CN103359917A - Preparation method of infrared chalcogenide glass lenses - Google Patents
Preparation method of infrared chalcogenide glass lenses Download PDFInfo
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- CN103359917A CN103359917A CN2013102276454A CN201310227645A CN103359917A CN 103359917 A CN103359917 A CN 103359917A CN 2013102276454 A CN2013102276454 A CN 2013102276454A CN 201310227645 A CN201310227645 A CN 201310227645A CN 103359917 A CN103359917 A CN 103359917A
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- chalcogenide glass
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Abstract
The invention discloses a preparation method of infrared chalcogenide glass lenses. The preparation method comprises the following steps of: (1) putting clean lumpish chalcogenide glass in a planetary ball mill, and sieving the chalcogenide glass subjected to ball milling to obtain chalcogenide glass powder with particle diameter being not more than 6.5 microns; (2) transferring the chalcogenide glass powder into a mould, pressing the mould, naturally cooling to the room temperature and demoulding to obtain chalcogenide glass lenses; and (3) warming the chalcogenide glass lenses in a precise annealing furnace with a protective atmosphere, slowly cooling to 80-100 DEG C, finally turning off a power supply of the annealing furnace, cooling the lenses to the room temperature with the furnace to obtain the uniform chalcogenide glass lenses. The infrared chalcogenide glass lenses prepared by the method are high in uniformity and are suitable for manufacturing of various infrared lenses and especially for manufacturing of various lens elements necessary for infrared night vision systems on vehicles, for security, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of glass mirror, especially relate to a kind of preparation method of infrared chalcogenide glass eyeglass.
Background technology
Chalcogenide glass is with sulphur, selenium beyond deoxygenation and the polonium in the periodic table of elements VIA family element or the glass that tellurium element chemical combination forms or sulphur, selenium or tellurium element and other element chemical combination form.As far back as 1870, the people such as S.Sellack just found that element sulphur can form separately glass, and found that red arsenic and arsenic selenide also can form stable glass.But until the fifties in last century, chalcogenide glass just begins saturating infrared optics performance because of its excellence and is subject to people and pays close attention to widely.Nineteen fifty, the people such as the R.Frerichs of the U.S. are to As
2S
3Glass restudies this optical material of rear deduction can be used for infrared system, from then on, has raised the chalcogenide glass research boom.
At present domestic and international commercial chalcogenide glass composition mainly contains a few class glass systems such as Ge-As-Se, As-Se, Ge-Sb-Se, As-S.The production firm of external chalcogenide glass mainly contains the Amorphous Materials company of the U.S., the Vitron Gmbh company of Germany and the Umicore company of France, domesticly have that Ningbo Shun's space is infrared, the companies such as the brilliant brightness of Beijing state and Hubei Xinhua light, University Of Ningbo's infra-red material and device experimental chamber also possess the ability that pilot product is provided in batches in addition.
As a kind of novel infrared optical material, chalcogenide glass compares germanium single crystal and zinc selenide (ZnSe) crystal has following relative merits: 1. with regard to seeing through range size, the Ge monocrystalline is the widest, secondly is the ZnSe crystal.2. with regard to thermal refractive index coefficient dn/dT, ZnSe is minimum, secondly is chalcogenide glass, is up to the Ge monocrystalline, and the dn/dT of chalcogenide glass is 1/9～1/5 of Ge monocrystal material, the poor performance decided advantage of the heat that disappears.3. with regard to the utilization of resources and manufacturing tooling cost, chalcogenide glass is preponderated most, mainly be lower to the rare loose resource consumption of Ge, and can adopt the accurate die pressing technology to make in batches eyeglass as amorphous material, and ZnSe and Ge monocrystalline often need the processing of single-point diamond turning process, its production efficiency is low, and cost is high.In general, chalcogenide glass has the advantages such as the dn/dT coefficient is lower, mass-producing preparation and fabrication cost is low, the Ge resource consumption is few.The Ge monocrystal material still is the most frequently used lens material of thermal infrared imager front end optical system at present.But the rapid growth in the commercial market causes in the rapid situation about enlarging of low-cost Infrared Lens element demand, especially from the development in future of the civilian night vision system such as vehicle-mounted, security protection, chalcogenide glass has become and has replaced in the infrared thermal imagery instrument system or part replaces the splendid candidate material of traditional Ge monocrystalline eyeglass.
The manufacturing of chalcogenide glass eyeglass mainly comprises chalcogenide glass preparation and processing.The chalcogenide glass preparation need to be carried out under the anhydrous atmosphere of anaerobic owing to the singularity of its raw material.Generally be to have in chalcogenide glass raw material (such as Ge, Sb or As and Se or the S etc.) quartz ampoule of packing into, with vacuum pump be evacuated to＜10
-3Handkerchief, then with acetylene or oxyhydrogen flame with the silica tube sealing by fusing, then the quartz ampoule that sealing by fusing is good is put into rocking furnace and is waved and found, and comes out of the stove at last and carries out shrend or air chilling, breaks quartz ampoule into pieces and can obtain the chalcogenide glass sample after annealing.
