CN116375336A - Preparation method of deep ultraviolet glass with low softening temperature for LED and related lens thereof - Google Patents
Preparation method of deep ultraviolet glass with low softening temperature for LED and related lens thereof Download PDFInfo
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- CN116375336A CN116375336A CN202310081074.1A CN202310081074A CN116375336A CN 116375336 A CN116375336 A CN 116375336A CN 202310081074 A CN202310081074 A CN 202310081074A CN 116375336 A CN116375336 A CN 116375336A
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- 239000011521 glass Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000002834 transmittance Methods 0.000 claims abstract description 17
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims abstract description 13
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 229910018068 Li 2 O Inorganic materials 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical group [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 238000003723 Smelting Methods 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000005304 optical glass Substances 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 8
- 230000005540 biological transmission Effects 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910000833 kovar Inorganic materials 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000000825 ultraviolet detection Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005283 halide glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000015842 Hesperis Nutrition 0.000 description 1
- 235000012633 Iberis amara Nutrition 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
Classifications
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/0013—Re-forming shaped glass by pressing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/02—Re-forming glass sheets
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/235—Heating the glass
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/0085—Compositions for glass with special properties for UV-transmitting glass
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B3/00—Simple or compound lenses
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to the technical field of special glass materials and preparation thereof, and discloses a deep ultraviolet low softening temperature for an LEDThe glass comprises the following components in percentage by weight: siO (SiO) 2 :68‑75％、Al 2 O 3 :2‑5％、B 2 O 3 :10‑15％、Na 2 5-9% of O, the balance being alkaline oxide, the alkali metal oxide being selected from BaO, caO, li 2 At least one of O. The weight percentage of the alkali metal oxide BaO, caO, li O is as follows: 0-3% of BaO, 0-2% of CaO and Li 2 O is 0-2%, has excellent deep ultraviolet ray transmission performance, and has a transmittance of more than 70% at a wavelength of 270nm at 3.5mm, and a thermal expansion coefficient of (48+/-3) x 10 < -7 >/DEG C within a range of 30-300 ℃; has low softening temperature, and the softening temperature is less than 600 ℃; and has good chemical stability and chemical resistance grade II.
Description
Technical Field
The invention relates to the technical field of special glass materials and preparation thereof, in particular to a preparation method of deep ultraviolet low softening temperature glass for LEDs and a related lens thereof.
Background
Ultraviolet is an electromagnetic wave commonly existing in nature, light with a wavelength smaller than 380nm in the sunlight spectrum is called ultraviolet (Ultraviolet Radiation), and has important effects on ultraviolet sterilization, ultraviolet fake detection, ultraviolet illumination and the like, and meanwhile strong ultraviolet can generate certain harm to human skin, eyes and the like. Ultraviolet rays are classified into three types of ultraviolet rays, namely ultraviolet rays-A (315-380 nm), ultraviolet rays-B (280-315 nm) and ultraviolet rays-C (100-280 nm) according to the wavelength range, most of ultraviolet rays which are contained in sunlight are absorbed by ozone layers in atmospheric layers after passing through the atmosphere, the ultraviolet spectrum region of the ultraviolet rays is called Sup>A 'solar blind zone', and if the 'solar blind zone' ultraviolet signals are detected in the atmosphere, the ultraviolet signals are basically judged to be generated by the emission of artificial aircrafts such as missiles, rockets and the like. Because the light emitted by the propeller flame of the aircraft contains intense 220-280nm wave band deep ultraviolet light, the 220-280nm ultraviolet light becomes characteristic light emitted by the aircraft. The ultraviolet detector detects characteristic ultraviolet light of flame of a propeller of the aircraft to judge the threat direction and degree, and sends out alarm information in real time so as to select proper time, effective interference is implemented, measures such as avoidance are taken, and attack of enemy is resisted. The ultraviolet detection field is a research hot spot in the international ultraviolet field at present, the wavelength range of detection is 185-280nm, no response is generated to the wavelength above 280nm, and the solar blind ultraviolet characteristic is truly realized. Therefore, the method has important significance for detecting the deep ultraviolet signals, especially the deep ultraviolet signals in the range of 185 nm-280 nm. However, since 185-280nm is far from deep ultraviolet, part of the radiation belongs to the vacuum ultraviolet region, the radiation capacity is extremely high, and according to the theory of the transmission loss of electromagnetic waves in a medium, the shorter the wavelength is, the larger the loss is, so that the varieties of ultraviolet-transmitting materials which can be commercialized in the world are few, and the transmittance at 185nm is low.
