CN203732747U - Metallic glass thin film micro device for plastic deformation processing - Google Patents
Metallic glass thin film micro device for plastic deformation processing Download PDFInfo
- Publication number
- CN203732747U CN203732747U CN201420043016.6U CN201420043016U CN203732747U CN 203732747 U CN203732747 U CN 203732747U CN 201420043016 U CN201420043016 U CN 201420043016U CN 203732747 U CN203732747 U CN 203732747U
- Authority
- CN
- China
- Prior art keywords
- thin film
- metallic glass
- glass thin
- micro device
- plastic deformation
- 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.)
- Expired - Fee Related
Links
- 239000005300 metallic glass Substances 0.000 title claims abstract description 17
- 238000012545 processing Methods 0.000 title claims abstract description 12
- 239000010409 thin film Substances 0.000 title abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 23
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 17
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000010287 polarization Effects 0.000 claims abstract description 12
- 230000005540 biological transmission Effects 0.000 claims abstract description 9
- 238000012216 screening Methods 0.000 claims abstract description 3
- 239000010953 base metal Substances 0.000 claims description 15
- 230000003287 optical effect Effects 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 48
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000956 alloy Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 229910045601 alloy Inorganic materials 0.000 abstract description 9
- 238000010891 electric arc Methods 0.000 abstract description 7
- 229910052786 argon Inorganic materials 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 238000005520 cutting process Methods 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 abstract description 4
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 230000009477 glass transition Effects 0.000 abstract description 2
- 241001025261 Neoraja caerulea Species 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000013077 target material Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 229910020639 Co-Al Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910020675 Co—Al Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000010884 ion-beam technique Methods 0.000 description 3
- 229910052747 lanthanoid Inorganic materials 0.000 description 3
- 150000002602 lanthanoids Chemical class 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 238000000646 scanning calorimetry Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 230000005469 synchrotron radiation Effects 0.000 description 1
Landscapes
- Diffracting Gratings Or Hologram Optical Elements (AREA)
Abstract
The utility model discloses a metallic glass thin film micro device for plastic deformation processing. A lanthanum based metallic glass thin film is high in thermoplasticity, low in glass transition temperature, high in flatness, and high in corrosion resistance; a structural formula of an alloy is La100-x-yCoxAly, wherein the x is an atomic percentage of the Co element, y is an atomic percentage of the Al element, 5 <= x <= 35, 5 <= y <= 35, 25 <= x+y <=50; more than four times of electric arc melting are carried out in a zirconium adsorption argon arc, so as to get a mixed-evenly alloy block; finally, a wire-electrode cutting method is used to get a target material meeting coating requirements; and a DC magnetron sputtering is used to get a metal glass film with a desired thickness. According to the metallic glass thin film micro device for plastic deformation processing, a 2D subwavelength transmission grating filtering piece with the polarization insensitive property is obtained; the grating unit is a convex square array; the height is 200nm, the square array cycle is 240nm, and the square side length is 120nm; and the metallic glass thin film micro device is not sensitive to the polarization of the incident light, can enhance the transmission rate of the incident light, and can realize the screening of the blue ray.
Description
Technical field
The utility model relates to micro-nano technology of preparing, particularly a kind of metallic glass film micro element for plastic yield processing.
Background technology
Traditional semiconducter process grows up on microelectronics integrated technique, and processing miniature parts is mainly used silicon materials, but due to the low mechanical strength of silicon chip, more and more can not meet the functional requirement of part in modern micro-optic and micro-system.For metal material, utilize the miniature parts of LIGA technology processing, although have good depth-to-width ratio, because technical limitation is difficult to be applied to dip plane and fine Precision Machining, while is the synchrotron radiation light source somewhat expensive of utilization wherein, has limited the range of application of this technology.Amorphous alloy (being commonly called as metallic glass) is that composed atom can not be arranged periodically and symmetric a kind of novel alloy material, due to its special micromechanism, make them there is superior mechanics, physics, chemistry and magnetic property, be particularly suitable for the preparation of micro element, but due to bulk amorphous alloy preparation difficulty, lack excellent ductility, cannot widespread use.Therefore the research of thin film of amorphous alloy is arisen at the historic moment, it had both inherited the advantage of amorphous alloy, as high strength, high rigidity, wear-resistant, corrosion-resistant, can in small scale, evade the shortcoming of bulk amorphous alloys poor ductility again simultaneously, be therefore with a wide range of applications.Yet most noncrystalline membrane supercooling liquid phase region is narrower, cause degree of stability not high, and glass transformation temperature is mostly at 250 ° more than C, for above shortcoming and restriction, we design and have prepared lanthanum base metal glass film.
