CN115353287A - Phi 40mm large-size optical fiber image inverter and surface processing method and application thereof - Google Patents

Phi 40mm large-size optical fiber image inverter and surface processing method and application thereof Download PDF

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Publication number
CN115353287A
CN115353287A CN202211107285.XA CN202211107285A CN115353287A CN 115353287 A CN115353287 A CN 115353287A CN 202211107285 A CN202211107285 A CN 202211107285A CN 115353287 A CN115353287 A CN 115353287A
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optical fiber
phi
fiber image
inverter
glass
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CN115353287B (en
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张磊
贾金升
王久旺
张敬
樊志恒
许慧超
于浩洋
王云
付杨
独雅婕
黄永刚
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China Building Materials Academy CBMA
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China Building Materials Academy CBMA
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/062Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/005Surface treatment of fibres or filaments made from glass, minerals or slags by mechanical means
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/11Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
    • C03C3/112Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
    • C03C3/115Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron
    • C03C3/118Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron containing aluminium
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/04Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings formed by bundles of fibres
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

Abstract

The invention discloses a phi 40mm large-size optical fiber image inverter and a surface processing method and application thereof, wherein the surface processing method comprises the following steps: grinding the phi 40mm large-size optical fiber image inverter by 7-10 microns of carborundum, and ultrasonically purifying the ground phi 40mm large-size optical fiber image inverter by using purified water; and the large-size optical fiber image inverter with the diameter of 40mm after the purification treatment is subjected to surface polishing treatment by using a polishing medium. The surface processing method of the phi 40mm large-size optical fiber image inverter can effectively improve the surface optical uniformity of the phi 40mm large-size optical fiber image inverter, the polished phi 40mm large-size optical fiber image inverter has a flat and smooth surface, no pit defects, low scratching rate, excellent polishing effect, smooth and easy cleaning surface, is beneficial to improving the surface quality, can reduce the use of auxiliary materials in various polishing processes to the maximum extent, and has the advantages of high polishing quality, low production cost and less surface defects.

Description

Phi 40mm large-size optical fiber image inverter and surface processing method and application thereof
Technical Field
The invention relates to the field of surface processing of glass rods and manufacturing of optical fiber image transmission elements, in particular to a phi 40mm large-size optical fiber image inverter and a surface processing method and application thereof.
Background
The optical fiber image transmission element comprises an optical fiber panel, an optical fiber image inverter, an optical fiber light cone, an optical fiber image transmission bundle and the like, is a photoelectric imaging element with excellent performance, and has the characteristics of simple structure, small volume, light weight, high resolution, large numerical aperture, small interstage coupling loss, clear and real image transmission, high light transmission efficiency, optical zero thickness in image transmission, capability of improving the edge image quality and the like. The optical fiber image transmission element is widely applied to various cathode ray tubes, image pickup tubes, charge-coupled Device (CCD) coupling, medical instrument display screens, high-definition television imaging and other instruments and equipment needing image transmission in the fields of military affairs, criminal investigation, night vision, aerospace, medical treatment and the like, is a high-tech top product in the photoelectronic industry, and plays an increasingly important role in the field of low-light night vision along with the development of information technology.
The optical fiber image inverter in which the size of the effective area is larger than phi 40mm is called a large-size optical fiber image inverter. The large-size optical fiber image inverter has the characteristics of large volume, high resolution, large visual field and the like, is stable in image transmission, is widely applied to aiming in aspects of machine vision, flight simulators and the like, and can be used for gun aiming of main battle tanks, periscope reconnaissance and monitoring, nuclear experiment image timely acquisition and low-light night vision systems of large armored vehicles, tanks and large ships. The large-size optical fiber image inverter is a hard optical fiber image transmission component which is prepared by carrying out close packing arrangement, hot melt pressing and twisting forming on thousands of optical fibers with unit fiber diameter smaller than 6 mu m and can transmit images. Each optical fiber in the optical fiber image inverter has good optical insulation, so that each optical fiber can independently transmit light and transmit an image without being influenced by other optical fibers, and the optical fiber image inverter as an optical coupling image transmission device has the characteristics of high resolution, zero distortion, high light transmission efficiency and the like, has the function of inverting images, and can obtain large-size, large-view-field and long-distance observation.