The chalcogenide glass eyeglass be processed with two kinds of cold working and precise compression moldings.The processing of chalcogenide glass cold working mode and germanium single crystal and ZnSe crystal is basically identical.Compare these traditional infrared crystalline materials, the sharpest edges of chalcogenide glass are to carry out precise compression molding.The accurate die pressing of chalcogenide glass relates generally to fine annealing technique etc. after design and fabrication, molding parameters and the mold pressing of processing and fabricating, mold pressing separatory membrane of precision die.
In above-mentioned technology, it is cut into slices, is polished to prefabrication after making chalcogenide glass, pick out the prefabrication of quality good (without inner striped, calculus, crystallization etc.) through optical detection, after carrying out mold pressing and processing, the final infrared optics eyeglass that obtains precision.Cutting, polishing and select in the process, not only need to expend a large amount of man power and materials, but also can cause the wasting of resources of a large amount of frits.In addition, in order to prepare the infrared chalcogenide glass of high uniformity, also carried out the improvement of many equipment and process for above-mentioned chalcogenide glass preparation process.But the improvement of the transformation of equipment and Technology, process is complicated, all needs to drop into a large amount of resources such as manpower and financial resources, and cost is higher.Be necessary to work out the simple cheaply chalcogenide glass of high uniformity of technique and the preparation method of eyeglass.
Summary of the invention
Technical problem to be solved by this invention is, for the deficiencies in the prior art, provide that a kind of cost is low, the preparation method of the simple infrared chalcogenide glass eyeglass of technique, the infrared chalcogenide glass eyeglass homogeneity that adopts the method to prepare is high, be applicable to prepare various Infrared Lens, be particularly useful for preparing the required various lens elements of infrared night vision system such as vehicle-mounted, security protection.
The present invention solves the problems of the technologies described above the technical scheme that adopts to be: a kind of preparation method of infrared chalcogenide glass eyeglass may further comprise the steps:
1) preparation chalcogenide glass powder: clean block chalcogenide glass is put into planetary ball mill, the weight ratio of grinding element and block chalcogenide glass is 5～8:1, ball milling 12～36h under the speed conditions of 200～1000r/min, then cross 2000 mesh sieves, obtain the chalcogenide glass powder of particle diameter≤6.5 μ m;
2) compression molding: chalcogenide glass powder obtained above is transferred in the mould, then under 350～450 ℃ of temperature, under the protective atmosphere condition with the mechanical pressure of 8～30MPa to glass powder mold pressing 1～5h, then naturally cool to room temperature, move back mould, obtain the chalcogenide glass eyeglass;
3) annealing: the chalcogenide glass eyeglass that will obtain through mold pressing; put into the fine annealing stove of protective atmosphere; under 270～330 ℃ of temperature, be incubated 5～10h; then with the speed slow cooling to 80 of 0.2～1.0 ℃/min～100 ℃; close at last the power supply of annealing furnace; make the chalcogenide glass eyeglass cool to room temperature with the furnace, namely obtain uniform chalcogenide glass eyeglass.
Preferably, in the step 1), described block chalcogenide glass is the chalcogenide glass scrap stock, first described chalcogenide glass scrap stock are immersed in the dehydrated alcohol before the use, be ultrasonic cleaning 1～3 time under 20～50kHz condition in frequency again, the single ultrasonic cleaning time is 10～30min, and then dry 30～60min under 120～150 ℃ of temperature obtains clean chalcogenide glass scrap stock.
Preferably, described block chalcogenide glass is block Ge-Sb-Se class chalcogenide glass.
Compared with prior art, advantage of the present invention is as follows: the present invention is by the size of control chalcogenide glass powder, and compression molding and annealing process in conjunction with suitable have made the chalcogenide glass eyeglass without striped, flawless high uniformity; Before mold pressing, utilize planetary ball mill to prepare first the chalcogenide glass powder, when therefore preparing the chalcogenide glass eyeglass, be not subjected to the shape of chalcogenide glass raw material, the restriction of size, flexibility ratio to material choice during preparation is large, the inventive method technique is simple simultaneously, utilization ratio to raw material can reach 100%, and without wastage of material, cost is low.The inventive method is applicable to prepare various Infrared Lens, is particularly useful for preparing the required various lens elements of infrared night vision system such as vehicle-mounted, security protection.
