CN102153283B - Method for preparing PbSe quantum dot doped fiber material - Google Patents
Method for preparing PbSe quantum dot doped fiber material Download PDFInfo
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- CN102153283B CN102153283B CN 201010546623 CN201010546623A CN102153283B CN 102153283 B CN102153283 B CN 102153283B CN 201010546623 CN201010546623 CN 201010546623 CN 201010546623 A CN201010546623 A CN 201010546623A CN 102153283 B CN102153283 B CN 102153283B
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- pbse
- doped fiber
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Abstract
The invention discloses a method for preparing a PbSe quantum dot doped fiber material. The fiber material is prepared from the following raw materials in percentage by mass: 45 to 75 percent of SiO2, 3 to 10 percent of B2O3, 3 to 10 percent of Al2O3, 5 to 20 percent of ZnO, 1 to 7 percent of AlF3, 10 to 25 percent of Na2O, 0.5 to 5 percent of PbO, 0.5 to 5 percent of Se, and 0.5 to 2 percent of C. The PbSe quantum dot doped fiber material is prepared by the following steps of: weighing the raw materials in mass percentage, putting the raw materials into a ball mill, fully mixing the raw materials uniformly, putting the mixture into a closed crucible, melting the mixture for 30 minutes to 2 hours at the high temperature of between 1,100 and 1,450 DEG C, then quickly cooling the melt to obtain light brown grass, and finally performing a thermal treatment process to obtain the brown black PbSe quantum dot doped fiber material. The PbSe quantum dot doped fiber material prepared by the method has the characteristics of simple process, low price, controllable quantum dot size and the like.
Description
(1) technical field
The present invention relates to optical communication technique and field of nano material preparation, be specifically related to the preparation method of the quantum dot-doped fiber optic materials of a kind of PbSe.The prepared quantum dot-doped fiber optic materials of PbSe of the present invention can be applicable to fiber amplifier.
(2) background technology
Quantum dot is a kind of accurate zero dimension semiconductor nanocrystal, its radius less than or close to the exciton Bohr radius.Because the strong confinement effect of quantum that its minimum size causes makes quantum dot show electricity, optics and the magnetism characteristic of many uniquenesses, thereby has caused that people pay close attention to greatly.Wherein the IV-VI semiconductor-quantum-point such as PbSe, PbS, because it has larger exciton Bohr radius (PbSe is 46nm, and PbS is 18nm), thereby causes strong quantum confined effect, shows strong fluorescence emission spectrum.By changing the size of quantum dot, can obtain the quantum dot of different fluorescent emission peak value wavelength, its fluorescent emission peak value wavelength nearly cover near-infrared band (1000-2300nm), research has shown that also quantum dot can be used as the good gain of light and amplification medium, and this makes quantum dot have very important application prospect aspect opto-electronic device.Particularly the IV-VI semiconductor-quantum-point is incorporated in the fiber optic materials (for example: glass, plastics), is optical-fiber type quantum dot light electronics device (for example quantum dot-doped fiber amplifier of PbSe) development and application, opened a fan gate.In addition, studies show that quantum dot-doped fiber amplifier has more excellent performance than conventional fiber amplifier, has the characteristics such as wide spectrum, high gain, lower noise.
The preparation method of quantum dot mainly contains: molecular beam epitaxial growth method, sol-gel method, scorification etc.Wherein to prepare the quantum dot doped-glass be one of focus of paying close attention to of people in recent years to scorification.A very large advantage utilizing the quantum dot-doped glass of this method preparation is can be by compatible mutually mode---optical fibre rod draws, and directly is drawn into quanta point optical fiber, thereby can further prepares the quantum dot light fiber amplifier with optical fiber technology of preparing now.Glass optical fiber has the characteristics such as chemical stability height and mechanicalness are strong with respect to plastic optical fiber.Therefore, quantum dot-doped glass is expected to become a kind of Novel Ultra-wide Band Fiber Amplifiers material.