The large-size optical fiber image inverter is a key device for manufacturing the large-view-field low-light-level imager, is mainly used in instruments and equipment such as a cathode ray tube, a camera tube, an image intensifier and the like which need to transmit images, has large requirements on imaging view fields, and enables the large-size optical fiber image inverter to be reused in detecting instruments and medical equipment. The key of manufacturing the large-size optical fiber image inverter is the working procedures of fusion pressing, torsion forming, cold processing and the like of a blank. The cold machining is the last process for manufacturing the large-size optical fiber image inverter, and directly influences the quality of the finished product of the optical fiber device, so that the requirement on the manufacturing process of the product is extremely high. The large-size optical fiber image inverter has large diameter, large surface area and large volume, and in the cold processing process, the larger the size of the optical fiber image inverter, the more difficult the surface processing process, the higher the fineness of the required operation, the more difficult the cold processing process, the higher the probability that the surface of the large-size optical fiber image inverter is corroded and scratched in the surface processing process, the defects of pits, protrusions and the like on the surface of the large-size optical fiber image inverter can be caused, and the defects of pits, protrusions and the like are increased due to the problems of uneven corrosion resistance and the like of the prepared core sheath material, and the manufacturing difficulty is high. In order to improve the surface smoothness and transmittance of the phi 40mm large-size optical fiber image inverter, the phi 40mm large-size optical fiber image inverter is generally subjected to surface polishing treatment, and commonly used polishing methods include a chemical polishing method and a mechanical polishing method, wherein the chemical polishing method is to perform chemical corrosion treatment on the surface of a glass rod by using an acid solution or an alkali solution, and has the defects that some effective chemical components on the surface of the glass rod are corroded or ion diffusion of a core-sheath interface is caused, the chemical solution has strong corrosion capability, is harmful to human bodies and the environment, and waste liquid cannot be recycled and is difficult to treat; the mechanical polishing method is a method for carrying out surface polishing treatment by using polishing powder, and has the defects of long processing period, low efficiency, high production cost, uneven polishing and the like, a large amount of auxiliary materials are required to be used, polishing media such as the polishing powder and the like are remained on the surface of a glass rod in the polishing treatment process, the polishing media are easily adhered to the surface of the glass rod and cannot be removed due to small particles, and the light transmission quality of a large-size optical fiber image inverter is influenced by the foreign particle fragments entering the surface, so that the internal image transmission quality is influenced.
Disclosure of Invention
The invention provides a surface processing method of a phi 40mm large-size optical fiber image inverter, aiming at solving the problems of low polishing efficiency, poor polishing effect, surface pit generation and the like in the traditional polishing method of the phi 40mm large-size optical fiber image inverter, in order to solve the surface polishing problem of the phi 40mm large-size optical fiber image inverter in the prior art and improve the surface quality of the large-size optical fiber image inverter.
In order to achieve the purpose, the invention adopts the technical scheme that:
a surface processing method of a phi 40mm large-size optical fiber image inverter comprises the following steps:
(1) Grinding the phi 40mm large-size optical fiber image inverter by 7-10 microns of carborundum, and ultrasonically purifying the ground phi 40mm large-size optical fiber image inverter by using purified water;
(2) And performing surface polishing treatment on the purified phi 40mm large-size optical fiber image inverter by using a polishing medium.
The polishing medium comprises the following substances in percentage by mass:
the content of rare earth oxide is 61-70%;
the content of the lubricant is 5-10%;
the water content is 20-25%;
1-5% of other substances;
the other substance is selected from at least one of zinc nitrate, sodium carbonate and potassium carbonate.
The rare earth oxide is cerium oxide and lanthanum oxide, the mass ratio of the cerium oxide to the lanthanum oxide is (12-16) to 1, and the granularity of the rare earth oxide is 0.5-3 mu m.
The lubricant is at least one of glycol and sodium dodecyl sulfate, and has the effects of suspending and dispersing the polishing medium, and being not easy to precipitate and stable; and/or the water is tap water or deionized water, preferably deionized water.
The granularity of the rare earth oxide is 1.0-2.0 mu m.
The time of the ultrasonic purification treatment is 50-80 minutes; the polishing treatment time is 0.5-2.0 hours; the polishing rotating speed of the phi 40mm large-size optical fiber image inverter is 150-300rad/min; the cleanliness of the polishing environment is above one hundred thousand grade; the grinding and grinding amount of the upper plane and the lower plane of the phi 40mm large-size optical fiber image inverter is 0.04mm.
The invention also provides a phi 40mm large-size optical fiber image inverter which is obtained after treatment according to the surface processing method.
