CN118164428A - Microchannel array and preparation method and application thereof - Google Patents
Microchannel array and preparation method and application thereof Download PDFInfo
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- CN118164428A CN118164428A CN202410290063.9A CN202410290063A CN118164428A CN 118164428 A CN118164428 A CN 118164428A CN 202410290063 A CN202410290063 A CN 202410290063A CN 118164428 A CN118164428 A CN 118164428A
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- 238000002360 preparation method Methods 0.000 title abstract description 20
- 239000011521 glass Substances 0.000 claims abstract description 224
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 11
- 238000005554 pickling Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 25
- 239000005385 borate glass Substances 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 239000005368 silicate glass Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 3
- 230000008030 elimination Effects 0.000 claims description 3
- 238000003379 elimination reaction Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 238000003491 array Methods 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 230000031700 light absorption Effects 0.000 description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 238000005491 wire drawing Methods 0.000 description 10
- 239000010985 leather Substances 0.000 description 8
- 238000005286 illumination Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910001953 rubidium(I) oxide Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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Classifications
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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
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
- C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B1/00—Devices without movable or flexible elements, e.g. microcapillary devices
- B81B1/002—Holes characterised by their shape, in either longitudinal or sectional plane
- B81B1/004—Through-holes, i.e. extending from one face to the other face of the wafer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00031—Regular or irregular arrays of nanoscale structures, e.g. etch mask layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00087—Holes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00539—Wet etching
-
- 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
-
- 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
- C03B37/14—Re-forming fibres or filaments, i.e. changing their shape
- C03B37/15—Re-forming fibres or filaments, i.e. changing their shape with heat application, e.g. for making optical fibres
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
- B81C2201/0128—Processes for removing material
- B81C2201/013—Etching
- B81C2201/0133—Wet etching
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- General Chemical & Material Sciences (AREA)
- Computer Hardware Design (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to a micro-channel array, a preparation method and application thereof, wherein the preparation method comprises the following steps: preparing a skin glass tube, a core glass rod and a glass filament; the sheath glass tube is acid-soluble, and the core glass rod and the glass filaments are acid-soluble; at least a portion of the glass filaments have a viscosity greater than the viscosity of the sheath-glass tube core glass rod; arranging glass filaments around a core glass rod, and then sleeving an epithelial glass tube to prepare a prefabricated rod; drawing the preform at high temperature and rotating to prepare monofilaments; arranging monofilaments to prepare plate sections, then performing high-temperature melting and pressing to prepare a blank plate, and slicing the blank plate to prepare a blank; and (5) pickling the blank to obtain the micro-channel array. The inner wall of the micro-channel array prepared by the invention is provided with the threaded microstructure, so that the specific surface area of the channel wall is greatly increased, and the absorption effect of the micro-channel array is obviously improved. The preparation method is suitable for micro-channel arrays with different specifications, and the preparation process is flexible to adjust, thereby providing a new idea for preparing the micro-channel arrays.
Description
Technical Field
The invention relates to the technical field of electronics, in particular to a micro-channel array and a preparation method and application thereof.
Background
The micro-channel array is a lamellar micro-channel array formed by millions of micro-scale glass channels, and has very large internal specific surface area. The micro-channel array can utilize the inner wall of the micro-channel to realize the absorption of gas, photons or particles, and has wide application in the fields of gas storage, light absorption, filtration, catalysis and the like.
Since the gas, photon or particle can be absorbed effectively only after entering the channel of the micro-channel array, the absorption effect is often improved by increasing the opening ratio of the micro-channel array in the prior art. But this method has limited improvement in the effect on the micro channel array since the aperture ratio cannot be infinitely increased.
Therefore, how to further enhance the absorption effect of the micro-channel array by adopting other ways has very important research significance.
Disclosure of Invention
The invention mainly aims to provide a micro-channel array, a preparation method and application thereof, and aims to solve the technical problem of how to further improve the absorption performance of the micro-channel array under the condition of a certain opening ratio, so that the micro-channel array is more practical.
