CN113024126B - Preparation method of glass microstructure with nanoscale holes - Google Patents
Preparation method of glass microstructure with nanoscale holes Download PDFInfo
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- CN113024126B CN113024126B CN202110283765.0A CN202110283765A CN113024126B CN 113024126 B CN113024126 B CN 113024126B CN 202110283765 A CN202110283765 A CN 202110283765A CN 113024126 B CN113024126 B CN 113024126B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/04—Re-forming tubes or rods
- C03B23/047—Re-forming tubes or rods by drawing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B33/00—Severing cooled glass
- C03B33/06—Cutting or splitting glass tubes, rods, or hollow products
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
- C03B37/02781—Hollow fibres, e.g. holey fibres
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/10—Non-chemical treatment
- C03B37/16—Cutting or severing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
- C03C25/68—Chemical treatment, e.g. leaching, acid or alkali treatment by etching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
A preparation method of a glass microstructure with nano-scale holes comprises the following steps of firstly, selecting two multi-component glasses with matched thermal properties and different chemical stabilities; the method comprises the following steps of (1) taking high-stability multi-component glass as substrate glass, inserting the low-stability multi-component glass into holes in the substrate glass, and obtaining a glass microstructure of the low-stability multi-component glass in nano-scale holes formed by the high-stability multi-component glass by adopting a tube-rod method and a multi-step stretching method according to the required number and diameter of the nano-scale holes; the glass microstructure is cut into a required thickness, ground and polished, is put into an erosion liquid to be immersed for a period of time, and is taken out and then is put into deionized water to be ultrasonically cleaned, so that the glass microstructure with uniform nano-scale holes is obtained. The number of the holes of the microstructure manufactured by the invention can reach more than one million, the hole diameter is uniform, and the size can be as low as nanometer.
Description
Technical Field
The invention belongs to the field of micro-nano optical devices, and particularly relates to a preparation method of a glass microstructure with nano-scale holes.
Background
With the rapid development of microelectronics and optoelectronics, and the gradual improvement of requirements on device performance, integration level and the like, the characteristic line width of the microelectronics and the optoelectronics has reached the sub-wavelength or nano-size. Optical fibers are the most commonly used transmission carrier in modern communications, and have been rapidly developed and widely used due to their distinct characteristics of compact and stable structure, no need for optical path adjustment, good heat dissipation, long service life, no need for maintenance, and the like. In recent years, micro-nano optical fibers such as nano cones, nano wires, photonic crystal fibers and the like are reported successively, and the development of micro-nano optoelectronic devices such as optical fiber sensors, optical fiber couplers, optical fiber beam splitters and the like is greatly promoted.
The micro-nano optical fiber has unique advantages in the aspects of construction and generation of sensors, couplers, resonant cavities and supercontinuum, but the optical fibers with the novel structures are not known so far, and much work needs to be systematically researched and explored. Such as: the structures of the nano-cone and the nano-wire optical fiber are single, no cladding or air is adopted as the cladding, but a composite waveguide structure is necessary for realizing the micro-nano photonic device with a specific function. For photonic crystal fibers, the minimum pore size reported at present is more than micron-scale, and submicron-scale or even nanometer-scale pore sizes have not been reported yet. The optical effects and phenomena associated with the further reduction of the aperture size are highly appreciated. On the other hand, the types of base materials currently used in research of micro-nano optical fibers include semiconductors, plastics, and quartz glass. In contrast, the multi-component glass matrix has continuous adjustability of physicochemical properties due to continuous adjustability of composition, particularly high solubility of rare earth ions, and excellent photo-thermal-electric stability capable of effectively resisting erosion of the external environment, so that the multi-component glass matrix has potential as a matrix material of the active micro-nano optical fiber. Furthermore, the more the number of times of drawing the hollow photonic crystal fiber is, the higher the possibility of deformation of the hollow is, which brings technical problems to further reduction of the diameter of the hollow hole in the drawing process.
