CN111574051A - PBG Er-doped3+Heavy metal oxide glass - Google Patents
PBG Er-doped3+Heavy metal oxide glass Download PDFInfo
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- CN111574051A CN111574051A CN202010504366.8A CN202010504366A CN111574051A CN 111574051 A CN111574051 A CN 111574051A CN 202010504366 A CN202010504366 A CN 202010504366A CN 111574051 A CN111574051 A CN 111574051A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
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- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/122—Silica-free oxide glass compositions containing oxides of As, Sb, Bi, Mo, W, V, Te as glass formers
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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Abstract
The invention relates to a PBG Er-doped fiber3+The heavy metal oxide glass comprises the following raw materials in percentage by mole: (37-57) PbO- (0-20) PbF2‑25Bi2O3‑18Ga2O3PbO and PbF2Is 57%; er doped with 1mol percent2O3(ii) a Calculating the mass required by each raw material according to the mol percentage of the raw materials, putting the raw materials into an agate mortar for grinding and stirring, and uniformly mixing; putting the mixture into a platinum crucible, and melting for 30 minutes at 900 ℃ in an electric furnace; pouring the molten glass on a preheated copper plate at 300 ℃,preserving the heat in a precise annealing furnace for 2 hours, and then cooling the furnace to room temperature to obtain the mid-infrared broadband luminous heavy metal oxide glass; the PBG glass prepared by the invention has the characteristics of high transparency, high luminous intensity, high stability and the like, the preparation process is simple, and mass production can be realized.
Description
Technical Field
The invention relates to heavy metal oxide glass, in particular to PBG (poly-p-phenylene benzobisoxazole) doped Er3+Heavy metal oxide glasses.
Background
Mid-infrared (2-5 μm) lasers have found wide application in many fields such as gas detection, medical surgery, military radar, etc. The band has strong absorption peaks of a plurality of common harmful gas molecules, such as ammonia gas (2.1 μm), hydrogen fluoride (2.5 μm), methane (2.35 μm and 3.3 μm), formaldehyde (3.5 μm), hydrogen chloride (3.5 μm), nitrous oxide (3.9 μm and 4.5 μm), sulfur dioxide (4 μm), carbon dioxide (4.25 μm), carbon monoxide (2.3 μm and 4.6 μm) and the like, so the mid-infrared laser can be applied to the related fields of gas detection, environmental protection and the like; taking 2.7 μm laser as an example, because the luminescence peak is positioned in the absorption peak of water molecules near 3 μm, and the laser has strong directionality and high power density, most of energy can be converged at one point, the laser can be used in the field of medical minimally invasive surgery; in addition, the mid-infrared laser can also be used in military fields such as heat source detection, night vision and the like.
Common methods for generating mid-infrared laser include: through optical parametric oscillation, difference frequency generation and nonlinear optical effects such as Raman effect in crystal or optical fiber; produced using a heterojunction semiconductor or quantum cascade semiconductor; and most commonly solid-state and fiber laser generation, etc. The core component of a solid state laser is the gain medium. The characteristics of the gain medium determine the output characteristics of the solid state laser. The gain medium of a general solid laser is made by doping a crystal or glass with rare earth ions or transition metal ions that can generate luminescence transitions. In general, the light-emitting range of the material doped with transition metal ions is generally broadband light emission, but the intensity of the light emission is also limited; in addition, the transition metal ion doped luminescent material generally has severe requirements on the matrix material and the required conditions, thereby limiting the application range. Common rare earth ions can generate mid-infrared light under different conditions, such as thulium (2.3 μm), erbium (2.7 μm, 3.5 μm), holmium (2.9 μm, 3.2 μm, 3.9 μm), dysprosium (2.9 μm, 4.3 μm), praseodymium (3.6 μm), and the like. Wherein erbium ion (Er)3+) Luminescence around 2.7 μm has been achieved in a variety of crystalline or glassy matrices due to the advantages of lower required doping concentrations, ease of implementation at low pump powers, higher luminescence intensities, etc.In addition, the erbium ions can realize effective pumping by using a commercial 980nm or 808nm laser diode without other co-doped ions, so that the cost of the erbium-doped luminescent material can be reduced, and the possibility of large-scale application of the erbium-doped luminescent material is ensured.
