CN109399945A - A kind of preparation method of high-performance optical fiber material - Google Patents
A kind of preparation method of high-performance optical fiber material Download PDFInfo
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- CN109399945A CN109399945A CN201811441787.XA CN201811441787A CN109399945A CN 109399945 A CN109399945 A CN 109399945A CN 201811441787 A CN201811441787 A CN 201811441787A CN 109399945 A CN109399945 A CN 109399945A
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- optical fiber
- fiber material
- performance optical
- heat treatment
- glass
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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
- C03C13/00—Fibre or filament compositions
-
- 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
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
Abstract
The invention discloses a kind of preparation methods of high-performance optical fiber material, it is made of the following raw material of mass percent: SiO2:45~75%, B2O3:3~10%, SiC:3~10%, ZnO:5~20%, MgO:1~7%, Na2O:10~25%, PbO:0.5~5%, Se:0.5~5%, C:0.5~2%；The high-performance optical fiber material is prepared as follows: weighing each raw material by above-mentioned mass percent, it puts and mixes well in the ball mill, it is placed in close crucible, in 1100~1450 DEG C of high-temperature fusion 30min~2h, then cooling rapidly, light brown glass is obtained, carries out heat treatment process finally to get the high-performance optical fiber material of brownish black is arrived.The high-performance optical fiber material of the method for the present invention preparation has the characteristics that simple process, cheap, quantum dot size is controllable.
Description
Technical field
The present invention relates to optical communication techniques and field of nano material preparation, and in particular to a kind of system of high-performance optical fiber material
Preparation Method.
Background technique
Quantum dot is a kind of quasi-zero dimension semiconductor nanocrystal, its radius is less than or close to exciton Bohr radius.By
The strong confinement effect of quantum caused by its minimum size makes quantum dot show many unique electricity, optics and magnetics special
Property, it is greatly paid close attention to so as to cause people.Wherein IV-VI semiconductor-quantum-point, such as PbSe, PbS, since it is with biggish
Exciton Bohr radius (PbSe 46nm, PbS 18nm) shows strong fluorescence hair so as to cause strong quantum confined effect
Penetrate spectrum.By changing the size of quantum dot, the quantum dot of different fluorescent emission peak value wavelength, fluorescent emission peak value can be obtained
Wavelength almost covers near infrared band (1000-2300nm), research also demonstrate quantum dot can be used as the good gain of light and
Amplification medium, this makes quantum dot have very important application prospect in terms of opto-electronic device.Especially by IV-VI semiconductor
Quantum dot is incorporated into fiber optic materials (such as: glass, plastics), is optical-fiber type quantum dot light electronics device (such as PbSe quantum
The fiber amplifier of point doping) it develops and applies, open a fan gate.In addition, research shows that quantum dot-doped optical fiber is put
Big device has superior performance than conventional fiber amplifier, has the characteristics that wide spectrum, high-gain, low noise.
The preparation method of quantum dot mainly has: molecular beam epitaxial growth method, sol-gal process, fusion method etc..Wherein melt
It is one of hot spot concerned by people in recent years that method, which prepares quantum dot-doped glass,.The quantum dot-doped glass prepared using the method
One very big advantage be can be by way of mutually compatible with optical fiber technology of preparing now --- optical fibre rod draw, come directly draw
Quanta point optical fiber is made, so as to further prepare quantum dot light fiber amplifier.Glass optical fiber has relative to plastic optical fiber
The features such as chemical stability height and strong mechanicalness.Therefore, quantum dot-doped glass is expected to put as a kind of Novel ultra wide band optical fiber
Big equipment material.
The direct band gap of PbSe body phase material can be 0.25eV, and corresponding wavelength is 4972.5nm.Relative to PbS, PbSe
Body phase material has wider band-gap energy, biggish exciton Bohr radius, PbSe quantum dot fluorescence quantum yield with higher.