Disclosure of Invention
The invention aims to provide a preparation method of a glass microstructure with uniform nano-scale holes, which solves the technical bottlenecks that the holes are not uniform in pore diameter and irregular in shape and even are closed due to collapse caused by directly drawing the holes.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme:
a method for preparing a glass microstructure with nano-scale holes comprises the following steps:
step 1: two kinds of multi-component glass with matched thermal properties and obviously different chemical stability are selected, one kind of multi-component glass is high-stability multi-component glass, the other kind of multi-component glass is low-stability multi-component glass, and the two kinds of multi-component glass can bear the processes of temperature rise and temperature reduction repeatedly to keep the properties of the glass unchanged;
step 2: the high-stability multi-component glass is used as substrate glass, the low-stability multi-component glass is inserted into the holes on the substrate glass, and a tube-rod method and a multi-step stretching method are adopted to obtain a glass microstructure with a required structure size according to the required number and diameter of the nano-scale holes;
and step 3: cutting the glass microstructure into required thickness, grinding and polishing, immersing the glass microstructure in an erosion liquid proved to be effective for a period of time, eroding the glass with low stability, taking out the glass, placing the glass in deionized water for ultrasonic cleaning, and thoroughly removing the low chemical stability glass and polishing powder and the like remained in the nanometer holes after being eroded to obtain the glass microstructure with uniform nanometer-scale holes.
Preferably, step 2 comprises the following sub-steps:
step 21: placing a low-stability glass preform into a drawing tower, drawing into a low-stability glass slim rod with the diameter of d, inserting the low-stability glass slim rod into a high-stability glass sleeve, and drawing and reducing by x times through the drawing tower to obtain a glass micro-structure rod A1, wherein the diameter of the low-stability glass slim rod in the glass micro-structure rod A1 is d/x;
step 22: on the cross section of a high-stability glass rod, drilling a multiplied by a number of holes with the diameter equal to the outer diameter of a glass micro-structural rod A1 by using a pre-forming machine, respectively inserting the multiplied by a number of glass micro-structural rods A1 into the holes, placing the glass micro-structural rods A1 into a wire drawing tower, and drawing and reducing the diameter by y times to obtain a glass micro-structural rod A2, wherein the diameter of the multiplied by a number of low-stability glass thin rods in the glass micro-structural rod A2 is d/x/y;
step 23: cutting the glass micro-structure rod A2 into required length and number, respectively sticking the outer cylindrical surfaces of the glass micro-structure rod A2 on a metal mould with polished surface by paraffin, grinding and polishing the outer cylindrical surface of the glass micro-structure rod A after the paraffin is solidified, and grinding and polishing the cross section of the glass micro-structure rod A2 into a square with maximum side length (the side length of the square is equal to the outer diameter of the A2 divided by the square root of 2) from a circle by turning at 90 ℃ for three times continuously; arranging the polished glass micro-structural rods A2 into a b x b square array, putting the square array into square holes with corresponding sizes in a high-stability glass rod, putting the square holes into a wire drawing tower, and drawing to reduce the size by z times to obtain glass micro-structural rods A3, wherein the diameters of (a x b) x (a x b) low-stability glass thin rods in the glass micro-structural rods A3 are d/x/y/z;
and step 24: repeating the step 23 according to the number and the diameter of the designed nano-scale holes to finally obtain the glass micro-structure rods An (n represents a non-0 natural number) with the required structure and size;
preferably, the two multi-component glasses include silicate glasses, borate glasses, phosphate glasses, germanate glasses, tellurate glasses, fluoride glasses, sulfide glasses, and their hybrid glasses, such as borosilicate glasses, germanium tellurate glasses, fluorine tellurate glasses, and the like; these multi-component glass systems are different in chemical stability, and generally, silicate glass ≈ borate glass ≈ germanate glass ≈ phosphate glass ≈ tellurite glass ≈ sulfide glass > fluoride glass, and glasses with different stability are selected as required to satisfy different technical requirements.
Preferably, the etching solution comprises hydrofluoric acid, hydrochloric acid, sulfuric acid, nitric acid, sodium hydroxide, potassium hydroxide and other solutions and mixed solutions of the hydrofluoric acid, the hydrochloric acid, the sulfuric acid, the nitric acid, the sodium hydroxide, the potassium hydroxide and the like in different mixing ratios, wherein the mixed solutions refer to different ratio mixing between acidic solutions and different ratio mixing between alkaline solutions; different acid-base solutions have different erosion capacities for multi-component glass systems with different compositions, and different acid-base solutions are selected for effectively eroding glass materials with low chemical stability.
The invention has the following beneficial technical effects:
the invention solves the technical problem that the nano-scale holes are difficult to be directly drawn due to too small size, adopts a relatively simple glass erosion technology, and can dissolve the glass with low chemical stability from the glass microstructure by adjusting the type and concentration of the chemical erosion liquid to leave the designed number of uniform nano-scale holes. The invention solves the technical bottlenecks that the pores are not uniform in pore diameter and irregular in shape and even are closed due to collapse caused by directly drawing the pores. The glass microstructure prepared by the invention has the advantages of more than one million empty holes, uniform aperture and low size of nano level. The glass microstructure prepared by the preparation method can guide light, heat and liquid, for example, glass optical fiber with nano-scale holes is prepared, and the glass microstructure has wide application prospect in the fields of optical fiber communication, optical fiber sensing, optical fiber laser and the like.
