CN103274597B - The method of the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve - Google Patents
The method of the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve Download PDFInfo
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Abstract
The present invention relates to the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve, comprise: bismuth-containing compound and aluminum contained compound are dissolved wiring solution-forming in a solvent, then micro porous molecular sieve is flooded, leave standstill, dry, thermal treatment, obtains mixing bismuth meal body; Loaded in graphite jig by above-mentioned bismuth meal body of mixing, then sinter with discharge plasma sintering oven, be cooled to room temperature, polishing, polishing, obtain near-infrared luminous glass.It is fast that the preparation method that the near-infrared luminous glass of bismuth is mixed in preparation provided by the invention has heat-up rate compared with conventional high-temperature scorification, sintering time is short, and there is not melting process in the sintering process that discharge plasma sintering prepares glass, belong to solid state sintering, during the glass preparation of same matrix, the sintering temperature of this method will, far below high-temperature fusion temperature, be a kind of method of energy-conserving and environment-protective in this approach.
Description
Technical field
The invention belongs to the preparation field of near-infrared luminous glass, particularly the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve.
Background technology
It is large that Fibre Optical Communication Technology has transmission capacity with it, and electromagnetism interference is strong, and the advantage such as good confidentiality and good operating stability becomes rapidly the main information transmission technology of modern society.And optical signal in Optical Fiber Transmission process due to reasons such as the loss of optical fiber self and dispersions, the decay of optical signal can be caused, this decay can have a strong impact on the long-distance transmissions of opticfiber communication, and fiber amplifier can the effectively decay of compensated optical signal in transmitting procedure, thus achieve the long-distance transmissions of opticfiber communication.Fiber amplifier (Optical Fiber Amplifier, OFA) be generally made up of gain media, pump light and input and output coupled structure, compared with traditional amplification mode, fiber amplifier does not need through complex processes such as opto-electronic conversion, electro-optic conversion and signal regenerations, can directly amplify optical signal, be a kind of novel all-optical amplifiers.Fiber amplifier practical at present mainly contains: erbium-doped fiber amplifier (EDFA), fiber Raman amplifier (SOA) and semiconductor optical amplifier (FRA) three class.Wherein erbium-doped fiber amplifier has the advantages such as gain is high, output rating is high, pumping efficiency is high, noise is low, channel interference is little, loss is low with it and becomes current the most widely used fiber amplifier.But the gain bandwidth making erbium-doped fiber amplifier maximum due to the restriction of rare earth ion self luminosity only has 75nm, thus limit its application in following ultra broadband high-capacity optical fiber communication system.Semiconductor optical amplifier also exists compared with erbium-doped fiber amplifier that noise is large, power compared with little, to the saturability of optical signal gain, during poor, sensitive to serial interference and polarization and coupling fiber, loss is large, poor work stability, be subject to the shortcomings such as the impact of envrionment temperature, make its performance and erbium-doped fiber amplifier still have larger gap.And fiber Raman amplifier has many advantages if optical fiber itself is as gain media, with fibre system, there is good compatibility; Gain wavelength is determined by the wavelength of pumping source, not by the restriction of other factors, as long as there is suitable pump light in theory, just can amplify the flashlight of any wavelength; High gain, channel interference are little, low noise figure, bandwidth range large (the maximum gain bandwidth realizing 300nm), satisfactory stability.But Raman Fiber Amplifier needs large pump power (optical fiber length being less than to 100m is greater than 1W) and more complicated structure can realize larger gain bandwidth, and this proposes larger challenge to existing opticfiber communication cable.Therefore, the obtained new fiber amplifier with ultrawide band high performance of research is the developing direction of current optical fiber amplifier.
The existing PDFA Praseodymium Doped Fiber Amplifier (Praseodymium-Doped Fiber Amplifier, PDFA) being operated in 1300nm at present; Be operated in the thulium doped fiber amplifier (Thulium-Doped Fiber Amplifier, TDFA) of l460nm; But based on rare earth ion, as the fiber amplifier of activator, due to the restriction of self luminosity, (rare earth ion is as the f-f forbidden transition of the near-infrared luminous electronics derived from 4f track of erbium, thulium, praseodymium etc., the impact that this transition is subject to environment due to the shielding of outer 6s, 5d orbital electron is less), being difficult to reentry has the luminescent material of larger gain bandwidth.Transition metal ion is as Cr
4+, Ni
2+etc. being by the less light emitting ionic of outer shell shielding effect, the impact that the luminescence of these ions is easily subject to host glass outfield can produce broad-band illumination in glass, but these ions require strict for glass matrix, only could produce broad-band illumination in minority glass matrix.Main group metal ion is as Bi, Pb, the effect that Tl etc. are subject to outer shell shielding due to outermost layer that their s, p valence electron is in electronic shell is less, be more vulnerable to the impact in host glass outfield and produce broad-band illumination, if find suitable glass matrix and glass preparation technique may make the material being used for amplifier with ultra broadband.
