本発明は、パルスレーザによる微小構造の形成方法に関し、特に、シリカガラスへのパルスレーザの集光照射によって、シリカガラスを局所的に改質させてレーザ改質領域を形成し、該レーザ改質領域をエッチングにより除去することにより、微小穴，微小溝，微小凹み等の微小構造を形成する方法に関する。 The present invention relates to a method for forming a microstructure using a pulsed laser, and in particular, a laser-modified region is formed by locally modifying silica glass by focused irradiation of the pulsed laser onto silica glass, and the laser modification. The present invention relates to a method for forming a minute structure such as a minute hole, a minute groove, and a minute recess by removing a region by etching.
微小穴，微小溝，微小凹み等の微小な構造を有するガラス材料は、マイクロノズルやバイオチップ・ケミストリーチップなどとしての利用が期待されている。そして、パルスレーザ、特にフェムト秒レーザを用いてガラスに微小構造を形成する手法では、３次元的な構造への加工を行うことが可能である等の長所を有している。 Glass materials having minute structures such as minute holes, minute grooves, and minute dents are expected to be used as micro nozzles, biochips, and chemistry chips. The technique of forming a microstructure on glass using a pulse laser, particularly a femtosecond laser, has an advantage that it can be processed into a three-dimensional structure.
フェムト秒レーザを用いてガラスに微小構造を形成する技術として、例えば特許文献１に示す技術が知られている。この技術は、シリカガラス等の透明材料からなる被加工材料に対し、パルスの持続時間がフェムト秒乃至ピコ秒オーダのパルスレーザを集光して照射し、上記パルスレーザの照射位置を、該被加工材料内において、少なくとも１箇所は該被加工材料の表面上である位置を含めて走査させ、上記被加工材料の上記パルスレーザが照射された部分を、フッ化水素酸やバッファードフッ酸を用いてエッチング処理により取り除き、該部分を孔とすることを特徴とするレーザ支援加工方法である。 As a technique for forming a microstructure on glass using a femtosecond laser, for example, a technique disclosed in Patent Document 1 is known. In this technique, a work material made of a transparent material such as silica glass is focused and irradiated with a pulse laser having a pulse duration of femtosecond to picosecond order, and the irradiation position of the pulse laser is determined. In the processing material, at least one place is scanned including the position on the surface of the processing material, and the portion of the processing material irradiated with the pulse laser is subjected to hydrofluoric acid or buffered hydrofluoric acid. It is a laser assisted processing method characterized in that it is removed by etching and used to form a hole.
しかしながら、特許文献１に係るレーザ支援加工方法では、微小構造、特に止まり穴のような構造を形成しようとする場合には、フッ化水素酸またはバッファードフッ酸によってエッチングを行った後の微小構造に、数度から十数度もの角度を有するテーパーが生じるという問題点があった。 However, in the laser-assisted processing method according to Patent Document 1, when a microstructure, particularly a structure such as a blind hole, is to be formed, the microstructure after etching with hydrofluoric acid or buffered hydrofluoric acid is used. In addition, there is a problem that a taper having an angle of several degrees to several tens of degrees occurs.
また、テーパーの角度はフッ化水素酸の濃度を低くすることにより、ある程度緩和することは可能である。しかし、フッ化水素酸の濃度を低下させると、微小構造の深さ方向へのエッチングの進行速度も低下するため、微小構造のエッチング工程にさらに多くの時間を要するという問題点があった。 The taper angle can be relaxed to some extent by reducing the concentration of hydrofluoric acid. However, when the concentration of hydrofluoric acid is reduced, the progress of the etching in the depth direction of the microstructure is also reduced, and there is a problem that more time is required for the etching process of the microstructure.
本発明は上記問題点に鑑みてなされたものであって、その目的とするところは、第１には、パルスレーザによる微小構造の加工において、微小構造に生じたテーパーの発生を抑え、深さ方向についてよりストレートな微小構造を形成することである。第２には、微小構造の深さ方向へのエッチングの進行速度がより速く効率的な、パルスレーザによるストレートな微小構造の形成方法を提供することである。 The present invention has been made in view of the above-mentioned problems. The object of the present invention is to suppress the generation of a taper generated in the microstructure in the processing of the microstructure by the pulse laser and to reduce the depth. It is to form a microstructure that is more straight in the direction. The second is to provide a method for forming a straight microstructure using a pulsed laser that is faster and more efficient in etching the microstructure in the depth direction.
