CN110407462B - Rare earth doped silicate glass and preparation method and application thereof - Google Patents
Rare earth doped silicate glass and preparation method and application thereof Download PDFInfo
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
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- 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
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
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- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
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- H01S3/063—Waveguide lasers, i.e. whereby the dimensions of the waveguide are of the order of the light wavelength
- H01S3/067—Fibre lasers
- H01S3/06708—Constructional details of the fibre, e.g. compositions, cross-section, shape or tapering
- H01S3/06716—Fibre compositions or doping with active elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
- H01S3/06—Construction or shape of active medium
- H01S3/063—Waveguide lasers, i.e. whereby the dimensions of the waveguide are of the order of the light wavelength
- H01S3/067—Fibre lasers
- H01S3/06754—Fibre amplifiers
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Abstract
Rare earth doped silicate glass and a preparation method and application thereof, the rare earth doped silicate glass is prepared from the following raw materials by mol percent of 50-65mol percent of SiO 2; 5-15 mol% of B2O 3; 15-30 mol% of CaCO 3; 3-8 mol% of Na2CO 3; 3-8 mol% of R2O 3; wherein R2O3 is one or more of Bi2O3, Er2O3 and Tm2O 3. The invention overcomes the defects of the prior art, has reasonable design, and adopts boron oxide to replace the common aluminum oxide in the prior art; because the boron element and the aluminum element are positioned in the same main group in the periodic table of the elements, the optical basicity of the boron oxide is lower than that of the aluminum oxide, and the melting point of the boron oxide is far lower than that of the aluminum oxide, the preparation method has obvious advantages; and by reasonably adjusting the formula of the matrix, co-doping various ions and increasing the concentration of the doped ions, the ultra-wideband luminescent material with simpler preparation method and good luminescent efficiency is obtained.
Description
Technical Field
The invention relates to the technical field of optical glass, in particular to rare earth doped silicate glass and a preparation method and application thereof.
Background
At present, the optical fiber communication technology is a main information transmission technology in modern society rapidly due to the advantages of large transmission capacity, strong electromagnetic interference resistance, good confidentiality, good working stability and the like. The attenuation of the optical signal can be caused by the loss and dispersion of the optical fiber in the optical fiber transmission process, the attenuation can seriously affect the long-distance transmission of the optical fiber communication, and the optical fiber amplifier can effectively compensate the attenuation of the optical signal in the transmission process, thereby realizing the long-distance transmission of the optical fiber communication. Journal of Mitsubishi wire industry corporation, journal of 3/4 mesh, 1998 filed a patent titled "bismuth-doped silica glass, optical fiber, and optical amplifier production method" (laid-open publication Hei 11-29334). They prepared bismuth-doped silica glass by using bismuth-exchanged zeolite as a dispersion medium and by integrating a sol-gel method and a high-temperature melting method, drawn corresponding optical fibers and realized optical amplification at a 1.3 μm position under a 0.81 μm pump. The fluorescence peak value of the glass is located near 1130nm, the maximum fluorescence full width at half maximum is 250nm, the maximum fluorescence lifetime is 650 mu s, and the stimulated emission cross section is about 1.0 multiplied by 10-20cm2. In 22.2.2001, gamboge, jing et al, filed a patent entitled "optical fiber and optical amplifier" (laid-open publication 2002-: al2O3-SiO2-Bi2O3 is melted at 1750 ℃ to draw a corresponding optical fiber, and the optical amplification at the position of 1.3 mu m under the pumping of 0.8 mu m is realized. In 2001, Fujimoto and Nakatsuka in Jpn.J.App.Phys.,40, (2001) L279 reported that when pentavalent bismuth ion Bi5+ doped A12O3-SiO2 glass is prepared under air at a high temperature of 1760 ℃, the transmittance in the infrared region is reduced to about 30% due to the existence of a large amount of bubbles, which greatly limits the practical application of the SiO 2-based glass. Qiu Jianrong et al at university of Zhejiang filed a series of patents titled "ytterbium-bismuth co-doped phosphate-based optical glass and preparation method thereof", "nano bismuth cluster doped silica-based optical glass and preparation method thereof", "bismuth ion doped crystal for tunable laser and broadband amplifier", "bismuth-doped germanium-based optical glass and preparation method of bismuth-doped high silica near-infrared broadband luminescent glass", "bismuth-nickel co-doped transparent silicate glass-ceramics and preparation method thereof" (patent publication No. 200710044174.8, 200510024483.X, 200510023597.2, 200410054216.2, 200410054217.7, 200710047760.8) on bismuth-doped glass as light amplification material.