Description of drawings
Fig. 1 is the compression molding schematic diagram that the inventive method prepares infrared chalcogenide glass eyeglass.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1: at first with Ge
28Sb
12Se
60The chalcogenide glass scrap stock immerse in the dehydrated alcohol, are ultrasonic cleaning 3 times under the 30kHz condition in frequency again, and the single ultrasonic cleaning time is 20min, and then dry 60min under 140 ℃ of temperature obtains clean Ge
28Sb
12Se
60The chalcogenide glass scrap stock; Then above-mentioned clean scrap stock are put into planetary ball mill, the weight ratio of grinding element and block chalcogenide glass is 6:1, and then ball milling 16h under the speed conditions of 400r/min crosses 2000 mesh sieves, obtains the chalcogenide glass powder of particle diameter≤6.5 μ m; The chalcogenide glass powder is transferred in the cylindrical mold, then under 380 ℃ of temperature, under the protective atmosphere condition with the mechanical pressure of 12MPa to glass powder mold pressing 1.5h, then naturally cool to room temperature, move back mould, obtain the chalcogenide glass eyeglass; The chalcogenide glass eyeglass is put into the fine annealing stove of protective atmosphere; under 300 ℃ of temperature, be incubated 6h, then with the speed slow cooling to 80 of 0.3 ℃/min ℃, close at last the power supply of annealing furnace; make the chalcogenide glass eyeglass cool to room temperature with the furnace, namely obtain uniform chalcogenide glass eyeglass.
Embodiment 2: at first with Ge
20Sb
15Se
65The chalcogenide glass scrap stock immerse in the dehydrated alcohol, are ultrasonic cleaning 3 times under the 30kHz condition in frequency again, and the single ultrasonic cleaning time is 20min, and then dry 50min under 130 ℃ of temperature obtains clean Ge
20Sb
15Se
65The chalcogenide glass scrap stock; Then above-mentioned clean scrap stock are put into planetary ball mill, the weight ratio of grinding element and block chalcogenide glass is 7:1, and then ball milling 20h under the speed conditions of 600r/min crosses 2000 mesh sieves, obtains the chalcogenide glass powder of particle diameter≤6.5 μ m; The chalcogenide glass powder is transferred in the cylindrical mold, then under 390 ℃ of temperature, under the protective atmosphere condition with the mechanical pressure of 10MPa to glass powder mold pressing 2h, then naturally cool to room temperature, move back mould, obtain the chalcogenide glass eyeglass; The chalcogenide glass eyeglass is put into the fine annealing stove of protective atmosphere; under 280 ℃ of temperature, be incubated 8h, then with the speed slow cooling to 95 of 0.5 ℃/min ℃, close at last the power supply of annealing furnace; make the chalcogenide glass eyeglass cool to room temperature with the furnace, namely obtain uniform chalcogenide glass eyeglass.
Embodiment 3: at first with Ge
30Sb
10Se
60The chalcogenide glass scrap stock immerse in the dehydrated alcohol, are ultrasonic cleaning 3 times under the 30kHz condition in frequency again, and the single ultrasonic cleaning time is 20min, and then dry 60min under 140 ℃ of temperature obtains clean Ge
30Sb
10Se
60The chalcogenide glass scrap stock; Then above-mentioned clean scrap stock are put into planetary ball mill, the weight ratio of grinding element and block chalcogenide glass is 7.5:1, and then ball milling 12h under the speed conditions of 900r/min crosses 2000 mesh sieves, obtains the chalcogenide glass powder of particle diameter≤6.5 μ m; The chalcogenide glass powder is transferred in the aspheric surface mould, then under 380 ℃ of temperature, under the protective atmosphere condition with the mechanical pressure of 14MPa to glass powder mold pressing 5h, then naturally cool to room temperature, move back mould, obtain the chalcogenide glass eyeglass; The chalcogenide glass eyeglass is put into the fine annealing stove of protective atmosphere; under 300 ℃ of temperature, be incubated 6h, then with the speed slow cooling to 100 of 0.7 ℃/min ℃, close at last the power supply of annealing furnace; make the chalcogenide glass eyeglass cool to room temperature with the furnace, namely obtain uniform chalcogenide glass eyeglass.
Embodiment 4: at first with Ge
15Sb
20Se
65The chalcogenide glass scrap stock immerse in the dehydrated alcohol, are ultrasonic cleaning 3 times under the 30kHz condition in frequency again, and the single ultrasonic cleaning time is 20min, and then dry 50min under 130 ℃ of temperature obtains clean Ge
15Sb
20Se
65The chalcogenide glass scrap stock; Then above-mentioned clean scrap stock are put into planetary ball mill, the weight ratio of grinding element and block chalcogenide glass is 8:1, and then ball milling 33h under the speed conditions of 1000r/min crosses 2000 mesh sieves, obtains the chalcogenide glass powder of particle diameter≤6.5 μ m; The chalcogenide glass powder is transferred in the aspheric surface mould, then under 410 ℃ of temperature, under the protective atmosphere condition with the mechanical pressure of 30MPa to glass powder mold pressing 1h, then naturally cool to room temperature, move back mould, obtain the chalcogenide glass eyeglass; The chalcogenide glass eyeglass is put into the fine annealing stove of protective atmosphere; under 320 ℃ of temperature, be incubated 9h, then with the speed slow cooling to 80 of 1.0 ℃/min ℃, close at last the power supply of annealing furnace; make the chalcogenide glass eyeglass cool to room temperature with the furnace, namely obtain uniform chalcogenide glass eyeglass.