The aim and the technical problems of the invention are realized by adopting the following technical proposal. The preparation method of the micro-channel array provided by the invention comprises the following steps:
(1) Preparing a skin glass tube, a core glass rod and a glass filament; the sheath glass tube is acid-soluble, and the core glass rod is easy to be acid-soluble; at least some of the foregoing glass filaments are acid soluble and have a viscosity greater than the viscosity of the foregoing sheath glass tube;
(2) Arranging the glass filaments around the core glass rod, and sleeving the core glass rod with the sheath glass tube to prepare a preform;
(3) Drawing the preform at high temperature and rotating to obtain monofilaments;
(4) Arranging the monofilaments to form a plate section;
(5) Carrying out high-temperature melting and pressing on the plate sections to form blank plates, and slicing the blank plates to form blanks;
(6) And (3) pickling the blank to obtain the micro-channel array.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
In some embodiments, according to the method of preparing a microchannel array of the present invention, in the step (1), the inner diameter of the sheath glass tube is 2 to 300mm, and the wall thickness is 0.2 to 10mm; the diameter of the core glass rod is 1.98-298 mm; the diameter of the glass filaments is 0.01-5 mm.
In some embodiments, according to the method for manufacturing a microchannel array described above, in the step (1), the difference between the viscosity of a part of the glass filaments and the viscosity of the sheath glass tube is equal to or greater than 5% with the viscosity of the sheath glass tube being 100%.
In some embodiments, according to the method of preparing a microchannel array of the present invention, in step (2), the glass filaments are closely and uniformly arranged around the core glass rod to form a layer;
Wherein the material of the glass filaments is the same as that of the core glass rod or the sheath glass tube.
In some embodiments, according to the method of manufacturing a microchannel array, the sheath glass tube, the core glass rod and the glass filaments are made of silicate glass or borate glass.
In some embodiments, according to the method of making a microchannel array described above, the difference in expansion coefficients of the sheath glass tube, the core glass rod, and the glass filaments is less than 30×10 -7/°c, and the difference in softening point temperature is less than 200 ℃.
In some embodiments, according to the method for preparing a microchannel array described above, in the step (3), the drawing speed is 0.1-10 m/min, the rotation speed is 100-10000 r/min, and the diameter of the monofilament is 0.03-5 mm.
The aim of the invention and the technical problems are also achieved by adopting the following technical proposal. According to the present invention, a microchannel array is provided, comprising:
an acid-resistant glass substrate; and
The micro-channel vertically penetrates through the upper bottom surface and the lower bottom surface of the acid-resistant glass substrate, the inner wall of the micro-channel is provided with a plurality of thread pits, and the thread extending direction of the thread pits is the axial direction of the micro-channel.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
In some embodiments, the micro-channels have a pore size of 0.02-4 mm according to the micro-channel array.
The aim of the invention and the technical problems are also achieved by adopting the following technical proposal. The application of any micro-channel array proposed according to the invention in image intensifier, high-energy ray detection, gas filtration or stray light elimination.
By means of the technical scheme, the micro-channel array, the preparation method and the application thereof have at least the following advantages:
According to the invention, the glass rod with the easily acid-soluble core and the acid-soluble skin glass are sleeved together, glass filaments are inserted between the glass rod with the easily acid-soluble core and the acid-soluble skin glass, at least part of the glass filaments are easily acid-soluble and have viscosity larger than that of the skin glass tube, the glass filaments are combined into the prefabricated rod, the glass filaments are enabled to leave threaded pits on the inner wall of the skin glass tube through rotary wire drawing, and then the glass with the easily acid-soluble core is removed through processes such as melt pressing and the like, so that a micro-channel array with a threaded micro-structure on the inner wall of the micro-channel is obtained, and the specific surface area of the channel wall of the micro-channel array is greatly increased, so that the absorption effect of the micro-channel array is remarkably improved. The preparation method is suitable for micro-channel arrays with different specifications, the preparation process is flexible to adjust, and micro-channel arrays with different thread inclination angles can be prepared by adjusting the rotation speed and the wire drawing speed during wire drawing; by adjusting the material and the diameter of the glass filaments, micro-channel arrays with different thread diameters, different thread depths and different thread intervals can be prepared, and a new idea is provided for preparing the micro-channel arrays.