Currently, external had some reports for preparing the quantum dot-doped glass of PbSe with fusion method.Chang etc. is incorporated into using PbSe
In SiO2-B2O3-ZnO-K2O parent glass batch, PbSe quantum dot borosilicate glass is obtained.In addition, in phosphate
In glass (Na2O-P2O5-Ga2O3-ZnO-MgO) substrate, Kolobkova etc. replaces PbO and Se using PbO and ZnSe or PbSe
Powder is obtained with certain density PbSe Quantum Dot Glass.The above work is all by using some more difficult volatilizations
Se compound (such as: ZnSe, PbSe etc.) volatile Se powder is replaced, to be prepared with certain density PbSe quantum dot
Doped-glass, but its higher cost；Or using the lower phosphate glass of melting temperature as substrate, but its chemical stability and
Mechanical performance is poor.It is domestic then without relevant report.
The problem to be solved by the invention is to provide a kind of preparation methods of high-performance optical fiber material, avoid using existing skill
The compound of the low volatility of the higher costs such as the PbSe or PbO that use in art and ZnSe, method is simple, cheap, amount
Sub- spot size is controllable.
Summary of the invention
The technical solution adopted by the present invention is that: a kind of preparation method of high-performance optical fiber material is as follows by mass percent
Raw material be made: SiO2:45~75%, B2O3:3~10%, SiC:3~10%, ZnO:5~20%, MgO:1~7%,
Na2O:10~25%, PbO:0.5~5%, Se:0.5~5%, C:0.5~2%.The high-performance optical fiber material is by following step
Rapid preparation: each raw material is weighed by above-mentioned mass percent, puts and mixes well in the ball mill, be placed in close crucible, 1100
~1450 DEG C of high-temperature fusion 30min~2h, it is then cooling rapidly, obtain light brown glass, finally carry out heat treatment process to get
To the high-performance optical fiber material of brownish black.
Further, heat treatment process of the present invention can specifically use following steps: by light brown glass in 500~700
DEG C heat treatment 30min~20h, taking-up are chilled to room temperature in air, obtain the high-performance optical fiber material.Further,
It is preferred that heat treatment temperature is 550~650 DEG C, heat treatment time is 3~10h.
Further, heat treatment process of the present invention can also specifically use following steps: by light brown glass in 400~
550 DEG C of Low Temperature Heat Treatment 30min~20h；Temperature is increased again to 550~700 DEG C, keeps the temperature 30min~10h, is taken out in air
It is chilled to room temperature, obtains the high-performance optical fiber material.Further, preferably Low Temperature Heat Treatment temperature is 450~530 DEG C,
It is preferred that the Low Temperature Heat Treatment time is 8~20h；It is preferred that after Low Temperature Heat Treatment, it is warming up to 550~650 DEG C, soaking time preferably 1~
8h。
Raw material composition of the invention: SiO2 and B2O3 is Network former, and SiC, ZnO are network intermediate, and Na2O is net
Network ectosome.SiC is used to adjust the Forming ability of glass, and ZnO facilitates quantum dot synthesis, can be reduced the volatilization of chalcogen, energy
The quantum dot size in glass is set to be distributed homogenization, Na2O accelerates glass to form reaction, reduces glass metal as cosolvent, MgO
Viscosity and surface tension, promote the clarification and homogenization of glass metal, and the effective nucleation agent as Quantum Dots Growth.PbO and
Introducing body of the Se as PbSe quantum dot.It is preferably added to excessive Se powder, so that the molar ratio of Se powder and PbO are greater than 1.Add
Entering excessive Se powder and allowing for Se element can largely be volatilized at high temperature, so that Se element containing in glass can be reduced
Amount.It joined a certain amount of C powder in glass batch simultaneously, play reduction, Se in glass melt is prevented to be partially oxidized,
To reduce the volatilization of Se element, the concentration of PbSe quantum dot in glass is improved.