1998, the quiet patent (special permission discloses flat 11-29334) waiting people to apply for being entitled as " mixing bismuth silica glass, optical fiber and image intensifer manufacture method " of Japanese Scientists liana.First bismuth ion is introduced in X zeolite by they, and then this zeolite is inserted SiO
2colloidal sol in, then through collosol and gel, drying, the 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 reaches, and 650us fluorescence halfwidth is also wide reach 250nm.But the technique that employing sol-gel method prepares glass is wayward, easily makes glass crack, be difficult to prepare structural glass or glass fiber material time dry.2002, this positive first-class people of bank adopts 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 obtain the fluorescence that peak value is positioned at 1000 ~ 1600nm, and can realize the light amplification of wavelength between 1000 ~ 1400nm.2004, the people such as Qiu Jianrong adopt high silica micropore glass flood bismuth nitrate solution then heat-treating methods prepare bismuth blended high silicon oxygen near-infrared super-broadband emission glass (CN1587136), this glass at the near band of 1.3um, can produce the broad-band illumination that halfwidth is about 300nm under the semiconductor laser pumping of 808nm.But high-temperature melting method also exists melt temperature height and fusion time long problem, thus causes the volatilization of bismuth, causes component wayward, even occurs dephasign.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve, the method is different from high-temperature melting method and sol-gel method, directly can sinter the powder after doping treatment into glass block fast through solid state sintering, there is the feature of energy-conserving and environment-protective.
The method of the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve of the present invention, comprising:
(1) bismuth-containing compound and aluminum contained compound are dissolved wiring solution-forming in a solvent, then flooded by micro porous molecular sieve, leave standstill, make solution and powder dipping evenly, dry, thermal treatment, obtains mixing bismuth meal body;
(2) loaded in graphite jig by above-mentioned bismuth meal body of mixing, then sinter with discharge plasma sintering oven, be cooled to room temperature, polishing, polishing, obtain near-infrared luminous glass.
In described step (1), bismuth-containing compound is one or more in bismuth oxide, bismuth hydroxide, Bismuth trinitrate, bismuth chloride, bismuth sulfate, bismuth subnitrate, bismuth subcarbonate, bismuth acetate.
In described step (1), aluminum contained compound is one or more in aluminum oxide, aluminium hydroxide, aluminum nitrate, aluminum chloride, aluminum isopropylate, plumbous subacetate.
In described step (1), solvent is one or more in water, hydrochloric acid, nitric acid, sulfuric acid, acetic acid.
In described step (1), micro porous molecular sieve is ZSM-n Series Molecules sieve.
In described step (1), dipping method is the one in excessive pickling process, equi-volume impregnating, vacuum impregnation technology.
In described step (1), time of repose is 12-24h.
Drying in described step (1) is dry in 80-100 DEG C of baking oven.
In described step (1), thermal treatment temp is 300-700 DEG C, and heat treatment time is 0-5h.
In described step (1), the molar fraction of mixing in bismuth meal body shared by bismuth-containing compound of gained is 0.01-5%, and the molar fraction shared by aluminum contained compound is 0-15%, and molar fraction shared by micro porous molecular sieve is 80 ~ 99.99%.
Be sintered in described step (2) in the furnace chamber of discharge plasma sintering oven, sinter under vacuum, inert atmosphere or reducing atmosphere, temperature rise rate is 50 ~ 200 DEG C/min, and sintering temperature is 1100 ~ 1500 DEG C, pressure is 10 ~ 100MPa, and soaking time is 1 ~ 10 minute.
The present invention proposes to utilize spark plasma sintering technology (SPS) to sinter the micro porous molecular sieve of bismuth doping, sintering process belongs to solid state sintering, do not need melting process, so low temperature, Fast Sintering can be realized, suppress the volatilization of bismuth, thus prepare the near-infrared super-broadband emission glass with excellent luminance performance.
beneficial effect
(1) it is fast that the preparation method that the near-infrared luminous glass of bismuth is mixed in preparation provided by the invention has heat-up rate compared with conventional high-temperature scorification, sintering time is short, and there is not melting process in the sintering process that discharge plasma sintering prepares glass, belong to solid state sintering, same matrix glass preparation time, the sintering temperature of this method will, far below high-temperature fusion temperature, be a kind of method of energy-conserving and environment-protective in this approach;
(2) volatilization that can effectively reduce or suppress bismuth because present method quick heating sintering time is short, makes component more controlled;
(3) glass prepared by the present invention adopts 800nm optical excitation can produce the fluorescence that peak value is about 1250nm, fluorescence halfwidth is about 270nm;
(4) the inventive method is a kind of near-net-shape technology, only needs simply polishing, polishing can obtain glass block.