In order to obtain stronger erbium ion 2.7 μm mid-infrared luminescence, rare earth doped crystals or glass is generally selected as a matrix material. For common laser crystals such as yttrium aluminum garnet crystal (YAG), yttrium vanadate crystal (YVO)4) Lithium yttrium fluoride crystals (YLF), etc., which generally have a relatively low moisture resistance, affecting their long-term use or storage, although their luminous intensity is generally higher than that of doped materials of glass matrix; the thermal expansion coefficient and the thermo-optic coefficient of the crystal are generally higher than those of glass materials, so that the output of the crystal is influenced by heat accumulation when the crystal works at high power or for a long time; in addition, the mass production of the crystals is generally complex in process or high in cost, and the glass can be produced in a large scale, and glass matrix materials with different physical properties can be obtained by adjusting the components of the glass or the production process according to the production requirements.
At present, the common intermediate infrared luminescent glass substrate materials include tellurate glass, phosphate glass, fluoride glass and the like, wherein zirconium fluoride (ZrF) is used4) ZBLAN (ZrF) as main component4-BaF2-LaF3-AlF3NaF) fluoride glasses are most widely used. The ZBLAN glass material has been widely used in the direction of fiber laser, super-continuum light source, etc. due to its characteristics of lower phonon energy, wider transmission window, etc. However, the ZBLAN material is difficult to realize large-scale low-cost production due to harsh manufacturing process conditions; the water absorption and the deliquescence are easy, and the chemical stability is poor; the glass transition temperature and the crystallization starting temperature have small difference, the thermal stability is poor and the like, and the application of the glass transition temperature and the crystallization starting temperature under high power or large scale is also limited. Heavy metal oxide glasses, another common mid-infrared luminescent material, have phonon energies close to or even lower than ZBLAN glasses, resulting in mid-infrared luminescence intensities higher than in fluoride glasses in heavy metal oxide glasses. The infrared cut-off wavelength can reach 8-10 mu m, far exceeds the infrared cut-off wavelength of fluoride glass, evenComparable to some chalcogenide glasses. In addition, the thermal and chemical stability of heavy metal oxide glasses far exceed that of fluoride glasses, and the difficulty and requirements of the manufacturing process are lower than those of fluoride glasses. Therefore, the performance of the heavy metal oxide glass as a mid-infrared luminescent material is superior to that of common fluoride glass.
In 1992, Dambaugh et al proposed a lead oxide (PbO), bismuth oxide (Bi)2O3) Gallium oxide (Ga)2O3) The EO heavy metal oxide glass is applied to a plurality of fields. The glass has higher thermal stability and chemical stability than fluoride glass, and the luminescent property of the glass in the middle infrared band is stronger than that of the fluoride glass. However, the EO glass tends to undergo severe devitrification due to a large amount of water absorption during the production process or to affect the luminous intensity in the vicinity of 3 μm, and therefore, improvement thereof is desired. Based on the purpose, we propose an improved PBG mid-infrared luminous heavy metal oxide glass material.
Disclosure of Invention
The invention aims to provide a PBG Er-doped Er for realizing broadband mid-infrared 2.7 mu m luminescence3+Heavy metal oxide glasses.