The C-band EDFA has a working window of 1530-1565 nm, has the characteristics of lowest optical fiber loss, large output power, high gain, independence on polarization, low noise index, independence on system bit rate and data format, simultaneous amplification of multi-path wavelength signals and the like, and is widely applied at present. The defect is that the gain bandwidth of the C-Band EDFA is only 35nm, only covers a part of a low-loss window of the quartz single-mode fiber, and limits the number of wavelength channels which can be accommodated by the fiber; in the patent, transition metal ions such as nickel and the like or ytterbium rare earth ions are co-doped to improve the infrared luminous intensity of bismuth, a germanate and phosphate system is adopted to improve the melting temperature of the glass, and the mechanical strength of the glass is improved through microcrystallization. However, the infrared luminous intensity of the original bismuth-doped glass is relatively weaker than that of rare earth ions used as an optical fiber amplifier, and the bismuth-doped glass is not beneficial to being used as an optical amplifier material; on the other hand, the strength of the glass can be improved by microcrystallizing the glass, but the microcrystals formed in the glass matrix easily cause reflection and refraction of light in the glass, which results in a decrease in light transmission efficiency and a decrease in light amplification effect.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides rare earth doped silicate glass and a preparation method and application thereof, overcomes the defects of the prior art, and obtains the ultra-wideband luminescent material with simpler preparation method and good luminescent efficiency by reasonably adjusting the matrix formula, co-doping various ions and increasing the concentration of the doped ions.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the rare earth doped silicate glass is prepared from the following raw materials in percentage by mole:
wherein R is2O3Is Bi2O3、Er2O3、Tm2O3One or more of them.
Preferably, the R2O3 is a mixture of Bi2O3, Er2O3 and Tm2O3, and the molar ratio of Bi2O3, Er2O3 and Tm2O3 is 3: 0.8-1.4: 0.6-1.2.
The invention also discloses a preparation method of the rare earth doped silicate glass, which comprises the following steps:
(1) weighing the raw materials according to the following molar ratio to obtain the required amount, and fully mixing the raw materials:
wherein R is2O3Is Bi2O3、Er2O3、Tm2O3One or more of the above;
(2) putting the mixed mixture powder into a high-temperature melting furnace, heating to 1200-1400 ℃, and preserving the temperature for 40-100 minutes to obtain molten glass liquid;
(3) pouring the obtained molten glass liquid onto a preheated mold, pressing, annealing at the temperature of 300-500 ℃ for 40-100 minutes, and naturally cooling to room temperature;
(4) taking out the sample, and grinding and polishing according to the required requirements to obtain the rare earth doped silicate glass.
Preferably, in the mixing in the step (1), the mixed raw materials are put into a mortar to be ground for 30 to 60 minutes.
The invention also discloses a preparation method of the bismuth-doped silicate glass optical waveguide amplifier, which comprises the steps of processing the bismuth-doped silicate glass into a cylindrical glass rod with the length of 0.8-1.5cm and the section diameter of 0.08-0.15cm, packaging, connecting lenses at two ends of the glass rod for coupling, packaging after coupling is finished, and leading out single-mode optical fibers at two ends of the glass rod.
The invention provides rare earth doped silicate glass and a preparation method and application thereof. The method has the following beneficial effects: boron oxide is adopted to replace aluminum oxide commonly used in the prior art; because the boron element and the aluminum element are positioned in the same main group in the periodic table of the elements, the optical basicity of the boron oxide is lower than that of the aluminum oxide, and the melting point of the boron oxide is far lower than that of the aluminum oxide, the preparation method has obvious advantages; and the ultra-wideband luminescent material with simpler preparation method and good luminous efficiency is obtained by reasonably adjusting the formula of the matrix, co-doping bismuth, erbium and thulium ions and increasing the concentration of doped ions.
Drawings
In order to more clearly illustrate the present invention or the prior art solutions, the drawings that are needed in the description of the prior art will be briefly described below.
