CN101798179A - Dichroic nanogold-particle-doped glass and preparation method thereof - Google Patents

Dichroic nanogold-particle-doped glass and preparation method thereof Download PDF

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Publication number
CN101798179A
CN101798179A CN 201010138093 CN201010138093A CN101798179A CN 101798179 A CN101798179 A CN 101798179A CN 201010138093 CN201010138093 CN 201010138093 CN 201010138093 A CN201010138093 A CN 201010138093A CN 101798179 A CN101798179 A CN 101798179A
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China
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glass
preparation
dichroic
gold
femtosecond laser
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曾惠丹
范茬兴
林振钰
杨一凡
陈国荣
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East China University of Science and Technology
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East China University of Science and Technology
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Abstract

The invention discloses a dichroic nanogold-particle-doped glass and a preparation method. The preparation method comprises the following steps: synthesizing gold-doped colorless and transparent glass at high temperature; carrying out secondary heat treatment at 500-600 DEG C; preparing glass doped with even purple gold particles the particle diameter of which is at nanoscales; finally, after the irradiation function of femto-second lasers, obtaining functional optical glass with different absorption coefficients to polarized light with different vibration directions.

Description

Has glass of dichroic, dopen Nano gold grain and preparation method thereof
Technical field
The present invention relates to glass of a kind of dopen Nano gold grain and preparation method thereof, particularly a kind of functionalization opticglass that femtosecond laser irradiation produces dichroic, dopen Nano gold grain and preparation method thereof that utilizes.Be applied to optics such as polarization chamber, photorectifier, amplifier.
Background technology
Utilize the glass of doping noble metal element to carry out the design of various nanometers or microtexture, have crucial directive significance for synthetic advanced material and optics field.In recent years, based on characteristics such as the surface plasma body resonant vibration (SPR) of nanometer precious metal particles, enhanced third-order nonlinear optical coefficients, mix glass materials such as gold and silver and have great application prospect, make it be subjected to people and more and more pay close attention in fields such as nonlinear material, optical element, nano photoelectric devices.The introducing of laser technology makes in the size of glass internal control precious metal particles, shape, and density and three-dimensional spatial distribution become possibility, and especially linearity and the nonlinear optical property to this glass material carried out maximum optimization.Document Appl.Phys.B94,459-465 (2009) have reported by the femtosecond laser radiation and have made the Yin Nami spherical particle of glass inside be transformed into anisotropic axiolitic silver nano-grain.Document J.Opt.A:Pure Appl.Opt.11065001 (2009) thus reported that also the shape that changes the inner silver nano-grain of glass by femtosecond laser produces optical dichroism.Up to the present, improve the shape and the arrangement of gold nano grain, further produce dichroic phenomenon and also do not report by using femtosecond laser.
In a word, remain a difficult problem by size, shape, density and the three-dimensional space arrangement that utilizes the inner precious metal particles of femtosecond laser regulating and controlling glass.In addition, the dichroism of utilizing femtosecond laser irradiation to produce, make its in the polarization chamber, fields such as spectrometric instrument (chromatographic instrument etc.), spectroscopic techniques research have huge application potential.
Summary of the invention
The objective of the invention is to propose a kind of functionalization opticglass that femtosecond laser irradiation produces dichroic, dopen Nano gold grain and preparation method thereof that utilizes.
That the present invention has is dichroic, the feature of the functionalization opticglass of dopen Nano gold grain is as follows:
By at high temperature synthesizing the colourless transparent glass of the gold that mixes, then it is carried out second heat treatment at 500~600 ℃, prepare mauve, doping contains big or small homogeneous, particle diameter is the gold grain glass of nanoscale.By under femtosecond laser irradiation, has the functionalization opticglass of different uptake factors for the polarization light of different direction of vibration at last.
That the present invention has is dichroic, the preparation method of the functionalization opticglass of dopen Nano gold grain is as follows:
