CN113604906B - Micro-nano optical phase change fiber for direct writing of static electricity and preparation method and application thereof - Google Patents
Micro-nano optical phase change fiber for direct writing of static electricity and preparation method and application thereof Download PDFInfo
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- CN113604906B CN113604906B CN202110768649.8A CN202110768649A CN113604906B CN 113604906 B CN113604906 B CN 113604906B CN 202110768649 A CN202110768649 A CN 202110768649A CN 113604906 B CN113604906 B CN 113604906B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
Abstract
The invention discloses an electrostatic direct writing micro-nano optical phase change fiber and a preparation method and application thereof, and belongs to the technical field of phase change material preparation. The invention firstly dissolves an organic precursor in a solvent to prepare a precursor solution, then adopts an electrostatic direct writing method to directly write the precursor solution into a precursor of the micro-nano optical phase-change fiber, and finally prepares the micro-nano optical phase-change fiber through post-treatment such as heating decomposition, calcination and the like. The preparation process provided by the invention has low cost, can prepare the optical phase-change fiber with one-dimensional extension space, and can control the shape of the micro-nano optical phase-change fiber according to the requirement. The micro-nano optical phase change fiber prepared by the invention can be used for optical logic, optical switches, optical modulation and the like, and is expected to be applied to a plurality of fields of optics, microelectronics, sensing and the like.
Description
Technical Field
The invention relates to an electrostatic direct writing micro-nano optical phase change fiber and a preparation method and application thereof, and belongs to the technical field of phase change material preparation.
Background
Because of the advantages of large bandwidth, low crosstalk, and high speed inherent in optical information transmission, it is highly desirable to achieve transmission and storage of information by optical means only. Thus, all-optical memories have evolved, i.e., memories that rely solely on light to effect "writing", "erasing", and "reading". Nonvolatile optical phase change materials are ideal materials for fabricating all-optical memories. Optical phase change materials are a class of materials with special physical properties. Under the induction of laser heat, the material can be converted between an amorphous state and a crystalline state, and macroscopically shows that optical properties, resistance characteristics and the like are greatly changed. In the microelectronics field, the storage of binary "0" states and "1" states can be realized by utilizing this property, and optical discs or phase change memories can be made according to this principle. The optical phase-change material which has been reported at present is mainly prepared into a film by a magnetron sputtering method, namely a planar optical phase-change material. The magnetron sputtering method is one of physical vapor deposition, argon is ionized by an electric field, and the ionized ions bombard a target material to enable particles on the target material to fall off, and then deposition is carried out, so that film coating is realized. The limitations of the magnetron sputtering method are that the magnetron sputtering method needs to draw by adopting a mode of customizing a mask plate aiming at complex patterns, however, the magnetron sputtering method has two limitations, namely, first, the economical and time aspects: when one pattern is replaced, a customized mask plate is required to be replaced, so that the preparation is not friendly enough under the condition that the sputtering pattern needs to be replaced frequently, and the customization of the mask plate is very time-consuming frequently; the mask plate is processed by chemical etching, laser drilling, electroforming and other modes, and has high requirements on the position and shape precision of the mask plate with fine patterns, so that the price of one fine metal mask plate is very high; second, the score line accuracy aspect: currently, a magnetron sputtering mask plate with higher cost performance has an error of about 50 micrometers in a line width of 500 micrometers, and the line width is difficult to be reduced to be below 50 micrometers. In addition, the conventional magnetron sputtering method is difficult to adjust the width of sputtered pattern lines by using the same mask plate, and the mask plate error is larger for narrow lines.
Therefore, it is necessary to provide a novel method for preparing micro-nano optical phase-change fibers to overcome the limitations that the traditional magnetron sputtering method requires a mask plate and only planar optical phase-change materials can be prepared.
Disclosure of Invention
The invention provides an electrostatic direct-writing micro-nano optical phase-change fiber, a preparation method and application thereof, and aims to solve the above limitations of the existing magnetron sputtering method for preparing the micro-nano optical phase-change fiber.
The technical scheme of the invention is as follows:
the electrostatic direct writing micro-nano optical phase change fiber comprises three elements of germanium, antimony and tellurium, wherein the chemical formula is GexSbyTez, and x, y and z are the mass parts of the corresponding elements, wherein x is more than or equal to 0 and less than or equal to 40, y is more than or equal to 0 and less than or equal to 40, z is more than or equal to 20 and less than or equal to 90, and x+y+z is more than or equal to 0 and less than or equal to 100.
Further defined, x is 20, y is 20, and z is 50.