The direct band gap of PbSe body phase material can be 0.25eV, and corresponding wavelength is 4972.5nm.With respect to PbS, the PbSe body phase material has wider band-gap energy, larger exciton Bohr radius, and the PbSe quantum dot has higher fluorescence quantum yield.At present, there were some to prepare the report of the quantum dot-doped glass of PbSe with scorification abroad.The employing PbSe such as Chang are incorporated into SiO
2-B
2O
3-ZnO-K
2In the O parent glass admixtion, obtained PbSe quantum dot borosilicate glass.In addition, at phosphate glass (Na
2O-P
2O
5-Ga
2O
3-ZnO-AlF
3) in the substrate, Kolobkova etc. adopt PbO and ZnSe or PbSe to replace PbO and Se powder, have obtained to have certain density PbSe Quantum Dot Glass.More than these work all be that Se compounds (such as ZnSe, PbSe etc.) by adopting some difficult volatilizations replace volatile Se powder, prepare to have the quantum dot-doped glass of certain density PbSe, but its cost is higher; Or adopt the lower phosphate glass of melt temperature as substrate, but its chemical stability and mechanical property are relatively poor.Domestic then do not have a relevant report.
(3) summary of the invention
Problem to be solved by this invention provides the preparation method of the quantum dot-doped fiber optic materials of a kind of PbSe, avoid using the compound of the higher low volatility of the PbSe of available technology adopting or the costs such as PbO and ZnSe, its method is simple, cheap, and quantum dot size is controlled.
Thinking of the present invention is: at first directly the hotchpotch PbO and the Se that generate the semiconductor nanocrystal quantum dot are joined in the parent glass admixtion, through fully obtaining glass after mixing, high-temperature fusion, the rapid cooling, then pass through thermal treatment process, thereby can obtain the quantum dot-doped fiber optic materials of quantum dot size and even density distribution.
The technical solution used in the present invention is:
The preparation method of the quantum dot-doped fiber optic materials of a kind of PbSe, made by the raw material that mass percent is following:
SiO
2 45～75％
B
2O
3 3～10％
Al
2O
3 3～10％
ZnO 5～20％
AlF
3 1～7％
Na
2O 10～25％
PbO 0.5～5％
Se 0.5～5％
C 0.5～2％
The quantum dot-doped fiber optic materials of described PbSe prepares as follows: take by weighing each raw material by above-mentioned mass percent, be placed on abundant mixing in the ball mill, place close crucible, at 1100～1450 ℃ of high-temperature fusion 30min～2h, then rapidly cooling, obtain light brown glass, heat-treat at last technique, namely obtain the quantum dot-doped fiber optic materials of PbSe of brownish black.
Further, thermal treatment process of the present invention can specifically adopt following steps: light brown glass in 500～700 ℃ of thermal treatment 30min～20h, is taken out and be chilled to room temperature in air, obtain the quantum dot-doped fiber optic materials of described PbSe.Further, preferred thermal treatment temp is 550～650 ℃, and heat treatment time is 3～10h.
Further, thermal treatment process of the present invention also can specifically adopt following steps: with light brown glass in 400～550 ℃ of low-temperature heat treatment 30min～20h; Raise again temperature to 550～700 ℃, insulation 30min～10h takes out and be chilled to room temperature in air, obtains the quantum dot-doped fiber optic materials of described PbSe.Further, preferred low-temperature heat treatment temperature is 450～530 ℃, and the preferred low-temperature heat treatment time is 8～20h; After the preferred low-temperature heat treatment, be warming up to 550～650 ℃, the preferred 1～8h of soaking time.