The phi 40mm large-size optical fiber image inverter comprises core glass and skin glass:
the core glass has a refractive index of 1.79-1.82 and consists of the following components in percentage by mol: siO 2 2 20-25%、B 2 O 3 19-27%、CaO 0.5-5%、SrO 1-5%、BaO 15-25%、TiO 2 10-15%、La 2 O 3 5-15%、Gd 2 O 3 7.1-10%、Nb 2 O 5 1-5%;
The sheath glass has a refractive index of 1.48-1.51 and consists of the following components in percentage by mole: siO 2 2 73.0-78.0%,Al 2 O 3 1.0-5.0%,B 2 O 3 1.0-5.0%,Na 2 O 0.1-2.9%,K 2 O 7.1-12.0%,MgO 5.1-10.0%,SrO 0.1-5.0%,ZnO 0.1-1.0%,F 2 1.1-2.5%。
The invention also provides an optical fiber image transmission element which comprises the phi 40mm large-size optical fiber image inverter.
The invention further provides an application of the phi 40mm large-size optical fiber image inverter in a low-light-level image intensifier.
Compared with the prior art, the surface processing method of the phi 40mm large-size optical fiber image inverter has the following characteristics:
(1) The surface optical uniformity of the phi 40mm large-size optical fiber image inverter can be effectively improved, the improvement of the surface quality is facilitated, the surface defects are few, the polished phi 40mm large-size optical fiber image inverter has a smooth and flat surface, low roughness, no pit defect and low scratching rate, and the corrosion resistance of a core-sheath glass material and the surface roughness and scratching performance indexes of the phi 40mm large-size optical fiber image inverter can be considered;
(2) According to the invention, the processing process of obtaining the smooth surface of the phi 40mm large-size optical fiber image inverter is realized through chemical and mechanical forces, a series of chemical reactions are generated between slurry formed by mixing micro particles and a chemical solution and the surface of the phi 40mm large-size optical fiber image inverter, the purposes of excellent polishing effect, high polishing efficiency and no impurity generation after polishing are realized, a transparent and smooth polishing surface is formed on the surface of the phi 40mm large-size optical fiber image inverter, and the surface is smooth and easy to clean;
(3) The invention can reduce the use of auxiliary materials in the polishing process of the phi 40mm large-size optical fiber image inverter to the maximum extent, the rare earth oxide can effectively improve the polishing effect, the polishing effect is excellent, the lubricant can prevent the polishing surface of the glass rod from being scratched, the scratching rate is reduced, and the addition of other substances is also beneficial to the improvement of the polishing quality and the reduction of the production cost;
(4) The surface processing method disclosed by the invention is low in production cost, low in energy consumption, non-toxic, green and environment-friendly, and can well meet the industrial production requirements.
Drawings
The invention is further explained below with reference to the drawings and the embodiments.
FIG. 1 is a schematic diagram of an internal structure of an optical fiber constituting a large-sized optical fiber inverter with a diameter of 40mm according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of total reflection of optical fibers of a large-sized fiber optic inverter with a diameter of 40mm according to an embodiment of the present invention.
Wherein 1 is light absorbing frit glass, 2 is core glass, and 3 is skin glass.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in further detail below. The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments, but the present invention is not limited thereto.
Referring to fig. 1 and 2, the sheath glass tube and the core glass rod are matched and then drawn into monofilaments, each monofilament comprises outer sheath glass 3 and inner core glass 2, a plurality of monofilaments are closely arranged to form a hexagonal body with a regular hexagonal cross section, light absorbing yarns formed by drawing light absorbing material glass 1 are arranged between every two adjacent monofilaments, the light absorbing yarns are inserted into the hexagonal body to form a primary composite rod, and the primary composite rod is drawn into primary multifilaments as shown in fig. 1.
In the present invention, the term "particle size" means the size of a particle, and when the particle is a sphere, the particle size is represented by the diameter of the sphere, when the particle is a cube, the particle size is represented by the side length of the cube, and when the particle is an irregular shape, the particle size is represented by the mesh size of a screen that can just screen out the particle.
The polishing medium comprises the following substances in percentage by mass:
the content of rare earth oxide is 61-70%;
the content of the lubricant is 5-10%;
the water content is 20-25%;
1-5% of other substances;
the other substances comprise at least one of zinc nitrate, sodium carbonate and potassium carbonate, and the substances can form a film layer with weak binding force on the surface of the glass rod in a short time. When the composition of the polishing medium is within the above range, the mechanical action and the chemical action reach an equivalent state in the polishing process, and in this case, the uniformity of the chemical action is good, so that the surface tension is small, the treatment consistency is good, and a good glass rod surface polishing effect can be obtained. The polishing rotating speed of the phi 40mm large-size optical fiber image inverter is set according to the polishing time, and the polishing rotating speed of the phi 40mm large-size optical fiber image inverter is preferably 150-300rad/min.