The preparation method of the micro-nano optical phase change fiber for direct writing of static electricity comprises the following steps:
the precursor solution comprises five-membered ring germanium (II) complex, trisilane antimony and disilane tellurium;
the static direct writing condition is as follows: the temperature is 15-30 ℃, the voltage is 5-25kV, the writing speed is 0.01-0.5cm/s, the moving speed of the receiving plate in the non-writing process is 0.2-2cm/s, the pen lifting/dropping interval is 0.5-2s, and the distance from the spray head to the glass slide is 3-10cm;
and step 3, carrying out heating calcination treatment on the organic precursor fiber obtained in the step 2 to obtain the micro-nano optical phase change fiber.
Further defined, the specific operation procedure of step 1 is:
and dissolving the five-membered ring germanium (II) complex, the trisilane antimony and the disilane tellurium in tetrahydrofuran, adding polymethyl methacrylate, and uniformly stirring to obtain a precursor solution.
Further defined, the total mass of the five-membered ring germanium (II) complex, the trisilane antimony and the disilane tellurium in the precursor solution accounts for 10% -30% of the mass of the precursor solution.
Further defined, the total mass of the five-membered ring germanium (II) complex, the trisilane antimony and the disilane tellurium in the precursor solution is 20% of the mass of the precursor solution, wherein the mass of the five-membered ring germanium (II) complex, the trisilane antimony and the disilane tellurium is 1.04g, 0.92g and 2.04g, respectively, and the tetrahydrofuran volume is 20mL.
Further defined, the polymethyl methacrylate has a molecular weight of 30 ten thousand.
Further defined, the specific operation procedure of the electrostatic direct writing in the step 2 is as follows:
firstly, placing a precursor solution in a spraying device of an electrostatic direct writing device;
then, fixing the glass slide on a receiving plate by adopting a non-metal clamp, and sequentially using deionized water, acetone and absolute ethyl alcohol as ultrasonic media to respectively ultrasonically clean the glass slide for 15min;
finally, the computer is debugged by presetting a track, parameters are set, and static direct writing is completed.
Further defined, the calcination treatment conditions in step 3 are: heating to 400 ℃ at a speed of 10 ℃/min under the protection of argon, maintaining for 90min, and naturally cooling to room temperature.
The method for preparing the all-optical memory by using the micro-nano optical phase change fiber comprises the following steps:
firstly, drawing micro-nano optical phase change fibers on a glass slide by adopting an electrostatic direct writing method;
then, the optical fiber with the coating layer partially stripped is tapered, and the tapered part is covered on the micro-nano phase change fiber;
and finally, packaging in vacuum or protective atmosphere to obtain the all-optical memory.
The invention has the following beneficial effects: the micro-nano optical phase-change fiber is prepared by adopting the electrostatic direct writing method, and the most remarkable advantage of the electrostatic direct writing is that the shape of the micro-nano optical phase-change fiber can be drawn according to the requirement, so that the limitation that only an optical phase-change material coating can be prepared by a magnetron sputtering method and a mask plate needs to be replaced frequently is overcome. The micro-nano optical phase change fiber prepared by the invention can be used for optical logic, optical switches, optical modulation, sensing and the like, and is expected to be applied to a plurality of fields of optics, electronics, sensing and the like.
Drawings
FIG. 1 is a schematic diagram of an electrostatic direct write device;
FIG. 2 is a schematic diagram of the chemical structures of five-membered ring germanium (II) complexes, trisilane antimony and disilane tellurium;
FIG. 3 is a schematic top view of the embodiment 1 before packaging the all-optical memory;
FIG. 4 is a schematic cross-sectional view of the taper of the all-optical memory fiber of example 1;
FIG. 5 is a schematic diagram of the conversion between the "0" state and the "1" state of the all-optical memory;
in the figure, 1-precursor solution, 2-injector, 3-metal needle, 4-electrode clamp, 5-receiving plate, 6-glass slide, 7-writing machine, 8-negative plate, 9-high voltage power supply, 10-ground wire, 11-jet, 15-micro-nano optical phase change fiber, 16-tapered optical fiber, 17-shell and 18-cavity.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
Example 1:
1. preparing a precursor solution:
the micro-nano optical phase change fiber Ge of the embodiment x Sb y Te z Where x=20, y=20, z=50.
According to the proportion, the total mass of the five-membered ring germanium (II) complex, the trisilane antimony and the disilane tellurium in the precursor solution accounts for 20% of the mass of the precursor solution, 1.04g of the five-membered ring germanium (II) complex, 0.92g of the trisilane antimony and 2.04g of the disilane tellurium are sequentially weighed, the molecular structural formula is shown in figure 2, the mixture is added into 20mL of tetrahydrofuran, 4g of PMMA with the molecular weight of about 30 ten thousand is added, and the mixture is stirred for 24 hours to obtain semitransparent to opaque sticky matters, namely the precursor solution.