FIG. 1 is a flow chart of a process for making the glass of the present invention;
FIG. 2 is a diagram showing the absorption spectrum of bismuth ions in bismuth-doped silicate glass;
FIG. 3 is an emission spectrum of bismuth ions in bismuth-doped silicate glass;
FIG. 4 is a graph of gain and noise figure versus pump power for an optical waveguide amplifier;
FIG. 5 is a graph of gain and noise figure of an optical waveguide amplifier versus signal light wavelength;
FIG. 6 is a graph comparing the absorption spectra of bismuth erbium thulium co-doped glass and single-doped glass;
FIG. 7 is a comparison of the emission spectra of the co-doped glasses described in examples three, four, and five;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings.
Example one
The rare earth doped silicate glass is prepared from the following raw materials in percentage by mole:
the preparation method comprises the following steps:
weighing the raw materials according to the required amount according to the molar ratio, putting the raw materials into a mortar for grinding for 40 minutes to fully mix the raw materials, pouring the mixed powder into a corundum crucible, putting the corundum crucible into a high-temperature melting furnace, heating to 1350 ℃, and then putting the corundum crucible into a heat preservation stage for heat preservation for 1 hour; after the heat preservation is finished, taking out the crucible, quickly pouring a molten sample on a preheated copper plate grinding tool, pressing, sending into an annealing furnace, and annealing at 350 ℃ for 60 minutes, wherein the function of the stage is to remove the internal stress of the glass and prevent the glass from cracking; and naturally cooling the bismuth-doped silicate glass after annealing is finished, taking out a sample, and grinding and polishing the sample according to the required requirements to obtain the bismuth-doped silicate glass.
In the embodiment, boron oxide is adopted to replace aluminum oxide commonly used in the prior art; as the boron element and the aluminum element are positioned in the same main group in the periodic table of the elements, the optical basicity of the boron oxide is lower than that of the aluminum oxide, and the melting point of the boron oxide is far lower than that of the aluminum oxide, the preparation method has obvious advantages. In the implementation, an UV/EV300UV-VIS spectrophotometer is adopted to measure the absorption spectrum of the glass sample, and a Zolix spectrophotometer is adopted to measure the emission spectrum of the sample under the excitation of a pump light source with power of 808nm and power of 100 mw; through measurement, the silicate glass sample obtained in the embodiment shows good luminescence in a wavelength range of near 400nm centered at 1300 nm.
As shown in fig. 2, which is an absorption spectrum of bismuth ions in the bismuth-doped silicate glass obtained in this example, it can be seen from the diagram that bismuth ions have two distinct absorption peaks at 500nm and 700nm, and a secondary distinct shoulder peak at 800nm, and these absorption peaks should be derived from energy level transition of Bi + ions;
and then, exciting the bismuth-doped silicate glass prepared by the experiment by using a pump light source with 808nm to obtain an emission spectrogram of bismuth ions in the bismuth-doped silicate glass shown in figure 3, wherein the radiation intensity of a vertical coordinate is a relative value, and a secondary peak appearing at 1420nm is an error of a measuring instrument. As can be seen from the figure, the prepared bismuth-doped glass has good near-infrared ultra-wideband luminescence, the luminescence center is 1310nm, the total luminescence interval reaches 400nm and covers the wavelength range of 1100-1500nm, and the full width at half maximum also reaches 200 nm. Thus, the bismuth-doped silicate glass obtained in the embodiment has good luminous feasibility.
Example two
Bismuth-doped silicate glass optical waveguide amplifier
The preparation method comprises the following steps:
processing the rare earth doped silicate glass prepared in the first embodiment into a cylindrical glass rod with the length of 1cm and the section diameter of 0.1cm, packaging, connecting lenses at two ends of the glass rod for coupling, packaging after coupling, and leading out single-mode optical fibers at two ends of the glass rod; and obtaining the bismuth-doped silicate glass optical waveguide amplifier after the packaging is finished.
In the embodiment, a 808nm pump light source is used as the pump input of the amplifier, a tunable small-signal laser source within the wavelength range of 1260, 1360nm is used as the input of the signal light, the two paths of input enter the amplifier after being coupled by the optical fiber coupler, and then the related data is obtained through the measurement of the optical spectrum analyzer and is analyzed.
