US20010017184A1 - Holographic grating and method of forming the same - Google Patents

Holographic grating and method of forming the same Download PDF

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Publication number
US20010017184A1
US20010017184A1 US09/735,556 US73555600A US2001017184A1 US 20010017184 A1 US20010017184 A1 US 20010017184A1 US 73555600 A US73555600 A US 73555600A US 2001017184 A1 US2001017184 A1 US 2001017184A1
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Prior art keywords
grating
grooves
negative
substrate
forming
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US09/735,556
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English (en)
Inventor
Masaru Koeda
Yuji Tanaka
Akio Soejima
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Shimadzu Corp
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Shimadzu Corp
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Assigned to SHIMADZU CORPORATION reassignment SHIMADZU CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SOEJIMA, AKIO, TANAKA, YUJI, KOEDA, MASARU
Publication of US20010017184A1 publication Critical patent/US20010017184A1/en
Priority to US10/459,463 priority Critical patent/US7129028B2/en
Abandoned legal-status Critical Current

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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/0005—Production of optical devices or components in so far as characterised by the lithographic processes or materials used therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/12—Generating the spectrum; Monochromators
    • G01J3/18—Generating the spectrum; Monochromators using diffraction elements, e.g. grating
    • G01J3/1838—Holographic gratings
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
    • G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
    • G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
    • G03H1/0276—Replicating a master hologram without interference recording
    • G03H1/028—Replicating a master hologram without interference recording by embossing
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
    • G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
    • G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
    • G03H1/024—Hologram nature or properties
    • G03H1/0244—Surface relief holograms
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
    • G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
    • G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
    • G03H1/0276—Replicating a master hologram without interference recording
    • G03H2001/0296—Formation of the master hologram
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
    • G03H2260/00—Recording materials or recording processes
    • G03H2260/50—Reactivity or recording processes
    • G03H2260/63—Indirect etching, e.g. lithography