Lanthanum base metal glass film prepared by this Project design possesses extremely low glass transformation temperature (minimum can reach 140 ° of C), proportioning is simple, thermoplasticity is excellent, flatness is high, and roughness is little, has very strong corrosion resistance simultaneously, degree of stability is high, having original advantage aspect clean shaping, be structured material desirable in micro-system and micro-machine-shaping, we utilize designed, designed this be the micro element that metallic film has successfully been prepared sub-wavelength dimensions.
Utility model content
The purpose of this utility model is to overcome the deficiencies in the prior art, and a kind of metallic glass film micro element for plastic yield processing is provided.
It is as follows that the utility model solves the technical scheme that its technical matters adopts:
A kind of metallic glass film micro element for plastic yield processing, the two-dimentional sub-wavelength transmission grating filter plate with polarization insensitive characteristic obtaining on lanthanum base metal glass film, raster unit is protruding quadrate array, height 200nm, quadrate array cycle 240nm, square length of side 120nm, this optical filter has the insensitive characteristic of incident light polarization, can improve the transmissivity of incident light, realize the screening to blue light.
The beneficial effect the utlity model has is: the utility model discloses a kind of glass transformation temperature low, flatness is high, roughness is little, thermoplasticity is good, superior and the corrosion resistant ternary lanthanum base metal glass film of clean crystallized ability, and successfully prepared two-dimentional sub-wavelength transmission grating filter plate and the simple one-dimensional grating of polarization insensitive characteristic, the excellent properties of this ternary lanthanum base film is with a wide range of applications it in the manufacture of nano impression and accurate micro-nano device.
Accompanying drawing explanation
Fig. 1 is La
53co
15al
32the XRD figure of film;
Fig. 2 is La
53co
15al
32the DSC figure of film;
Fig. 3 is La
53co
15al
32the mechanical property figure of film;
Fig. 4 is La
53co
15al
32the AFM figure of film;
Fig. 5 is micro element preparation flow figure;
Fig. 6 is that raster unit is projection square, cycle 240nm, the two-dimentional sub-wavelength transmission grating filter plate figure with polarization insensitive characteristic of length of side 120nm;
Fig. 7 is live width 150nm, cycle 300nm, the simple line grating figure of one dimension of dark 200nm.
Embodiment
Step 1: the La that is 99.9% by purity, the Al that the Co that purity is 99.95% and purity are 99.95% is by La
100-x-yco
xal
y,wherein x is the atomic percentage of La element, y is the atomic percentage of Co element, 5≤x≤35,5≤y≤35,25≤x+ y≤50, in the argon gas electric arc of zirconium absorption, electric arc melting more than four times, obtains the alloy block mixing, afterwards alloy block is cast and prepared the initial target of 2 inches by copper mold, finally utilize line cutting to obtain meeting the target of plated film requirement;
Step 2: the target that the method for employing d.c. sputtering obtains step 1 and substrate are put into the good operation room of vacuum tightness and obtained the good lanthanum base metal glass film of density;
Step 3: the structure that characterizes gained sample with X-ray diffraction;
Step 4: obtain thermal parameters with poor formula scanning calorimetry;
Step 5: the mechanical property that adopts testing machine for mechanical properties test resulting materials;
Step 6: the surfaceness that adopts atomic force microscope testing film;
Step 7: by the flatness of ZYGO interferometer measurement film surface;
Step 8: utilize focused ion beam (FIB) technology to process the antistructure that obtains required micro element on monocrystalline silicon, using this as mould;
Step 9: the silicon mould having prepared and La-Co-Al metallic glass film sample are placed in marking press machine chamber up and down, pressure and heating-up temperature are set, carry out 3 minutes recession temperature of hot pressing heat-insulation pressure keeping and remove pressure, after sample is cooling, mould and sample are separated;
Step 10: in absolute ethyl alcohol, the sample of preparation is carried out to ultrasonic cleaning, finally obtain the required lanthanum base metal glass film micro element contrary with mould structure.
embodiment 1
This embodiment adopts the method for magnetron sputtering to prepare the La that thickness 200nm is thick
53co
15al
32metallic glass film, and with this film preparation raster unit be projection square, cycle 240nm, the two-dimentional sub-wavelength transmission grating filter plate with polarization insensitive characteristic of length of side 120nm.