本発明者は、深さ方向についてストレートな微小構造を効率よく形成するには、シリカガラスと被加工部分とのエッチングレートのバランスが重要であることを見出し、本発明を完成させた。 The present inventor has found that the balance of the etching rate between the silica glass and the part to be processed is important for efficiently forming a straight microstructure in the depth direction, and has completed the present invention.
すなわち、請求項１記載の発明は、シリカガラスにパルスレーザの集光照射を行ってパルスレーザの焦点近傍の該シリカガラスを改質させ、該パルスレーザまたは該シリカガラスを走査させながら改質させて該シリカガラスの表面を１ヶ所以上含んだレーザ改質領域を形成し、該レーザ改質領域をエッチングにより除去して該被加工物に微小構造を形成する方法において、該エッチングの工程で水酸化カリウム水溶液をエッチャントとして用いることを特徴とするシリカガラスへの微小構造の形成方法である。 That is, the invention according to claim 1 is characterized by modifying the silica glass near the focal point of the pulse laser by condensing and irradiating the silica glass with a pulsed laser, and modifying the silica laser while scanning the pulse laser or the silica glass. In the method of forming a laser modified region including at least one surface of the silica glass and removing the laser modified region by etching to form a microstructure on the workpiece, A method for forming a microstructure on silica glass, characterized in that an aqueous potassium oxide solution is used as an etchant.
請求項２記載の発明は、請求項１記載の構成に加えて、前記パルスレーザのパルス幅が、１ｐｓ以下であることを特徴とする、シリカガラスへの微小構造の形成方法である。 The invention described in claim 2 is a method for forming a microstructure in silica glass, in addition to the structure described in claim 1, wherein the pulse width of the pulse laser is 1 ps or less.
請求項３記載の発明は、請求項１〜２のいずれかに記載の構成に加えて、前記パルスレーザの波長が、該被加工物を透過する波長を有することを特徴とする、シリカガラスへの微小構造の形成方法である。 In addition to the structure in any one of Claims 1-2, invention of Claim 3 has the wavelength which the said pulse laser has a wavelength which permeate | transmits this workpiece, To silica glass characterized by the above-mentioned This is a method for forming a microstructure.
請求項４記載の発明は、請求項１〜３のいずれかに記載の構成に加えて、前記水酸化カリウム水溶液の濃度が０.１ｗｔ％〜５０ｗｔ％の間にあることを特徴とする、シリカガラスへの微小構造の形成方法である。 The invention according to claim 4 is characterized in that, in addition to the structure according to any one of claims 1 to 3, the concentration of the potassium hydroxide aqueous solution is between 0.1 wt% and 50 wt%. This is a method for forming a microstructure on glass.
本発明のシリカガラスへの微小構造の形成方法によれば、シリカガラスへのエッチャントとして通常用いられない水酸化カリウム水溶液を用いることにより、パルスレーザによって改質されたシリカガラスの改質領域を選択的にエッチングさせることができ、シリカガラスに形成される微小構造のテーパーの発生を抑えて、深さ方向についてストレートな微小構造を形成することができるという効果を奏する。 According to the method for forming a microstructure in silica glass of the present invention, a modified region of silica glass modified by a pulsed laser is selected by using an aqueous potassium hydroxide solution that is not normally used as an etchant for silica glass. Thus, it is possible to form a fine microstructure straight in the depth direction by suppressing the occurrence of a taper of the microstructure formed in the silica glass.
また本発明によれば、好ましい濃度及び液温の水酸化カリウム水溶液を用いることにより、微小構造の深さ方向へのエッチングの進行速度を飛躍的に高めることが出来るという効果を奏する。 Further, according to the present invention, by using a potassium hydroxide aqueous solution having a preferable concentration and liquid temperature, there is an effect that the progress of etching in the depth direction of the microstructure can be dramatically increased.
