JP2005306702A - Method of forming micro-hole having tapered shape - Google Patents
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本発明は、テーパー形状を有する微小穴の製造方法に関し、特に、石英ガラスへのパルスレーザの集光照射によって、石英ガラスを局所的に改質させ、その改質部分をエッチングにより除去する、テーパー形状を有する微小穴の形成方法に関する。 The present invention relates to a method of manufacturing a microscopic hole having a tapered shape, and in particular, a tapered glass in which quartz glass is locally modified by focused irradiation of a pulsed laser onto quartz glass, and the modified portion is removed by etching. The present invention relates to a method for forming a minute hole having a shape.
パルスレーザを用いて、材料にテーパーを有する穴を形成する手法としては、例えば特許文献１に示す技術が従来知られている。この方法は、材料の表面にパルス幅が１ｐｓ未満のパルスレーザ、すなわちフェムト秒レーザを集光照射することによって穴を形成するものであり、光路中にコーン形状レンズ対を導入し、これらの間隔を変化させることによってビーム強度を変化させ、穴のテーパー角度を制御するという手法である。 As a technique for forming a hole having a taper in a material using a pulse laser, for example, a technique disclosed in Patent Document 1 is conventionally known. In this method, a hole is formed by focusing and irradiating a pulse laser having a pulse width of less than 1 ps, that is, a femtosecond laser, on the surface of the material. This is a method of changing the beam intensity by changing the angle and controlling the taper angle of the hole.
また、特許文献２に係る従来技術によると、シリカガラスにフェムト秒レーザを照射してシリカの構造に変化を与え、その後にフッ酸やバッファードフッ酸によってエッチングを行い、穴を形成している。 Further, according to the prior art according to Patent Document 2, the silica glass is irradiated with a femtosecond laser to change the structure of the silica, and then etched with hydrofluoric acid or buffered hydrofluoric acid to form a hole. .
しかしながら特許文献１に係る技術においては、形成される穴の内周面は荒いものとなる。一般に、フェムト秒レーザのレーザアブレーションでは、パルス幅が極端に短いために、レンズにより集光すると、焦点付近ではレーザ強度が１０ＴＷ／ｃｍ↑２に達する。これにより焦点付近では、プラズマの発生を伴う材料の改質が極めて短時間で発生するが、テーパーを有する穴の内周面を鏡面レベルの平滑面にしたという報告は今までにない。また従来の、テーパーを有する穴の形成方法では、コーン形状レンズ対を導入するなど複雑な光学系を用いる上、これらの調整は困難であるという問題点があった。 However, in the technique according to Patent Document 1, the inner peripheral surface of the hole to be formed is rough. Generally, in laser ablation of a femtosecond laser, since the pulse width is extremely short, when focused by a lens, the laser intensity reaches 10 TW / cm ↑ 2 near the focal point. As a result, in the vicinity of the focal point, the material modification accompanied by the generation of plasma occurs in a very short time, but there has never been a report that the inner peripheral surface of the tapered hole has been made a smooth surface at a mirror surface level. Further, the conventional method for forming a hole having a taper has a problem that it is difficult to adjust these in addition to using a complicated optical system such as introducing a cone-shaped lens pair.
また、特許文献２に係る技術は、ストレートな穴の形成方法に関する技術であるが、形成された穴は、わずかにテーパーを有する形状であった。 Moreover, although the technique which concerns on patent document 2 is a technique regarding the formation method of a straight hole, the formed hole was a shape which has a taper slightly.
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には簡素な光学系を用いたレーザによる、テーパーを有する微小穴の加工において、微小穴に生じたテーパーの角度量を調節することである。第２には、鏡面レベルで平滑な内周面を有する、テーパーを有する微小穴を形成することである。 The present invention has been made in view of the above-mentioned problems, and the object of the present invention is first to occur in a minute hole in processing of a minute hole having a taper by a laser using a simple optical system. Adjusting the amount of taper angle. The second is to form a tapered microhole having a smooth inner peripheral surface at a mirror surface level.