Step 1: the La that is 99.9% by purity, the Al that the Co that purity is 99.95% and purity are 99.95% is by La
53co
15al
32in the argon gas electric arc that proportioning is adsorbed at zirconium, electric arc melting is five times, obtains the alloy block mixing, and afterwards alloy block is cast and is prepared the initial target of 2 inches by copper mold, finally utilizes line cutting to obtain meeting the target of plated film requirement;
Step 2: vacuum chamber is put in target and quartz glass substrate that step 1 is obtained, 5 * 10
-4pa-6 * 10
-4in the vacuum tightness of Pa, by low tension, from argon gas and on target cathode surface, introduce magnetic field, utilize magnetically controlled DC sputtering, with the power of 60W, the rate of sedimentation of (20+/-0.5) nm/s, sputter 10s, the lanthanum base metal glass film of acquisition 200um;
Step 3: characterize the structure of gained sample with X-ray diffraction, the X-ray diffractogram that Fig. 1 is this sample, illustrates that this film sample is non-crystaline amorphous metal structure;
Step 4: obtain thermal parameters with poor formula scanning calorimetry, the DSC figure that Fig. 2 is this sample;
Step 5: adopt the mechanical property of testing machine for mechanical properties test resulting materials as Fig. 3;
Step 6: with AFM, measure the roughness of film sample, the AFM figure that Fig. 4 is this sample, roughness is less than 1 nanometer, only has 0.3nm;
Step 7: the flatness with ZYGO interferometer measurement film surface, be less than 2 apertures, flatness is very high.
Step 8: utilize focused ion beam (FIB) technology on monocrystalline silicon, to process raster unit for depression square, degree of depth 200nm, cycle 240nm, the quadrate array of length of side 120nm, usings this as mould;
Step 9: the silicon mould having prepared and La-Co-Al metallic glass film sample are placed in marking press machine chamber up and down, 240 ° of C of pressure 300N and temperature are set, carry out 3 minutes recession temperature of hot pressing heat-insulation pressure keeping and remove pressure, after sample is cooling, mould and sample are separated;
Step 10: in absolute ethyl alcohol, the sample of preparation is carried out to ultrasonic cleaning, finally on lanthanum base metal glass film, obtain raster unit for projection square, cycle 240nm, the two-dimentional sub-wavelength transmission grating filter plate with polarization insensitive characteristic of length of side 120nm.The preparation flow of micro element as shown in Figure 5.
By known this embodiment 1 of Fig. 1 ~ Fig. 4, obtained the lanthanum base metal glass film of thickness 200nm, and on lanthanum base metal glass film, obtained the two-dimentional sub-wavelength transmission grating filter plate (Fig. 6) with polarization insensitive characteristic.The performance of the lanthanide series metal glass film that this embodiment obtains is as shown in table 1.The lanthanum base metal glass film glass transition temperature of this proportioning is lower, elastic modulus is large, be applicable to structural stability to require high, the material that is difficult for the protruding two-dimensional complex array grating filter plate of deformation, according to surface plasma bulk effect, we have designed cycle 240nm, thickness 200nm and array are shaped as two-dimentional protruding square array, when light and the interaction of our film surface sub-wavelength structure, realized matching well incident wave resultant surface resonance wave vector, this, intercouple in process, restricted gender and non-radiation type due to surface plasma primitive, stop energy along metal surface conduction decay, the concussion of region plasma wave excites enhancing, therefore improved the transmissivity of filter plate, while is due to the symmetry of periodic structure, avoided the impact of the polarization of incident light.We can also realize the different frequency filtering to incident light by adjusting grating cycle size and thickness.
Table 1 La
53co
15al
32film performance
?
embodiment 2
This embodiment adopts the method for magnetron sputtering to prepare the La of thickness 200nm
72co
18al
10metallic glass film, utilizes this film to make one-dimensional grating.
Step 1: the La that is 99.9% by purity, the Al that the Co that purity is 99.95% and purity are 99.95% is by La
72co
18al
10in the argon gas electric arc that proportioning is adsorbed at zirconium, electric arc melting is five times, obtains the alloy block mixing, and afterwards alloy block is cast and is prepared the initial target of 2 inches by copper mold, finally utilizes line cutting to obtain meeting the target of plated film requirement;
Step 2: vacuum chamber is put in target and quartz glass substrate that step 1 is obtained, 5 * 10
-4pa-6 * 10
-4in the vacuum tightness of Pa, by low tension, from argon gas and on target cathode surface, introduce magnetic field, utilize magnetically controlled DC sputtering, with the power of 60W, the rate of sedimentation of (20+/-0.5) nm/s, sputter 10s, the lanthanum base metal glass film sample of acquisition 200nm;
Step 3: the structure that characterizes gained sample with X-ray diffraction;
Step 4: obtain thermal parameters with poor formula scanning calorimetry;
Step 5: the mechanical property that adopts testing machine for mechanical properties test resulting materials;
Step 6: the roughness of measuring film sample with AFM;
Step 7: by the flatness of ZYGO interferometer measurement film surface;
Step 8: utilize focused ion beam (FIB) technology to process one-period 300nm on monocrystalline silicon, the line grating mould of dark 200nm;
Step 9: the silicon mould having prepared and La-Co-Al metallic glass film sample are placed in marking press machine chamber up and down, 150 ° of C of pressure 160N and temperature are set, carry out 3 minutes recession temperature of hot pressing heat-insulation pressure keeping and remove pressure, after sample is cooling, mould and sample are separated;
Step 10: in absolute ethyl alcohol, the sample of preparation is carried out to ultrasonic cleaning, finally obtain the simple grating of one dimension (Fig. 7) of cycle 300nm on lanthanum base metal glass film.