以下、本発明を実施するための最良の形態について説明する。本実施形態は、予め全面研磨を行ったシリカガラス１に対して、載置台２とパルスレーザ３、エッチング液槽５を用いた、微小穴，微小溝，微小凹み等の微小構造の形成方法である。 Hereinafter, the best mode for carrying out the present invention will be described. This embodiment is a method for forming a micro structure such as a micro hole, a micro groove, or a micro dent using a mounting table 2, a pulse laser 3, and an etching solution tank 5 on silica glass 1 that has been polished on the entire surface in advance. is there.
本実施形態に用いるパルスレーザ３は、加工閾値以上のレーザ強度を有している必要がある。具体的には、パルスレーザ３のパルス幅は１５０ｆｓ〜１ｐｓで、繰返し周期１ｋＨｚ〜３００ｋＨｚ、波長７８０ｎｍ〜８００ｎｍ、平均出力１Ｗ前後のものが使用可能である。しかしながら、微小構造の内面をより平滑にするためには、パルスレーザ３の繰返し周期を大きくして、レーザ強度は小さく抑えることが好ましい。 The pulse laser 3 used in the present embodiment needs to have a laser intensity equal to or higher than a processing threshold. Specifically, the pulse width of the pulse laser 3 is 150 fs to 1 ps, a repetition period of 1 kHz to 300 kHz, a wavelength of 780 nm to 800 nm, and an average output of about 1 W can be used. However, in order to make the inner surface of the microstructure more smooth, it is preferable to increase the repetition period of the pulse laser 3 and to keep the laser intensity small.
本発明に用いるパルスレーザとしては、１ｐｓ以下のパルス幅を持つパルスレーザが好ましい。なぜならば、パルス幅の短いレーザは１０ＴＷ／ｃｍ２以上のレーザ強度を有しており、シリカガラスが当該強度を有するパルスレーザを多光子吸収することで、シリカガラスの改質を引き起こすことができるためである。多光子吸収されたパルスレーザは熱拡散をほとんど起こさず、レーザ集光照射部近傍のみを改質させることができるため、本実施形態のような微小加工には非常に好適である。As the pulse laser used in the present invention, a pulse laser having a pulse width of 1 ps or less is preferable. This is because a laser with a short pulse width has a laser intensity of 10 TW / cm2 or more, and silica glass can cause modification of the silica glass by absorbing the multi-photon of the pulse laser having the intensity. Because. A multi-photon-absorbed pulse laser hardly causes thermal diffusion and can modify only the vicinity of the laser focused irradiation part. Therefore, it is very suitable for microfabrication like this embodiment.
また、シリカガラス内部での改質を空間選択的に起こすためには、パルスレーザの波長がシリカガラスを透過する波長であることが好ましい。なぜならば、シリカガラスにパルスレーザを照射する際に、使用するパルスレーザの波長がシリカガラスの固有吸収内であると、シリカガラスの表面でレーザの吸収が起こって当該部分が改質してしまうために、シリカガラス内部への加工を行う際の妨げになりやすいからである。 Further, in order to spatially selectively modify the inside of the silica glass, the wavelength of the pulse laser is preferably a wavelength that transmits the silica glass. Because, when irradiating the silica glass with the pulse laser, if the wavelength of the pulse laser used is within the intrinsic absorption of the silica glass, the absorption of the laser occurs on the surface of the silica glass and the part is modified. For this reason, it tends to be an obstacle when processing into the silica glass.
図１に示すように、本実施形態１に用いるシリカガラス１は、予め研磨を行い、載置台２に設置する。上記条件に適合したパルスレーザ３を、レンズ３ｂで集光してシリカガラス１に照射し、パルスレーザの焦点３ｃの近傍のシリカガラスの改質を行う。そして載置台をＸＹＺステージ等の手段により移動させて焦点３ｃを走査させながらシリカガラスの改質を行っていき、シリカガラス１の表面の少なくとも１ヶ所を含んだ所望の領域に、シリカガラス１の改質領域４を形成する。 As shown in FIG. 1, the silica glass 1 used in Embodiment 1 is previously polished and placed on the mounting table 2. The pulsed laser 3 conforming to the above conditions is condensed by the lens 3b and applied to the silica glass 1 to modify the silica glass near the focal point 3c of the pulsed laser. Then, the silica glass 1 is modified while moving the mounting table by means such as an XYZ stage and scanning the focal point 3c, and the silica glass 1 is placed in a desired region including at least one part of the surface of the silica glass 1. A modified region 4 is formed.