Raw material of the present invention forms: SiO
2And B
2O
3Be Network former, Al
2O
3, ZnO is the network intermediate, Na
2O is network outer body.Al
2O
3Be used for regulating the formation ability of glass, ZnO helps quantum dot synthetic, can reduce the volatilization of sulfur family element, can make the quantum dot size distribution homogenization in the glass, Na
2O is as solubility promoter, AlF
3Accelerate glass and form reaction, reduce viscosity and the surface tension of glass metal, promote the clarification and homogenization of glass metal, and as the effective nucleation agent of Quantum Dots Growth.PbO and Se are as the introducing body of PbSe quantum dot.The excessive Se powder of preferred adding is so that the molar ratio of Se powder and PbO is greater than 1.Adding excessive Se powder is to consider that the Se element at high temperature can be volatilized in a large number, thereby can reduce the content of Se element in glass.In glass batch, add simultaneously a certain amount of C powder, played reductive action, prevented that Se is partially oxidized in the glass melt, thereby reduced the volatilization of Se element, improved the concentration of PbSe quantum dot in glass.
Key problem in technology of the present invention is that the growth size of quantum dot is controlled, distribution density is controlled, thereby reaches the controlled of optical property.Heat treatment process guarantees to generate the quantum dot crystal grain of certain density and certain size.Heat treatment process is that the devitrification of glass process is Pb
2+And Se
2-The process of ion diffusion comprises that nucleus forms and crystal two stages of growth, and thermal treatment temp is higher, and nucleus growth speed is faster, and heat treatment time is longer, and the PbSe quantum dot size in the glass is larger.Therefore, by control heat treatment time and temperature, can obtain the quantum dot-doped fiber optic materials of different size PbSe, have good or even desirable absorption and emission spectrum at this wave band of 1000-2300nm (communication band).
Compared with prior art, technique effect of the present invention is: the quantum dot-doped fiber optic materials of PbSe of the inventive method preparation has the characteristics such as technique is simple, cheap, quantum dot size is controlled, can be by compatible mutually mode---optical fibre rod draws with optical fiber technology of preparing now, directly be drawn into quanta point optical fiber, thereby can further prepare the quantum dot light fiber amplifier, have the performance more excellent than conventional fiber amplifier, have the characteristics such as wide spectrum.
(4) description of drawings
Fig. 1 is the transmission electron microscope picture of 6nmPbSe quantum dot among the embodiment one;
Fig. 2 is the fluorescent emission spectrogram of 6nmPbSe quantum dot among the embodiment one;
Fig. 3 is the transmission electron microscope picture of 9nmPbSe quantum dot among the embodiment two;
Fig. 4 is the fluorescent emission spectrogram of 9nmPbSe quantum dot among the embodiment two;
Fig. 5 is the transmission electron microscope picture of 5.5nmPbSe quantum dot among the embodiment six;
Fig. 6 is the fluorescent emission spectrogram of 5.5nmPbSe quantum dot among the embodiment six.
(5) embodiment
The present invention is described further below in conjunction with specific embodiment:
Embodiment one:
Be 58%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 9%ZnO, 2%AlF
3, 16%Na
2O, 3%PbO, 3%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 29.0g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:4.5g, Na
2CO
3: 13.7g, PbO:1.5g; Chemical pure AlF
33H
2O:1.6g, Se:1.5g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 550 ℃ of thermal treatment 5h, take out and in air, be chilled to room temperature, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 6nm.The transmission electron microscope picture of the quantum dot-doped fiber optic materials of prepared PbSe (scale is 20nm) as shown in Figure 1, the fluorescent emission spectrogram as shown in Figure 2, its full width at half maximum is 275nm.
Embodiment two:
Be 58%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 9%ZnO, 2%AlF
3, 16%Na
2O, 3%PbO, 3%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 29.0g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:4.5g, Na
2CO
3: 13.7g, PbO:1.5g; Chemical pure AlF
33H
2O:1.6g, Se:1.5g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 600 ℃ of thermal treatment 5h, take out and in air, be chilled to room temperature, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 9nm.The transmission electron microscope picture of the quantum dot-doped fiber optic materials of prepared PbSe (scale is 20nm) as shown in Figure 3, the fluorescent emission spectrogram as shown in Figure 4, its full width at half maximum is 506nm.