The purpose of the invention is realized as follows:
PBG Er-doped3+The heavy metal oxide glass is characterized by comprising the following raw materials in percentage by mole: (37-57) PbO- (0-20) PbF2-25Bi2O3-18Ga2O3PbO and PbF2Is 57%; er doped with 1mol percent2O3。
The preparation method comprises the following steps:
the method comprises the following steps: calculating the mass required by each raw material according to the molar percentage of the raw materials, weighing the high-purity raw materials with corresponding mass by using a high-precision electronic balance, putting the raw materials into an agate mortar for grinding and stirring, and uniformly mixing;
step two: putting the mixture into a platinum crucible, and melting for 30 minutes at 900 ℃ in an electric furnace;
step three: pouring the molten glass onto a preheated copper plate at 300 ℃, preserving the heat for 2 hours in a precision annealing furnace, and then cooling the glass to room temperature along with the furnace to obtain the mid-infrared broadband luminous heavy metal oxide glass;
the process was carried out in a glove box filled with dry nitrogen and oxygen.
Compared with the prior art, the invention has the beneficial effects that:
compared with the prior common fluoride glass such as ZBLAN glass, fluorine indium-based glass and fluorine aluminum-based glass, the PBG glass has higher thermal stability than the three fluoride glasses; under the condition that the conditions such as doping concentration, pumping power, sample thickness and the like are the same, the luminous intensity and FWHM of the PBG glass at the position of 2.7 mu m are superior to those of the three fluoride glasses;
the invention relates to a PBG Er-doped fiber3+The heavy metal oxide glass has high luminous intensity and high luminous bandwidth.
Drawings
FIG. 1 is a DSC differential thermal analysis curve of a PBG glass of the present invention;
FIG. 2 is a graph of absorption versus transmission for a PBG glass of the present invention;
FIG. 3 is a comparison of the emission band at 2.7 μm for the PBG glass of the present invention with several fluoride glasses.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Er capable of realizing broadband mid-infrared 2.7 mu m luminescence3+The preparation method of the ion-doped heavy metal oxide glass comprises the following steps: composition of matrix glass: the mole percentage of each raw material of the glass matrix can be expressed as: (37-57) PbO- (0-20) PbF2-25Bi2O3-18Ga2O3PbO and PbF2The total mol percent is 57 percent, and Er is doped with 1mol percent2O3(ii) a The preparation method of the luminescent glass comprises the following steps: calculating the mass ratio of high-purity raw materials according to the mol percentage, grinding and stirring to fully mix various raw materials, putting the mixture into a platinum crucible, heating in an electric furnace at 900 ℃ for 30min, pouring molten glass on a preheated copper plate, placing the molten glass in a precise annealing furnace, and preserving heat at 300 DEG CAnd after 2h, cooling to room temperature along with the furnace, and cutting and polishing the prepared glass sample according to the test or application requirements. The invention relates to a preparation method of novel erbium ion doped heavy metal oxide glass capable of realizing broadband mid-infrared 2.7 mu m luminescence. Has important application in the fields of mid-infrared luminescent materials, mid-infrared fiber lasers and the like.
The purpose of the invention is realized as follows: by modifying the formulation of the original EO glass, lead fluoride (PbF) is added thereto2) To remove hydroxyl (OH) in the glass-) Increasing the size of erbium ion (Er)3+) The purpose of the emission intensity in the vicinity of 2.7 μm.
PBG Er-doped3+The heavy metal oxide glass comprises the following raw materials in percentage by mol: (37-57) PbO- (0-20) PbF2-25Bi2O3-18Ga2O3，PbF2The content can be adjusted according to specific requirements, PbO and PbF2Is 57%; doped with 1% Er3+In oxide form (Er)2O3) And (4) introducing.
The preparation of the sample comprises the following steps:
1. calculating the mass required by each raw material according to the molar percentage of the raw materials, weighing the high-purity raw materials with corresponding mass by using a high-precision electronic balance, putting the raw materials into an agate mortar for grinding and stirring, and uniformly mixing;
2. putting the mixture into a platinum crucible, and melting for 30 minutes at 900 ℃ in an electric furnace;
3. pouring molten glass onto a preheated copper plate at 300 ℃, preserving heat for 2 hours in a precision annealing furnace, and then cooling to room temperature along with the furnace;
4. and cutting and polishing the prepared glass sample according to the test or application requirements.