ここでパルスレーザ３による改質は、シリカガラス１に貫通穴等のようにシリカガラス１を貫通する微小構造を形成する場合は、シリカガラス裏面１ａを起点として、表側に向かって焦点を走査させて行うことが好ましい。一方で、止まり穴等のようにシリカガラス１を貫通しない微小構造を形成する場合は、シリカガラス１の加工領域のうち表側から最も深い部分を起点として、表側に向かって焦点を走査させて行うことが好ましい。その理由は、照射されたレーザが改質されたシリカガラスによって屈折・散乱してしまうことを防ぐためである。 Here, in the modification by the pulse laser 3, when a fine structure penetrating the silica glass 1 such as a through hole is formed in the silica glass 1, the focal point is scanned from the silica glass back surface 1a to the front side. It is preferable to carry out. On the other hand, when forming a minute structure that does not penetrate the silica glass 1 such as a blind hole, the focus is scanned toward the front side from the deepest part from the front side in the processed region of the silica glass 1. It is preferable. The reason is to prevent the irradiated laser from being refracted and scattered by the modified silica glass.
図２に示すように、シリカガラス１は、パルスレーザ３の集光照射後にエッチング槽５内に浸漬させ、シリカガラス１の改質領域４をエッチングにより除去する。エッチング層の中に入れるエッチャント６としては、水酸化カリウム水溶液を用いる。水酸化カリウム水溶液の濃度は、５０ｗｔ％のものから０.１ｗｔ％の希薄な水溶液まで適用可能である。５０ｗｔ％より大きい濃度の水酸化カリウム水溶液はシリカガラス１の未改質領域をエッチングし易く、この未改質領域のエッチングによってテーパーが生じるのを防ぐためである。 As shown in FIG. 2, the silica glass 1 is immersed in the etching tank 5 after the focused irradiation of the pulse laser 3, and the modified region 4 of the silica glass 1 is removed by etching. As the etchant 6 to be put into the etching layer, an aqueous potassium hydroxide solution is used. The concentration of the potassium hydroxide aqueous solution is applicable from 50 wt% to a dilute aqueous solution of 0.1 wt%. This is because the potassium hydroxide aqueous solution having a concentration of more than 50 wt% easily etches the unmodified region of the silica glass 1 and prevents the taper from being generated by the etching of the unmodified region.
また、エッチャント６である水酸化カリウム水溶液の液温は、２０℃から６０℃の範囲内、特に５０℃から６０℃の範囲内にあることが好ましい。なぜならば、エッチャント６の液温が６０℃より高いとシリカガラス１の未改質領域をエッチングし易くなり、逆にエッチャント６の液温が２０℃より低いと微小構造の深さ方向へのエッチングの進行が殆ど進行しなくなるからである。 The liquid temperature of the potassium hydroxide aqueous solution as the etchant 6 is preferably in the range of 20 ° C. to 60 ° C., particularly in the range of 50 ° C. to 60 ° C. This is because, when the liquid temperature of the etchant 6 is higher than 60 ° C., the unmodified region of the silica glass 1 is easily etched, and conversely, when the liquid temperature of the etchant 6 is lower than 20 ° C., etching in the depth direction of the microstructure is performed. This is because the progression of is hardly progressed.
エッチングにより改質領域４を除去したシリカガラス１から、付着した水酸化カリウム水溶液を洗浄等の手段により除去する。このようにして、微小穴，微小溝，微小凹み等の微小構造を有するシリカガラスが提供される。 The adhered potassium hydroxide aqueous solution is removed from the silica glass 1 from which the modified region 4 has been removed by etching, by means such as washing. In this way, silica glass having a microstructure such as a minute hole, a minute groove, and a minute dent is provided.