請求項１記載の発明は、石英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石英ガラスを改質させ、該改質部分をエッチングにより除去して該被加工物に微小穴を形成する方法において、エッチャントであるフッ酸の濃度をＣ［ｗｔ％］、該改質部分の直径をＤ０［μｍ］、該改質部分の直径方向のエッチングレートをＥＤ［μｍ/ｈ］、該改質部分の長さ方向のエッチングレートをＥＬ［μｍ/ｈ］、非改質部分のエッチングレートをＥ０［μｍ/ｈ］、そして形成される微小穴の側面に生じるテーパー角度をθ［ｄｅｇ］とすると、Ｃとθ及びエッチング時間ｔ［ｈ］との関係が、以下の式で表されることを特徴とする、石英ガラスへの微小穴の形成方法である。 According to the first aspect of the present invention, the quartz glass is irradiated with focused laser light to modify the quartz glass in the vicinity of the focal point of the pulse laser, and the modified portion is removed by etching so that the work piece is minutely formed. In the method of forming a hole, the concentration of hydrofluoric acid as an etchant is C [wt%], the diameter of the modified portion is D 0 [μm], and the etching rate in the diameter direction of the modified portion is E D [μm / h], the etching rate in the length direction of the modified portion is E L [μm / h], the etching rate of the non-modified portion is E 0 [μm / h], and the taper generated on the side surface of the formed microhole When the angle is θ [deg], the relationship between C, θ, and etching time t [h] is expressed by the following equation, and this is a method for forming a microhole in quartz glass.
形成される微小穴は、石英ガラス表面と内部のエッチングの時間差と、改質部分と非改質部分のエッチング速度の違いにより、表面の直径が大きく中心の直径が小さい、テーパー形状の微小穴が形成される。 Due to the difference in etching time between the quartz glass surface and inside, and the difference in etching rate between the modified part and the non-modified part, the formed microhole is a tapered microhole with a large surface diameter and a small central diameter. It is formed.
ここで、濃度Ｃ[ｗｔ％]のフッ酸を用いた場合のエッチングレートは、微小穴の直径が石英ガラスの改質部分の直径Ｄ０［μｍ］よりも小さいうちは、改質部分の直径方向のエッチングレートＥＤ［μｍ/ｈ］となる。一方、改質部分がエッチングにより除去され、微小穴の直径がＤ０より大きくなると、フッ酸は未改質部分のエッチングを行うため、エッチングレートはＥＤよりも小さいＥ［μｍ/ｈ］となる。すなわち、各々の場合の微小穴の直径Ｄ［μｍ］とＥＤ、Ｅ、Ｃおよび時間ｔ［ｈ］との関係は、微小穴の直径Ｄ0である時の時間ｔ＝Ｄ０／ＥＤ（Ｃ）［ｈ］を境にして、以下のように表される。 Here, the etching rate in the case of using hydrofluoric acid having a concentration of C [wt%] is as long as the diameter of the minute hole is smaller than the diameter D 0 [μm] of the modified portion of the quartz glass. The etching rate E D in the direction is [μm / h]. On the other hand, modified portion is removed by etching, the diameter of the minute hole is greater than D 0, hydrofluoric acid for etching the unmodified portion, the etching rate is smaller E [μm / h] than E D Become. That is, the diameter D [[mu] m] and E D of the micro holes in each case, E, relation between the C and the time t [h], the time t = D 0 / E D when the diameter D 0 of the minute hole (C) Expressed as follows, with [h] as the boundary.
一方、エッチングで形成される微小穴の深さは、レーザ照射部の深さ方向のエッチングレートＥＬ［μｍ/ｈ］より求められ、微小穴の深さＬ［μｍ］とｃ、ｔ[ｈ]との関係は、以下のように表される。 On the other hand, the depth of the minute hole formed by etching is obtained from the etching rate E L [μm / h] in the depth direction of the laser irradiation portion, and the depth L [μm] of the minute hole and c, t [h] ] Is expressed as follows.
ここで、上記のＤ，Ｌとテーパー角度θは、幾何的に以下の式により求められる。 Here, the above D and L and the taper angle θ are obtained geometrically by the following equations.