There have been many studies on ultraviolet-transmitting materials at home and abroad, and these ultraviolet-transmitting materials are mainly concentrated on fluoride single crystals, halide glasses and quartz glass materials. Fluoride crystals (such as CaF2 and MgF2 crystals) are difficult to process and prepare due to the difficulty in single crystal growth and are expensive, and the fluoride crystals have inherent defects due to anisotropy, poor chemical stability and small geometric dimensions, so that the fluoride crystals have limited application; the halide glass contains fluoride or chloride, so that in the high-temperature melting process of the glass, the halide has a certain degree of erosion on the platinum crucible, the cost and the production safety hidden trouble are increased, the preparation condition is strict, and the price is high; although the transmittance of the high-purity quartz glass reaches 91% at 254nm, the quartz glass has high melting temperature, strict requirements on preparation conditions, high price and large difference between the thermal expansion coefficient and that of the kovar alloy, and can not be directly sealed with the kovar alloy, so that the application range is limited, and the application of the high-purity quartz glass is also limited.
The ultraviolet-transmitting glass material has good uniformity, high transmittance, controllable geometric shape and low price, and is the first choice material for the fields of national defense science and technology, high technology and the like. The ultraviolet-transmitting glass material has been developed in the early 70 th century in China, and is widely applied to the aspects of power grid safety monitoring, forest fire alarm, large-scale integrated circuit lithography, crop pest control, ultraviolet optical lenses, ultraviolet spectrometers and other special optical instruments, and the like, and the ultraviolet-transmitting glass material for the field of deep ultraviolet detection is lacking at present. The foreign ultraviolet-transmitting glass material products mainly comprise German Schottky 8337B and American Conning 9471 ultraviolet-transmitting glass materials, the transmittance of the German Schottky 8337B and the American Corning 9471 ultraviolet-transmitting glass materials at 200nm is 40% and 35% (the thickness is 1 mm), and the transmittance at 185nm is lower, so that the requirements of detecting the ultraviolet can not be met.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a preparation method of deep ultraviolet glass with low softening temperature for LEDs and a related lens thereof.
(II) technical scheme
To achieve the above object, the present inventionThe technical scheme is as follows: the deep ultraviolet glass with low softening temperature for the LED is characterized in that: the components in percentage by weight are: siO (SiO) 2 :68-75％、Al 2 O 3 :2-5％、B 2 O 3 :10-15％、Na 2 5-9% of O and the balance of alkaline oxide.
Preferably, the alkali metal oxide is selected from BaO, caO, li 2 At least one of O.
Preferably, the weight percentage of the alkali metal oxide BaO, caO, li O is as follows:
BaO:0-3％、CaO:0-2％、Li 2 O:0-2％。
preferably, the glass and the lens have a thickness of 3.5mm, a transmittance at a wavelength of 270nm of 70% or more, a thermal expansion coefficient in the range of 30 to 300 ℃ of (48.+ -. 3). Times.10-7/. Degree.C, and a softening point of 600 ℃ or less.
Preferably, the transition metal oxide Fe contained in the glass and the lens 2 O 3 The total amount is less than 3PPm.