As shown in fig. 4, which is a graph of the relationship between the gain and noise figure of the optical waveguide amplifier and the pump power, since it can be known that the luminescence center of the bismuth-doped silicate glass is located at a wavelength of 1310nm, the wavelength of the signal light is selected to be 1310nm, and as can be seen from fig. 4, the signal gain becomes larger as the pump power increases, wherein when the pump power is less than 400mw, the influence of the pump power on the gain is large, but when the pump power is higher than 400mw, the influence of the pump power on the gain is small; for the noise figure, the noise figure of the amplifier is always decreasing with increasing pump power, but the noise of the amplifier is still around 4.5dB at 500 mw.
In view of the above results, in order to achieve both the efficiency and performance of the amplifier, in this measurement, the pump power is fixed at 400mw, the graph of the gain and noise figure of the optical waveguide amplifier versus the optical wavelength is shown in fig. 5, the gain of the optical waveguide amplifier has a maximum value at the 1310nm wavelength position, which is about 6.08dB, which is also the luminescence center of the bismuth ion emission spectrum, at both sides of this position, the gain of the amplifier shows a downward trend, wherein the gain at 1260nm is about 4.5dB, the gain at 1360nm is about 4.1dB, and it is not difficult to see from the trend of the curve that the amplifier still has an amplifying effect on signals outside the 1260-, 1360nm wavelength range, and the gain is smaller as the wavelength position of the signals is farther from 1310 nm. The relationship of the noise figure of the amplifier to the wavelength is similar to the relationship of gain to wavelength, with high noise over the entire measurement band.
In summary, the bismuth-doped silicate glass optical waveguide amplifier shows good amplification characteristics, which illustrates the feasibility of using the glass described in the first embodiment to make the amplification material, and also demonstrates the feasibility of the manufacturing method of the optical waveguide amplifier, and the combination of the two has a wide application prospect.
EXAMPLE III
The bismuth-erbium-thulium co-doped silicate glass is prepared from the following raw materials in percentage by mole:
wherein R is2O3Is Bi2O3、Er2O3And Tm2O3And Bi2O3、Er2O3And Tm2O3In a molar ratio of 3:0.8: 1.2.
Example four
The bismuth-erbium-thulium co-doped silicate glass is prepared from the following raw materials in percentage by mole:
wherein R is2O3Is Bi2O3、Er2O3And Tm2O3And Bi2O3、Er2O3And Tm2O3In a molar ratio of 3:1.0: 1.0.
EXAMPLE five
The bismuth-erbium-thulium co-doped silicate glass is prepared from the following raw materials in percentage by mole:
wherein R is2O3Is Bi2O3、Er2O3And Tm2O3And Bi2O3、Er2O3And Tm2O3In a molar ratio of 3:1.4: 0.6.
The glass making methods and processes of the third, fourth and fifth embodiments remain the same as in the first embodiment; and the absorption spectra of the glass samples prepared in the third embodiment, the fourth embodiment and the fifth embodiment are measured by a UV/EV300UV-VIS spectrophotometer, and the absorption spectra of the bismuth-erbium-thulium co-doped glass and the single-doped glass are compared as shown in FIG. 6; as can be seen, a plurality of absorption peaks were observed in the absorption spectrum of the co-doped glass, and these peaks were suspected to have new peaks in addition to the absorption peaks corresponding to each ion when doped individually. Thus showing that all the dopants are well mixed and exist in the form of luminescent ions in the co-doped glass, and energy transfer exist among the three ions.
Measuring emission spectra of the glass samples prepared in the third, fourth and fifth examples under the excitation of 808nm pump light source with power of 100mw by using a Zolix spectrophotometer, as shown in FIG. 7; the concentrations of bismuth ions of the glasses corresponding to the three embodiments are the same, and the concentrations of erbium ions and thulium ions are different, so that all glasses have ultra-wideband near-infrared emission at 1200nm-1800nm, but the difference of the luminous intensities of peaks and troughs is large. In all, the glass samples prepared in the three examples have the best luminescence curve.