The foregoing description is only an overview of the present invention, and is intended to provide a better understanding of the present invention, as it is embodied in the following description, with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic illustration of a preform structure in some embodiments of the invention;
FIG. 2 is a schematic illustration of two different preform structures in some embodiments of the invention.
Detailed Description
In order to further describe the technical means and effects adopted by the invention to achieve the preset aim, the following is a micro-channel array, a preparation method thereof, a specific implementation, a structure, a characteristic and effects thereof according to the invention, and the specific implementation, the structure, the characteristic and the effects thereof are described in detail below with reference to the accompanying drawings and the preferred embodiment. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
Some embodiments of the present invention provide a method for preparing a microchannel array, comprising the steps of:
(1) Preparing a skin glass tube, a core glass rod and a glass filament; the sheath glass tube is acid-soluble, and the core glass rod is easy to be acid-soluble; at least some of the foregoing glass filaments are acid soluble and have a viscosity greater than the viscosity of the foregoing sheath glass tube;
(2) Arranging the glass filaments around the core glass rod, and sleeving the core glass rod with the sheath glass tube to form a preform, as shown in FIG. 1;
(3) Drawing the preform at high temperature and rotating to obtain monofilaments;
(4) Arranging the monofilaments to form a plate section;
(5) Carrying out high-temperature melting and pressing on the plate sections to form blank plates, and slicing the blank plates to form blanks;
(6) And (3) pickling the blank to obtain the micro-channel array.
Specifically, in step (1), at least a portion of the glass filaments have a viscosity greater than that of the sheath glass tube, because the glass filaments are to leave depressions in the sheath glass tube during subsequent thermal processing, and the portion is to be readily soluble in acid so that it can be removed during subsequent pickling, thereby increasing the specific surface area of the microchannel. The viscosity of the glass filaments determines the morphology of the depressions, i.e. the radius of the depressions, which influences the specific surface area. Thus, the viscosity of the glass filaments is an important factor affecting the specific surface area. By controlling the viscosity and diameter of the glass filaments, threaded depressions of different diameters can be prepared. In the step (2), the structural schematic diagram of the prepared preform is shown in fig. 1, and the sizes of the sheath glass tube, the core glass rod and the glass filaments in the preform are matched. The glass filaments arranged around the core glass rod may be one layer or may be multiple layers.
In the step (3), the rotation speed and the drawing speed determine the thread inclination angle α, and threads having different inclination angles can be prepared by adjusting the rotation speed and the drawing speed during drawing. Wherein 0 DEG < alpha < 90 deg.
In step (4), the monofilaments are arranged to form cylindrical plate segments, for example, the cross section of the plate segments may be regular hexagon or regular triangle, etc. Preferably, the plate sections are regular hexagonal fiber bundles, and the distance between opposite sides is 20-300 mm.
In step (5), the plate segment is melted and pressed at a high temperature to form a blank, for example, the melting and pressing can be performed by a mechanical automatic melting and pressing technology, the melting and pressing temperature is 400-700 ℃, the pressure is 1-3 multiplied by 10 5 N, and the vacuum degree is less than 1 multiplied by 10 -2 Pa. Then, the blank plate is subjected to processes of slicing, rounding, polishing and the like to prepare a blank; preferably, the resulting blank has a coaxiality of 50 μm, a parallelism of 2 μm and a flatness of 0.1. Mu.m.
In the step (6), preferably, the blank is subjected to acid etching by 0.1-1 mol/L hydrochloric acid or nitric acid solution, the acid dissolution temperature is 10-70 ℃ and the time is 0.5-24 h, and finally an ultrasonic cleaner with the frequency of 40-150 KHz is adopted for cleaning, so that all the acid-soluble glass in the blank is washed off, and the micro-channel array with internal threads is obtained.
According to the preparation method of the micro-channel array, provided by the invention, the inner wall of the micro-channel array is provided with the threaded microstructure, so that the specific surface area of the channel wall is greatly increased, and the absorption effect of the micro-channel array is obviously improved. The preparation method is suitable for micro-channel arrays with different specifications, and the preparation process is flexible to adjust, thereby providing a new idea for preparing the micro-channel arrays.