Take by weighing various composition materials by forming calculated amount, its composition molar percentage is SiO 2: Na 2O:CaO:MgO: PbO: Au 2O 3=40%-80%: 5%-20%: 5%-20%: 0%-20%: 0%-10%: 0.005%-0.5%.Adopt the preparation of heating for multiple times method, be about to above-mentioned raw materials and fully grind and be mixed evenly, insert in quartz crucible or the platinum crucible, put into high-temperature smelting pot; At 1450-1700 ℃ of following fusion 1-5 hour, make raw materials melt become liquid, and melt is mixed.After melt thermostatically heating 1-5 hour, from the high temperature stove, take out crucible, and melt in the crucible is poured into fast on the mould of prior preheating and formed glass sample, glass sample put into 500-600 ℃ stove, slowly cooling annealing is 18-36 hour, glass after the annealing can obtain the golden colourless transparent glass that mixes through processing such as cutting, polishings; And then will mix the gold glass carried out second heat treatment 5-24 hour at 450-600 ℃, can obtain separating out the red-purple glass of nm gold particles; At last by femtosecond laser is focused on glass inner certain a bit, utilize software and workplatform control sample to move and carry out irradiation experiment.
That the present invention has is dichroic, the parameter of the functionalization femtosecond laser that opticglass uses of dopen Nano gold grain is:
Femtosecond laser frequency ν=1 kilohertz (kHZ), pulse wavelength X=400 nanometers (nm), the numerical aperture NA=0.2-0.8 of focusing objective len, recurrence interval τ=120-150 femtosecond (fs), depth of focus h=50-700 micron (μ m), scan velocity V=5-500 micron per second (μ m/s), the ENERGY E of each pulse=0.3-50 milliwatt (mW).
The present invention has, and functionalization opticglass dichroic, the dopen Nano gold grain is that doping contains big or small homogeneous, diameter is the nm gold particles of 3~5m, has the functionalization opticglass of different uptake factors for the polarization light of different direction of vibration, in the polarization chamber, field such as spectrometric instrument (chromatographic instrument etc.), spectroscopic techniques research has huge application potential.
Description of drawings
Having of obtaining in Fig. 1 example 1 is dichroic, the abosrption spectrogram of the transmission electron microscope TEM photo of the glass of dopen Nano gold grain and different directions polarized light
Embodiment
Following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1
The preparation molar percentage is 20Na earlier 2O6CaO70SiO 24PbO0.01Au 2O 3Glass.Adopting quartz sand, soda ash, lime carbonate, plumbous oxide and hydrochloro-auric acid is main raw material, take by weighing earlier 42.0 gram quartz sands, 21.2 gram soda ash, 6.0 gram lime carbonate, 8.93 gram plumbous oxide and 0.039g chloric acid gold respectively, with above-mentioned raw materials fully grind be mixed even, insert in quartz crucible or the platinum crucible, put into high-temperature smelting pot; 1500 ℃ of following fusions 2 hours, make raw materials melt become liquid, and melt is mixed.After the melt thermostatically heating 2 hours, from the high temperature stove, take out crucible, and melt in the crucible is poured into fast on the mould of prior preheating and formed glass sample, glass sample put into 500 ℃ stove, slowly cooling annealing is 24 hours, glass after the annealing can obtain the golden colourless transparent glass that mixes through processing such as cutting, polishings; And then the glass of the gold that will mix can obtain the golden colourless transparent glass that mixes 500 ℃ of processing such as polishing; And then will mix the gold glass carried out second heat treatment 12 hours at 500 ℃, can obtain separating out the glass of nm gold particles; At last by femtosecond laser is focused on glass inner certain a bit, utilize software and workplatform control sample to move and carry out irradiation experiment.Laser parameter is respectively: femtosecond laser frequency ν=1 kilohertz (kHZ), pulse wavelength X=400 nanometers (nm), the numerical aperture NA=0.6 of focusing objective len, recurrence interval τ=120 femtoseconds (fs), depth of focus h=300 micron (μ m), scan velocity V=50 micron per second (μ m/s), the ENERGY E of each pulse=2.5 milliwatts (mW).
Fig. 1 is dichroic for having in the example 1, the glass of dopen Nano gold grain in 350-550nm and 550-750nm wavelength region, the abosrption spectrogram to different directions polarization light of identical radiation areas.From figure, can clearly observe, in the 350-550nm wavelength region, sample is for the uptake factor of the horizontal polarization light uptake factor greater than vertical polarization light, and in the 550-750nm wavelength region, situation is just in time opposite, and sample is for the uptake factor of the horizontal polarization light uptake factor less than vertical polarization light.