Because the depth of the pits on the surface of the large-size optical fiber image inverter with the diameter of 40mm is generally several micrometers, the pits can be completely removed by polishing for 2-5 times, the integral height of the optical fiber image inverter before grinding can be measured, the integral height of the optical fiber image inverter after grinding can be measured, and when the grinding amount of the upper plane and the lower plane reaches 0.04mm, the grinding is finished. In order to prevent the phi 40mm large-size optical fiber image inverter from being polluted in the polishing process, a clean room is selected for polishing, and the cleanliness of the polishing environment is over one hundred thousand.
The high-refractive-index core glass material has a proper thermal expansion coefficient, and the average linear thermal expansion coefficient within the range of 30-300 ℃ is (89 +/-4) multiplied by 10 -7 /° c; having a high refractive index, n D 1.79 to 1.82; has good anti-precipitationCrystallization performance, wherein the crystallization temperature is more than 850 ℃; the chemical stability of water resistance and acid resistance is better than II level, and the preparation method has the advantages of good transparency to visible radiation, good chemical stability and the like.
The sheath glass is low-refractive-index glass made of SiO 2 -Al 2 O 3 -B 2 O 3 -RO-R 2 Of O-glass system, and incorporating F 2 Introduction of alkali metal oxide RO and alkaline earth metal oxide R as glass fining agent to eliminate bubbles and reduce refractive index of glass 2 O is used for improving the anti-crystallization performance and the high-temperature viscosity characteristic of the glass, the lower limit of the crystallization temperature of the glass is improved, a certain amount of ZnO is introduced to adjust the viscosity of the glass, the crystallization performance is effectively improved, and a skin layer glass formula and a manufacturing process which meet the requirements in the field of optical fiber image transmission elements can be obtained.
The parameters and the measuring method and the measuring instrument for the core sheath glass used for the optical fiber image transmission element are as follows:
(1) Refractive index n D Refractive index of glass at [ lambda =589.3nm];
(2) Average coefficient of thermal expansion alpha of 30-300 DEG C 30/300 [10 -7 /℃];
(3) Crystallization temperature T of glass c (℃)。
Wherein the refractive index n of the glass D Measuring by using a refractive index tester; the linear expansion coefficient of 30 to 300 ℃ is measured by a horizontal expansion instrument and expressed as an average linear expansion coefficient, and is measured by a method specified in ISO 7991, and the devitrification resistance temperature of the glass is measured by a protocol for measuring the liquefaction temperature of the glass by a gradient furnace method specified in ASTM C829-1981.
All "mole percent mol.%, based on the total molar amount of the final glass composition, are detailed herein in tables 1 and 2 for the chemical compositions (mol.%) of the core glass and skin glass examples, respectively.
TABLE 1 chemical composition (mol.%) and glass Properties of core glass examples
Figure BDA0003841157660000071
Table 2 chemical composition (mol.%) and glass properties of skin glass examples
Figure BDA0003841157660000081
The raw materials and the requirements of the core sheath glass material for preparing the phi 40mm large-size optical fiber image inverter in the following examples are as follows:
the raw materials used for the core glass and the requirements of the raw materials are as follows:
quartz sand (high purity, 150 μm oversize below 1%, 45 μm undersize below 30%, fe 2 O 3 Less than 0.01 wt.%), boric acid or boric anhydride (less than 10% for oversize products with a size of 400 μm and less than 10% for undersize products with a size of 63 μm), calcium carbonate (analytically pure, with an average particle size of 250 μm), strontium carbonate (analytically pure, with a purity of 99.0% or more), barium nitrate (analytically pure, with a purity of 99.0% or more), titanium dioxide (chemically pure), lanthanum oxide (5N), gadolinium oxide (5N), and niobium pentoxide (5N).
The raw materials and the requirements of the raw materials used by the skin layer glass are as follows:
quartz sand (high purity, 1% or less of 150 μm oversize, 30% or less of 45 μm undersize, fe) 2 O 3 Less than 1 PPm), aluminum hydroxide or alumina (analytically pure, average particle size 50 μm), boric acid or boric anhydride (400 μm oversize below 10% and 63 μm undersize below 10%), sodium carbonate (industrial soda), potassium carbonate or potassium nitrate (analytically pure, purity not less than 99.0%), basic magnesium carbonate (chemically pure, average particle size 50 μm), magnesium fluoride (analytically pure, average particle size 45 μm oversize below 1%), strontium carbonate (analytically pure, purity not less than 99.0%), zinc oxide (analytically pure).