In some embodiments, according to the method of preparing a microchannel array of the present invention, in the step (1), the inner diameter of the sheath glass tube is 2 to 300mm, and the wall thickness is 0.2 to 10mm; the diameter of the core glass rod is 1.98-298 mm; the diameter of the glass filaments is 0.01-5 mm.
Specifically, the inner diameter of the glass tube is too small, the preparation efficiency is low, and the requirement on wiredrawing equipment is too high if the inner diameter is too large; when the wall thickness of the skin glass tube is too small, the skin glass tube is easy to deform in preparation, and when the wall thickness is too large, the increase of the specific surface area of the whole micro-channel array is not facilitated; therefore, the inner diameter of the glass tube is controlled to be 2-300 mm, and the wall thickness is controlled to be 0.2-10 mm. The diameter of the glass filaments is too small, the requirements on the wire drawing process are high, and the glass filaments are easy to break; when the diameter of the glass filaments is too large, the skin glass tube is easily deformed. Thus, the diameter of the glass filaments is controlled to be 0.01 to 5mm.
In some embodiments, according to the method for manufacturing a microchannel array described above, in the step (1), the difference between the viscosity of a part of the glass filaments and the viscosity of the sheath glass tube is equal to or greater than 5% with the viscosity of the sheath glass tube being 100%. In particular, under the condition, the formation of clear internal thread pits is more favorable, and the preparation efficiency is improved.
In some embodiments, according to the method of preparing a microchannel array of the present invention, in step (2), the glass filaments are closely and uniformly arranged around the core glass rod to form a layer; wherein the material of the glass filaments is the same as that of the core glass rod or the sheath glass tube.
Specifically, only the glass filaments contacting the glass tube can form the internal thread concave on the surface of the glass tube, and the technical purpose can be realized by only arranging one layer of glass filaments.
The material of the glass filaments is the same as that of the core glass rod or the sheath glass tube. Wherein the glass filaments with the same material as the core glass rod are core glass filaments, and the glass filaments with the same material as the sheath glass tube are sheath glass filaments, as shown in fig. 2. In fig. 2 (a), all glass filaments are made of the same material as the core glass rod, and under this condition, only two glass materials are used for processing. In fig. 2 (b), the material of a part of the glass filaments is the same as that of the core glass rod, and the material of a part of the glass filaments is the same as that of the sheath glass tube. Under the condition, on one hand, only two glass materials are used, so that the processing is convenient; on the other hand, the core glass filaments leave thread dents on the skin glass tube and are removed in the pickling process, and the skin glass filaments are fused with the skin glass tube in the hot working process and are not removed in the pickling process, thereby playing a role of deepening the thread dents.
In some embodiments, according to the method of manufacturing a microchannel array, the sheath glass tube, the core glass rod and the glass filaments are made of silicate glass or borate glass.
Specifically, silicate glass can be selected as the skin glass tube, the expansion coefficient is (30-80) ×10 -7/DEG C, and the softening point is 400-650 ℃. For example, the sheath glass tube has a total content of ：SiO2,70.5～74.5mo1％;PbO,12.0～12.5mo1％;Bi2O3,0～2.0mol％;Na2O、K2O、Rb2O and Cs 2 O of 5.8 to 7.7mol%; baO and MgO, 4.6-6.7mol% of the catalyst; a1 2O3,1.1～3.0mo1％;TiO2, 0-2.0 mo1%.
The core glass rod and the glass filaments can be borate glass. The glass filaments can be borate glass with high viscosity, the expansion coefficient is (30-90) multiplied by 10 -7/DEG C, and the softening point is 450-700 ℃. The core glass rod can be made of high-viscosity borate glass or low-viscosity borate glass. The expansion coefficient of the low-viscosity borate glass is (20-100) multiplied by 10 -7/DEG C, and the softening point is 400-700 ℃. For example, the borate glass selected for the core glass rod and glass filaments has a total content of ：SiO2,30.3～36.4mo1％;Bi2O3,18.9～20.2mo1％;La2O3,5.9～6.1mol％;BaO and CaO of 33.7 to 39.4 mole percent 1%; a1 2O3,1.6～2.3mo1％;TiO2, 2.0 to 2.9mo1%. The viscosity of the borate glass can be adjusted by adjusting the composition of the glass, for example, increasing the content of SiO 2 and A1 2O3 in the glass composition.