Claims (3)
1. the preparation method of an infrared chalcogenide glass eyeglass is characterized in that may further comprise the steps:
1) preparation chalcogenide glass powder: clean block chalcogenide glass is put into planetary ball mill, the weight ratio of grinding element and block chalcogenide glass is 5～8:1, ball milling 12～36h under the speed conditions of 200～1000r/min, then cross 2000 mesh sieves, obtain the chalcogenide glass powder of particle diameter≤6.5 μ m;
2) compression molding: chalcogenide glass powder obtained above is transferred in the mould, then under 350～450 ℃ of temperature, under the protective atmosphere condition with the mechanical pressure of 8～30MPa to glass powder mold pressing 1～5h, then naturally cool to room temperature, move back mould, obtain the chalcogenide glass eyeglass;
3) annealing: the chalcogenide glass eyeglass that will obtain through mold pressing; put into the fine annealing stove of protective atmosphere; under 270～330 ℃ of temperature, be incubated 5～10h; then with the speed slow cooling to 80 of 0.2～1.0 ℃/min～100 ℃; close at last the power supply of annealing furnace; make the chalcogenide glass eyeglass cool to room temperature with the furnace, namely obtain uniform chalcogenide glass eyeglass.
2. the preparation method of a kind of infrared chalcogenide glass eyeglass according to claim 1, it is characterized in that in the step 1), described block chalcogenide glass is the chalcogenide glass scrap stock, first described chalcogenide glass scrap stock are immersed in the dehydrated alcohol before the use, be ultrasonic cleaning 1～3 time under 20～50kHz condition in frequency again, the single ultrasonic cleaning time is 10～30min, and then dry 30～60min under 120～150 ℃ of temperature obtains clean chalcogenide glass scrap stock.
3. the preparation method of a kind of infrared chalcogenide glass eyeglass according to claim 1 and 2 is characterized in that described block chalcogenide glass is block Ge-Sb-Se class chalcogenide glass.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336379A (en) * | 2018-11-30 | 2019-02-15 | 湖北新华光信息材料有限公司 | A kind of chalcogenide glass waste residue reuse method and gained glass |
| CN114956554A (en) * | 2022-04-21 | 2022-08-30 | 宁波大学 | Preparation method for improving mechanical strength of chalcogenide glass and chalcogenide glass |
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| JPH01313339A (en) * | 1988-06-10 | 1989-12-18 | Kubota Ltd | Mold for hot press molding of glass powder |
| JPH05279062A (en) * | 1992-04-02 | 1993-10-26 | Matsushita Electric Ind Co Ltd | Method for molding glass lens |
| CN101117264A (en) * | 2007-06-29 | 2008-02-06 | 上海晶采建材厂 | Process for making glass mosaic |
| CN101293738A (en) * | 2008-05-12 | 2008-10-29 | 中国科学院上海硅酸盐研究所 | Infrared transmission glass material and preparation method thereof |
-
2013
- 2013-06-07 CN CN2013102276454A patent/CN103359917A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01313339A (en) * | 1988-06-10 | 1989-12-18 | Kubota Ltd | Mold for hot press molding of glass powder |
| JPH05279062A (en) * | 1992-04-02 | 1993-10-26 | Matsushita Electric Ind Co Ltd | Method for molding glass lens |
| CN101117264A (en) * | 2007-06-29 | 2008-02-06 | 上海晶采建材厂 | Process for making glass mosaic |
| CN101293738A (en) * | 2008-05-12 | 2008-10-29 | 中国科学院上海硅酸盐研究所 | Infrared transmission glass material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336379A (en) * | 2018-11-30 | 2019-02-15 | 湖北新华光信息材料有限公司 | A kind of chalcogenide glass waste residue reuse method and gained glass |
| CN109336379B (en) * | 2018-11-30 | 2021-10-01 | 湖北新华光信息材料有限公司 | Sulfur glass waste residue recycling method and obtained glass |
| CN114956554A (en) * | 2022-04-21 | 2022-08-30 | 宁波大学 | Preparation method for improving mechanical strength of chalcogenide glass and chalcogenide glass |
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Application publication date: 20131023 |