The core sheath glass used by the phi 40mm large-size optical fiber image inverter has the following properties:
(1) The thermal property matching is good, and the thermal expansion coefficients are similar; the core glass has a coefficient of thermal expansion (3-10) x 10 higher than that of the sheath glass -7 /° c, such thermal property matchingThe bending strength, the tensile strength and the torsional strength of the optical fiber can be greatly improved.
(2) The drawn optical fiber has good compatibility matching of chemical properties, harmful ion diffusion or chemical reaction does not occur on the core and skin interfaces of the drawn optical fiber, the number of internal spot defects of the prepared optical fiber image transmission element is small, and the size of the internal spot defects is smaller than 50 mu m;
(3) The prepared optical fiber image transmission element has excellent fixed pattern noise performance, the transmittance is more than 65% in the wavelength range of 500-600nm, and no obvious multifilament boundary is observed under a 10-fold microscope.
(4) The softening point temperature of the fiber core glass is 30-100 ℃ higher than that of the skin layer glass, and the skin layer glass frit can be tightly attached to the fiber core glass frit during fiber drawing; the viscosity of the core glass and the sheath glass is approximately close to each other at the drawing temperature, which is beneficial to the stability of the fiber diameter. The two glasses are matched to draw the optical fiber filament, and neutralization reaction and harmful ion diffusion do not occur at the interface of the core and the sheath.
The fiber core material glass rod used by the phi 40mm large-size optical fiber image inverter of the invention uses rare earth oxide to improve the refractive index of glass, and after the refractive index of the core material glass of the optical fiber image transmission element is improved, the effective numerical aperture of the glass can be improved, and various performances of an optical fiber panel, the optical fiber image inverter, an optical fiber light cone and the like can be improved well.
The present invention will be further illustrated by the following specific examples.
Example 1
Preparing a polishing medium according to the following substances in percentage by mass:
the content of cerium oxide is 60%; the content of lanthanum oxide is 5%; the content of ethylene glycol is 10 percent; the content of deionized water is 20 percent; 5% of sodium carbonate; both the cerium oxide and lanthanum oxide had a particle size of 1.5. Mu.m. And uniformly mixing the substances to obtain the polishing medium.
The lubricant provided by the invention has the effects of suspending and dispersing the polishing medium, and being not easy to precipitate and stable;
a surface processing method of a phi 40mm large-size optical fiber image inverter comprises the following steps:
(1) Grinding a room with the cleanliness of more than one hundred thousand grades by using 10-micron carborundum, wherein the grinding and grinding amount of the upper plane and the lower plane of the phi 40mm large-size optical fiber image inverter is 0.04mm, and ultrasonically purifying the ground glass rod for 1 hour by using purified water;
(2) Polishing the purified phi 40mm large-size optical fiber image inverter by using a polishing medium for 1 hour, wherein the rotating speed of the phi 40mm large-size optical fiber image inverter is 200rad/min until the surface of the phi 40mm large-size optical fiber image inverter is observed by using a 10-fold microscope to have no pit defect.
The core sheath glass used for the large-size optical fiber image inverter with the diameter of 40mm is prepared according to the following method:
the preparation method of the core glass comprises the following steps:
first, the raw materials were selected in accordance with the glass composition of example 1 of Table 1, and oxides of valence-changing elements such as Fe were required in the glass raw materials 2 O 3 Etc. are strictly controlled to obtain finished glass Fe 2 O 3 The content is less than 150PPm, and the ingredients meet the glass chemical composition shown in the table 1, then a platinum crucible is used for melting for 6 hours at the temperature of 1550 ℃, in the glass melting process, the glass is stirred for 2 to 3 times to ensure that the glass is melted uniformly, after the glass is melted, the temperature is reduced to 1420 ℃ for clarification for 2 hours, then the molten glass liquid is cast into the specified requirements of a test product, annealing is carried out, the annealing process is carried out, the temperature is maintained for 2 hours at 605 ℃, the temperature is reduced to 100 ℃ within 24 hours, and then the glass is cooled to the room temperature along with a furnace. The test performance is shown in table 1, wherein (1) the refractive index is 1.81; (2) Average linear expansion coefficient of 85 x 10 at 30-300 DEG C -7 /℃。
The preparation method of the skin layer glass comprises the following steps:
the glass compositions of example 1 of Table 2 were selected and the oxides of the valence-changing elements, such as Fe, were required in the glass raw materials 2 O 3 Etc. are strictly controlled to obtain finished glass Fe 2 O 3 The content is less than 1PPm, and the ingredients meet the glass chemical composition shown in the table 2, then a pure platinum crucible is used for melting for 6 hours at the temperature of 1550 ℃, in the glass melting process, the glass is stirred for 2 to 3 times, and the glass is preparedAfter the uniform melting, drawing the molten glass into a glass tube, and then annealing, wherein the test performance is shown in table 2, wherein (1) the refractive index is 1.48; (2) Average linear expansion coefficient of 85 x 10 at 30-300 DEG C -7 /° c; (3) the devitrification temperature of the glass is 910 ℃.
