EP1999498A1 - Composants optiques antireflets à large bande avec surfaces incurvées et leur procédé de fabrication - Google Patents

Composants optiques antireflets à large bande avec surfaces incurvées et leur procédé de fabrication

Info

Publication number
EP1999498A1
EP1999498A1 EP07727292A EP07727292A EP1999498A1 EP 1999498 A1 EP1999498 A1 EP 1999498A1 EP 07727292 A EP07727292 A EP 07727292A EP 07727292 A EP07727292 A EP 07727292A EP 1999498 A1 EP1999498 A1 EP 1999498A1
Authority
EP
European Patent Office
Prior art keywords
silicon
needle
structures
optical device
optical component
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.)
Withdrawn
Application number
EP07727292A
Other languages
German (de)
English (en)
Inventor
Konrad Bach
Daniel Gaebler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
X Fab Semiconductor Foundries GmbH
Original Assignee
X Fab Semiconductor Foundries GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by X Fab Semiconductor Foundries GmbH filed Critical X Fab Semiconductor Foundries GmbH
Publication of EP1999498A1 publication Critical patent/EP1999498A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/118—Anti-reflection coatings having sub-optical wavelength surface structures designed to provide an enhanced transmittance, e.g. moth-eye structures
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings

Definitions

  • the present invention generally relates to manufacturing methods and curved-surface optical components having a refractive power (a positive or negative refractive power for incident light rays).
  • the light is in a given wavelength range, with the invention, an anti-reflection of the optically active surface (the curved surface) is to be achieved.
  • Antireflective optically effective, curved surfaces which thus produce a negative or positive bundling effect for light rays impinging on the surface, has been causing problems since the emergence of the first antireflection coatings at the beginning of the 20th century.
  • Antireflective coatings based on the interference phenomena require homogeneous properties of the applied layers, in particular, the thicknesses must be carefully matched. All known processes that produce this type of antireflective coating are affected by this problem.
  • Another problem is the adhesive strength of the applied layers and the effectiveness over an often very limited wavelength range. Only complicated coating systems enable antireflection over a larger wavelength range.
  • Corresponding layer systems make very high demands on the layer homogeneity and tend to reduce the adhesive strength by the combination of the mechanical layer stresses that occur.
  • layer materials are not suitable for every wavelength range.
  • Electronic, opto-electronic, sensory or micromechanical components often have as integral components optical components which require curved surfaces for processing optical signals, the overall efficiency of these optical components being very much dependent on the proportion of the radiation component coupled into the surface.
  • Efficient antireflection coating is also important in these cases, whereby the compatibility of the processes for producing the antireflection coatings with the further integration processes is also an important aspect.
  • the complex structures of the conventional anti-reflection structures lead to complex and thus costly production steps, whereby a broadband effect of the anti-reflection layers is nevertheless rarely achieved. Overview of the invention.
  • the invention is based on the object for optical components with curved surfaces, as they occur as components of optoelectronic integrated circuits, as individual components or as purely optical components of devices to specify such an expression of the surface, creating a significantly reduced reflection over a wide (or: wide) wavelength range is achieved.
  • a layer is produced on a base material with a curved surface, which produces an almost gradual adjustment of the refractive index of the base material into the surrounding medium, at least for the light wavelength range considered, without complex layer systems being required and the desired "globally curved" geometry the surface of the base material is maintained.
  • a self-organizing etching process which can act directly on the surface when it is composed essentially of silicon, or which can be used to produce a suitable structure in other base materials.
  • a reactive plasma atmosphere having at most two different gas components with oxygen and a reactive gas for etching silicon is produced by setting process parameters which develop a self-masking effect for producing a nanostructure. The etching takes place without further working gases and is carried out as a one-step process.
  • the silicon surface is exposed to the action of the etching plasma without any further process steps taking place; in particular, no further measures are necessary to achieve a targeted micro-masking of the silicon surface.
  • practical "freedom from defects" is achieved, in the sense that substantially no additional defects, such as in the form of etch by-products, are produced by the reactive plasma.
  • crystal defects are substantially avoided, whereby the semiconductor properties are not changed by the etching process, if this is important for the further production of the curved surface.