Accompanying drawing explanation
X-ray diffraction analysis (XRD) collection of illustrative plates of Fig. 1 glass prepared by embodiment 1;
The transmitted spectrum of Fig. 2 glass prepared by embodiment 2;
Fig. 3 fluorescence spectrum that glass produces under 800nm optical excitation prepared by embodiment 3.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Load weighted Bismuth trinitrate and aluminum nitrate (mol ratio=1:5) are put into beaker, and adding 1mL concentration is that they dissolve by the nitric acid of 1mol/L, and the distilled water adding 0.5mL after dissolving again makes liquor capacity reach 1.5mL; Add 2.42gZSM-5 powder according to proportioning, after ultrasonic, form incipient impregnation, leave standstill 24 hours, make solution and powder dipping evenly.By leaving standstill the powder after 24 hours, to put into 80 DEG C of loft drier dry, transfers in crucible, put into retort furnace 450 DEG C of sintering soak 2 hours after drying by powder, obtain after having calcined bismuth-containing compound concentration be 0.2mol% mix bismuth meal body.After finally the powder prepared being loaded graphite jig, put into SPS equipment and sinter.SPS preparation process is carried out under high-purity argon gas condition.Temperature rise rate is 90 DEG C/min; Sintering temperature is 1200 DEG C; Soaking time is 3min; During sintering, institute's applied pressure is 80MPa.Sinter rear closedown instrument power source, cool to room temperature with the furnace.Sample obtains glass block through processes such as polishing, polishings after taking out.X-ray diffraction analysis (XRD) collection of illustrative plates of prepared glass as shown in Figure 1.
Embodiment 2
Load weighted bismuth chloride and aluminum chloride (mol ratio=1:3) are put into beaker, and adding 2mL concentration is that they dissolve by the hydrochloric acid of 2mol/L, and the distilled water adding 1mL after dissolving again makes liquor capacity reach 3mL; Add 3.63gZSM-11 powder according to proportioning, after ultrasonic, form incipient impregnation, leave standstill 24 hours, make solution and powder dipping evenly.By leaving standstill the powder after 24 hours, to put into 90 DEG C of loft drier dry, transfers in crucible, put into retort furnace 550 DEG C of sintering soak 1 hour after drying by powder, obtain bismuth-containing compound concentration be 1mol% mix bismuth meal body.After finally the powder prepared being loaded graphite jig, put into SPS equipment and sinter.SPS preparation process is carried out under high-purity argon gas condition.Temperature rise rate is 80 DEG C/min; Sintering temperature is 1250 DEG C; Soaking time is 4min; During sintering, institute's applied pressure is 70MPa.Sinter rear closedown instrument power source, cool to room temperature with the furnace.Sample obtains glass block through processes such as polishing, polishings after taking out.The transmitted spectrum of prepared glass as shown in Figure 2.
Embodiment 3
Load weighted bismuth oxide and aluminium hydroxide (mol ratio=1:6) are put into beaker, and adding 2mL concentration is that they dissolve by the nitric acid of 1mol/L, and the distilled water adding 1mL after dissolving again makes liquor capacity reach 3mL; Add 4.84gZSM-5 powder according to proportioning, after ultrasonic, form incipient impregnation, leave standstill 24 hours, make solution and powder dipping evenly.By leaving standstill the powder after 24 hours, to put into 80 DEG C of loft drier dry, transfers in crucible, put into retort furnace 450 DEG C of sintering soak 2 hours after drying by powder, obtain bismuth-containing compound concentration be 0.5mol% mix bismuth meal body.After finally the powder prepared being loaded graphite jig, put into SPS equipment and sinter.SPS preparation process is carried out under high-purity argon gas condition.Temperature rise rate is 100 DEG C/min; Sintering temperature is 1300 DEG C; Soaking time is 3min; During sintering, institute's applied pressure is 60MPa.Sinter rear closedown instrument power source, cool to room temperature with the furnace.Sample obtains glass block through processes such as polishing, polishings after taking out.Prepared glass adopts 800nm optical excitation to produce the fluorescence that peak value is about 1250nm, fluorescence halfwidth is about 270nm.