本発明を、以下の実施例を用いて詳細に説明する。
［実施例１］
本実施例は、本発明の実施形態における、テーパーを有する微小構造の形成方法に関するものである。サンプルとして全面研磨された合成シリカガラス基板５ｍｍ×５ｍｍ×３ｍｍを用いた。またレーザによるサンプル内部の改質には、パルス幅１５０ｆｓ、平均出力１Ｗ、繰返し周期２００ｋＨｚのフェムト秒レーザを用い、該シリカガラス基板に深さ２ｍｍ、直径８μｍのストレートなレーザ改質領域を形成した。The invention is explained in detail using the following examples.
[Example 1]
The present example relates to a method for forming a microstructure having a taper in the embodiment of the present invention. A synthetic silica glass substrate 5 mm × 5 mm × 3 mm polished on the entire surface was used as a sample. In addition, a femtosecond laser having a pulse width of 150 fs, an average output of 1 W, and a repetition period of 200 kHz was used to modify the inside of the sample with a laser, and a straight laser modified region having a depth of 2 mm and a diameter of 8 μm was formed on the silica glass substrate. .
ここでエッチャントとして３０ｗｔ％の水酸化カリウム水溶液を用いて２４時間エッチングを行った場合、エッチングされた微小構造の直径は１５μｍ、深さは６９６μｍとなり、テーパー角度は０．３８°となった。また、この微小構造の(a)表面及び(b)断面を光学顕微鏡により観察したところ、図３に示すとおりになった。 Here, when etching was performed for 24 hours using a 30 wt% potassium hydroxide aqueous solution as an etchant, the etched microstructure had a diameter of 15 μm, a depth of 696 μm, and a taper angle of 0.38 °. Further, when the (a) surface and (b) cross section of the microstructure were observed with an optical microscope, the microstructure was as shown in FIG.
［比較例１］
比較例として、従来シリカガラスへのエッチャントとして広く用いられていたフッ化水素酸を用いて、同様の微小構造形成工程を行った。実施例１と同様に、サンプルとして全面研磨された合成シリカガラス基板５ｍｍ×５ｍｍ×３ｍｍを用いた。またレーザによるサンプルの改質には、パルス幅１５０ｆｓ、平均出力１Ｗ、繰返し周期２００ｋＨｚのフェムト秒レーザを用い、該シリカガラス基板に深さ２ｍｍ、直径８μｍのストレートなレーザ改質領域を形成した。[Comparative Example 1]
As a comparative example, the same microstructure formation process was performed using hydrofluoric acid which has been widely used as an etchant for silica glass. As in Example 1, a synthetic silica glass substrate 5 mm × 5 mm × 3 mm polished on the entire surface was used as a sample. The sample was modified by a laser using a femtosecond laser having a pulse width of 150 fs, an average output of 1 W, and a repetition period of 200 kHz, and a straight laser modified region having a depth of 2 mm and a diameter of 8 μm was formed on the silica glass substrate.
該シリカガラス基板のエッチングには、１ｗｔ％のフッ化水素酸を用いて２４時間エッチングを行った。エッチングされた微小構造の直径は１５μｍ、深さは２０８μｍとなり、テーパー角度は１．９４°となった。また、この微小構造の(a)表面及び(b)断面を光学顕微鏡により観察したところ、図４に示すとおりになった。 The silica glass substrate was etched using 1 wt% hydrofluoric acid for 24 hours. The etched microstructure had a diameter of 15 μm, a depth of 208 μm, and a taper angle of 1.94 °. Further, when the (a) surface and (b) cross section of the microstructure were observed with an optical microscope, the microstructure was as shown in FIG.
１ シリカガラス
２ 載置台
３ パルスレーザ
３ａ パルスレーザ発光源
３ｂ レンズ
３ｃ 焦点
４ レーザ改質領域
５ エッチング槽
６ エッチャント
７ ヒータ
DESCRIPTION OF SYMBOLS 1 Silica glass 2 Mounting stand 3 Pulse laser 3a Pulse laser emission source 3b Lens 3c Focus 4 Laser modification area | region 5 Etching tank 6 Etchant 7 Heater
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| JP2004370268AJP4630971B2 (en) | 2004-12-21 | 2004-12-21 | Microstructure formation method using pulsed laser |
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| JP2004370268AJP4630971B2 (en) | 2004-12-21 | 2004-12-21 | Microstructure formation method using pulsed laser |
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| JP2006176355Atrue JP2006176355A (en) | 2006-07-06 |
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