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、石英ガラスへの微小穴の形成方法である。 According to a second aspect of the present invention, in addition to the configuration of the first aspect, the pulse width of the pulse laser is 1 ps or less, and the method for forming a microhole in quartz glass.
本発明に用いるパルス幅の短いレーザ、特に１ｐｓ以下のパルス幅を持つパルスレーザでは、１０ＴＷ／ｃｍ２以上のレーザ強度を容易に実現できる。このようなパルスレーザを用いるとき、石英ガラスにおいてパルスレーザの多光子吸収が生じ、石英ガラスの改質を引き起こすことができる。またパルス幅が極端に短いために、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。 With a laser having a short pulse width used in the present invention, particularly a pulse laser having a pulse width of 1 ps or less, a laser intensity of 10 TW / cm 2 or more can be easily realized. When such a pulse laser is used, multiphoton absorption of the pulse laser occurs in the quartz glass, which can cause modification of the quartz glass. Further, since the pulse width is extremely short, the pulsed laser that has absorbed multiphotons hardly causes thermal diffusion, and only the vicinity of the laser focused irradiation part can be modified.
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、石英ガラスへの微小穴の形成方法である。 According to a third aspect of the present invention, in addition to the structure of the first or second aspect, the wavelength of the pulse laser has a wavelength that transmits the workpiece. This is a method of forming a microhole.
石英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石英ガラスの固有吸収内であると、石英ガラスの表面でレーザの吸収が起こり、改質が行われて、石英ガラス内部への加工を行う際の妨げになりやすい。したがって、石英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石英ガラスを透過する波長であることがより好ましい。 When irradiating the quartz glass with a pulsed laser, if the wavelength of the pulsed laser used is within the intrinsic absorption of the quartz glass, the laser will be absorbed on the surface of the quartz glass, and the modification will be carried out. It tends to be a hindrance when performing the processing. Therefore, in order to cause spatial modification selectively in the quartz glass, it is more preferable that the wavelength of the pulse laser is a wavelength that transmits the quartz glass.
本発明の石英ガラスへの微小穴の形成方法によれば、エッチング液の濃度を選択することにより、石英ガラスに形成される微小穴のテーパー角度をコントロールできるため、テーパー量のコントロールを光学系に委ねる必要がなくなる。これにより、簡素な光学系を用いたレーザ加工で、微小穴に生じたテーパーの角度量を調節することが出来るという効果を奏する。 According to the method for forming microholes in the quartz glass of the present invention, the taper angle of the microholes formed in the quartz glass can be controlled by selecting the concentration of the etching solution. There is no need to leave it. Thereby, there is an effect that the angle amount of the taper generated in the minute hole can be adjusted by laser processing using a simple optical system.
また本発明によれば、平均面粗さＲａが５ｎｍ未満の、非常に平滑な内面を有する、テーパーを有する微小穴を得ることができるという効果を奏する。 Moreover, according to this invention, there exists an effect that the micro hole which has a very smooth inner surface whose average surface roughness Ra is less than 5 nm, and has a taper can be obtained.
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石英ガラス１に対して、載置台２とパルスレーザ３、エッチング液槽４を用いた、テーパーを有する微小穴の形成方法である。 Hereinafter, the best mode for carrying out the present invention will be described. The present embodiment is a method for forming a microscopic hole having a taper using a mounting table 2, a pulse laser 3, and an etching solution tank 4 with respect to quartz glass 1 which has been polished on the whole surface in advance.
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〜２５０ｋＨｚ、波長８００ｎｍ前後、平均出力１Ｗ前後のものが使用可能である。しかしながら、エッチング速度の制御をより精密にして、テーパーを有する微小穴を安定的に形成するためには、またテーパーを有する微小穴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 250 kHz, a wavelength of about 800 nm, and an average output of about 1 W can be used. However, in order to make the control of the etching rate more precise and form a tapered microhole stably, and to make the inner surface of the tapered microhole more smooth, the repetition period of the pulse laser 3 It is preferable to keep the laser intensity small by increasing.
