CN103274597A - Method for preparing near-infrared luminescent glass by bismuth ion-doped microporous molecular sieve - Google Patents
Method for preparing near-infrared luminescent glass by bismuth ion-doped microporous molecular sieve Download PDFInfo
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Abstract
The invention relates to a method for preparing near-infrared luminescent glass by a bismuth ion-doped microporous molecular sieve. The method comprises the following steps of: dissolving a bismuth compound and an aluminium compound into a solvent and preparing a solution; dipping the microporous molecular sieve into the solution, standing still, drying and carrying out heat treatment to obtain bismuth-doped powder; putting the bismuth-doped powder into a graphite mould, and then sintering the powder by a discharge plasma sintering furnace; and cooling to the room temperature, grinding and polishing to obtain the near-infrared luminescent glass. Compared with the traditional high-temperature melting method, the method for preparing the near-infrared luminescent glass is rapid in temperature rise rate and short in sintering time; the melting process does not occur in the sintering process of the glass prepared by discharge plasma sintering, so that the sintering belongs to solid phase sintering; and when being used for preparing glass with the same substrate, the method has the sintering temperature much lower than the high temperature melting temperature, thus being energy-saving and environment-friendly.
Description
Technical field
The invention belongs to the preparation field of near-infrared luminous glass, particularly a kind of bismuth ion doped micropore molecular sieve prepares the method for near-infrared luminous glass.
Background technology
It is big that Fibre Optical Communication Technology has transmission capacity with it, and anti-electromagnetic interference is strong, and advantages such as good confidentiality and good operating stability become modern society's main information transmission technology rapidly.And optical signal in the Optical Fiber Transmission process owing to reasons such as the loss of optical fiber self and chromatic dispersions, can cause the decay of optical signal, this decay can have a strong impact on the long-distance transmissions of opticfiber communication, and the effectively decay of compensated optical signal in transmission course of fiber amplifier, thereby realized the long-distance transmissions of opticfiber communication.Fiber amplifier (Optical Fiber Amplifier, OFA) generally formed by gain media, pump light and input and output coupled structure, compare with traditional amplification mode, fiber amplifier does not need through complex processes such as opto-electronic conversion, electric light conversion and signal regenerations, can directly amplify optical signal, be a kind of novel full image intensifer.The fiber amplifier of practicability mainly contains at present: erbium-doped fiber amplifier (EDFA), fiber Raman amplifier (SOA) and semiconductor optical amplifier (FRA) three classes.Wherein erbium-doped fiber amplifier has advantages such as gain is high, output rating is high, pumping efficiency is high, noise is low, channel interference is little, loss is low and becomes present the most widely used fiber amplifier with it.But because the restriction of rare earth ion self luminosity makes the gain bandwidth of erbium-doped fiber amplifier maximum have only 75nm, thereby limited it in following ultra broadband high-capacity optical fiber Application in Communication Systems.Semiconductor optical amplifier compares with erbium-doped fiber amplifier and exists that noise is big, power is less, poor, sensitive to serial interference and polarization to the saturability of optical signal gain, during with the optical fiber coupling loss big, poor work stability, be subject to the shortcomings such as influence of envrionment temperature, make its performance and erbium-doped fiber amplifier still have bigger gap.And fiber Raman amplifier has many advantages such as optical fiber itself as gain media, has good compatibility with fibre system; Gain wavelength is determined by the wavelength of pumping source, is not subjected to the restriction of other factors, as long as suitable pump light is arranged in theory, just can amplify the flashlight of any wavelength; High gain, channel interference are little, low noise figure, bandwidth range big (maximum can realize the gain bandwidth of 300nm), satisfactory stability.But Raman Fiber Amplifier needs big pump power (for length less than the optical fiber of 100m greater than 1W) and more complicated structure can realize bigger gain bandwidth, and this has proposed bigger challenge to existing opticfiber communication cable.Therefore, to make the new fiber amplifier with ultrawide band high performance be the developing direction of current fiber amplifier in research.
At present the existing PDFA Praseodymium Doped Fiber Amplifier that is operated in 1300nm (Praseodymium-Doped Fiber Amplifier, PDFA); Be operated in l460nm thulium doped fiber amplifier (Thulium-Doped Fiber Amplifier, TDFA); But be based on rare earth ion as the fiber amplifier of activator because restriction (the f-f forbidden transition of the electronics in the near-infrared luminous 4f of the deriving from track of rare earth ion such as erbium, thulium, praseodymium etc. of self luminosity, this transition since the shielding of outer 6s, 5d orbital electron to be subjected to the influence of environment less), being difficult to reentry has the luminescent material of bigger gain bandwidth.Transition metal ion is as Cr
4+, Ni
2+Deng being the light emitting ionic that is subjected to the outer shell shielding effect less, the luminous influence that is subjected to the host glass outfield easily of these ions can produce broad-band illumination in glass, but these ions are strict for glass matrix, only could produce broad-band illumination in the minority glass matrix.Main group metal ion such as Bi, Pb, Tl etc. since their s, outermost layer that the p valence electron is in electronic shell to be subjected to the effect of outer shell shielding littler, be more vulnerable to the influence in host glass outfield and produce broad-band illumination, if find suitable glass matrix and glass preparation technology to make to have the material that is used for amplifier of ultra broadband.