Definitions

  • the present invention relates to a grating or diffraction grating as a wavelength separating/selecting element used in a spectroscope or a branching filter, and particularly, the present invention relates to a holographic grating formed by a holographic exposure method, and a method of manufacturing the same.
  • a grating or diffraction grating is a wavelength separating/selecting element used in a spectroscope, a branching filter, or the like.
  • a mechanical method wherein grating grooves are mechanically engraved by a ruling engine; and a holographic exposure method, wherein interference fringes by interference of two beams are exposed and developed in a photoresist layer coated on a base plate, so that a resist pattern having a section in a sine wave form is manufactured.
  • the diffraction grating formed by the holographic exposure method is generally called as a holographic grating.
  • the grating Since the grating is a precision instrument and requires many procedures to manufacture the same, it generally takes a long time, that is, tens of hours to hundreds of hours, to manufacture the grating, and it is impossible to mass-produce the gratings. Therefore, the grating is very expensive such that a unit price for the grating is several million Yen, and it is inevitable that there are individual differences in performances of the gratings.
  • a negative grating is formed with a resin from one original grating, and a replica grating is again formed from the negative grating, so that replica gratings are supplied in the market.
  • a general method for mass-producing the replica grating is as follows.
  • a thin oil film or a metal film made of gold, platinum or the like, which is weak in adhesion, is formed as a parting or separating agent on a lattice surface of a negative grating, and an aluminum thin film is formed by a vacuum deposition on the thin oil film or the metal film.
  • a replica base plate (glass base plate) is attached onto the aluminum thin film by an adhesive, and after setting of the adhesive, the glass base plate is separated from the original or mold.
  • the aluminum thin film is shifted to the glass base plate, and accordingly, there is obtained the replica grating in which grating grooves of the negative grating are transferred.
  • the transferring method as described above is not suitable for mass production. Namely, (1) since the grating grooves are formed in the original grating by the holographic exposure method, the photoresist layer coated on a front surface of the base plate is made of resin and has low intensity; (2) the adhesion force between the base plate and the photoresist layer is low as compared with an adhesion force of a single material; (3) the base plate and the photoresist layer are different in expansion coefficient, strength, and hardness. Therefore, in a parting or separating step, a breakage is likely to occur, and for example, at the time of parting, the grating groove becomes deficient, the resist is torn, or an entire resist layer is peeled off from the base plate. As a result, it is able to obtain only about ten sheets of replicas from the one sheet of the original grating. Also, the breakage of the grating is frequent, and a manufacturing efficiency is poor.
  • a replica should be manufactured by using an original grating in which grating grooves are directly engraved in a base plate instead of engraving the grooves in the photoresist layer, and the following method has been attempted.
  • a method wherein after exposing a photoresist layer provided on a base plate, the photoresist layer is etched by a known reactive ion beam etching (RIBE) method until the photoresist layer is completely deleted, and a grating pattern on the resist is transferred to a base plate itself as it is.
  • RIBE reactive ion beam etching
  • an object of the invention is to provide a holographic grating, which has an excellent durability, less stray light value, and a high diffraction efficiency while a change of diffraction efficiency in a wide wavelength range is small.
  • a mixed gas of a fluorine based gas and oxygen (O 2 ) is used as an etching gas used in the reactive ion beam etching (RIBE) with respect to an optical glass base plate, a direct engravement to the base plate becomes excellent.
  • a groove pattern for the grating formed by the exposure in the photoresist layer has a groove depth deeper than one time or more of a groove depth to be obtained finally.
  • a selection ratio (etching speed with respect to a base plate)/(etching speed with respect to a resist layer), which is defined according to a kind of the etching gas and materials of the base plate or the resist, becomes an issue in many cases.
  • the base plate which is an object for etching is not smoothly removed so that a production efficiency is poor, or on the contrary, only the base plate is removed or etched and the sectional form of the grating grooves does not become a desirable one. Therefore, normally, the selection ratio is adjusted by providing a mixed gas containing a halogen based gas as an etching gas such that the etching speed of the base plate is the same or more as that of the resist.
  • a method for manufacturing a grating of the invention in which the etching with respect to the optical base plate can be made excellently.
  • a resist pattern which has the depth deeper than that of the grating grooves to be desired finally, is formed in the resist layer on the optical glass base plate in advance, and then a mixed gas of a fluorine based gas and oxygen, which is adjusted such that the etching speed with respect to the resist is faster than the etching speed with respect to the base plate, is used as the etching gas to engrave the grooves in the optical base plate itself. Accordingly, excellent effects in the following have been found.
  • the resist pattern is set to be greater than the depth of the desired grating groove in advance, and by the ion beam etching, the resist pattern is formed to have the desired groove depth finally. Therefore, the deterioration of the grating grooves and the surface roughness thereof due to the damage in the etching, which were problems conventionally, are reduced for the portion of the selection ratio (ratio of the etching speeds of the optical glass base plate with respect to the resist), and rather, surface roughness can be reduced to be smaller than that of the original resist pattern, so that the scattered light component is further reduced. Thus, the excellent grating having a low stray light value can be formed.
  • carbon in the gas is deposited on the front surface of the photoresist to become a carbon rich condition, to thereby prevent the etching.