  • this structure serves as a basis for the production of the surfaces of other base materials, these advantageous properties can also be utilized for the steps required for this purpose.
  • the production of a stencil on the basis of microstructuring processes well known for crystalline silicon An efficient adjustment of the refractive index in the curved surfaces is achieved by adjusting the aspect ratio of the reactive plasma atmosphere resulting needle-like structures to a value of 4 or greater by controlling the process time, wherein a masking of the silicon surface, whether by photoresist or other substances such Aluminum, gold, titanium, polymers, water, or any surface contaminants, etc. is not required.
  • the needle-like structures produced have a form which is best suited for use on curved surfaces in the visible light and also in the infrared range.
  • the shape of the needle-like structures produced by the self-organized masking of the etching also has a "pyramid-like" shape in addition to the aspect ratio of greater than 4, resulting in a very tapered needle end, whereas at the foot of the above needle-like tapered shape, a relatively flat leaking region is created can be, the shallow ends.
  • the lateral dimensions increase significantly toward the foot. Between the circumscribed pyramid-like structures with needle tip remains a clear distance, at least 50 nm, so that in spite of high needle density too close to each other standing needles are prevented. Such too dense needles would converge to a larger entity and bring the etching process to a halt here.
  • the forms specified with the given circumscriptions are not all the same, but in the mean and in the statistical distribution they have regular and individually sharply demarcated forms. Nevertheless, their density distribution results in about 50 "pyramid-like needles" per square micrometer, in any case well below 100 needles per micron 2 , with a height of the pyramid-like needles of above 400 nm, especially in the range around 500 nm and at about the same depth of a gap between the pyramid-like needles. Between adjacent such needles of at least 50 nm wide gap remains, the first at the bottom of the pyramid-like course, where the foot area relatively flat, runs down almost shallow, converges.
  • the pyramid should not be understood as having only four pages; even more pages are possible as well, up to a versatile pyramidal shape and towards an approximately round shape in cross section.
  • a profilometer needle of the profilometer exerts a pressure between 0.1 and 10 mg on the sample to be measured (the nano-surface with the pyramidal needles).
  • the profilometer needle is very pointed, but increases in diameter quickly, so that when moving on a sample a 5 ⁇ m deep well with a width of 1 micron can not be resolved exactly in the measurement image.
  • a pressure of typically 5 mg and a movement of the profilometer needle at a rate of up to 100 ⁇ m / sec on the nanostructure no adverse effect on the reflection properties of the nanostructure was observed, as would occur if the pyramidal needle structure were destroyed.
  • the (total) reflection is below 0.7% for a wavelength range between 400 nm and about 800 nm (scattered and direct reflection). In an extended range between 180 nm and 3000 nm, the (total) reflection is below 2%, with practically only the scattered reflection contributing. Reflection is a physical property of the nanostructure that is reproducible, measurable, and comparable to another structure. Without intending to limit the invention by the following discussion, studies suggest that efficient self-organized masking (as "self-marking”) is achieved by the etching process itself rather than by existing or specially added materials.
  • the structures produced by the method show no edge shading at high edges. It is thus possible, for example, to structure surfaces of a few ⁇ m, even if the surface is enclosed by a 5 ⁇ m high structure, so that great flexibility results in the production of corresponding curved surfaces of optical components and the positioning of the refractive index matching layer thereon.
  • the structuring of the silicon is done by the plasma in the RIE process. These structures are deepened by the etching process, resulting in the structures in the nanometer range with enormous aspect ratios.
  • the structure thus produced has a low-defect nanostructure surface, which can be produced on the base material of the optical component.
  • a height of the free-standing pyramid-like needles is at least 400 nm and a gap of at least 50 nm. The height is between 400 nm and 1000 nm, which can be read from images of the electron beam microscope image, as described in more detail below.
  • the pictorial representation is intended to replace a limited possible structural description of the pyramid-like needles and their environment. For comparison, reference may be made to the John Hancock Center in Chicago, which is about 350m high, slightly pyramid-like, and has a lateral foot measurement (with no shallow, relatively shallow leakage) of about 85m.
  • This structure is constructed in a reduced by a factor of 10 9 form in, for example, silicon, often side by side and difficult to visualize on this scale with the current imaging techniques and clearly described. On the one hand, this task is not simple, but on the other hand, it is essentially fulfilled by measuring and presenting the effects of these structures.