図１に示すように、本実施形態１に用いる石英ガラス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で集光して石英ガラス１に照射し、パルスレーザの焦点３ｃの近傍の石英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を走査させることで、石英ガラス１の表面の少なくとも１ヶ所を含んだ所望の領域に、石英ガラス１の改質領域４を形成する。ここでパルスレーザ３による改質は、石英ガラス裏面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。その理由は、改質された石英ガラスによるレーザの屈折・散乱を防ぐためである。 As shown in FIG. 1, the quartz 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 irradiated onto the quartz glass 1 to modify the quartz glass near the focal point 3c of the pulsed laser. Then, by moving the mounting table by means such as an XYZ stage and scanning the focal point 3c, the modified region 4 of the quartz glass 1 is formed in a desired region including at least one place on the surface of the quartz glass 1. Here, the modification by the pulse laser 3 is preferably performed by scanning the focal point from the quartz glass back surface 1a to the front side. The reason is to prevent laser refraction and scattering by the modified quartz glass.
石英ガラス１はパルスレーザ３の集光照射後、エッチング槽４内に浸漬させる。エッチング層の中は、数式１で求められる濃度のフッ酸水溶液を用いる。フッ酸水溶液の濃度は、１０ｗｔ％のものから０.１ｗｔ％の希薄な水溶液まで適用可能である。エッチングは石英ガラス１の表面の改質部分から内部に進行していくが、石英ガラスの表面と内部とのエッチングの時間差が生じるため、またパルスレーザ３による改質部分４のエッチング速度は非改質部分に比べて速いため、表面の直径よりも中心の直径が小さい、テーパー形状の微小穴が形成される。 The quartz glass 1 is immersed in the etching tank 4 after the focused irradiation of the pulse laser 3. In the etching layer, a hydrofluoric acid aqueous solution having a concentration calculated by Equation 1 is used. The concentration of the hydrofluoric acid aqueous solution is applicable from 10 wt% to a dilute aqueous solution of 0.1 wt%. Etching proceeds from the modified portion on the surface of the quartz glass 1 to the inside. However, the etching time difference between the surface and the inside of the quartz glass occurs, and the etching rate of the modified portion 4 by the pulse laser 3 is not modified. Since it is faster than the quality part, a tapered microhole having a central diameter smaller than the surface diameter is formed.
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穴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石英ガラス１０ｍｍ×１０ｍｍ×４ｍｍ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、石英ガラスに改質部分を形成した。
The present example relates to a method for forming a microhole having a taper in the embodiment of the present invention. Synthetic quartz glass 10 mm × 10 mm × 4 mm polished on the entire surface was used as a sample. Further, for the modification inside the sample by a laser, a modified portion was formed in quartz glass using a femtosecond laser having a pulse width of 150 fs, an average output of 1 W, and a repetition period of 200 kHz.
ここでエッチャントとして１０ｗｔ％，１ｗｔ％，０.１ｗｔ％のフッ酸水溶液を用いた場合、テーパー角度の制御は、±０.０５°以内の高い再現性を有していた。ここで上記方法により形成した、直径１１１μｍ，テーパー角度１０.４°の微小穴の断面を露出させ、その断面を走査型電子顕微鏡（ＳＥＭ）により観察し、内面粗度を原子間力顕微鏡（ＡＦＭ）により評価を行った。このときの電子顕微鏡像及び原子間力顕微鏡像はそれぞれ、図２及び図３に示すとおりになった。そして、断面の平均面粗さＲａは５ｎｍとなり、微小穴の表面は非常に平滑となった。 Here, when 10 wt%, 1 wt%, and 0.1 wt% hydrofluoric acid aqueous solution was used as the etchant, the control of the taper angle had high reproducibility within ± 0.05 °. Here, a cross-section of a microhole having a diameter of 111 μm and a taper angle of 10.4 ° formed by the above method is exposed, the cross-section is observed with a scanning electron microscope (SEM), and the inner surface roughness is measured by an atomic force microscope (AFM). ). The electron microscope image and the atomic force microscope image at this time were as shown in FIGS. 2 and 3, respectively. The average surface roughness Ra of the cross section was 5 nm, and the surface of the microhole was very smooth.