In some embodiments, according to the method of making a microchannel array described above, the difference in expansion coefficients of the sheath glass tube, the core glass rod, and the glass filaments is less than 30×10 -7/°c, and the difference in softening point temperature is less than 200 ℃. Specifically, under the condition, the control of the hot working process in the step is simpler, and the yield of finished products is higher.
In some embodiments, according to the method for preparing a microchannel array described above, in the step (3), the drawing speed is 0.1-10 m/min, the rotation speed is 100-10000 r/min, and the diameter of the monofilament is 0.03-5 mm.
Specifically, if the wire drawing speed is too high and a certain thread inclination angle is to be obtained, a higher rotation speed is required, and the equipment requirement is higher; if the wire drawing rate is too low, the preparation efficiency is low, so that the wire drawing rate is controlled to be 0.1-10 m/min. The rotational speed should be matched to the drawing rate. Therefore, the wire drawing speed is controlled to be 0.1-10 m/min, and the rotating speed is controlled to be 100-10000 r/min.
The diameter of the monofilament is too small, so that the requirement on wiredrawing equipment is high; and if the diameter of the monofilament is too large, the whole specific surface area of the prepared micro-channel array is smaller. Thus, the diameter of the monofilament is controlled to be 0.03 to 5mm.
The invention provides a micro-channel array, comprising: an acid-resistant glass substrate; and the micro-channel vertically penetrates through the upper bottom surface and the lower bottom surface of the acid-soluble-resistant glass substrate, the inner wall of the micro-channel is provided with a plurality of thread pits, and the thread extending direction of the thread pits is the axial direction of the micro-channel.
In some embodiments, the micro-channels have a pore size of 0.02-4 mm according to the micro-channel array.
The invention provides application of any micro-channel array in an image intensifier, high-energy ray detection, gas filtration or stray light elimination.
The invention will be further described with reference to specific examples, which are not to be construed as limiting the scope of the invention, but rather as falling within the scope of the invention, since numerous insubstantial modifications and adaptations of the invention will now occur to those skilled in the art in light of the foregoing disclosure.
Unless otherwise indicated, materials, reagents, and the like referred to below are commercially available products well known to those skilled in the art; unless otherwise indicated, the methods are all methods well known in the art. Unless otherwise defined, technical or scientific terms used should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Example 1:
(1) Selecting acid-soluble silicate glass as leather pipe glass, wherein the expansion coefficient is 75 multiplied by 10 -7/DEG C, the softening point is 530 ℃ to prepare the leather glass pipe with the inner diameter of 30mm and the wall thickness of 4mm; selecting acid-soluble borate glass as core glass, wherein the expansion coefficient is 80 multiplied by 10 -7/DEG C, the softening point is 580 ℃, and casting and molding the core glass rod with the diameter of 28mm; the same borate glass is selected to prepare glass filaments, and the glass filaments are core glass filaments with the diameter of 1mm.
(2) The glass filaments, i.e., core glass filaments, were uniformly and tightly wrapped around a core glass rod in a single layer, and then a sheath glass tube was sleeved to make a preform, as shown in fig. 2 (a).
(3) The preform is drawn at a high temperature of 800-900 ℃ and rotated at a drawing speed of 1m/min and a rotating speed of 2000r/min to prepare the monofilament with a diameter of 0.5 mm.
(4) The monofilaments were cut into 100mm segments and arranged in a die neatly into plate segments with hexagonal cross sections, with a distance between opposite sides of 30mm.
(5) The plate section is formed into a blank by high-temperature hot-melting and pressing, the melting and pressing temperature is 580 ℃, the pressure is 2 multiplied by 10 5 N, and the vacuum degree is less than 1 multiplied by 10 -2 Pa.
(6) The blank plate is rounded by a grinder, sliced by an inner circle slicer, ground by a grinder and polished by a polisher, and the blank is prepared. The thickness of the blank is 1mm, the coaxiality is 50 mu m, the parallelism is 2 mu m, and the flatness is 0.1 mu m.