  • Claimed is a method for producing an optical component.
  • the production of a globally curved surface takes place in a base material. Due to the (globally) curved shape, rays of light incident on the curved surface are changed in their propagation direction, in the sense of refraction. The rays of light also enter the curved surface.
  • a refractive index adjusting layer is formed with a nanometer structure in the base material. This preserves the global curvature of the surface.
  • the adaptation layer is formed using the described process. Includes are
  • the gas components are oxygen and a reactive gas for etching silicon, without an intermediate step. In particular, no further gas components are involved.
  • the aspect ratio of the needle-like structures formed in the plasma atmosphere is set to a value of at least four.
  • the base material of the optical component may be directly silicon (claims 19 to 26, claims 10 to 13), which may be further treated as needed after patterning, e.g. At least partially converted to oxide, or from needle-like silicon structures, layers can be made by molding, so that these structures then allow a gradual refractive index transition in a variety of materials.
  • the base material can also simultaneously obtain its global surface curvature by molding (claim 5), thus providing a great flexibility in the selection of materials and an efficient manufacturing method for the antireflection of the curved surfaces.
  • the surface structure according to the invention for globally curved geometries can therefore be used in a large number of possible components, for example optoelectronic circuits (claim 15, 22, 31), but also in absorption elements for control and measurement purposes (claim 23, 32), whereby almost all incident on the curved surface light intensity can be absorbed and thus detected.
  • a significant increase in the efficiency of components can be achieved, which are designed for a radiation (claim 33), such as a lens, wherein one or both surfaces can be effectively anti-reflection.
  • the temperature of the silicon wafer and the ratio of the working gases at the reaction point on the silicon surface are suitably adjusted.
  • the temperature of the silicon surface is set at 27 ° C., preferably in the range ⁇ 5 ° C.
  • process pressure and plasma power are properly matched as set forth in the following description to obtain the desired aspect ratio while reducing the rate of contamination and low crystal defect density.
  • the ratio of not more than two working gases is adjusted so that etching removal and self-masking balance each other out. This ensures both the structuring and the required freedom from defects (no additional defects due to the etching regime).
  • the absolute parameter values can be efficiently adjusted to the proportion of the open (or free) silicon surface which serves as the basis for the curved surface design. If the Si surface is covered to a high surface area by a mask layer, for example oxide or silicon nitride, since for example only certain areas of the surface or a template should receive a corresponding needle structure, this can be achieved at least by increasing the reactive gas content, for example the SF 6 share, be compensated, especially if the SF 6 simultaneous reduction of oxygen content and simultaneous increase of process pressure.
  • a mask layer for example oxide or silicon nitride
  • Another suitable method comprises generating a reactive plasma atmosphere with oxygen and a reactive gas consisting of a mixture of HCl and BCI3, for etching silicon without further process steps by setting process parameters that have a self-masking effect to produce a nanostructure with needle-like structures unfold. Also in this case, a self-organizing masking effect can be achieved so that the above-described properties (or shapes) of the nanostructures are obtained.
  • a nanoscale nanostructure comprising randomly distributed monocrystalline needle-like silicon structures formed on a monocrystalline silicon base layer, wherein the aspect ratio of the needle-like silicon structures is 4 or greater, and the crystal defect density in the silicon structures is not higher is as is in the silicon base layer.
  • These structures may then be further processed as needed, as previously described, to produce the curved surface finish therefrom.
  • the nanostructure which thus has silicon structures with lateral dimensions that are typically below the wavelength of visible light, can thus be used efficiently as a layer in devices in which a gradual change in the refractive index between silicon or other base material and a, the medium surrounding the base material is desired. On In this way, an adjustment of the refractive index between the base material and the medium is achieved. As a result, the reflection behavior and / or the transmission behavior of optoelectronic components provided with curved surfaces to achieve the desired optical effect can be significantly improved.
  • the object of the invention has, inter alia, the advantages that a broadband anti-reflection is achieved with curved silicon surfaces or other optically active surfaces, wherein, if silicon is the base material, no material needs to be applied, but only the surface is modified. There are no adhesion problems, no layer stresses and no restrictions in the optical wavelength range.