Embodiment three:
Be 58%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 9%ZnO, 2%AlF
3, 16%Na
2O, 3%PbO, 3%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 29.0g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:4.5g, Na
2CO
3: 13.7g, PbO:1.5g; Chemical pure AlF
33H
2O:1.6g, Se:1.5g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 650 ℃ of thermal treatment 5h, take out and in air, be chilled to room temperature, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 13nm.
Embodiment four:
Be 58%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 9%ZnO, 2%AlF
3, 14%Na
2O, 4%PbO, 4%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 29.0g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:4.5g, Na
2CO
3: 12.0g, PbO:2.0g; Chemical pure AlF
33H
2O:1.6g, Se:2.0g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 530 ℃ of low-temperature heat treatment 12h, the temperature to 650 that raises again ℃, insulation 1h.Taking-up is chilled to room temperature in air, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 8nm.
Embodiment five:
Be 58%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 9%ZnO, 2%AlF
3, 14%Na
2O, 4%PbO, 4%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 29.0g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:4.5g, Na
2CO
3: 12.0g, PbO:2.0g; Chemical pure AlF
33H
2O:1.6g, Se:2.0g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 530 ℃ of low-temperature heat treatment 12h, the temperature to 650 that raises again ℃, insulation 3h.Taking-up is chilled to room temperature in air, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 11nm.
Embodiment six:
Be 58%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 11%ZnO, 2%AlF
3, 14%Na
2O, 3%PbO, 3%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 29.0g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:5.5g, Na
2CO
3: 12.0g, PbO:1.5g; Chemical pure AlF
33H
2O:1.6g, Se:1.5g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 500 ℃ of low-temperature heat treatment 10h, the temperature to 550 that raises again ℃, insulation 3h.Taking-up is chilled to room temperature in air, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 5.5nm.The transmission electron microscope picture of the quantum dot-doped fiber optic materials of prepared PbSe (scale is 50nm) as shown in Figure 5, the fluorescent emission spectrogram as shown in Figure 6, its full width at half maximum is 508nm.
Embodiment seven:
Be 56%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 11%ZnO, 2%AlF
3, 16%Na
2O, 3%PbO, 3%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 28.0g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:5.5g, Na
2CO
3: 13.7g, PbO:1.5g; Chemical pure AlF
33H
2O:1.6g, Se:1.5g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 500 ℃ of low-temperature heat treatment 10h, the temperature to 550 that raises again ℃, insulation 3h.Taking-up is chilled to room temperature in air, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 7nm.
Embodiment eight:
Be 53%SiO according to glass formula
2, 4%B
2O
3, 4%Al
2O
3, 14%ZnO, 2%AlF
3, 16%Na
2O, 3%PbO, 3%Se and 1%C (wt.%) take by weighing analytical pure SiO
2: 26.5g, B
2O
3: 2.0g, Al
2O
3: 2.0g, ZnO:7.0g, Na
2CO
3: 13.7g, PbO:1.5g; Chemical pure AlF
33H
2O:1.6g, Se:1.5g and C:0.5g.Place ball mill to stir above-mentioned chemical feedstocks, taking-up is placed in the airtight corundum crucible, then puts into cabinet-type electric furnace, at 1400 ℃ of high-temperature fusion 1h, then melt is poured on the metal pattern, and cool to room temperature obtains light brown glass rapidly.
Then glass is put into cabinet-type electric furnace, at 500 ℃ of low-temperature heat treatment 10h, the temperature to 550 that raises again ℃, insulation 3h.Taking-up is chilled to room temperature in air, can obtain the quantum dot-doped fiber optic materials that the PbSe quantum dot size is about 10nm.
The above has introduced preferred embodiment of the present invention, but the expert that need to know this area can make some modifications and variations to the present invention in the situation of not leaving intention of the present invention and scope, the present invention ought to comprise all such modifications and variation, as long as they are in these claims limited range.