1998, the quiet patent (special permission discloses flat 11-29334) that waits the people to apply for being entitled as " mixing bismuth silica glass, optical fiber and image intensifer manufacture method " of Japanese scientist's liana.They at first introduce bismuth ion in the X zeolite, and then this zeolite is inserted SiO
2Colloidal sol in, pass through collosol and gel, drying again, processes such as high-temperature fusion just can obtain 800nm and excite and produce the fluorescent glass that peak value is positioned at 1.3um, and its luminescent lifetime reach the also wide 250nm of reaching of 650us fluorescence halfwidth.But it is wayward that the employing sol-gel method prepares the technology of glass, when dry glass cracked, and is difficult to prepare structural glass or glass fiber material.2002, this positive first-class people of bank adopts the scorification preparation to mix bismuth alumina silicate glass (the open 2003-283028 of special permission), this glass adopts the optical excitation of 400～850nm can access the fluorescence that peak value is positioned at 1000～1600nm, and can realize the light amplification of wavelength between 1000～1400nm.2004, people such as Qiu Jianrong adopt high silica micropore glass dipping bismuth nitrate solution then heat-treating methods prepare bismuth blended high silicon oxygen near-infrared super-broadband emission glass (CN1587136), this glass produces the broad-band illumination that halfwidth is about 300nm near can the frequency band at 1.3um under the semiconductor laser pumping of 808nm.But high-temperature melting method exists the high and long problem of fusion time of melt temperature, thereby causes the volatilization of bismuth, causes component wayward, even dephasign occurs.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of bismuth ion doped micropore molecular sieve prepares near-infrared luminous glass, this method is different from high-temperature melting method and sol-gel method, can directly sinter the powder after the doping treatment into the glass block fast through solid state sintering, have the characteristics of energy-conserving and environment-protective.
A kind of bismuth ion doped micropore molecular sieve of the present invention prepares the method for near-infrared luminous glass, comprising:
(1) bismuth-containing compound and aluminum contained compound are dissolved wiring solution-forming in solvent, with the micro porous molecular sieve dipping, leave standstill then, make solution and powder dipping evenly, dry, thermal treatment obtain mixing the bismuth meal body;
(2) the above-mentioned bismuth meal body of mixing is packed in the graphite jig, carry out sintering with the discharge plasma sintering oven then, be cooled to room temperature, polishing, polishing namely get near-infrared luminous glass.
Bismuth-containing compound is one or more in bismuth oxide, bismuth hydroxide, Bismuth trinitrate, bismuth chloride, bismuth sulfate, bismuth subnitrate, bismuth subcarbonate, the bismuth acetate in the described step (1).
Aluminum contained compound is one or more in aluminum oxide, aluminium hydroxide, aluminum nitrate, aluminum chloride, aluminum isopropylate, the plumbous subacetate in the described step (1).
Solvent is one or more in water, hydrochloric acid, nitric acid, sulfuric acid, the acetic acid in the described step (1).
Micro porous molecular sieve is ZSM-n series molecular sieve in the described step (1).
Dipping method is a kind of in excessive pickling process, equi-volume impregnating, the vacuum impregnation technology in the described step (1).
Time of repose is 12-24h in the described step (1).
Drying in the described step (1) is dry in the 80-100 ℃ of baking oven.
Thermal treatment temp is 300-700 ℃ in the described step (1), and heat treatment time is 0-5h.
In the described step (1) gained mix that the shared molar fraction of bismuth-containing compound is 0.01-5% in the bismuth meal body, the shared molar fraction of aluminum contained compound is 0-15%, the shared molar fraction of micro porous molecular sieve is 80～99.99%.
Be sintered in the furnace chamber of discharge plasma sintering oven in the described step (2), carry out sintering under vacuum, inert atmosphere or reducing atmosphere, temperature rise rate is 50～200 ℃/min, and sintering temperature is 1100～1500 ℃, pressure is 10～100MPa, and soaking time is 1～10 minute.
The present invention proposes to utilize the micro porous molecular sieve of discharge plasma Fast Sintering technology (SPS) sintering bismuth doping, sintering process belongs to solid state sintering, do not need melting process, so can realize low temperature, Fast Sintering, suppress the volatilization of bismuth, thereby prepare the near-infrared super-broadband emission glass with excellent luminescent properties.