Because of the PBG glass to OH in the glass-Is relatively sensitive to the content of OH-Too high a content will greatly reduce the luminous intensity at 2.7 μm and at the same time easily cause devitrification of the glass, thus requiring the water content in the raw materials and the preparation process. Except for the requirement of anhydrous grade of raw materials, all preparation processes except the cutting and polishing processes are full ofDry nitrogen (N)2) And oxygen (O)2) And preferably the mix is placed in a glove box for 24 hours prior to melting to allow sufficient physical removal of water.
The prepared glass samples have higher luminous intensity and full width at half maximum (FWHM) than several fluoride glasses with the same doping concentration when pumped by a 980nm commercial laser diode.
With 10% PbF2Is a specific embodiment. After the mass of each component is obtained through calculation, weighing a high-purity raw material with corresponding mass by using a high-precision electronic balance, putting the raw material into an agate mortar for grinding and stirring, and uniformly mixing; putting the mixture into a 30ml platinum crucible, and melting for 30 minutes at 900 ℃ in an electric furnace; pouring the molten glass onto a preheated copper plate at 300 ℃, preserving the heat for 2 hours in a precision annealing furnace, and then cooling the glass to room temperature along with the furnace. The whole preparation process is filled with dry N2And O2Was cut into 10 × 10 × 2mm3Polishing the thin sheet, and carrying out related optical tests; grinding appropriate amount of leftover material into powder, and performing DSC differential thermal analysis test on 10mg of powder.
The DSC differential thermal analysis results are shown in figure 1. The transition temperature (T) of the PBG glass can be seen from the graphg) At 310 ℃ and crystallization onset temperature (T)x) 391 ℃, the corresponding thermal stability parameter Δ T ═ Tx-Tg81 ℃ is higher than common fluoride glasses, indicating higher thermal stability than fluoride glasses.
FIG. 1 is a comparison of the mid-infrared emission spectra at 2.7 μm under the same conditions for PBG glass and three other fluoride glasses. It can be seen from the figure that PBG is superior to fluoride glass in both intensity and emission bandwidth, and thus can be applied to mid-infrared broadband emission. The absorption and transmission test results are shown in FIG. 2, in which (a) is the absorption spectrum from the ultraviolet band edge to 2 μm of the PBG glass, and (b) is the transmission spectrum from the 2 μm to the infrared band edge of the PBG glass. Er visible from the absorption spectrum3+The absorption peaks in visible light and near infrared wave bands can be obviously identified, and the Er is proved3+Presence in PBG glass and due to Er3+Has absorption peaks at about 800nm and 980nm, due toThe commercial laser with the corresponding wavelength can be used for pumping, so that the possibility of large-scale and low-cost application is ensured; as can be seen from the transmission spectrum, the infrared band edge of the PBG glass is 8 μm and higher than that of fluoride glass (generally about 6 μm), which shows that the transmission performance of the PBG glass in the middle infrared band is better than that of the fluoride glass. Further, OH in the vicinity of 3 μm can be calculated from the transmission spectrum locally amplified-Has an absorption coefficient of 0.04cm-1It is shown that the PBG glass has a low water content, which contributes to the formation of the glass and the 2.7 μm luminescence.
The 2.7 μm mid-infrared emission spectrum under 980nm laser diode pumping is shown in FIG. 3. The luminous intensity of the glass is sequentially PBG glass, fluorine indium-based glass, ZBLAN glass and fluorine aluminum-based glass from strong to weak; the full width at half maximum of the luminous band is PBG glass, ZBLAN glass, fluorine indium base glass and fluorine aluminum base glass in sequence from wide to narrow, and the corresponding FWHM values are shown in the attached table. The test result shows that the light emitting characteristic of the PBG glass near 2.7 mu m is superior to that of the three fluoride glasses, and the PBG glass is beneficial to the application of the PBG glass in the middle infrared band.