本実施例は、請求項１における数式からの、具体的な数値の導出に関するものである。実施例１と同様に、サンプルとして全面研磨された合成石英ガラス１０ｍｍ×１０ｍｍ×４ｍｍ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、石英ガラスに改質部分を形成した。 The present embodiment relates to the derivation of specific numerical values from the mathematical expression in claim 1. As in Example 1, a synthetic quartz glass 10 mm × 10 mm × 4 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 modified portion was formed in quartz glass.
石英ガラスのエッチングには、１.５ｗｔ％のフッ酸を用いた。この時、直径Ｄ＝８μｍの改質部分へのエッチングによる微小穴の直径・深さの経時変化は、例えば図５・図６のように示された。これらの関係から、該改質部分の直径方向のエッチングレートＥＤ（１.５）＝６.４、該改質部分の長さ方向のエッチングレートＥＬ（１.５）＝３２、非改質部分のエッチングレートＥ（１.５）＝０.６７と求められた。この値を請求項１の公式にあてはめることにより、θとｔの関係を表す近似式は、ｔ＝１.２５［ｈ］を境にして、以下のように求められた。 For etching quartz glass, 1.5 wt% hydrofluoric acid was used. At this time, the time-dependent changes in the diameter and depth of the microhole due to the etching into the modified portion having the diameter D = 8 μm are shown in FIGS. 5 and 6, for example. From these relationships, the etching rate E D (1.5) = 6.4 in the diameter direction of the modified portion, the etching rate E L (1.5) = 32 in the length direction of the modified portion, The etching rate E (1.5) of the quality part was determined to be 0.67. By applying this value to the formula of claim 1, an approximate expression representing the relationship between θ and t was obtained as follows with t = 1.25 [h] as a boundary.
本発明のテーパーを有する微小穴は、非常に平滑な内面をもつ微小径の穴であるため、その内部に流体を流すことも可能で、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への適用が可能である。 The tapered micro-hole of the present invention is a micro-diameter hole with a very smooth inner surface, so it is possible to allow fluid to flow through it and can be applied to micro nozzles, biochips, chemistry chips, etc. It is.
１ 石英ガラス
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 改質部分
DESCRIPTION OF SYMBOLS 1 Quartz glass 2 Mounting stand 3 Pulse laser 3a Pulse laser emission source 3b Lens 3c Focus 4 Modified part
Claims (3)
パルスレーザの焦点近傍の石英ガラスを改質させ、
該改質部分をエッチングにより除去して該被加工物に微小穴を形成する方法において、
エッチャントであるフッ酸の濃度をＣ［ｗｔ％］、
該改質部分の直径をＤ０［μｍ］、
該改質部分の直径方向のエッチングレートをＥＤ［μｍ/ｈ］、
該改質部分の長さ方向のエッチングレートをＥＬ［μｍ/ｈ］、
非改質部分のエッチングレートをＥ０［μｍ/ｈ］、
そして形成される微小穴の側面に生じるテーパー角度をθ［ｄｅｇ］とすると、
Ｃとθ及びエッチング時間ｔ［ｈ］との関係が、
で表されることを特徴とする、石英ガラスへの微小穴の形成方法。 Condensed irradiation of pulsed laser on quartz glass,
The quartz glass near the focal point of the pulse laser is modified,
In the method of removing the modified portion by etching to form a microhole in the workpiece,
The concentration of hydrofluoric acid as an etchant is C [wt%],
The diameter of the modified portion is D 0 [μm],
The etching rate in the diameter direction of the modified portion is E D [μm / h],
The etching rate in the length direction of the modified portion is E L [μm / h],
The etching rate of the unmodified portion is E 0 [μm / h],
Then, if the taper angle generated on the side surface of the formed microhole is θ [deg],
The relationship between C, θ, and etching time t [h] is
A method for forming microholes in quartz glass, characterized by:
The method for forming a microhole in quartz glass according to any one of claims 1 to 2, wherein the wavelength of the pulse laser has a wavelength that transmits the workpiece.
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