Key problem in technology of the invention is that the growth size of quantum dot is controllable, distribution density is controllable, to reach optical property
It is controllable.Heat treatment process guarantees to generate the quantum dot crystal grain of certain density and certain size.Heat treatment process, that is, devitrification of glass
Process is the process of Pb2+ and Se2- ion diffusion, including nucleus is formed and two stages of crystal growth, and heat treatment temperature is higher,
Nucleus growth speed is faster, and heat treatment time is longer, and the PbSe quantum dot size in glass is bigger.Therefore, at by control heat
Time and temperature are managed, available difference size high-performance optical fiber material has in 1000-2300nm (communication band) this wave band
There are good, even ideal absorption and emission spectra.
Compared with prior art, the technical effects of the invention are that: the method for the present invention preparation high-performance optical fiber material tool
There is the features such as simple process, cheap, quantum dot size is controllable, the side mutually compatible with optical fiber technology of preparing now can be passed through
Formula --- optical fibre rod is drawn, and is directly drawn into quanta point optical fiber, so as to further prepare quantum dot light fiber amplifier, tool
There is performance more superior than conventional fiber amplifier, has the characteristics that wide spectrum.
Specific embodiment
To keep the purposes, technical schemes and advantages of the application clearer, below by the technical solution in embodiment into
Row clearly and completely describes.
Embodiment one:
According to glass formula be 58%SiO2,4%B2O3,4%SiC, 9%ZnO, 2%MgO, 16%Na2O, 3%PbO,
3%Se and 1%C (wt.%) weighs analysis pure SiO2:29.0g, B2O3:2.0g, SiC:2.0g, ZnO:4.5g, Na2CO3:
13.7g PbO:1.5g；Chemistry pure MgO3H2O:1.6g, Se:1.5g and C:0.5g.Above-mentioned chemical raw material is placed in ball mill
It stirs evenly, taking-up is placed in closed corundum crucible, is then put into cabinet-type electric furnace, in 1400 DEG C of high-temperature fusion 1h, so
Melt is poured on metal mold afterwards, rapid cooling to room temperature obtains light brown glass.
Then glass is put into cabinet-type electric furnace, in 550 DEG C of heat treatment 5h, taking-up is chilled to room temperature in air, can be with
Obtain the high-performance optical fiber material that PbSe quantum dot size is about 6nm.
Embodiment two:
According to glass formula be 58%SiO2,4%B2O3,4%SiC, 9%ZnO, 2%MgO, 16%Na2O, 3%PbO,
3%Se and 1%C (wt.%) weighs analysis pure SiO2:29.0g, B2O3:2.0g, SiC:2.0g, ZnO:4.5g, Na2CO3:
13.7g PbO:1.5g；Chemistry pure MgO3H2O:1.6g, Se:1.5g and C:0.5g.Above-mentioned chemical raw material is placed in ball mill
It stirs evenly, taking-up is placed in closed corundum crucible, is then put into cabinet-type electric furnace, in 1400 DEG C of high-temperature fusion 1h, so
Melt is poured on metal mold afterwards, rapid cooling to room temperature obtains light brown glass.
Then glass is put into cabinet-type electric furnace, in 600 DEG C of heat treatment 5h, taking-up is chilled to room temperature in air, can be with
Obtain the high-performance optical fiber material that PbSe quantum dot size is about 9nm.
Embodiment three:
According to glass formula be 58%SiO2,4%B2O3,4%SiC, 9%ZnO, 2%MgO, 16%Na2O, 3%PbO,
3%Se and 1%C (wt.%) weighs analysis pure SiO2:29.0g, B2O3:2.0g, SiC:2.0g, ZnO:4.5g, Na2CO3:
13.7g PbO:1.5g；Chemistry pure MgO3H2O:1.6g, Se:1.5g and C:0.5g.Above-mentioned chemical raw material is placed in ball mill
It stirs evenly, taking-up is placed in closed corundum crucible, is then put into cabinet-type electric furnace, in 1400 DEG C of high-temperature fusion 1h, so
Melt is poured on metal mold afterwards, rapid cooling to room temperature obtains light brown glass.