(7) The blank is eroded by 0.5mol/L hydrochloric acid solution, the acid dissolution temperature is 50 ℃ and the time is 2 hours, finally, an ultrasonic cleaner with the frequency of 100KHz is adopted for cleaning, and all the glass easy to be acid-dissolved is washed off, so as to obtain a micro-channel array, and the aperture of the micro-channel is 395 mu m.
The light absorption performance of the micro-channel array is tested by a spectrophotometer under the illumination of 400-1100 nm wavelength, and the light absorption rate is 92%.
Example 2:
(1) Selecting acid-soluble silicate glass as leather pipe glass, wherein the expansion coefficient is 75 multiplied by 10 -7/DEG C, the softening point is 530 ℃ to prepare the leather glass pipe with the inner diameter of 30mm and the wall thickness of 4mm; the same silicate glass is selected to prepare glass filaments, which are sheath glass filaments with the diameter of 1mm; selecting acid-soluble borate glass as core glass, wherein the expansion coefficient is 80 multiplied by 10 -7/DEG C, the softening point is 580 ℃, and casting and molding the core glass rod with the diameter of 28mm; the same borate glass is selected to prepare glass filaments, and the glass filaments are core glass filaments with the diameter of 1mm.
(2) The two glass filaments, the sheath glass filament and the core glass filament, are uniformly and closely spaced around the core glass rod in a single layer, and then the sheath glass tube is sleeved to produce a preform, as shown in fig. 2 (b).
(3) The preform is drawn at a high temperature of 800-900 ℃ and rotated at a drawing speed of 1m/min and a rotating speed of 2000r/min to prepare the monofilament with a diameter of 0.5 mm.
(4) The monofilaments were cut into 100mm segments and arranged in a die neatly into plate segments with hexagonal cross sections, with a distance between opposite sides of 30mm.
(5) The plate section is formed into a blank by high-temperature hot-melting and pressing, the melting and pressing temperature is 580 ℃, the pressure is 2 multiplied by 10 5 N, and the vacuum degree is less than 1 multiplied by 10 -2 Pa.
(6) The blank plate is rounded by a grinder, sliced by an inner circle slicer, ground by a grinder and polished by a polisher, and the blank is prepared. The thickness of the blank is 1mm, the coaxiality is 50 mu m, the parallelism is 2 mu m, and the flatness is 0.1 mu m.
(7) The blank is eroded by 0.5mol/L hydrochloric acid solution, the acid dissolution temperature is 50 ℃ and the time is 2 hours, finally, an ultrasonic cleaner with the frequency of 100KHz is adopted for cleaning, and all the glass easy to be acid-dissolved is washed off, so that a micro-channel array is obtained, and the aperture of the micro-channel is 370 mu m.
The light absorption performance of the micro-channel array is tested by a spectrophotometer under the illumination of 400-1100 nm wavelength, and the light absorption rate is 98%.
Example 3:
(1) Selecting acid-soluble silicate glass as leather pipe glass, wherein the expansion coefficient is 75 multiplied by 10 -7/DEG C, the softening point is 530 ℃ to prepare the leather glass pipe with the inner diameter of 30mm and the wall thickness of 4mm; selecting low-viscosity acid-soluble borate glass as core glass, wherein the expansion coefficient is 85 multiplied by 10 -7/DEG C, the softening point is 565 ℃, and casting and molding the core glass rod with the diameter of 28mm; the acid-soluble borate glass with high viscosity is selected to prepare the acid-soluble glass filaments, the expansion coefficient is 80 multiplied by 10 -7/DEG C, and the filament diameter is 1mm at the softening point of 580 ℃.
(2) The glass filaments were uniformly and tightly wrapped around a core glass rod in a single layer, and then a sheath glass tube was sleeved to make a preform, as shown in FIG. 1.
(3) The preform is drawn at a high temperature of 800-900 ℃ and rotated at a drawing speed of 1m/min and a rotating speed of 2000r/min to prepare the monofilament with a diameter of 0.5 mm.
(4) The monofilaments were cut into 100mm segments and arranged in a die neatly into plate segments with hexagonal cross sections, with a distance between opposite sides of 30mm.