2. Electrostatic direct write preparation of organic precursor fibers:
adopting an electrostatic direct writing device as shown in fig. 1, firstly, sequentially using deionized water, acetone and absolute ethyl alcohol as ultrasonic media for a glass slide 6, respectively ultrasonically cleaning for 15min to clean the surface, and then drying in an oven for later use. Then, the precursor solution configured in the step one is placed in a spraying device of an electrostatic direct writing device. The pretreated slide 6 is then fixed to the receiving plate 5. Then, debugging is carried out by using a preset track of a computer, the distance between a spray head and a glass slide is adjusted to be 5.4cm (if the distance is too short, the solvent is not completely volatilized, so that the written optical phase change fiber precursor is gathered and deformed, and if the distance is too long, jet flow is branched), a new glass slide is replaced after the debugging is finished, and static direct writing is carried out according to the preset track, so that a 2mm machine precursor fiber is obtained. Wherein the preset track is a straight line of 2 mm; the specific conditions of static direct writing are as follows: the temperature is 25 ℃, the voltage is 10kV, the writing speed is 0.05cm/s, the moving speed of the receiving plate in the non-writing process is 0.5cm/s, and the pen lifting/dropping interval is 1s.
3. Post-treating the organic precursor fiber to prepare micro-nano optical phase change fiber;
calcining the organic precursor fiber obtained in the second step under the protection of argon, wherein the calcining treatment conditions are as follows: heating to 400 ℃ at a speed of 10 ℃/min, maintaining for 90min, and naturally cooling to room temperature. Because the organic precursor fiber is an organic substance containing metal atoms or ions, the substance can be subjected to chemical reaction under certain conditions (such as heating), the metal atoms or ions are reduced into metal simple substances, complex reactions can be generated after a plurality of organic precursors are mixed, and metal bonds are formed, so that the alloy is prepared.
4. Preparing an all-optical memory:
firstly, tapering the optical fiber with the coating layer partially stripped so that the diameter of the narrowest part is 25 micrometers to obtain a tapered optical fiber 16;
then, covering the tapered optical fiber 16 on the micro-nano optical phase change fiber 15 prepared in the third step, so as to ensure that the tapered part is covered on the micro-nano optical phase change fiber 15, as shown in fig. 3;
finally, packaging in an atmosphere with nitrogen as a protective gas to isolate the manufactured device from air and prevent oxidization, wherein the cross section of the obtained taper part of the all-optical memory optical fiber is shown in fig. 4.
The micro-nano optical phase change fiber 15 is used as an information storage unit, the tapered optical fiber 16 is used as a unit for triggering the micro-nano optical phase change fiber 15 to generate phase change, and the triggering mode is as follows: the tapering optical fiber conducts pulse laser, and an evanescent field of the tapering area of the optical fiber enables part of light in the optical fiber to leak, and the part of light generates laser heat induction on the micro-nano optical phase change fiber 15 to trigger the micro-nano optical phase change fiber 15 to generate phase change.
Fig. 5 is a schematic diagram of conversion between "0" state and "1" state of an all-optical memory, in which information is stored in a micro-nano phase change fiber, and a part of light leaks due to an evanescent field of a tapering region of the optical fiber, and the part of light reacts with the micro-nano phase change fiber. When the input ultrashort pulse light energy is higher, and the surface temperature of the phase change material is higher than the melting temperature Tm, the atomic configuration in the crystal is rearranged, and the phase change material is converted from a crystalline state to an amorphous state, namely, a RESET process occurs; when the input ultrashort pulse light energy is relatively low, so that the surface temperature of the phase change material is higher than the crystallization temperature Tc and lower than the melting temperature Tm, the phase change material is converted from an amorphous state to a crystalline state, namely a SET process occurs. The crystalline state energy is lower, as the "0" state, and the amorphous state energy is higher, as the "1" state. Since the GST material has a nonvolatile property, maintenance of an amorphous state does not require a continuous energy, so that it can be maintained, and thus "writing" or "erasing" can be achieved by input light. When the input ultra-short pulse light energy is lower, the surface temperature is lower than the crystallization temperature Tc, and the crystalline state of the ultra-short pulse light energy is not changed. The refractive index of the crystalline state and the amorphous state of the optical phase change material are greatly different, and the characteristic can be used for information reading. When information is read, input light passes through the phase change material, and the output light is different due to different refractive indexes of the phase change material, so that the state of the phase change material can be known through detection of the output light, and information reading is realized. In summary, the all-optical memory can realize writing, erasing and reading through one optical fiber, and a plurality of memories can store more information in parallel.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (5)