Example 2
Preparing a polishing medium according to the following substances in percentage by mass:
the content of cerium oxide was 57%; the content of lanthanum oxide is 4%; the ethylene glycol content is 4%; the content of the sodium dodecyl sulfate is 5 percent; the content of deionized water is 25%; 5% of zinc nitrate; particle size of cerium oxide 1 μm particle size of lanthanum oxide 2.0 μm. And uniformly mixing the substances to obtain the polishing medium.
The lubricant provided by the invention has the effects of suspending and dispersing the polishing medium, and being not easy to precipitate and stable;
a surface processing method of a phi 40mm large-size optical fiber image inverter comprises the following steps:
(1) Grinding rooms with cleanliness of more than one hundred thousand grades by 7-micron carborundum, wherein the grinding and grinding amount of the upper plane and the lower plane of the phi 40mm large-size optical fiber image inverter is 0.04mm, and ultrasonically purifying the ground glass rod for 50 minutes by using purified water;
(2) Polishing the purified phi 40mm large-size optical fiber image inverter for 0.5 hour by using a polishing medium, wherein the rotating speed of the phi 40mm large-size optical fiber image inverter is 300rad/min; the large-size optical fiber image inverter with diameter of 40mm is suitable for observing the surface by a 10-fold microscope without pit defects.
The core sheath glass of the large-size optical fiber image inverter with the diameter of 40mm is prepared according to the following method:
the preparation method of the core glass comprises the following steps:
referring to table 1, example 2, the actual composition of the glass uses the same raw materials and raw material requirements as those of example 1 in table 1, the glass is melted at 1500 ℃ for 8 hours, the glass is stirred for 2 times in the glass melting process to melt the glass uniformly, the temperature is reduced to 1400 ℃ after the glass is melted, the glass is clarified for 1.5 hours, then the molten glass liquid is cast into the specified requirements of a test product, the annealing is carried out, the annealing process is carried out, the temperature is maintained for 1.5 hours at 600 ℃, the temperature is reduced to 100 ℃ after 23 hours, and the glass is cooled to room temperature along with a furnace.
The basic properties of the test specimens are shown in table 1 using the same test conditions as in example 1. (1) a refractive index of 1.81; an average linear expansion coefficient of 91X 10-7/DEG C at 30-300 ℃.
The preparation method of the skin layer glass comprises the following steps:
actual composition of glass referring to table 2, example 2, the basic properties of the samples are shown in table 2 using the same raw materials and raw material requirements as in table 2, example 1, and employing a melt process regime of melting at 1450 ℃ for 10 hours and the same test conditions as in example 1. (1) a refractive index of 1.49; (2) Average linear expansion coefficient of 82 x 10 at 30-300 DEG C -7 /° c; and (3) the crystallization temperature of the glass is 915 ℃.
Example 3
Preparing a polishing medium according to the following substances in percentage by mass:
the content of cerium oxide is 65%; the content of lanthanum oxide is 5%; the content of ethylene glycol is 5 percent; the content of tap water is 22%; 1% of zinc nitrate; 2% of sodium carbonate; the particle size of cerium oxide was 0.5 and that of lanthanum oxide was 3.0. Mu.m. And uniformly mixing the substances to obtain the polishing medium.
The lubricant provided by the invention has the effects of suspending and dispersing the polishing medium, and being not easy to precipitate and stable;
a surface processing method of a phi 40mm large-size optical fiber image inverter comprises the following steps:
(1) Grinding a room with the cleanliness of more than one hundred thousand grades by using 8-micron carborundum, wherein the grinding and grinding amount of the upper plane and the lower plane of the phi 40mm large-size optical fiber image inverter is 0.04mm, and ultrasonically purifying the ground glass rod by using purified water for 80 minutes;
(2) Polishing the purified phi 40mm large-size optical fiber image inverter for 2.0 hours by using a polishing felt and a polishing medium, wherein the rotating speed of the phi 40mm large-size optical fiber image inverter is 150rad/min; the large-size optical fiber image inverter with diameter of 40mm is suitable for observing the surface by a 10-fold microscope without pit defects.