The peaks appearing in the figure are analyzed one by one, the position of the first peak is about 1330nm, and the bismuth ion luminescence can be determined to be caused by bismuth ion luminescence, but compared with the first embodiment, the bismuth ion luminescence peak is slightly red-shifted, the distance is about 20nm, and the biggest possible reason is that the peak value is right-shifted due to the superposition of the peak of the thulium ion at 1435nm and the luminescence peak of the bismuth ion; the reason why the trough is caused by that the intensity after the superposition of the bismuth ion luminescence and the thulium ion luminescence at the 1390nm position is still not as strong as that of the ion luminescence at the luminescence center, but the absolute luminescence intensity at the position is not weak; the second peak is followed by a wave trough with a more obvious downward sliding, and then two closely connected peaks are respectively arranged at 1520nm and 1560nm, for the two peaks, the two peaks are considered to be caused by the transition luminescence of erbium ions, wherein 1520nm does not exclude the influence of the mutual superposition of the luminescence of thulium ions and erbium ions; the main peak of erbium 1560nm is followed by a very severely degraded trough, which is also caused by the absence of ion luminescence bands in the spectrum with the width of 1580-1750 nm; after 1700nm, a significant increase in the intensity of luminescence is observed, which is the luminescence brought about by the luminescence center of the thulium ion at 1800 nm.
And through observation of several main luminescence peaks, it can be seen that the increase of the concentration of erbium ions has a negative effect on the luminescence of other ions, which is caused by energy transfer between ions on the one hand, and on the other hand, erbium ions may have stronger absorption to pump light energy, but the pump energy is limited, so that the larger the concentration of erbium ions is, the stronger the luminous effect of erbium ions is, and the weaker the other two ions are. The luminous intensity at 1435nm and 1800nm can be raised by properly increasing the thulium ion concentration, which is shown in the emission spectrum of the glass by raising the height of several wave trough positions, so that the whole luminous curve is more flat. Therefore, after the doping concentrations of the three ions of bismuth, erbium and thulium are reasonably adjusted, the optical performance of the rare earth doped silicate glass can be better improved.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. The rare earth doped silicate glass is characterized by being prepared from the following raw materials in percentage by mole:
SiO2:50-65mol%；
B2O3:5-15mol%；
CaCO3:15-30mol%；
Na2CO3:3-8mol%；
R2O3:3-8mol%；
wherein, R is2O3Is Bi2O3、Er2O3、Tm2O3And Bi2O3、Er2O3And Tm2O3In a molar ratio of 3:0.8: 1.2.
2. The preparation method of the rare earth doped silicate glass is characterized by comprising the following steps:
(1) the starting materials according to claim 1 are weighed out in the required amounts in the respective molar ratios and mixed thoroughly:
(2) putting the mixed mixture powder into a high-temperature melting furnace, heating to 1200-1400 ℃, and preserving the temperature for 40-100 minutes to obtain molten glass liquid;
(3) pouring the obtained molten glass liquid onto a preheated mold, pressing, annealing at the temperature of 300-500 ℃ for 40-100 minutes, and naturally cooling to room temperature;
(4) taking out the sample, and grinding and polishing according to the required requirements to obtain the rare earth doped silicate glass.
3. The method of producing a rare earth-doped silicate glass according to claim 2, characterized in that: when mixing in the step (1), the mixed raw materials are put into a mortar to be ground for 30 to 60 minutes.
4. A method for preparing an optical waveguide amplifier of bismuth-doped silicate glass is characterized by comprising the following steps: the rare earth-doped silicate glass prepared according to claim 1 is processed into a cylindrical glass rod having a length of 0.8 to 1.5cm and a cross-sectional diameter of 0.08 to 0.15cm, and is encapsulated, and then lenses are connected to both ends of the glass rod for coupling, and after the coupling is completed, the encapsulation is performed, and a single-mode optical fiber is used for leading out at both ends of the glass rod.
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| CN113113844B (en) * | 2021-03-18 | 2022-11-15 | 北京大学 | Gain material for silicon-based optical waveguide amplifier and laser and preparation method thereof |
| CN114477764B (en) * | 2022-01-26 | 2023-04-21 | 华南理工大学 | Bismuth-thulium co-doped gain glass with high-efficiency broadband and preparation method thereof |
| CN114656144A (en) * | 2022-05-07 | 2022-06-24 | 四川和泰光纤有限公司 | Near-infrared luminous tin-bismuth doped aluminosilicate glass optical rod and preparation method thereof |
| CN116217071A (en) * | 2023-02-21 | 2023-06-06 | 云南大学 | Rare earth ion doped borosilicate laser glass and preparation method and application thereof |
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