Embodiment 4
Load weighted bismuth acetate and aluminum nitrate (mol ratio=1:7) are put into beaker, and adding 1mL concentration is that they dissolve by the nitric acid of 1mol/L, adds 0.5mL distilled water again and make liquor capacity reach 1.5mL after dissolving; Add 2.42gZSM-5 powder according to proportioning, after ultrasonic, form incipient impregnation, be placed on vacuum in room temperature in vacuo loft drier and leave standstill 24 hours, make solution and powder dipping evenly.By leaving standstill the powder after 24 hours, to put into 80 DEG C of loft drier dry, transfers in crucible, put into retort furnace 400 DEG C of sintering soak 3 hours after drying by powder, obtain bismuth-containing compound concentration be 0.1mol% mix bismuth meal body.After finally the powder prepared being loaded graphite jig, put into SPS equipment and sinter.SPS preparation process is carried out under high-purity argon hydrogen gas mixture condition.Temperature rise rate is 100 DEG C/min; Sintering temperature is 1350 DEG C; Soaking time is 2min; During sintering, institute's applied pressure is 50MPa.Sinter rear closedown instrument power source, cool to room temperature with the furnace.Sample obtains glass block through processes such as polishing, polishings after taking out.
Embodiment 5
Load weighted Bismuth trinitrate and aluminium hydroxide (mol ratio=1:9) are put into beaker, adding 2mL concentration is that they dissolve by the nitric acid of 3mol/L, the distilled water of 20mL is added again after dissolving, by 4.84gZSM-5 powder dipping in the solution, then evaporation drying in 100 DEG C of loft drier is placed on, after drying, powder is transferred in crucible, puts into retort furnace 600 DEG C of sintering soak 1 hour, obtain bismuth-containing compound concentration be 0.05mol% mix bismuth meal body.After finally the powder prepared being loaded graphite jig, put into SPS equipment and sinter.SPS preparation process is carried out under high-purity argon gas condition.Temperature rise rate is 100 DEG C/min; Sintering temperature is 1400 DEG C; Soaking time is 1min; During sintering, institute's applied pressure is 30MPa.Sinter rear closedown instrument power source, cool to room temperature with the furnace.Sample obtains glass block through processes such as polishing, polishings after taking out.
Claims (10)
1. a method for the near-infrared luminous glass of bismuth ion doped micropore molecular sieve, comprising:
(1) bismuth-containing compound and aluminum contained compound are dissolved wiring solution-forming in a solvent, then flooded by micro porous molecular sieve, leave standstill, dry, thermal treatment, obtains mixing bismuth meal body;
(2) loaded in graphite jig by above-mentioned bismuth meal body of mixing, then sinter with discharge plasma sintering oven, be cooled to room temperature, polishing, polishing, obtain near-infrared luminous glass.
2. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, is characterized in that: in described step (1), bismuth-containing compound is one or more in bismuth oxide, bismuth hydroxide, Bismuth trinitrate, bismuth chloride, bismuth sulfate, bismuth subnitrate, bismuth subcarbonate, bismuth acetate.
3. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, is characterized in that: in described step (1), aluminum contained compound is one or more in aluminum oxide, aluminium hydroxide, aluminum nitrate, aluminum chloride, aluminum isopropylate, plumbous subacetate.
4. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, is characterized in that: in described step (1), solvent is one or more in water, hydrochloric acid, nitric acid, sulfuric acid, acetic acid.
5. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, is characterized in that: in described step (1), micro porous molecular sieve is ZSM-n Series Molecules sieve.
6. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, is characterized in that: in described step (1), dipping method is the one in excessive pickling process, equi-volume impregnating, vacuum impregnation technology.
7. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, is characterized in that: the time of repose in described step (1) is 12-24h, and drying is dry in 80-100 DEG C of baking oven.
8. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, is characterized in that: in described step (1), thermal treatment temp is 300-700 DEG C, and heat treatment time is 0-5h.
9. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, it is characterized in that: in described step (1), the molar fraction of mixing in bismuth meal body shared by bismuth-containing compound of gained is 0.01-5%, molar fraction shared by aluminum contained compound is 0-15%, and molar fraction shared by micro porous molecular sieve is 80 ~ 99.99%.
10. the method for the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve according to claim 1, it is characterized in that: be sintered in described step (2) in the furnace chamber of discharge plasma sintering oven, sinter under vacuum, inert atmosphere or reducing atmosphere, temperature rise rate is 50 ~ 200 DEG C/min, sintering temperature is 1100 ~ 1500 DEG C, pressure is 10 ~ 100MPa, and soaking time is 1 ~ 10 minute.
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| CZ201264A3 (en) * | 2012-01-30 | 2013-04-24 | Vysoká skola chemicko - technologická v Praze | Optical luminescent sodium-aluminium-silicate glass doped with metal oxides and intended for photonics |
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| CN1587136A (en) * | 2004-09-02 | 2005-03-02 | 中国科学院上海光学精密机械研究所 | Method for preparing bismuth blended high silicon oxygen and infrared broad band luminous glass |
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