The core sheath glass used for the large-size optical fiber image inverter with the diameter of 40mm is prepared according to the following method:
the preparation method of the core glass comprises the following steps:
referring to table 1, example 3, the actual composition of the glass uses the same raw materials and raw material requirements as those of example 1 in table 1, melting is carried out at 1480 ℃ for 10 hours, in the glass melting process, the glass is stirred for 3 times to melt the glass uniformly, after the glass is melted, the temperature is reduced to 1380 ℃ to clarify for 2.5 hours, then the molten glass liquid is cast into specified test product requirements, annealing is carried out, the annealing process is carried out after 2.5 hours of heat preservation at 595 ℃ and 20 hours of temperature reduction to 100 ℃, and then furnace cooling is carried out to room temperature
The basic properties of the test specimens are shown in table 1 using the same test conditions as in example 1. (1) a refractive index of 1.80; average linear expansion coefficient of 93 x 10 at 30-300 deg.C -7 /℃。
The preparation method of the skin layer glass comprises the following steps:
actual composition of glass referring to table 2, example 3, using the same raw materials and raw material requirements as in table 2, example 1, and employing a melting schedule of melting at 1500 ℃ for 8 hours and the same test conditions as in example 1, the basic properties of the samples are shown in table 1. (1) a refractive index of 1.50; (2) Average linear expansion coefficient of 86 x 10 at 30-300 DEG C -7 /° c; (3) the devitrification temperature of the glass is 910 ℃.
Example 4
Preparing a polishing medium according to the following substances in percentage by mass:
the content of cerium oxide is 60%; the content of lanthanum oxide is 4%; the content of sodium dodecyl sulfate is 10 percent; the content of tap water is 25%; 1% of potassium carbonate; the particle size of cerium oxide was 1.5 μm and the particle size of lanthanum oxide was 2.0. Mu.m. And uniformly mixing the substances to obtain the polishing medium.
The lubricant provided by the invention has the effects of suspending and dispersing the polishing medium, and being not easy to precipitate and stable;
a surface processing method of a phi 40mm large-size optical fiber image inverter comprises the following steps:
(1) Grinding a room with the cleanliness of more than one hundred thousand grades by using 9-micron carborundum, wherein the grinding and grinding amount of the upper plane and the lower plane of the phi 40mm large-size optical fiber image inverter is 0.04mm, and ultrasonically purifying the ground glass rod for 1 hour by using purified water;
(2) The phi 40mm large-size optical fiber image inverter after the purification treatment is polished by a polishing medium for 1.5 hours, and the rotating speed of the phi 40mm large-size optical fiber image inverter is 250rad/min.
The core sheath glass used by the phi 40mm large-size optical fiber image inverter is prepared according to the following method:
the preparation method of the core glass comprises the following steps:
referring to table 1, example 4, the actual composition of the glass uses the same raw materials and raw material requirements as those of example 1 in table 1, the glass is melted at 1450 ℃ for 5 hours, the glass is stirred for 2-3 times in the glass melting process to be uniformly melted, the temperature is reduced to 1390 ℃ after the glass is melted, the glass is clarified for 2 hours, then the molten glass liquid is cast into the specified requirements of a test product, the annealing process is carried out, the temperature is maintained at 610 ℃ for 2 hours, the temperature is reduced to 100 ℃ for 24 hours, and the glass is cooled to room temperature along with a furnace,
the basic properties of the test specimens are shown in table 1 using the same test conditions as in example 1. (1) a refractive index of 1.82; an average linear expansion coefficient of 89 x 10 at 30-300 deg.C -7 /℃。
The preparation method of the skin layer glass comprises the following steps:
actual composition of glass referring to table 2, example 4, using the same raw materials and raw material requirements as in table 2, example 1, and taking the melting process regime and test conditions to melt at 1480 c for 7 hours, the basic properties of the samples are shown in table 1. (1) a refractive index of 1.51; (2) Average linear expansion coefficient of 88 x 10 at 30-300 DEG C -7 /° c; (3) the glass had a crystallization temperature of 905 ℃.