(5) The plate section is formed into a blank by high-temperature hot-melting and pressing, the melting and pressing temperature is 580 ℃, the pressure is 2 multiplied by 10 5 N, and the vacuum degree is less than 1 multiplied by 10 -2 Pa.
(6) The blank plate is rounded by a grinder, sliced by an inner circle slicer, ground by a grinder and polished by a polisher, and the blank is prepared. The thickness of the blank is 1mm, the coaxiality is 50 mu m, the parallelism is 2 mu m, and the flatness is 0.1 mu m.
(7) The blank is eroded by 0.5mol/L hydrochloric acid solution, the acid dissolution temperature is 50 ℃ and the time is 2 hours, finally, an ultrasonic cleaner with the frequency of 100KHz is adopted for cleaning, and all the glass easy to be acid-dissolved is washed off, so as to obtain a micro-channel array, and the aperture of the micro-channel is 395 mu m.
The light absorption performance of the micro-channel array is tested by a spectrophotometer under the illumination of 400-1100 nm wavelength, and the light absorption rate is 91%.
Example 4:
the difference from example 1 is that in step (1), the diameter of the core glass rod was 26mm and the filament diameter of the glass filaments was 2mm.
The light absorption performance of the microchannel array was tested and the light absorption rate was 93%.
Example 5:
The difference from example 1 is that in step (1), the diameter of the core glass rod was 22mm and the filament diameter of the glass filaments was 4mm.
The light absorption performance of the micro-channel array is tested by a spectrophotometer under the illumination of 400-1100 nm wavelength, and the light absorption rate is 90%.
Example 6:
The difference from example 1 is that in step (3), a drawing rate of 1m/min and a rotation speed of 1000r/min were carried out to obtain a monofilament having a diameter of 0.5 mm.
The light absorption performance of the microchannel array was tested and the light absorption rate was 90%.
Comparative example 1:
(1) Silicate glass is selected as the glass of the leather tube, the expansion coefficient is 75 multiplied by 10 -7/DEG C, the softening point is 530 ℃ and the leather glass tube is manufactured, the inner diameter is 30mm and the wall thickness is 4mm; borate glass is selected as acid-soluble core glass, the expansion coefficient is 80 multiplied by 10 -7/DEG C, the softening point is 580 ℃, and the core glass rod is formed by casting and molding, and the diameter is 30mm.
(2) And placing the core glass rod into a skin glass tube to prepare the prefabricated rod.
(3) Drawing the preform at a high temperature of 800-900 ℃ at a drawing speed of 1m/min to obtain the monofilament with the diameter of 0.5 mm.
(4) The monofilaments were cut into 100mm segments and arranged in a die neatly into plate segments with hexagonal cross sections, with a distance between opposite sides of 30mm.
(5) The plate section is formed into a blank by high-temperature hot-melting and pressing, the melting and pressing temperature is 580 ℃, the pressure is 2 multiplied by 10 5 N, and the vacuum degree is less than 1 multiplied by 10 -2 Pa.
(6) The blank plate is rounded by a grinder, sliced by an inner circle slicer, ground by a grinder and polished by a polisher, and the blank is prepared. The thickness of the blank is 1mm, the coaxiality is 50 mu m, the parallelism is 2 mu m, and the flatness is 0.1 mu m.
(7) The blank is eroded by 0.5mol/L hydrochloric acid solution, the acid dissolution temperature is 50 ℃ and the time is 2 hours, finally, an ultrasonic cleaner with the frequency of 100KHz is adopted for cleaning, and all the glass easy to be acid-dissolved is washed off, so as to obtain a micro-channel array, and the aperture of the micro-channel is 395 mu m.
The light absorption performance of the micro-channel array is tested by a spectrophotometer under the illumination of 400-1100 nm wavelength, and the light absorption rate is 35%.
Comparative example 2:
The difference from example 1 is that in step (3), the preform was drawn at a high temperature of 800 to 900℃at a drawing rate of 1m/min and a rotation speed of 0r/min, to obtain a monofilament having a diameter of 0.5 mm.
The light absorption performance of the micro-channel array is tested by a spectrophotometer under the illumination of 400-1100 nm wavelength, and the light absorption rate is 81%.