The preparation method of the deep ultraviolet low softening temperature glass lens for the LED comprises the following steps:
step one, mixing: weighing the raw materials according to the weight percentage, wherein the lining material of the mixer is stainless steel or quartz (preferably quartz), and the mixing time is 30-50 minutes to form mixed raw materials;
step two, charging and melting: the feeding temperature is 1450 ℃, the materials are fed again after being fully melted, the total feeding is 2 times, and the feeding interval is about 4 hours; heating to 1350-1500 ℃ after the charging is finished, wherein the heating time is 1-2 hours; smelting at 1350-1500 deg.c for 8 hr; cooling from 1300-1500deg.C to 1300-1400 deg.C for 1-2 hr, and discharging at 1200-1350 deg.C; the mixed raw materials are melted under the protection of reducing atmosphere;
step three, glass molding and annealing: after the mixture is melted, the melted glass liquid is put into a heat-resistant mould with the temperature of 500-600 ℃ by a mechanical or casting molding mode to obtain preset molded glass, and then annealing treatment is carried out; annealing: cooling to 470-520 deg.c, 100 deg.c per hour, and naturally cooling to 200-400 deg.c to obtain semi-finished glass product or prefabricated glass product;
and fourthly, placing the prefabricated member into an optical glass molding machine, heating to 600-650 ℃ within 3-10 minutes, and maintaining the pressure for 2-5 seconds to obtain the lens with the PV value of 1 micron.
Preferably, the gas in the reducing atmosphere is carbon monoxide, and the carbon monoxide gas reducing atmosphere is obtained by placing a small crucible containing tartaric acid or citric acid in a melting furnace for heat preservation for 1.5-2.5 hours.
(III) beneficial effects
Compared with the prior art, the invention provides the preparation method of the glass with the deep ultraviolet and low softening temperature for the LED and the related lens thereof, which has the following beneficial effects:
1. the preparation method of the glass with low softening temperature and the glass with low softening temperature for the LED has excellent deep ultraviolet transmittance, the transmittance at the wavelength of 270nm is more than 70% at 3.5mm, and the thermal expansion coefficient is (48+/-3) multiplied by 10 < -7 >/DEG C within the range of 30-300 ℃; has low softening temperature, and the softening temperature is less than 600 ℃; and has good chemical stability and chemical resistance grade II.
2. The preparation method of the glass with the deep ultraviolet low softening temperature for the LED and the related lens is characterized in that the glass with the thickness of 3mm and the transmittance of the glass at the wavelength of 270nm is more than 70 percent, the preparation method of the glass is simple, environment-friendly and pollution-free, no heavy metal ions are introduced, the melting temperature is lower, the deep ultraviolet region within the range of 205 nm-280 nm has the characteristics of high ultraviolet transmittance, proper thermal expansion coefficient, low softening temperature, excellent chemical stability and the like, is suitable for sealing with kovar alloy, can be used for sealing a deep ultraviolet detection window material, and can also be used for manufacturing ultraviolet lamps, ultraviolet optical windows, ultraviolet spectrometers, optical instruments and camera lenses which require high ultraviolet-visible light transmittance, and the like.
3. Glass with deep ultraviolet and low softening temperature for LED and preparation method of related lens thereof, li 2 O、Na 2 O、K 2 O is an alkali metal oxide, an exo-glass network oxide, in a phosphate glass systemThe glass has the advantages that the glass mainly plays a role of network bond breaking to generate non-bridging oxygen, the ultraviolet-transmitting performance of the glass is related to the bridging oxygen quantity in the glass, the ultraviolet-transmitting limit moves to the short wave direction when the bridging oxygen quantity is large, the transmittance is increased, and otherwise, the transmittance is reduced.
4. The preparation method of the glass with deep ultraviolet and low softening temperature for the LED and the related lens thereof adds SiO 2 And B 2 O 3 Li added 2 O、Na 2 O、K 2 O but first repairs [ PO 4 ]、[SiO 4 ]And [ BO ] 3 ]Break point between, will [ BO ] 3 ]Conversion of the triangular layered structure into [ BO ] 4 ]The tetrahedron strengthens network connection, increases the amount of bridging oxygen, reduces the non-bridging oxygen content, and leads the ultraviolet intrinsic absorption to move to the short wave direction.
5. Glass with deep ultraviolet and low softening temperature for LED and preparation method of related lens thereof, na 2 The introduction of O can reduce the phase separation and crystallization tendency of the glass, but the ultraviolet transmittance can be greatly reduced when the weight percentage content is more than 2 percent.