Drawings
FIG. 1 is a flow chart of a method for making a glass microstructure having nano-scale voids according to the present invention;
FIG. 2 is a diagram of the preparation process of example 1 proposed by the present invention;
wherein, the (1) -037# slim rod 1; (2) -138# sleeve 1; (3) -8 × 8 holes 1 with a hole diameter of 1.5 mm; (4) -15 × 15 square array 1; (5) -9 × 9 square array 1;
FIG. 3 is a diagram of the preparation process of example 2 proposed by the present invention;
wherein, the (6) -037# slim rod 2; (7) -138# cannula 2; (8) -8 × 8 holes 2 with a hole diameter of 1.5 mm; (9) -15 × 15 square array 2; (10) -8 x 8 square array 2;
Detailed Description
The technical scheme of the invention is described in detail in the following by combining the embodiment of the invention and the attached drawings:
as shown in fig. 1, two self-made multicomponent glasses were first screened: HSD-037 (borosilicate glass, hereinafter 037 #) and HSD-138 (silicate glass, hereinafter 138 #) have the properties set forth in the following table:
as can be seen from the table, the thermal properties of the 037# and 138# glasses are quite similar, while the chemical stability is significantly different, and are suitable for use as the low stability glass (037 #) and the high stability glass (138 #) respectively in the present invention.
Example 1:
as shown in fig. 2, a glass microstructure having 1080 × 1080 pores and 82nm pores was prepared;
1) Placing a 037# prefabricated rod with the diameter of 10mm into a drawing tower, and drawing a 037# thin rod with the diameter of 1.5mm at about 780 ℃;
2) Inserting a 037# slim rod 1 (1) with the diameter of 1.5mm into a 138# sleeve 1 (2) with the inner diameter of 1.5mm and the outer diameter of 24mm, and reducing the diameter by 16 times at about 790 ℃ through a drawing tower to obtain a glass microstructure rod A1 with the diameter of 93.75 mu m and the outer diameter of 1.5 mm;
3) On a section of a 138# rod having an outer diameter of 30.40mm, 8X 8 hollow holes 1 (3) having a hole diameter of 1.5mm were drilled by a preform machine at a center-to-center spacing of 2.5mm, and then glass microstructure rods A1 were inserted into the 64 total hollow holes, respectively, and put together in a drawing tower and reduced by 15.2 times at about 800 ℃ to obtain glass microstructure rods A2 having an outer diameter of 2mm in which 8X 8 037# rods having a diameter of about 6.17 μm were scattered;
4) Cutting the glass micro-structure rod A2 into required length and number, adhering paraffin to a metal mold with polished surface one by one, grinding and polishing the outer cylindrical surface of the glass micro-structure rod A2 after the paraffin is solidified, and grinding and polishing the original circular cross section with the outer diameter of 2mm into a square cross section with the side length of about 1.414mm by turning the glass micro-structure rod A2 for three times continuously at 90 ℃. The polished samples were then arranged in a 15X 15 square array 1 (4), placed together in a 138# sleeve with square holes having sides of about 21.21mm, the 138# sleeve having an outer diameter of 30mm, and then placed again in a draw tower and reduced by a factor of 15 at about 800 ℃ to give glass microstructured rods A3 having an outer diameter of 2mm interspersed with 120X 120 037# fine rods having a diameter of about 411 nm;
5) The circular cross section of the glass microstructure rod A3 was ground again to a square cross section having a side length of about 1.414mm, respectively, by the same method as in step 4), and then arranged into a 9 × 9 square array 1 (5), and put together into a 138# sleeve having a square hole having a side length of about 12.73mm, the 138# sleeve having an outer diameter of 20mm, and then put into a drawing tower again, and reduced by 5 times at about 790 ℃, to obtain a glass microstructure rod A4 having an outer diameter of 4mm in which 1080 × 1080 number of 037# fine rods having a diameter of about 82.2nm were scattered;
6) The glass microstructure rod A4 was cut to a desired thickness, ground and polished, and then immersed in a commercially available hydrochloric acid solution having a concentration of 36% for 2 to 3 hours. After being taken out, the sample is put into deionized water for ultrasonic cleaning for 10 minutes to remove residues of 037# glass, polishing powder and the like which are etched away and possibly exist in the nano-pores, so that a glass microstructure with 1080X 1080 pores and 82nm pore diameters is formed.
