CN109180011B - PbTe/CdTe double quantum dot co-doped borosilicate glass and preparation process thereof - Google Patents

PbTe/CdTe double quantum dot co-doped borosilicate glass and preparation process thereof Download PDF

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CN109180011B
CN109180011B CN201810902490.2A CN201810902490A CN109180011B CN 109180011 B CN109180011 B CN 109180011B CN 201810902490 A CN201810902490 A CN 201810902490A CN 109180011 B CN109180011 B CN 109180011B
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朱世新
杨雍
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SUZHOU RONGRUI ELECTRONIC TECHNOLOGY Co.,Ltd.
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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
    • 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
    • C03C14/006—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 microcrystallites, e.g. of optically or electrically active material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00—Annealing glass products
    • 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
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/16—Microcrystallites, e.g. of optically or electrically active material

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Abstract

The invention discloses PbTe/CdTe double quantum dot codoped borosilicate glass and a preparation process thereof, wherein the PbTe/CdTe double quantum dot codoped borosilicate glass comprises the following raw materials in percentage by mole: SiO 2245‑75％、B2O36‑12％、Na2O 4‑8％、Al2O30.1‑3％、ZnTe 2.5‑9％、PbO 1.2‑2.4％、CdO 1‑2％、CaO 5‑9％、ZnO 4‑6％、SrF21‑2％、Mg2B2O50.1‑0.6％、La2O3+Pr2O3+Nb2O50.1 to 1 percent. The invention mixes PbTe quantum dots and CdTe quantum dots in a borosilicate glass system by a melting method, realizes the comprehensive coverage of visible light, near infrared light and intermediate infrared light, has the spectral response range of 500-2100nm, and regulates and controls the growth size and growth speed of the quantum dots by different heat treatment processes.