5. The preparation method of the glass with deep ultraviolet and low softening temperature for the LED and the related lens thereof not only greatly improves the chemical stability, but also reduces the expansion coefficient, and more expensive, the structure does not reduce the amount of bridging oxygen, and the ultraviolet absorption limit and the ultraviolet transmittance can be ensured. Al (Al) 2 O 3 The weight percentage of the glass is 2.0-5.0 percent, the glass resistance is reduced, and the transition temperature is reduced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The deep ultraviolet glass with low softening temperature for the LED is characterized in that: the components in percentage by weight are: siO (SiO) 2 :68、Al 2 O 3 :5％、B 2 O 3 :14、Na 2 9% of O and the balance of alkaline oxide. The weight percentage of the alkali metal oxide BaO, caO, li O is as follows: 1% of BaO, 1.5% of CaO and Li 2 O:1.5％。
Example two
The deep ultraviolet glass with low softening temperature for the LED is characterized in that: the components in percentage by weight are: siO (SiO) 2 :70％、Al 2 O 3 :4％、B 2 O 3 :13％、Na 2 7% of O and the balance of alkaline oxide. The weight percentage of the alkali metal oxide BaO, caO, li O is as follows: baO 2%, caO 2%, li 2 O:2％。
Example III
The deep ultraviolet glass with low softening temperature for the LED is characterized in that: the components in percentage by weight are: siO (SiO) 2 :69％、Al 2 O 3 :3％、B 2 O 3 :12％、Na 2 9% of O and the balance of alkaline oxide. The weight percentage of the alkali metal oxide BaO, caO, li O is as follows: baO 3%, caO 2%, li 2 O:2％。
Example IV
The deep ultraviolet glass with low softening temperature for the LED is characterized in that: the components in percentage by weight are: siO (SiO) 2 :72％、Al 2 O 3 :3％、B 2 O 3 :13％、Na 2 6% of O and the balance of alkaline oxide. The weight percentage of the alkali metal oxide BaO, caO, li O is as follows: baO 3%, caO 1.5%, li 2 O:1.5％。
Example five
The deep ultraviolet glass with low softening temperature for the LED is characterized in that: the components in percentage by weight are: siO (SiO) 2 :71％、Al 2 O 3 :2％、B 2 O 3 :15％、Na 2 9% of O and the balance of alkaline oxide. The weight percentage of the alkali metal oxide BaO, caO, li O is as follows: 1% of BaO, 1% of CaO and 1% of Li 2 O:1％。
Wherein the alkali metal oxide is selected from BaO, caO, li 2 At least one of O.
Transition metal oxide Fe contained in the glass and lens 2 O 3 The total amount is less than 3PPm.
The preparation method of the deep ultraviolet low softening temperature glass lens for the LED comprises the following steps:
step one, mixing: weighing the raw materials according to the weight percentage, wherein the lining material of the mixer is stainless steel or quartz (preferably quartz), and the mixing time is 30-50 minutes to form mixed raw materials;
step two, charging and melting: the feeding temperature is 1450 ℃, the materials are fed again after being fully melted, the total feeding is 2 times, and the feeding interval is about 4 hours; heating to 1350-1500 ℃ after the charging is finished, wherein the heating time is 1-2 hours; smelting at 1350-1500 deg.c for 8 hr; cooling from 1300-1500deg.C to 1300-1400 deg.C for 1-2 hr, and discharging at 1200-1350 deg.C; the mixed raw materials are melted under the protection of reducing atmosphere;
step three, glass molding and annealing: after the mixture is melted, the melted glass liquid is put into a heat-resistant mould with the temperature of 500-600 ℃ by a mechanical or casting molding mode to obtain preset molded glass, and then annealing treatment is carried out; annealing: cooling to 470-520 deg.c, 100 deg.c per hour, and naturally cooling to 200-400 deg.c to obtain semi-finished glass product or prefabricated glass product;
and fourthly, placing the prefabricated member into an optical glass molding machine, heating to 600-650 ℃ within 3-10 minutes, and maintaining the pressure for 2-5 seconds to obtain the lens with the PV value of 1 micron.