Example 2:
as shown in fig. 3, a glass microstructure having 960 × 960 pores and a pore diameter of 82nm was prepared;
1) Placing a 037# prefabricated rod with the diameter of 10mm into a drawing tower, and drawing a 037# thin rod with the diameter of 1.5mm at about 780 ℃;
2) Inserting 037# slim rod 2 (6) with a diameter of 1.5mm into 138# sleeve 2 (7) with an inner diameter of 1.5mm and an outer diameter of 30.5mm, and reducing by 20.3 times at about 790 ℃ through a drawing tower to obtain glass microstructure rod A1 with a diameter of 73.77 μm and an outer diameter of 1.5 mm;
3) On the section of the 138# rod having an outer diameter of 30mm, 8X 8 holes 2 (8) having a hole diameter of 1.5mm were drilled by a preform machine with a center-to-center spacing of 2.7mm, and then glass microstructure rods A1 were inserted into the total of 8X 8 holes, respectively, and put together in a drawing tower and reduced by 15 times at about 800 ℃ to obtain glass microstructure rods A2 having an outer diameter of 2mm in which 8X 8 037# fine rods having a diameter of about 4.92 μm were scattered;
4) Cutting the glass micro-structure rod A2 into required length and number, adhering paraffin to a metal mold with polished surface one by one, grinding and polishing the outer cylindrical surface of the glass micro-structure rod A2 after the paraffin is solidified, and grinding and polishing the original circular cross section with the outer diameter of 2mm into a square cross section with the side length of about 1.414mm by turning the glass micro-structure rod A2 for three times continuously at 90 ℃. The polished samples were then arranged in a 15X 15 square array 2 (9), placed together in a 138# sleeve with square holes of about 21.21mm side length, the 138# sleeve having an outer diameter of 30mm, and then placed again in a draw tower and reduced by a factor of 15 at about 800 ℃ to give glass microstructured rods A3 having an outer diameter of 2mm interspersed with 120X 120 037# fine rods of about 328nm diameter;
5) The circular cross section of the glass microstructure rod A3 was ground again to a square cross section having a side length of about 1.414mm, respectively, in the same manner as in the step 4), and then arranged into an 8X 8 square array 2 (10), which was put together into a 138# sleeve having square holes having a side length of about 11.31mm and an outer diameter of 16mm, and then put into a drawing tower again and reduced by 4 times at about 790 ℃ to obtain a glass microstructure rod A4 having an outer diameter of 4mm in which 960X 960 # fine rods 037 having a diameter of about 82nm were scattered;
6) The glass microstructure rod A4 was cut to a desired thickness, ground and polished, and then immersed in a commercially available hydrochloric acid solution having a concentration of 36% for 2 to 3 hours. After removal, the sample was placed in deionized water and subjected to ultrasonic cleaning for 10 minutes to remove any residues of 037# glass, polishing powder, and the like, which were etched away, from the nanopores, thereby forming a glass microstructure having 960 × 960 nanopores and a pore size of 82 nm.
In other embodiments, the hydrochloric acid etching solution may be replaced by an acidic mixed solution or an alkaline mixed solution of hydrofluoric acid, hydrochloric acid, sulfuric acid, nitric acid, sodium hydroxide, potassium hydroxide, and the like, and their different mixing ratios. The time of erosion in the erosion liquid is different according to the properties of the selected glass and the erosion liquid, and is from several minutes to tens of hours or days, and the time of ultrasonic cleaning is also different correspondingly.
Two multi-component glasses may also be replaced by borate glasses, phosphate glasses, germanate glasses, tellurate glasses, fluoride glasses, sulfide glasses and their hybrid glasses, such as borosilicate glasses, germanium tellurate glasses, fluorine tellurate glasses, etc., ordered according to stability: silicate glass is approximately equal to borate glass, germanate glass, phosphate glass, tellurate glass and fluoride glass, and two kinds of multi-component glass with different stability are selected.
The above is a complete implementation process of the present embodiment.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make modifications, alterations, additions or substitutions within the spirit and scope of the present invention.