  • the rough surface occurs by continuing the etching while the carbon is deposited on the front surface of the photoresist, and in the extreme case, the shape of the resist pattern is damaged, or the front surface of the grating becomes clouded whitey.
  • the ion beam is irradiated from a direction substantially vertical to the grooving direction at a slant upper side of the base plate, a sectional form of the obtained grating grooves becomes slightly close to a blazed holographic grating. Therefore, there can be formed a high performance grating having a higher diffraction efficiency than that of the conventional holographic grating while an advantage of the holographic grating, that is, a wide using wavelength range, is maintained. Also, since it is possible to adjust which element should be increased between the sine wave shape and the blazed shape, there can be formed the grating having an efficiency distribution optimal to the spectroscope to be used.
  • FIGS. 1 ( a ) through 1 ( h ) are schematic views for explaining an embodiment of a holographic grating and a replica grating according to the present invention.
  • FIG. 2 is a schematic view for explaining a structural example of a holographic exposing device.
  • numeral 1 designates a base plate or substrate made of optical glass.
  • the base plate is a blank for an original of a diffraction grating, and can be any kind as long as the base plate can be optically polished and the resist can be coated thereon.
  • the optical glass is low in coefficient of expansion by a thermal change, and is excellent as a material for the base plate of the diffraction grating which is an optical element.
  • a low-expansion crystal glass such as BK7, BSC2, Pyrex glass, soda glass, quartz glass, “ZERODUR” (manufactured by Scott Glasswerke), or “CRYSTORON” (manufactured by HOYA CORPORATION), can be used satisfactorily, and in the invention, BK7 glass is used as an example in the present embodiment.
  • BK7 glass approximately 60 mm ⁇ 60 mm ⁇ 11.3 mm
  • the BK7 glass is optically polished to form a concave grating, and a front surface thereof is cleaned by ultrasonic cleaning.
  • a photoresist layer 2 is formed on the front surface of the base plate 1 .
  • the photoresist can be any kind as long as the holographic exposure can be made, and for example, MP1400 (manufactured by “SHIPLEY FAR EAST LTD.”), OFPR 500 (manufactured by “TOKYO OHKA KOGYO LTD.”), or the like, can be used as the photoresist.
  • MP1400 manufactured by “SHIPLEY FAR EAST LTD.”
  • OFPR 500 manufactured by “TOKYO OHKA KOGYO LTD.”
  • the MP1400 is baked in a convection oven at 90° C. for 30 minutes to form the photoresist layer 2 having a thickness of 300 nm.
  • the formed diffraction grating pattern 21 of the photoresist has a sectional form in the sine wave form.
  • the groove depth (amplitude of the sine wave form) of the diffraction grating pattern 21 of the photoresist can be determined by controlling the exposure time and, the development time, and in the embodiment, the groove depth is 200 nm.
  • FIG. 1( d )′ shows a part of the sectional form of the groove taken out from FIG. 1( d ) and enlarged.
  • the sectional form of the groove is made to have a shape slightly inclined from the sine wave, so that the holographic grating has two advantages, i.e. due to the sinewave-formed section, a change of the diffraction efficiency in the wide wavelength band is small, and due to a blazed grating having a serrated sectional form, the diffraction efficiency is high. Also, by changing the incident angle of the ion beam, an inclination amount of the sectional form can be adjusted, and by adjusting a ratio of the sine wave form to the blazed form, the diffraction efficiency distribution is adjusted, so that the grating optimal to the spectroscope is made.
  • the etching gas to be used is not limited to the mixed gas of CF 4 and O 2 , and the etching gas can be a mixed gas of the fluorine based gas, such as ChF 3 , CBrF 3 , or the like, and O 2 .
  • the objects are to form a resist pattern having a groove depth, which may be more than 1.5 times, deeper than the groove depth of the diffraction grating to be obtained finally; to eliminate the carbon rich condition on the etching surface by using the etching gas in which O 2 is mixed; and to reduce the surface roughness by adjusting the selection ratio of the etching.
  • the incident angle of ions assuming that the direction of the normal line of the base line is zero degree, as the incident angle is increased, a peak value of the diffraction efficiency becomes larger.
  • the incident angle of ions can be freely set in the range of 10 degrees to 80 degrees, and the incident angle itself is not important.
  • the peak of the efficiency will be approximately 220 nm, to constitute the efficiency distribution optimal for use in an ultraviolet visible spectroscope.
  • the efficiency in the conventional holographic grating, in which the diffraction grating grooves are formed of the resist, is about 30 percent.
  • the efficiency in the diffraction grating of the present embodiment is 39 percent, resulting in the approximately 30 percent increase or improvement as compared with the conventional one.
  • the original grating After cleaning the original grating in which the etching is completed, coating by a material optimal to the wavelength range to be used is carried out in a vacuum deposition device (FIG. 1( e )).
  • a vacuum deposition device (FIG. 1( e )).
  • the original grating since the original grating has a sufficiently high reflectance, the original grating may be sufficiently usable as it is.
  • the original grating is coated with gold (Au), platinum (Pt), or an X-ray multilayer film to thereby increase the reflectance and durability, and then, the coated grating is used.
  • gold (Au), platinum (Pt), or an X-ray multilayer film to thereby increase the reflectance and durability, and then, the coated grating is used.
  • aluminum (Al) which has a high reflectance in a range from an ultraviolet region to a visible region, is coated.
  • a method for forming a replica grating from the original grating will be explained (refer to FIG. 1( f )).
  • a thin oil film (thickness of about 1 nm) is formed as a parting agent by, for example, a silicone grease on the original grating, and then an aluminum thin film (thickness of 0.2 ⁇ m) is vacuum-deposited thereon.
  • a negative base plate (glass base plate or the like) is attached thereto by an adhesive.
  • the adhesive is not limited thereto, and other thermosetting resin having the thermal resistance, such as urea resin, melanin resin, and phenolic resin, can be used as the adhesive. If BENEF IX VL (manufactured by “ADELL Co., Ltd.”), that is a visible light hardening resin, is used as the adhesive, an effect of a thermal distortion can be reduced. Also, the elastic adhesive EP-001 (manufactured by Cemedine Co., Ltd.) can be also used as the adhesive.