This embodiment 2 has obtained the lanthanum base metal glass film of thickness 200nm and with its processing, has obtained live width 150nm, cycle 300nm, the simple line grating of one dimension of dark 200nm.The performance of the lanthanide series metal glass film that this embodiment obtains is as shown in table 2.The lanthanide series metal glass film glass transformation temperature of this proportioning is very low, and elastic modulus is lower, is applicable to the rapid processing to the relatively low micro element simple in structure of rigidity requirement.
Table 2 La
72co
18al
10film performance
Claims (1)
1. the metallic glass film micro element for plastic yield processing, it is characterized in that, the two-dimentional sub-wavelength transmission grating filter plate with polarization insensitive characteristic obtaining on lanthanum base metal glass film, raster unit is protruding quadrate array, height 200nm, quadrate array cycle 240nm, square length of side 120nm, this optical filter has the insensitive characteristic of incident light polarization, can improve the transmissivity of incident light, realizes the screening to blue light.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420043016.6U CN203732747U (en) | 2014-01-23 | 2014-01-23 | Metallic glass thin film micro device for plastic deformation processing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420043016.6U CN203732747U (en) | 2014-01-23 | 2014-01-23 | Metallic glass thin film micro device for plastic deformation processing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203732747U true CN203732747U (en) | 2014-07-23 |
Family
ID=51202809
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201420043016.6U Expired - Fee Related CN203732747U (en) | 2014-01-23 | 2014-01-23 | Metallic glass thin film micro device for plastic deformation processing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN203732747U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110794499A (en) * | 2019-10-31 | 2020-02-14 | 歌尔股份有限公司 | Light filter |
-
2014
- 2014-01-23 CN CN201420043016.6U patent/CN203732747U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110794499A (en) * | 2019-10-31 | 2020-02-14 | 歌尔股份有限公司 | Light filter |
| WO2021082053A1 (en) * | 2019-10-31 | 2021-05-06 | 潍坊歌尔微电子有限公司 | Optical filter |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103805920A (en) | Metallic glass film for plastic deformation processing and preparation method of micro-component of metallic glass film | |
| Bollmann | Interference effects in the electron microscopy of thin crystal foils | |
| CN103033496B (en) | A kind of wide area surface strengthens the preparation method of Raman scattering substrate | |
| CN103996719B (en) | Based on the Meta Materials optical pickocff and preparation method thereof of dielectric-dielectric-metal structure | |
| CN102925869B (en) | Method for preparing amorphous/nanometer crystal multilayer-structure film | |
| CN103938130B (en) | The preparation method of nanoporous nickel block body | |
| CN103911587A (en) | Application of amorphous alloy material source, composite material and preparation method thereof | |
| CN203732747U (en) | Metallic glass thin film micro device for plastic deformation processing | |
| WO2006111068A1 (en) | A ce-base amorphous metallic plastic | |
| Ma et al. | Large size metallic glass gratings by embossing | |
| CN1552940A (en) | High heat stability block ferromagnetic metal glas synthetic method | |
| Nishio et al. | Ideally ordered metal hole arrays with high aspect ratios prepared from anodic porous alumina | |
| CN102234746B (en) | Zinc-based massive amorphous alloy and preparation method thereof | |
| CN108417475A (en) | A kind of preparation method of the metal Nano structure array based on interface induced growth | |
| Sun et al. | Hierarchical macro to nano press molding of optical glasses by using metallic glasses | |
| CN105463402A (en) | Nanometer twin crystallization surface manufacturing method for diamond needle tip array template coining | |
| CN102268618A (en) | High specific strength light titanium-based amorphous alloy | |
| Huang et al. | Study on silicon nanopillars with ultralow broadband reflectivity via maskless reactive ion etching at room temperature | |
| CN1285925C (en) | Production for aluminium-material X-ray assembled lens | |
| CN101200279B (en) | High-sensitivity nickel/silicon composite micro-cantilever and preparation method thereof | |
| CN103303860A (en) | Method for generating 0-50nm of random-height nano step on surface of Si | |
| Liu et al. | Morphology and structure evolution of metallic nanowire arrays prepared by die nanoimprinting | |
| JP2010179586A (en) | Material for forming mold, mold material, molding mold, and method for manufacturing optical lens element | |
| CN101979995B (en) | Method for measuring micro-nano film line elongation and film surface elongation | |
| CN101187006A (en) | Double target co-sputtering method for preparing Zr doped ITO film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140723 Termination date: 20170123 |