Claims (4)
1. the preparation method of the quantum dot-doped fiber optic materials of PbSe, made by the raw material that mass percent is following:
The quantum dot-doped fiber optic materials of described PbSe prepares as follows: take by weighing each raw material by above-mentioned mass percent, be placed on abundant mixing in the ball mill, place close crucible, at 1100～1450 ℃ of high-temperature fusion 30min～2h, then rapidly cooling, obtain light brown glass, heat-treat at last technique, namely obtain the quantum dot-doped fiber optic materials of PbSe of brownish black;
Described thermal treatment process adopts scheme 1, and is specific as follows: light brown glass in 500～700 ℃ of thermal treatment 30min～20h, is taken out and be chilled to room temperature in air, obtain the quantum dot-doped fiber optic materials of described PbSe;
Perhaps described thermal treatment process adopts scheme 2, specific as follows: with light brown glass in 400～550 ℃ of low-temperature heat treatment 30min～20h, temperature to 550～700 ℃ of raising again, insulation 30min～10h, taking-up is chilled to room temperature in air, obtain the quantum dot-doped fiber optic materials of described PbSe.
2. the preparation method of the quantum dot-doped fiber optic materials of PbSe according to claim 1 is characterized in that: in the described scheme 1, with light brown glass in 550～650 ℃ of thermal treatment 3～10h.
3. the preparation method of the quantum dot-doped fiber optic materials of PbSe according to claim 1 is characterized in that: in the described scheme 2, with light brown glass in 450～530 ℃ of low-temperature heat treatment 8～20h, temperature to 550～650 ℃ of raising again, insulation 1～8h.
4. one of according to claim 1～3 the preparation method of the quantum dot-doped fiber optic materials of described PbSe is characterized in that the molar ratio of Se powder and PbO is greater than 1.
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| CN102674692A (en) * | 2012-04-25 | 2012-09-19 | 程潇羽 | Preparation method for high-density PbSe quantum dot silicate glass |
| CN103043912B (en) * | 2012-12-16 | 2015-04-08 | 青岛文创科技有限公司 | Preparation method of quantum dot optical fiber core |
| CN104556692B (en) * | 2014-12-17 | 2017-01-18 | 武汉理工大学 | PbSe quantum dot doped germanate glass and preparation method thereof |
| CN104529152B (en) * | 2014-12-17 | 2017-03-08 | 武汉理工大学 | A kind of CdSe quantum dot doped-glass and preparation method thereof |
| CN104556678B (en) * | 2015-01-19 | 2017-06-20 | 华南理工大学 | A kind of preparation method of quantum dot-doped microcrystalline glass optical fiber |
| CN106830679A (en) * | 2017-04-06 | 2017-06-13 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of the quantum dot-doped alumina silicate glass high of vulcanized lead |
| CN107147003A (en) * | 2017-05-27 | 2017-09-08 | 杭州电子科技大学 | Lead selenide quantum dot as gain media mode locked fiber laser |
| CN108975681A (en) * | 2017-05-31 | 2018-12-11 | Tcl集团股份有限公司 | High temperature resistant quanta point material and preparation method thereof |
| CN108519714A (en) * | 2018-06-27 | 2018-09-11 | 浙江工业大学 | A kind of sodium Boroalumino silicate glasses near-infrared broadband PbSe quantum dot light fiber amplifiers |
| CN112159099A (en) * | 2020-09-23 | 2021-01-01 | 中国科学院上海光学精密机械研究所 | Method for inducing precipitation of quantum dots in glass by picosecond laser |
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| CN1284738C (en) * | 2000-12-22 | 2006-11-15 | 康宁股份有限公司 | Treating soot preforms with a reducing agent |
| US6711918B1 (en) * | 2001-02-06 | 2004-03-30 | Sandia National Laboratories | Method of bundling rods so as to form an optical fiber preform |
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| US4141710A (en) * | 1976-08-23 | 1979-02-27 | Siemens Aktiengesellschaft | Method for producing light conducting fibers |
| CN1380265A (en) * | 2000-12-28 | 2002-11-20 | 彭波 | Optical fibre of light-guide wave path glass and its optical fibre and optical amplifier |
| CN101441295A (en) * | 2008-12-11 | 2009-05-27 | 浙江工业大学 | Method for preparing quantum point optical fiber core |
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