaction area on the surface of a plate with fine acicular titanium dioxide groups, characterized in that a static reaction area Ar is obtained.
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CN105883912A (en) * 2016-05-15 2016-08-24 北京工业大学 Method for preparing self-support titanium dioxide three-dimensional micro-nano structure

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105883912A (en) * 2016-05-15 2016-08-24 北京工业大学 Method for preparing self-support titanium dioxide three-dimensional micro-nano structure

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