Beneficial effect
(1) the preparation provided by the invention preparation method that mixes the near-infrared luminous glass of bismuth compares with the conventional high-temperature scorification that to have a heat-up rate fast, sintering time is short, and melting process does not take place in the sintering process that the discharge plasma sintering prepares glass, belong to solid state sintering, same matrix glass preparation the time, the sintering temperature of this method will be far below the high-temperature fusion temperature, so this method is a kind of method of energy-conserving and environment-protective;
(2) because present method quick heating sintering time weak point can effectively reduce or suppress the volatilization of bismuth, make component more controlled;
(3) the prepared glass of the present invention adopts the 800nm optical excitation can produce peak value to be about the fluorescence that 1250nm, fluorescence halfwidth are about 270nm;
(4) the inventive method is a kind of near-net-shape technology, only needs simple polishing, polishing can obtain the glass block.
Description of drawings
Fig. 1 is X-ray diffraction analysis (XRD) collection of illustrative plates of embodiment 1 prepared glass;
Fig. 2 is the transmitted spectrum of embodiment 2 prepared glass;
The fluorescence spectrum that Fig. 3 produces under the 800nm optical excitation for embodiment 3 prepared glass.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
With load weighted Bismuth trinitrate and aluminum nitrate (mol ratio=1:5) put into beaker, the nitric acid that adds 1mL concentration and be 1mol/L dissolves them, the distilled water that adds 0.5mL after the dissolving again makes liquor capacity reach 1.5mL; Add the 2.42gZSM-5 powder according to proportioning, after ultrasonic, form incipient impregnation, left standstill 24 hours, make solution and powder dipping evenly.To put into 80 ℃ of loft drier dry with leaving standstill powder after 24 hours, after the drying powder transferred in the crucible, puts into 450 ℃ of calcining insulations of retort furnace 2 hours, and what obtain bismuth-containing compound concentration after calcining is finished and be 0.2mol% mixes the bismuth meal body.At last prepared powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under the high-purity argon gas condition.Temperature rise rate is 90 ℃/min; Sintering temperature is 1200 ℃; Soaking time is 3min; Institute's applied pressure is 80MPa during sintering.Close instrument power source after sintering is finished, cool to room temperature with the furnace.Sample obtains the glass block through processes such as polishing, polishings after taking out.The X-ray diffraction analysis of prepared glass (XRD) collection of illustrative plates as shown in Figure 1.
Embodiment 2
With load weighted bismuth chloride and aluminum chloride (mol ratio=1:3) put into beaker, the hydrochloric acid that adds 2mL concentration and be 2mol/L dissolves them, the distilled water that adds 1mL after the dissolving again makes liquor capacity reach 3mL; Add the 3.63gZSM-11 powder according to proportioning, after ultrasonic, form incipient impregnation, left standstill 24 hours, make solution and powder dipping evenly.To put into 90 ℃ of loft drier dry with leaving standstill powder after 24 hours, after the drying powder transferred in the crucible, puts into 550 ℃ of calcining insulations of retort furnace 1 hour, and what obtain bismuth-containing compound concentration and be 1mol% mixes the bismuth meal body.At last prepared powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under the high-purity argon gas condition.Temperature rise rate is 80 ℃/min; Sintering temperature is 1250 ℃; Soaking time is 4min; Institute's applied pressure is 70MPa during sintering.Close instrument power source after sintering is finished, cool to room temperature with the furnace.Sample obtains the glass block through processes such as polishing, polishings after taking out.The transmitted spectrum of prepared glass as shown in Figure 2.
Embodiment 3
With load weighted bismuth oxide and aluminium hydroxide (mol ratio=1:6) put into beaker, the nitric acid that adds 2mL concentration and be 1mol/L dissolves them, the distilled water that adds 1mL after the dissolving again makes liquor capacity reach 3mL; Add the 4.84gZSM-5 powder according to proportioning, after ultrasonic, form incipient impregnation, left standstill 24 hours, make solution and powder dipping evenly.To put into 80 ℃ of loft drier dry with leaving standstill powder after 24 hours, after the drying powder transferred in the crucible, puts into 450 ℃ of calcining insulations of retort furnace 2 hours, and what obtain bismuth-containing compound concentration and be 0.5mol% mixes the bismuth meal body.At last prepared powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under the high-purity argon gas condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1300 ℃; Soaking time is 3min; Institute's applied pressure is 60MPa during sintering.Close instrument power source after sintering is finished, cool to room temperature with the furnace.Sample obtains the glass block through processes such as polishing, polishings after taking out.Prepared glass adopts the 800nm optical excitation to produce peak value to be about the fluorescence that 1250nm, fluorescence halfwidth are about 270nm.