The gas in the reducing atmosphere is carbon monoxide, and the carbon monoxide gas reducing atmosphere is obtained by placing a small crucible filled with tartaric acid or citric acid into a melting furnace and preserving the temperature for 1.5-2.5 hours.
The chemical composition (wt.%) and glass properties of the specific examples are shown in the following table
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The deep ultraviolet glass with low softening temperature for the LED is characterized in that: the components in percentage by weight are: siO (SiO) 2 :68-75％、Al 2 O 3 :2-5％、B 2 O 3 :10-15％、Na 2 5-9% of O and the balance of alkaline oxide.
2. The deep ultraviolet low softening temperature glass for LEDs of claim 1, wherein: the alkali metal oxide is selected from BaO, caO, li 2 At least one of O.
3. The deep ultraviolet low softening temperature glass for LEDs of claim 1, wherein: the weight percentage of the alkali metal oxide BaO, caO, li O is as follows:
BaO:0-3％、CaO:0-2％、Li 2 O:0-2％。
4. the deep ultraviolet low softening temperature glass for LEDs of claim 1, wherein: the glass and lens have a thickness of 3.5mm, a transmittance at a wavelength of 270nm of 70% or more, a thermal expansion coefficient in the range of 30-300 ℃ of (48+ -3). Times.10-7/. Degree.C, and a softening point of 600 ℃ or less.
5. The deep ultraviolet low softening temperature glass for LEDs of claim 1, wherein: transition metal oxide Fe contained in the glass and lens 2 O 3 The total amount is less than 3PPm.
6. A preparation method of a deep ultraviolet glass lens with low softening temperature for an LED is characterized by comprising the following steps: the method comprises the following steps:
step one, mixing: weighing the raw materials according to the weight percentage, wherein the lining material of the mixer is stainless steel or quartz (preferably quartz), and the mixing time is 30-50 minutes to form mixed raw materials;
step two, charging and melting: the feeding temperature is 1450 ℃, the materials are fed again after being fully melted, the total feeding is 2 times, and the feeding interval is about 4 hours; heating to 1350-1500 ℃ after the charging is finished, wherein the heating time is 1-2 hours; smelting at 1350-1500 deg.c for 8 hr; cooling from 1300-1500deg.C to 1300-1400 deg.C for 1-2 hr, and discharging at 1200-1350 deg.C; the mixed raw materials are melted under the protection of reducing atmosphere;
step three, glass molding and annealing: after the mixture is melted, the melted glass liquid is put into a heat-resistant mould with the temperature of 500-600 ℃ by a mechanical or casting molding mode to obtain preset molded glass, and then annealing treatment is carried out; annealing: cooling to 470-520 deg.c, 100 deg.c per hour, and naturally cooling to 200-400 deg.c to obtain semi-finished glass product or prefabricated glass product;
and fourthly, placing the prefabricated member into an optical glass molding machine, heating to 600-650 ℃ within 3-10 minutes, and maintaining the pressure for 2-5 seconds to obtain the lens with the PV value of 1 micron.
7. The method for preparing the glass lens with low softening temperature for the deep ultraviolet rays for the LED, which is characterized in that: the gas in the reducing atmosphere is carbon monoxide, and the carbon monoxide gas reducing atmosphere is obtained by placing a small crucible filled with tartaric acid or citric acid into a melting furnace and preserving the temperature for 1.5-2.5 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310081074.1A CN116375336A (en) | 2023-02-08 | 2023-02-08 | Preparation method of deep ultraviolet glass with low softening temperature for LED and related lens thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310081074.1A CN116375336A (en) | 2023-02-08 | 2023-02-08 | Preparation method of deep ultraviolet glass with low softening temperature for LED and related lens thereof |
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| CN202310081074.1A Pending CN116375336A (en) | 2023-02-08 | 2023-02-08 | Preparation method of deep ultraviolet glass with low softening temperature for LED and related lens thereof |
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