Claims (3)
1. A method for preparing a glass microstructure with nano-scale holes is characterized by comprising the following steps:
step 1: selecting two kinds of multi-component glass with matched thermal properties and different chemical stabilities, wherein one kind of multi-component glass is high-stability multi-component glass, and the other kind of multi-component glass is low-stability multi-component glass;
the two kinds of multi-component glass comprise silicate glass, borate glass, phosphate glass, germanate glass, tellurate glass, fluoride glass, sulfide glass and mixed glass thereof;
step 2: the method comprises the following steps of (1) taking high-stability multi-component glass as substrate glass, inserting low-stability multi-component glass into holes in the substrate glass, and obtaining a glass microstructure with a required structure size by adopting a tube-rod method and a multi-step stretching method according to the required number and diameter of nano-scale holes;
and step 3: cutting the glass microstructure into required thickness, grinding and polishing, immersing the glass microstructure in an erosion liquid for a period of time, taking out the glass microstructure, placing the glass microstructure in deionized water for ultrasonic cleaning, and forming a glass microstructure with uniform nano-scale holes along with the removal of low-stability multi-component glass;
step 2 comprises the following substeps:
step 21: placing a low-stability glass preform into a wire drawing tower, drawing into a low-stability glass slim rod with the diameter of d, inserting the low-stability glass slim rod into a high-stability glass sleeve, and drawing and reducing by x times through the wire drawing tower to obtain a glass micro-structural rod A1, wherein the diameter of the low-stability glass slim rod in the glass micro-structural rod A1 is d/x;
step 22: drilling a multiplied by a number of holes with the hole diameter equal to the outer diameter of a glass micro-structural rod A1 on the cross section of a high-stability glass rod by using a preform machine, respectively inserting the multiplied by a number of glass micro-structural rods A1 into the holes, placing the glass micro-structural rods A1 into a wire drawing tower, drawing and reducing the diameter by y times to obtain a glass micro-structural rod A2, wherein the diameter of the multiplied by a number of low-stability glass thin rods in the glass micro-structural rod A2 is d/x/y;
step 23: cutting the glass micro-structure rod A2 into required length and number, respectively sticking the outer cylindrical surfaces of the glass micro-structure rod A2 on a metal mould with polished surface by paraffin, grinding and polishing the outer cylindrical surfaces of the glass micro-structure rod A after the paraffin is solidified, and grinding and polishing the cross section of the glass micro-structure rod A2 into a square with maximum side length from a circle by turning the glass micro-structure rod A three times continuously at 90 ℃; arranging the polished glass micro-structural rods A2 into a b x b square array, putting the square array into square holes with corresponding sizes in a high-stability glass rod, putting the square holes into a wire drawing tower, and drawing and reducing by z times to obtain glass micro-structural rods A3, wherein the diameters of (a x b) x (a x b) low-stability glass thin rods in the glass micro-structural rods A3 are d/x/y/z;
step 24: and (5) repeating the step (23) according to the number and the diameter of the designed nano-scale holes to finally obtain the glass micro-structural rods An with the required structure and size, wherein n represents a non-0 natural number.
2. The method of claim 1, wherein the two types of multicomponent glass can be repeatedly subjected to temperature raising and lowering processes while maintaining the glass properties.
3. The method of claim 1, wherein the etching solution comprises hydrofluoric acid, hydrochloric acid, sulfuric acid, nitric acid, sodium hydroxide, potassium hydroxide solution, and their mixture solutions in different mixing ratios.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5264722A (en) * | 1992-06-12 | 1993-11-23 | The United States Of America As Represented By The Secretary Of The Navy | Nanochannel glass matrix used in making mesoscopic structures |
| CN102015240A (en) * | 2008-04-21 | 2011-04-13 | 康宁股份有限公司 | Glass structure having sub-micron and nano-size bandgap structures and method for producing same |
| CN102515487A (en) * | 2011-11-22 | 2012-06-27 | 中国建筑材料科学研究总院 | Preparation method of high-precision superfine glass rods |
| CN108483899A (en) * | 2018-03-20 | 2018-09-04 | 华南理工大学 | One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7707854B2 (en) * | 2007-03-16 | 2010-05-04 | Ut-Battelle, Llc | Method of producing microchannel and nanochannel articles |
| US9828284B2 (en) * | 2014-03-28 | 2017-11-28 | Ut-Battelle, Llc | Thermal history-based etching |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5264722A (en) * | 1992-06-12 | 1993-11-23 | The United States Of America As Represented By The Secretary Of The Navy | Nanochannel glass matrix used in making mesoscopic structures |
| CN102015240A (en) * | 2008-04-21 | 2011-04-13 | 康宁股份有限公司 | Glass structure having sub-micron and nano-size bandgap structures and method for producing same |
| CN102515487A (en) * | 2011-11-22 | 2012-06-27 | 中国建筑材料科学研究总院 | Preparation method of high-precision superfine glass rods |
| CN108483899A (en) * | 2018-03-20 | 2018-09-04 | 华南理工大学 | One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof |
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