Example 5
Preparing a polishing medium according to the mass percentage of the substance in the example 1;
a surface processing method of a phi 40mm large-size optical fiber image inverter is as in example 1;
the core sheath glass used for the large-size optical fiber image inverter with the diameter of 40mm is prepared according to the following method:
the preparation method of the core glass comprises the following steps:
actual glass composition referring to table 1, example 5, the basic properties of the samples are shown in table 1 using the same raw materials and raw material requirements as in table 1, and using the same melting process schedule and test conditions. (1) a refractive index of 1.79; average linear expansion coefficient of 87 multiplied by 10 at 30-300 DEG C -7 /℃。
The preparation method of the skin layer glass comprises the following steps:
actual composition of the glass referring to table 2, example 5, using the same raw materials and raw material requirements as in table 2, example 1, and using the same melting process regime and test conditions, the basic properties of the samples are shown in table 1. (1) a refractive index of 1.51; (2) Average linear expansion coefficient of 84 x 10 at 30-300 DEG C -7 /° c; and (3) the crystallization temperature of the glass is 905 ℃.
The data obtained by the embodiment can show that the phi 40mm large-size optical fiber image inverter has the advantages of good surface processing quality, high surface polishing quality, low production cost, few surface defects and the like, does not contain heavy metal oxide which seriously harms the environment, and can be applied to large-size low-light-level image intensifiers.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. A surface processing method of a phi 40mm large-size optical fiber image inverter is characterized by comprising the following steps:
(1) Grinding the phi 40mm large-size optical fiber image inverter by 7-10 microns of carborundum, and ultrasonically purifying the ground phi 40mm large-size optical fiber image inverter by purified water;
(2) And performing surface polishing treatment on the purified phi 40mm large-size optical fiber image inverter by using a polishing medium.
2. The surface processing method of a phi 40mm large-size optical fiber image inverter as claimed in claim 1, wherein the polishing medium comprises the following substances in percentage by mass:
the content of rare earth oxide is 61-70%;
the content of the lubricant is 5-10%;
the water content is 20-25%;
1-5% of other substances;
the other substance is selected from at least one of zinc nitrate, sodium carbonate and potassium carbonate.
3. The surface processing method of a phi 40mm large-size optical fiber image inverter as claimed in claim 2, wherein the rare earth oxide is cerium oxide and lanthanum oxide, and the mass ratio of the cerium oxide to the lanthanum oxide is (12-16): 1 the granularity of the rare earth oxide is 0.5-3 mu m.
4. The method for surfacing a phi 40mm large-sized optical fiber inverter according to claim 3, wherein the lubricant is at least one of ethylene glycol and sodium dodecyl sulfate; and/or the water is tap water or deionized water.
5. The surface processing method of a phi 40mm large-sized optical fiber inverter according to claim 3, wherein the particle size of the rare earth oxide is 1.0-2.0 μm.
6. The surface processing method of a phi 40mm large-sized optical fiber inverter according to any one of claims 1 to 5, wherein the ultrasonic cleaning treatment time is 50 to 80 minutes; the polishing treatment time is 0.5-2.0 hours; the polishing rotating speed of the phi 40mm large-size optical fiber image inverter is 150-300rad/min; the cleanliness of the polishing environment is above one hundred thousand grade; the grinding and grinding amount of the upper plane and the lower plane of the phi 40mm large-size optical fiber image inverter is 0.04mm.
7. A large-sized fiber optic inverter having a diameter of 40mm, obtained by treating the same according to the surface processing method of any one of claims 1 to 6.
8. The phi 40mm large-sized fiber optic inverter of claim 7, wherein the phi 40mm large-sized fiber optic inverter comprises a core glass and a skin glass:
the core glass has a refractive index of 1.79-1.82 and consists of the following components in percentage by mole: siO 2 2 20-25%、B 2 O 3 19-27%、CaO 0.5-5%、SrO 1-5%、BaO 15-25%、TiO 2 10-15%、La 2 O 3 5-15%、Gd 2 O 3 7.1-10%、Nb 2 O 5 1-5%;
The sheath glass has a refractive index of 1.48-1.51 and consists of the following components in percentage by mole: siO 2 2 73.0-78.0%,Al 2 O 3 1.0-5.0%,B 2 O 3 1.0-5.0%,Na 2 O 0.1-2.9%,K 2 O 7.1-12.0%,MgO 5.1-10.0%,SrO 0.1-5.0%,ZnO 0.1-1.0%,F 2 1.1-2.5%。
9. An optical fiber image-transmitting member comprising a large-sized optical fiber inverter of phi 40mm according to claim 7 or 8.
10. Use of the optical fiber image transfer element of claim 9 in a micro-optical image intensifier.
CN202211107285.XA 2022-09-09 2022-09-09 Phi 40mm large-size optical fiber image inverter and surface processing method and application thereof Active CN115353287B (en)

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