  • the antireflection coating also has the advantage that the direct reflection is significantly lower than the scattered reflection and thus can be suppressed by suitable measures (apertures, dark frames, etc.) in their effects.
  • the excellent homogeneity of the antireflective coating over a large area minimizes the control effort for finished components enormously. For example, for microlens arrays not every lens has to be measured individually.
  • the described RIE silicon etching process is used.
  • the generated structures can be converted by an oxidation of silicon into oxide, whereby the anti-reflection is also applicable to curved oxide surfaces.
  • Other surface processes, such as nitriding or other treatments can be carried out without problems after the generation of the needle-like structure.
  • the produced silicon or oxide nanostructure in the curved surface can also be transferred by molding to other materials, for example to produce a stamping tool for other materials.
  • Fig. 1 is an electron micrograph of a RIE etched
  • 2 is an electron micrograph with an obliquely incident electron beam, from which the homogeneity of the distribution of the silicon needles and the depth of the spaces between the needles are visible,
  • FIG. 3 a shows the receptacle from FIG. 3 turned so that the [001] direction is vertical
  • FIG. 4 a shows the electron micrograph of FIG. 2 with an obliquely incident electron beam, from which the homogeneity of the distribution of the silicon needles and the depth of the interspaces between the needles are visible, here a left-hand section, FIG.
  • 4b shows the electron micrograph of FIG. 2 with obliquely incident electron beam, from which the homogeneity of the distribution of the silicon needles and the depth of the interspaces between the needles are visible, here an intermediate section,
  • 4c shows the electron micrograph of FIG. 2 with an obliquely incident electron beam, from which the homogeneity of the distribution of the silicon needles and the depth of the interspaces between the needles are visible, here a right section,
  • FIG. 5 shows the electron micrograph of FIG. 2 with an obliquely incident electron beam, from which the homogeneity of the distribution of the silicon needles and the depth of the interspaces between the needles are visible, here a front section
  • 6 shows the electron micrograph of FIG. 2 with obliquely incident electron beam, from which the homogeneity of the distribution of the silicon needles and the depth of the interspaces between the needles are visible, here completely,
  • FIG. 7 shows corresponding results of reflection of light on a curved surface with an anti-reflection layer, which is produced on the basis of a needle-like structure, as also shown in the preceding figures, FIG.
  • FIG. 8b shows the curved-surface optical component after forming a needle-like nanostructure
  • FIG. 1 shows a silicon-containing component 1 with a nanostructure 2 which has a monocrystalline silicon base layer 3 on which needle-like silicon structures 4 are formed.
  • needle-like silicon structures are to be understood as "pyramid-like" structures that have a tip with lateral dimensions of a few nanometers, wherein the tip increases significantly downwards in its lateral dimension, so that in the lower part of the structure has a lateral dimension of some ten nanometers or up to 100 nm is achieved.
  • the silicon base layer 3 is limited in this embodiment by a mask layer 5, which may be composed of silicon dioxide, silicon nitride or the like, wherein the needle-like silicon structures 4 are formed up to an edge region 5 a of the mask layer 5.
  • the silicon base layer 3 is a part of a 6 inch diameter silicon wafer with a (100) surface orientation that has a p-type doping giving a resistivity of 10 ohm.cm.
  • the base layer 3 may have any desired crystal orientation with any predoping.
  • the base layer 3 may be formed substantially of amorphous or polycrystalline silicon.
  • FIG. 2 shows an enlarged section of the nanostructure 2, wherein the angle of incidence of the probing electron beam is irradiated with an inclination angle of approximately 17 ° in order to more clearly show the size relationships in the lateral direction and in the height or thickness direction of the pyramidal structures 4.
  • the silicon structures 4 have a height which is on average about 1000 nm, so that in some embodiments a height is reached which is greater than the wavelengths of visible light.
  • the scale with 2 microns 10 scale parts are plotted in Figure 2. In Figure 1, it is 500 nm per scale part.
  • the height entered as a measure in FIG. 2 is to be converted from 603 nm to the real height. It is also possible to convert the vertical extent by up to 60% for lower pyramid-like needles, which achieve their effects from about 400 nm. This is done by compression of Figure 2 in the height direction to 40% of the height shown. But also pyramid-like structures 4 with a mean height in the range of 400 nm show excellent optical properties in many applications. Thus, for example, for an average height of 400 nm, excellent antireflection in the visible wavelength range and up to 3000 nm was observed.
  • a mean maximum height of the silicon structures 4 can also be substantially 1000 nm.
  • FIGS. 1 and 2 show that the lateral dimension of the silicon structures (at the foot) is less than 100 nm or a few tens of nanometers (significantly less), so that on average an aspect ratio of height to lateral dimension of 4 or higher is achieved becomes.