Then glass is put into cabinet-type electric furnace, in 650 DEG C of heat treatment 5h, taking-up is chilled to room temperature in air, can be with
Obtain the high-performance optical fiber material that PbSe quantum dot size is about 13nm.
Example IV:
According to glass formula be 58%SiO2,4%B2O3,4%SiC, 9%ZnO, 2%MgO, 14%Na2O, 4%PbO,
4%Se and 1%C (wt.%) weighs analysis pure SiO2:29.0g, B2O3:2.0g, SiC:2.0g, ZnO:4.5g, Na2CO3:
12.0g PbO:2.0g；Chemistry pure MgO3H2O:1.6g, Se:2.0g and C:0.5g.Above-mentioned chemical raw material is placed in ball mill
It stirs evenly, taking-up is placed in closed corundum crucible, is then put into cabinet-type electric furnace, in 1400 DEG C of high-temperature fusion 1h, so
Melt is poured on metal mold afterwards, rapid cooling to room temperature obtains light brown glass.
Then glass is put into cabinet-type electric furnace, in 530 DEG C of Low Temperature Heat Treatment 12h, then increases temperature to 650 DEG C, keeps the temperature
1h.Taking-up is chilled to room temperature, the high-performance optical fiber material that available PbSe quantum dot size is about 8nm in air.
Embodiment five:
According to glass formula be 58%SiO2,4%B2O3,4%SiC, 9%ZnO, 2%MgO, 14%Na2O, 4%PbO,
4%Se and 1%C (wt.%) weighs analysis pure SiO2:29.0g, B2O3:2.0g, SiC:2.0g, ZnO:4.5g, Na2CO3:
12.0g PbO:2.0g；Chemistry pure MgO3H2O:1.6g, Se:2.0g and C:0.5g.Above-mentioned chemical raw material is placed in ball mill
It stirs evenly, taking-up is placed in closed corundum crucible, is then put into cabinet-type electric furnace, in 1400 DEG C of high-temperature fusion 1h, so
Melt is poured on metal mold afterwards, rapid cooling to room temperature obtains light brown glass.
Then glass is put into cabinet-type electric furnace, in 530 DEG C of Low Temperature Heat Treatment 12h, then increases temperature to 650 DEG C, keeps the temperature
3h.Taking-up is chilled to room temperature, the high-performance optical fiber material that available PbSe quantum dot size is about 11nm in air.
Preferred embodiment of the invention is described above, but needs to know the expert of this field without departing from wound of the invention
Some modifications and variations can be made to the present invention in the case where meaning and range, the present invention ought to include all such modifications and
Variation, as long as they are in the claims limited range.
Claims (3)
1. a kind of preparation method of high-performance optical fiber material, which comprises the following steps: according to following mass percent
Weigh raw material: SiO2:45~75%, B2O3:3~10%, SiC:3~10%, ZnO:5~20%, MgO:1~7%, Na2O:
10~25%, PbO:0.5~5%, Se:0.5~5%, C:0.5~2%；It puts and mixes well in the ball mill, be placed in closed earthenware
It is then cooling rapidly in 1100~1450 DEG C of high-temperature fusion 30min~2h in crucible, light brown glass is obtained, hot place is finally carried out
Science and engineering skill is to get the high-performance optical fiber material for arriving brownish black.
2. the preparation method of high-performance optical fiber material according to claim 1, it is characterised in that: the heat treatment process
For by light brown glass in 500~700 DEG C of heat treatment 30min~20h, taking-up is chilled to room temperature in air, obtains described
High-performance optical fiber material.
3. the preparation method of high-performance optical fiber material according to claim 1, it is characterised in that: the heat treatment process
By light brown glass in 400~550 DEG C of Low Temperature Heat Treatment 30min~20h, then to increase temperature to 550~700 DEG C, keeping the temperature
30min~10h, taking-up are chilled to room temperature in air, obtain the high-performance optical fiber material.
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| CN201811441787.XA CN109399945A (en) | 2018-11-29 | 2018-11-29 | A kind of preparation method of high-performance optical fiber material |
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Application publication date: 20190301 |