1. A preparation method of an electrostatic direct writing micro-nano optical phase change fiber is characterized in that the phase change fiber comprises three elements of germanium, antimony and tellurium, and the chemical formula is Ge x Sb y Te z Wherein x, y and z are the mass parts of the corresponding elements, x is 20, y is 20 and z is 50;
the method comprises the following steps:
step 1, preparing a precursor solution;
sequentially weighing 1.04g of five-membered ring germanium (II) complex, 0.92g of trisilane antimony and 2.04g of disilane tellurium, adding into 20mL of tetrahydrofuran, adding 4g of PMMA, and stirring for 24 hours to obtain a precursor solution, wherein the total mass of the five-membered ring germanium (II) complex, trisilane antimony and disilane tellurium in the precursor solution accounts for 20% of the mass of the precursor solution;
step 2, obtaining an organic precursor fiber by adopting an electrostatic direct writing method;
the static direct writing condition is as follows: the temperature is 15-30 ℃, the voltage is 5-25kV, the writing speed is 0.01-0.5cm/s, the moving speed of the receiving plate in the non-writing process is 0.2-2cm/s, the pen lifting/dropping interval is 0.5-2s, and the distance from the spray head to the glass slide is 3-10cm;
and step 3, carrying out heating calcination treatment on the organic precursor fiber obtained in the step 2 to obtain the micro-nano optical phase change fiber.
2. The method for preparing an electrostatic direct writing micro-nano optical phase change fiber according to claim 1, wherein the polymethyl methacrylate has a molecular weight of 30 ten thousand.
3. The method for preparing the electrostatic direct writing micro-nano optical phase change fiber according to claim 1, wherein the specific operation process of the electrostatic direct writing in the step 2 is as follows:
firstly, placing a precursor solution in a spraying device of an electrostatic direct writing device;
then, fixing the glass slide on a receiving plate by adopting a non-metal clamp, and sequentially using deionized water, acetone and absolute ethyl alcohol as ultrasonic media to respectively ultrasonically clean the glass slide for 15min;
finally, the computer is debugged by presetting a track, parameters are set, and static direct writing is completed.
4. The method for preparing the electrostatic direct writing micro-nano optical phase change fiber according to claim 1, wherein the calcining treatment conditions in the step 3 are as follows: heating to 400 ℃ at a speed of 10 ℃/min under the protection of argon, maintaining for 90min, and naturally cooling to room temperature.
5. The method for preparing the all-optical memory by using the micro-nano optical phase-change fiber obtained by the preparation method as claimed in claim 1 is characterized by comprising the following steps:
firstly, drawing micro-nano optical phase change fibers on a glass slide by adopting an electrostatic direct writing method;
then, the optical fiber with the coating layer partially stripped is tapered, and the tapered part is covered on the micro-nano phase change fiber;
and finally, packaging in vacuum or protective atmosphere to obtain the all-optical memory.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792900A (en) * | 2008-05-08 | 2010-08-04 | 气体产品与化学公司 | Binary and ternary metal chalcogenide materials and method of making and using the same |
| CN104099578A (en) * | 2013-04-11 | 2014-10-15 | 气体产品与化学公司 | Method of making a multicomponent film |
| CN104389046A (en) * | 2014-11-21 | 2015-03-04 | 天津工业大学 | Nano phase change and energy storage luminescent fibers and preparation method thereof |
| CN111320145A (en) * | 2020-02-24 | 2020-06-23 | 中国科学院上海微***与信息技术研究所 | Phase change material, phase change memory unit and manufacturing method thereof |
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| US10808316B2 (en) * | 2018-05-10 | 2020-10-20 | International Business Machines Corporation | Composition control of chemical vapor deposition nitrogen doped germanium antimony tellurium |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792900A (en) * | 2008-05-08 | 2010-08-04 | 气体产品与化学公司 | Binary and ternary metal chalcogenide materials and method of making and using the same |
| CN104099578A (en) * | 2013-04-11 | 2014-10-15 | 气体产品与化学公司 | Method of making a multicomponent film |
| CN104389046A (en) * | 2014-11-21 | 2015-03-04 | 天津工业大学 | Nano phase change and energy storage luminescent fibers and preparation method thereof |
| CN111320145A (en) * | 2020-02-24 | 2020-06-23 | 中国科学院上海微***与信息技术研究所 | Phase change material, phase change memory unit and manufacturing method thereof |
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