Embodiment 4
With load weighted bismuth acetate and aluminum nitrate (mol ratio=1:7) put into beaker, the nitric acid that adds 1mL concentration and be 1mol/L dissolves them, adds 0.5mL distilled water after the dissolving again and makes liquor capacity reach 1.5mL; Add the 2.42gZSM-5 powder according to proportioning, form incipient impregnation through ultrasonic back, be placed on that vacuum left standstill 24 hours in the room temperature vacuum drying oven, make solution and powder dipping even.To put into 80 ℃ of loft drier dry with leaving standstill powder after 24 hours, after the drying powder transferred in the crucible, puts into 400 ℃ of calcining insulations of retort furnace 3 hours, and what obtain bismuth-containing compound concentration and be 0.1mol% mixes the bismuth meal body.At last prepared powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under high-purity argon hydrogen gas mixture condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1350 ℃; Soaking time is 2min; Institute's applied pressure is 50MPa during sintering.Close instrument power source after sintering is finished, cool to room temperature with the furnace.Sample obtains the glass block through processes such as polishing, polishings after taking out.
Embodiment 5
(mol ratio=1:9) is put into beaker with load weighted Bismuth trinitrate and aluminium hydroxide, adding 2mL concentration is that the nitric acid of 3mol/L dissolves them, the distilled water that adds 20mL after the dissolving again, the 4.84gZSM-5 powder is immersed in the solution, be placed on evaporation drying in 100 ℃ of loft drier then, after the drying powder is transferred in the crucible, put into 600 ℃ of retort furnaces calcining insulation 1 hour, what obtain bismuth-containing compound concentration and be 0.05mol% mixes the bismuth meal body.At last prepared powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.The SPS preparation process is carried out under the high-purity argon gas condition.Temperature rise rate is 100 ℃/min; Sintering temperature is 1400 ℃; Soaking time is 1min; Institute's applied pressure is 30MPa during sintering.Close instrument power source after sintering is finished, cool to room temperature with the furnace.Sample obtains the glass block through processes such as polishing, polishings after taking out.
Claims (10)
1. a bismuth ion doped micropore molecular sieve prepares the method for near-infrared luminous glass, comprising:
(1) bismuth-containing compound and aluminum contained compound are dissolved wiring solution-forming in solvent, with the micro porous molecular sieve dipping, leave standstill then, dry, thermal treatment obtain mixing the bismuth meal body;
(2) the above-mentioned bismuth meal body of mixing is packed in the graphite jig, carry out sintering with the discharge plasma sintering oven then, be cooled to room temperature, polishing, polishing namely get near-infrared luminous glass.
2. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: bismuth-containing compound is one or more in bismuth oxide, bismuth hydroxide, Bismuth trinitrate, bismuth chloride, bismuth sulfate, bismuth subnitrate, bismuth subcarbonate, the bismuth acetate in the described step (1).
3. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: aluminum contained compound is one or more in aluminum oxide, aluminium hydroxide, aluminum nitrate, aluminum chloride, aluminum isopropylate, the plumbous subacetate in the described step (1).
4. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: solvent is one or more in water, hydrochloric acid, nitric acid, sulfuric acid, the acetic acid in the described step (1).
5. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: micro porous molecular sieve is ZSM-n series molecular sieve in the described step (1).
6. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: dipping method is a kind of in excessive pickling process, equi-volume impregnating, the vacuum impregnation technology in the described step (1).
7. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, and it is characterized in that: the time of repose in the described step (1) is 12-24h, and drying is dry in the 80-100 ℃ of baking oven.
8. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: thermal treatment temp is 300-700 ℃ in the described step (1), and heat treatment time is 0-5h.
9. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: gained mixes that the shared molar fraction of bismuth-containing compound is 0.01-5% in the bismuth meal body in the described step (1), the shared molar fraction of aluminum contained compound is 0-15%, and the shared molar fraction of micro porous molecular sieve is 80～99.99%.
10. a kind of bismuth ion doped micropore molecular sieve according to claim 1 prepares the method for near-infrared luminous glass, it is characterized in that: be sintered in the furnace chamber of discharge plasma sintering oven in the described step (2), under vacuum, inert atmosphere or reducing atmosphere, carry out sintering, temperature rise rate is 50～200 ℃/min, sintering temperature is 1100～1500 ℃, pressure is 10～100MPa, and soaking time is 1～10 minute.
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| CN111847883A (en) * | 2020-08-31 | 2020-10-30 | 贵州赛义光电科技有限公司 | Fluorescent glass ceramic and preparation method thereof |
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