From examples 1, 4 and 5, it is seen that the diameter of the glass filaments has an effect on the light absorption properties of the microchannel array. When the diameter of the glass filament is smaller, the generated thread dent is denser, but the depth of the dent is shallower; at this time, if the diameter of the glass filaments is properly increased, the generated thread dents are deepened, which is advantageous for the increase of the specific surface area. However, if the diameter of the glass filament is further increased, the generated thread dent is sparse, and the depth of the dent generated by the increase of the curved surface radius of the glass filament is not necessarily further deepened, the specific surface area is reduced, and the light absorptivity is reduced.
According to examples 1 and 6, it is understood that the rotation speed is increased and the inclination angle of the thread dent is increased, and the denser the thread dent is produced, the larger the specific surface area is, and the light absorbing performance is improved.
Comparing example 1 with comparative example 1, the light absorption performance of the micro-channel array with internal thread microstructure prepared by the present invention is significantly higher than that of the micro-channel array with smooth inner wall.
Comparing example 1 with comparative example 2, the light absorption performance of the micro-channel array with the internal thread micro-structure prepared by the present invention is significantly higher than that of the micro-channel array with the straight stripe micro-structure. This is because the diameter of the glass filaments is reduced during rotation, and when the same diameter glass filaments are used, the internal thread microstructure produced by the glass filaments is denser than the straight thread microstructure, so that the specific surface area of the inner wall of the microchannel is larger, and the light absorption performance is improved.
The technical features of the claims and/or the description of the present invention may be combined in a manner not limited to the combination of the claims by the relation of reference. The technical scheme obtained by combining the technical features in the claims and/or the specification is also the protection scope of the invention.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (10)
1. A method of preparing a microchannel array comprising the steps of:
(1) Preparing a skin glass tube, a core glass rod and a glass filament; the sheath glass tube is acid-resistant, and the core glass rod is easy to be acid-soluble; at least a portion of the glass filaments are acid soluble and have a viscosity greater than the viscosity of the sheath glass tube;
(2) Arranging the glass filaments around the core glass rod, and sleeving the sheath glass tube to prepare a preform;
(3) Drawing the preform rod at high temperature and rotating the preform rod to prepare monofilaments;
(4) Arranging the monofilaments to form a plate section;
(5) Carrying out high-temperature melting and pressing on the plate sections to form blank plates, and slicing the blank plates to form blanks;
(6) And (3) pickling the blank to obtain the micro-channel array.
2. The method according to claim 1, wherein in the step (1), the inner diameter of the skin glass tube is 2 to 300mm and the wall thickness is 0.2 to 10mm; the diameter of the core glass rod is 1.98-298 mm; the diameter of the glass filaments is 0.01-5 mm.
3. The production method according to claim 1, wherein in the step (1), a difference between the viscosity of a part of the glass filaments and the viscosity of the sheath glass tube is 5% or more, based on the viscosity of the sheath glass tube as 100%.
4. The method of claim 1, wherein in step (2), the glass filaments are closely and uniformly arranged around the core glass rod, surrounding a layer;
wherein the material of the glass filaments is the same as that of the core glass rod or the sheath glass tube.
5. The method according to claim 1, wherein the material of the sheath glass tube, the core glass rod and the glass filaments is silicate glass or borate glass.
6. The method of claim 1, wherein the difference in coefficients of expansion of the sheath glass tube, the core glass rod, and the glass filaments is less than 30 x 10 -7/°c and the difference in softening point temperature is less than 200 ℃.
7. The method according to claim 1, wherein in the step (3), the drawing rate is 0.1 to 10m/min, the rotation speed is 100 to 10000r/min, and the diameter of the monofilament is 0.03 to 5mm.
8. A microchannel array comprising:
an acid-resistant glass substrate; and
The micro-channel vertically penetrates through the upper bottom surface and the lower bottom surface of the acid-soluble-resistant glass substrate, the inner wall of the micro-channel is provided with a plurality of thread pits, and the thread extending direction of the thread pits is the axial direction of the micro-channel.
9. The microchannel array according to claim 8, wherein the microchannels have a pore size of 0.02-4 mm.
10. Use of a micro-channel array according to any one of claims 8-9 in an image intensifier, high energy radiation detection, gas filtration or elimination of stray light.
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