Claims (3)

1. have glass dichroic, the dopen Nano gold grain it is characterized in that by will mix the gold colourless transparent glass carry out second heat treatment at 500~600 ℃, prepare mauve, doping contains big or small homogeneous, particle diameter is the glass of the gold grain of nanoscale.And then utilize femtosecond laser irradiation, have the functionalization opticglass of different uptake factors for the polarization light of different direction of vibration.
2. the preparation method with glass of dichroic, dopen Nano gold grain as claimed in claim 1 is characterized in that the preparation method is as follows:
Take by weighing various composition materials by forming calculated amount, its composition molar percentage is SiO 2: Na 2O: CaO: MgO: PbO: Au 2O 3=40%-80%: 5%-20%: 5%-20%: 0%-20%: 0%-10%: 0.005%-0.5%.Adopt the preparation of heating for multiple times method, be about to above-mentioned raw materials and fully grind and be mixed evenly, insert in quartz crucible or the platinum crucible, put into high-temperature smelting pot; At 1450-1700 ℃ of following fusion 1-5 hour, make raw materials melt become liquid, and melt is mixed.After melt thermostatically heating 1-5 hour, from the high temperature stove, take out crucible, and melt in the crucible is poured into fast on the mould of prior preheating and formed glass sample, glass sample put into 500-600 ℃ stove, slowly cooling annealing is 18-36 hour, glass after the annealing can obtain the golden colourless transparent glass that mixes through processing such as cutting, polishings; And then will mix the gold glass carried out second heat treatment 5-24 hour at 450-600 ℃, can obtain separating out the glass of nm gold particles; At last by femtosecond laser is focused on glass inner certain a bit, utilize software and workplatform control sample to move and carry out irradiation experiment.
3. have the preparation method of the glass of dichroic, dopen Nano gold grain according to claim 2, it is characterized in that the parameter of the femtosecond laser that uses is:
Femtosecond laser frequency v=1 kilohertz (kHZ), pulse wavelength X=400 nanometers (nm), the numerical aperture NA=0.2-0.8 of focusing objective len, recurrence interval τ=120-150 femtosecond (fs), depth of focus h=50-700 micron (μ m), scan velocity V=5-500 micron per second (μ m/s), the ENERGY E of each pulse=0.3-50 milliwatt (mW).
CN 201010138093 2010-04-02 2010-04-02 Dichroic nanogold-particle-doped glass and preparation method thereof Pending CN101798179A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103145343A (en) * 2013-03-06 2013-06-12 宁波大学 Metal nanoparticle glass composite block material and preparation method thereof
CN113267842A (en) * 2021-05-19 2021-08-17 福州高意光学有限公司 Glass polaroid and manufacturing method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1138640A2 (en) * 2000-03-29 2001-10-04 Heraeus Quarzglas GmbH & Co. KG Method and apparatus for heat treatment of synthetic quartz glass
CN1448733A (en) * 2003-04-11 2003-10-15 中国科学院上海光学精密机械研究所 Method for preparing noble metal nano microstructure grating
JP2004226811A (en) * 2003-01-24 2004-08-12 Institute Of Physical & Chemical Research Micro optical element and its manufacturing method
CN1583629A (en) * 2004-06-01 2005-02-23 中国科学院上海光学精密机械研究所 Method for manufacturing ultraviolet pulse laser irradiation assisted nano-doped glass
US20060107696A1 (en) * 2003-07-31 2006-05-25 Arisawa Mfg. Co., Ltd. Method for producing polarizing glass

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1138640A2 (en) * 2000-03-29 2001-10-04 Heraeus Quarzglas GmbH & Co. KG Method and apparatus for heat treatment of synthetic quartz glass
JP2004226811A (en) * 2003-01-24 2004-08-12 Institute Of Physical & Chemical Research Micro optical element and its manufacturing method
CN1448733A (en) * 2003-04-11 2003-10-15 中国科学院上海光学精密机械研究所 Method for preparing noble metal nano microstructure grating
US20060107696A1 (en) * 2003-07-31 2006-05-25 Arisawa Mfg. Co., Ltd. Method for producing polarizing glass
CN1583629A (en) * 2004-06-01 2005-02-23 中国科学院上海光学精密机械研究所 Method for manufacturing ultraviolet pulse laser irradiation assisted nano-doped glass

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103145343A (en) * 2013-03-06 2013-06-12 宁波大学 Metal nanoparticle glass composite block material and preparation method thereof
CN103145343B (en) * 2013-03-06 2015-11-18 宁波大学 A kind of metal nanoparticle composite block glass material and preparation method thereof
CN113267842A (en) * 2021-05-19 2021-08-17 福州高意光学有限公司 Glass polaroid and manufacturing method thereof

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Application publication date: 20100811