  • Si slice temperature 27 degrees Celsius
  • Plasma power 100 W
  • Self-adjusting BIAS DC potential between the plasma atmosphere and the surface to be etched: varies by 350 V.
  • process time of up to 20 min is also useful. Then the process results in an extremely high-quality antireflective coating of the surface nanostructured with the needles.
  • gas flow rates were between 50 sccm for the reactive gas, so SF 6, C n F m or HCl / BCl 3 provided to 150 bar.
  • oxygen gas flow rates 20 to 200 sccm are provided.
  • the temperature of the substrate, and thus the base layer 3 is set to a range of 27 ° C ⁇ 5 ° C.
  • corresponding parameter values for other etching systems and other degrees of coverage of the silicon base layer 3 to be structured with the pyramidal structures can be determined. For example, a lower coverage of the silicon base layer due to a lower gas flow rate of the reactive gas.
  • the Si needles 4 having a height of about 1000 nm were generally randomly distributed at the areas not masked by the mask layer 5.
  • the mask layer 5 e.g. Silicon oxides or silicon nitrides.
  • Machined disks with similar structures become completely black and showed a reflection of less than 0.4% for the wavelength range of 400 nm to 1000 nm, at the same time excellent homogeneity of this property over the entire wafer (disk).
  • the investigations showed a still excellent anti-reflection behavior with reflections below 2%. The reflections recorded here (practically only) the reflections in all solid angles.
  • the crystal damage caused by the plasma-assisted single-stage structuring process and the contamination are very low and are below the detection limit in the exemplary embodiments shown. No residual substances could be detected after the plasma structuring process and the crystal quality of the silicon structures is almost identical to the crystal quality of the silicon base layer before the etching process.
  • the needle sections of the pyramid-like needles are almost atomically pointed at their end 4a.
  • the lateral dimensions of the end 4a are only a few nanometers.
  • individual network planes (111) of the monocrystalline needle section can be clearly seen without crystal defects caused by the etching being recognizable.
  • FIG. 3 shows, from a pyramid-like needle 4, a single tip 4a or an end region with this tip 4a.
  • the needles are almost atomically pointed at their end 4a, ie, the lateral dimensions of the end 4a are only a few nanometers and are thus smaller than 10 nm.
  • the crystal direction is also perpendicular to Surface of the silicon base layer 3 registered. This direction corresponds to a [001] direction, since for the shown Embodiment, the surface orientation is a (100) orientation.
  • the end region extends with the pointed end 4a substantially along the [001] direction with only a slight deviation of less than 10 °, so that the structural elements are nearly perpendicular with only a few degrees deviation from the normal to the surface of the base layer 3 are aligned.
  • FIG. 3a is the direction [001] oriented vertically. With the figures 3, 3a, the inclination of the side wall of a pyramid-like needle can be roughly determined. It is about 4 ° to the normal [001].
  • the surface which is severely rugged after the process, significantly increases their surface area, which significantly alters their properties.
  • the increased surface area offers a much larger attack surface for attaching molecules and can thus significantly increase the sensitivity of sensors.
  • the pyramidal structures 4 are interesting in that they are smaller in lateral size than the wavelength of light (VIS / NIR) and by their needle shape, ie by the small lateral dimension of the end region 4a and the relatively large dimension at the foot pyramidal structure, and the high aspect ratios give a nearly perfect gradient layer.
  • the refractive index gradually changes from the refractive index of the silicon to the refractive index of the medium surrounding the nanostructure 2, for example, air, so that a corresponding layer having the structures 4 can be referred to as a refractive index matching layer between two media.
  • Figure 7 shows a corresponding measurement of the direct and scattered reflections typically achieved. It can be seen that in a range from about 400 nm to 800 nm, the total reflection is dominated by the scattered reflection and is very low. For this wavelength range, the total reflection is 0.7% or even less.
  • FIG. 8c shows the component 8 in a further embodiment, wherein the base material 8a is made of a different material, which in the embodiment shown is provided in a deformable state.
  • a variety of polymeric materials may be applied or transferred into a deformable state by appropriate treatment to allow subsequent surface structuring.
  • This has a Template 9 a single or multiple curved surface 9b, which is a template material 9a formed.
  • the surface 9b has a layer 9c with a nanostructure which has the geometric properties as described above in connection with the nanostructure 4.
  • the template 9 may be a silicon carrier, in which in addition to the surface 9b and the layer 9c is incorporated.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Surface Treatment Of Optical Elements (AREA)