In summary, the following steps: the invention provides a novel 2.7 mu m mid-infrared broadband light-emitting heavy metal oxide glass material. The glass matrix comprises the following chemical components in percentage by mole: (37-57) PbO- (0-20) PbF2-25Bi2O3-18Ga2O3(PBG glass), PbO and PbF2Is 57% in the form of an oxide (Er)2O3) Er is introduced by external doping3+Ions. The PBG glass prepared by the invention has the characteristics of high transparency, high luminous intensity, high stability and the like, the preparation process is simple, and mass production can be realized. The needed pumping light source is a 980nm laser, so that the device can be applied to a plurality of fields such as medical operation, gas monitoring and sensing and the like in a large scale. In addition, due to its excellent thermal stability and processability, this glass also has important potential applications in the field of fiber lasers.
Claims (3)
1. PBG Er-doped3+The heavy metal oxide glass is characterized by comprising the following raw materials in percentage by mole: (37-57) PbO- (0-20) PbF2-25Bi2O3-18Ga2O3PbO and PbF2Is 57%; er doped with 1mol percent2O3。
2. The PBG doped Er of claim 13+The heavy metal oxide glass is characterized by being prepared by the following method:
the method comprises the following steps: calculating the mass required by each raw material according to the molar percentage of the raw materials, weighing the high-purity raw materials with corresponding mass by using a high-precision electronic balance, putting the raw materials into an agate mortar for grinding and stirring, and uniformly mixing;
step two: putting the mixture into a platinum crucible, and melting for 30 minutes at 900 ℃ in an electric furnace;
step three: pouring the molten glass onto a preheated copper plate at 300 ℃, preserving the heat for 2 hours in a precision annealing furnace, and then cooling the glass to room temperature along with the furnace to obtain the mid-infrared broadband luminous heavy metal oxide glass.
3. The PBG doped Er of claim 23+Heavy metal oxide glass, characterized in that the method is carried out in a glove box filled with dry nitrogen and oxygen.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104098270A (en) * | 2014-07-16 | 2014-10-15 | 中国科学院上海光学精密机械研究所 | Erbium-doped gallium aluminum acid salt laser glass for 2.7 [mu]m medium infrared rays and preparation method thereof |
| US20160280586A1 (en) * | 2013-03-20 | 2016-09-29 | University Of Leeds | Glass |
| CN111646695A (en) * | 2020-06-02 | 2020-09-11 | 苏州凯文堡尼光电科技有限公司 | Heavy metal oxide glass with broadband mid-infrared light emitting characteristic and preparation method thereof |
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- 2020-06-05 CN CN202010504366.8A patent/CN111574051A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160280586A1 (en) * | 2013-03-20 | 2016-09-29 | University Of Leeds | Glass |
| CN104098270A (en) * | 2014-07-16 | 2014-10-15 | 中国科学院上海光学精密机械研究所 | Erbium-doped gallium aluminum acid salt laser glass for 2.7 [mu]m medium infrared rays and preparation method thereof |
| CN111646695A (en) * | 2020-06-02 | 2020-09-11 | 苏州凯文堡尼光电科技有限公司 | Heavy metal oxide glass with broadband mid-infrared light emitting characteristic and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| BO WANG ET AL.: "Excited state absorption cross sections of 4I13/2 of Er3+ in ZBLAN", 《OPTICAL MATERIALS》 * |
| E.P.伯廷: "《X射线光谱分析的原理和应用》", 31 January 1983, 国防工业出版社 * |
| HIROKI YAMAUCHI ET AL.: "Spectroscopic properties of Tm3+ ions in PbO–PbF2–Bi2O3–Ga2O3 glasses for S-band optical amplifications", 《JOURNAL OF APPLIED PHYSICS》 * |
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