  • the negative base plate When the negative base plate is separated from the original grating (mold or matrix) after the adhesive is hardened, the negative base plate is separated at the parting agent as the boundary. After parting, the parting agent remained on the surface of the negative base plate is cleaned by a solvent, such as Freon, and removed. Accordingly, there can be obtained the negative grating having a front surface in which the diffraction grating grooves for the original grating are transferred (FIG. 1( g )).
  • the resist layer is peeled off from the base plate at the step of parting or separating the negative base plate, so that the durability was poor.
  • the grooves are directly engraved in the BK7 glass base plate, the grating is excellent in durability, and a large number of replicas or reproductions can be formed.
  • the fine diffraction grating grooves may change, so that the grooves of the original grating and the grooves of the negative grating bite each other to thereby disable the separation.
  • the surface roughness after transfer is solved, and the stray light is held down to be low.
  • the replica grating of the embodiment is mounted in an ultraviolet visible spectrophotometer UV1200 (manufactured by Shimadzu Corporation) to compare a stray light value thereof with that of the conventional grating, while the stray light value of the conventional grating is 0.024%, the stray light value of the grating of the invention is 0.0061%, so that the stray light value can be improved to be extremely excellent. Since the stray light value includes a value contained in the spectrophotometer itself other than that of the grating, it is possible to say that the stray light value of the grating itself can be minimized to the limit.
  • the method of forming the replica grating is the same as in the negative grating.
  • a parting agent layer and an aluminum thin film are formed, and after a replica base plate is bonded by the adhesive, the separation is carried out.
  • the grooves of the negative grating are again transferred, and as a result, the replica grating has the same grooves as those of the original grating.
  • a large number of replica grating is formed.
  • the coating is peeled off and the original grating is coated again, so that the original grating can be used again.
  • the grating is extremely excellent in durability, and it becomes possible to reproduce thousands of sheets of replica gratings from one sheet of the original grating. This enables not only to supply the replica grating at a low cast in the market, but also to reduce the unevenness of the performance of the replica grating, resulting in the effect that the grating with a stable quality can be provided.
  • the holographic grating according to the present invention is structured such that diffraction grating grooves, which are conventionally used to be engraved in the resist, are directly engraved in the glass base plate, the durability of the grating can be extremely improved. Therefore, in the steps of forming the replicas or reproductions, there is no inconvenience that the resist is peeled off or the grooves are chipped at the time of separation, and thousands of sheets of the replica gratings can be reproduced from one sheet of the original grating, so that the unit price can be extremely lowered. Also, since the original grating is common, there is no unevenness in performances of replicas formed from the common original grating, so that the stable quality can be guaranteed.
  • the groove height of the grating pattern formed in the resist is set high one time or more relative to the groove height of the grating to be obtained finally, and then, a selection ratio is adjusted such that the etching speed with respect to the resist is faster than the etching speed with respect to the base plate. Therefore, the surface roughness of the front surface of the grating obtained as a result of the etching is reduced partly by the selection ratio, and rather, the surface damage due to the etching is reduced, resulting in an incomparable effect that the excellent grating with the low stray light value can be formed.
  • the reactive ion beam etching step since the mixed gas of the fluorine based gas and oxygen is adopted as the etching gas with respect to the optical glass base plate, in addition to adjusting the section ratio in the etching, the carbon rich condition on the etching surface can be solved, to thereby increase the etching efficiency. At the same time, there can be solved the problem of the cloudiness of the front surface of the grating.
  • the ion beam is irradiated from the direction, which is vertical to the grooving direction of the resist pattern and is inclined with respect to the normal line of the base plate, so that the sectional form of the grating grooves has a substantially sine wave slightly close to the serrated form (inclined toward the incident direction of the ions). Therefore, there can be formed the grating which has both advantage such that due to the sinewave-formed section of the holographic grating, a change of the diffraction efficiency is small in the wide wavelength band, and due to the blazed grating having a serrated sectional form, the diffraction efficiency is high.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Diffracting Gratings Or Hologram Optical Elements (AREA)
  • Photosensitive Polymer And Photoresist Processing (AREA)
  • Holo Graphy (AREA)
  • Surface Treatment Of Glass (AREA)
US09/735,556 2000-02-25 2000-12-14 Holographic grating and method of forming the same Abandoned US20010017184A1 (en)

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JP2000048686A JP2001235611A (ja) 2000-02-25 2000-02-25 ホログラフィック・グレーティング

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US20030228106A1 (en) * 1999-11-25 2003-12-11 Ken Hashimoto Method of making diffraction grating device, diffraction grating device, and apparatus for making diffraction grating device
US20040063051A1 (en) * 2000-07-11 2004-04-01 Afromowitz Martin A. Method for fabricating 3-D structures with smoothly-varying topographic features in photo-sensitive epoxy resists
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US20050130072A1 (en) * 2003-11-27 2005-06-16 Shimadzu Corporation Blazed holographic grating, method for producing the same and replica grating
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US20100164128A1 (en) * 2007-04-26 2010-07-01 Enns John B Lithographic method for forming mold inserts and molds
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JP2001235611A (ja) 2001-08-31
US20030213768A1 (en) 2003-11-20
US7129028B2 (en) 2006-10-31
CN1310346A (zh) 2001-08-29

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