Abstract

La présente invention concerne un procédé et des composants optiques qui comportent une nanostructure (4) sur une surface incurvée pour leur conférer une propriété antireflet à large bande. La nanostructure est fabriquée à l'aide d'un procédé auto-masquant à une étape de cuisson de silicium (3) sur la surface incurvée.
EP07727292A 2006-03-24 2007-03-23 Composants optiques antireflets à large bande avec surfaces incurvées et leur procédé de fabrication Withdrawn EP1999498A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006013670A DE102006013670A1 (de) 2006-03-24 2006-03-24 Breitbandig entspiegelte optische Bauteile mit gekrümmten Oberflächen
PCT/EP2007/052818 WO2007110392A1 (fr) 2006-03-24 2007-03-23 Composants optiques antireflets à large bande avec surfaces incurvées et leur procédé de fabrication

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EP1999498A1 true EP1999498A1 (fr) 2008-12-10

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US (1) US20090180188A1 (fr)
EP (1) EP1999498A1 (fr)
DE (1) DE102006013670A1 (fr)
WO (1) WO2007110392A1 (fr)

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DE112013005487B4 (de) 2012-11-16 2022-07-07 Nalux Co., Ltd. Verfahren zur Herstellung einer Form für eine Antireflexionsstruktur und einer Form für ein optisches Gitter
DE102013106392B4 (de) * 2013-06-19 2017-06-08 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Herstellung einer Entspiegelungsschicht
JP2016532317A (ja) 2013-09-27 2016-10-13 ダンマークス テクニスク ユニバーシテットＤａｎｍａｒｋｓ Ｔｅｋｎｉｓｋｅ Ｕｎｉｖｅｒｓｉｔｅｔ ナノ構造化されたシリコン系太陽電池およびナノ構造化されたシリコン系太陽電池を製造する方法
JP6074560B2 (ja) 2014-03-21 2017-02-08 ナルックス株式会社 光学素子の製造方法及び光学素子用成型型の製造方法
CN105047590B (zh) * 2015-08-11 2017-12-15 上海华力微电子有限公司 一种具有蓝宝石基片的光谱反射计
JP2018077304A (ja) * 2016-11-08 2018-05-17 株式会社デンソー 撮像装置
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US20090180188A1 (en) 2009-07-16
WO2007110392A1 (fr) 2007-10-04

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