Description

PbTe/CdTe double quantum dot co-doped borosilicate glass and preparation process thereof
Technical Field
The invention relates to the technical field of glass manufacturing, in particular to PbTe/CdTe double quantum dot co-doped borosilicate glass and a preparation process thereof.
Background
Borosilicate glass, also known as borosilicate glass, has excellent thermal stability, chemical stability, mechanical properties, processing properties, optical properties, and the like. Compared with common glass, the borosilicate glass has low content of alkali metal oxide and higher content of boron oxide, and the basic component comprises 70-80% of SiO2、6％-15％B2O3、4％-10％Na2O, wherein, Na2O is B2O3Oxygen vacancies in the crystal lattice provide free oxygen to [ BO3]The layered triangular units are orderly connected into [ BO ] by sharing oxygen atoms4]A frame-like tetrahedron structure of [ BO ]4]And [ SiO ]4]Further constructing a complete network structure as B2O3With SiO2The co-heating synthesis of uniform and stable glass creates conditions.
The quantum dot is a semiconductor nano structure which restrains conduction band electrons, valence band holes and excitons in three spatial directions, has good quantum surface effect, quantum size effect, quantum confinement effect and quantum tunnel effect, and when the three-dimensional nano scale of the quantum dot is smaller than the exciton Bohr radius of a corresponding semiconductor material, the movement of a current carrier is limited, so that the continuous energy band of the semiconductor is changed into discrete energy level. Common quantum dots are composed of group IV, II-VI, IV-VI, or III-V elements, such as Si quantum dots, Ge quantum dots, CdS quantum dots, CdSe quantum dots, CdTe quantum dots, ZnSe quantum dots, PbS quantum dots, PbSe quantum dots, InP quantum dots, InAs quantum dots, and the like. With the rapid development of the communication industry and the solar photovoltaic industry, the chemical modification of quartz glass by adopting quantum dots has become a research hotspot of technicians in the field. At present, quantum dot doped glass has low emission spectrum coverage rate, cannot absorb all visible light wave bands and mid-infrared wave bands in sunlight, has narrow photoluminescence spectrum range, and needs to further improve photoelectric conversion rate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide PbSe quantum dot doped borosilicate glass and a preparation process thereof.
The technical scheme of the invention is summarized as follows:
a PbTe/CdTe double quantum dot codoped borosilicate glass comprises the following raw materials in percentage by mole: SiO 2245-75％、B2O36-12％、Na2O 4-8％、Al2O30.1-3％、ZnTe 2.5-9％、PbO 1.2-2.4％、CdO 1-2％、CaO 5-9％、ZnO 4-6％、SrF21-2％、Mg2B2O50.1-0.6％、La2O3+Pr2O3+Nb2O50.1-1％。
Preferably, the La is2O3、Pr2O3And Nb2O5The molar ratio of (2-3): (1.5-2): 1.
the invention also provides a preparation process of the PbTe/CdTe double quantum dot codoped borosilicate glass, which comprises the following steps:
s1: uniformly mixing the glass raw materials according to the mole percentage, heating to 1250-;
s2: when the temperature of the glass melt is reduced to 1000-1200 ℃, the glass melt is cast on a graphite mold for molding, and then annealing treatment is carried out for 3 hours at the temperature of 550-570 ℃;
s3: and carrying out heat treatment on the annealed glass, and cutting and polishing after the PbTe quantum dots and the CdTe quantum dots are separated out to obtain the PbTe/CdTe double-quantum-dot co-doped borosilicate glass.
Preferably, the heat treatment process is as follows: heating the glass at the constant temperature of 600 ℃ for 1-2h at 550 ℃ and then raising the temperature to 750 ℃ at the rate of 3-5 ℃/min, preserving the heat for 1-5h, raising the temperature to 900 ℃ at the rate of 10-15 ℃/min, preserving the heat for 1-3h, then lowering the temperature to 600 ℃ at the rate of 15-20 ℃/min, and finally lowering the temperature to room temperature at the rate of 8-10 ℃/min.
The invention has the beneficial effects that:
(1) the invention takes ZnTe, PbO and CdO as precursors of double quantum dots, firstly precipitates PbTe quantum dots and CdTe quantum dots in a borosilicate glass system, can simultaneously cover a visible light region and near and intermediate infrared light regions, expands a spectral response range, has an absorption wavelength and a luminescence wavelength of 500-2100nm, and regulates and controls the growth size and the growth speed of the quantum dots by different heat treatment processes, wherein the heat treatment process is Pb2+、Cd2+、Te2-The diffusion process comprises two stages of nucleation and crystal growth.
(2) The invention uses SiO2And B2O3As network formers, in the borosilicate glass system, [ SiO ] is formed4]、[BO4]Covalently bonded network structure, Al2O3And ZnO as network intermediate to reduce crystallization tendency, Na2O and CaO are network exosomes to provide free oxygen and promote boroxine [ BO ]3]Conversion to boroxotetrahedra [ BO ] consisting entirely of bridge oxygens4]So as to convert the two-dimensional layered structure into a three-dimensional frame structure, improve the stability of the borosilicate glass, destroy Si-O bonds, reduce the softening point, and reduce La2O3、Pr2O3、Nb2O5Form rare earth oxide composition, improve glass plasticity, facilitate molding, and have SrF2Has good optical properties, reduced light reflectivity, Mg2B2O5As a reinforcing material, the glass can accelerate the generation of crystal nucleus and the growth of crystal, and improve the strength, rigidity, impact resistance and flame retardant property of the glass matrix.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
Example 1
A PbTe/CdTe double quantum dot codoped borosilicate glass comprises the following raw materials in percentage by mole: SiO 2245％、B2O312％、Na2O 8％、Al2O33％、ZnTe 9％、PbO 2.4％、CdO 2％、CaO 9％、ZnO6％、SrF22％、Mg2B2O50.6％、La2O3+Pr2O3+Nb2O51 percent; wherein, La2O3、Pr2O3And Nb2O5In a molar ratio of 2: 1.5: 1.
the preparation process of the PbTe/CdTe double quantum dot codoped borosilicate glass comprises the following steps:
s1: uniformly mixing the glass raw materials according to the mol percentage, heating to 1250 ℃ under the condition of nitrogen, and melting for 1h under the condition of heat preservation to obtain a glass melt;
s2: when the temperature of the glass melt is reduced to 1000 ℃, casting the glass melt on a graphite mould for forming, and then annealing for 3 hours at the temperature of 550 ℃;
s3: heating the annealed glass at the constant temperature of 550 ℃ for 1h, heating to 700 ℃ at the speed of 3 ℃/min, preserving heat for 1h, heating to 820 ℃ at the speed of 10 ℃/min, preserving heat for 1h, then cooling to 550 ℃ at the speed of 15 ℃/min, finally cooling to room temperature at the speed of 8 ℃/min, precipitating PbTe quantum dots and CdTe quantum dots, and obtaining the PbTe/CdTe double quantum dot codoped borosilicate glass after cutting and polishing.
Example 2
A PbTe/CdTe double quantum dot codoped borosilicate glass comprises the following raw materials in percentage by mole: SiO 2260％、B2O39％、Na2O 6％、Al2O31.5％、ZnTe 5.8％、PbO 1.8％、CdO 1.5％、CaO 7％、ZnO 5％、SrF21.5％、Mg2B2O50.3％、La2O3+Pr2O3+Nb2O50.6 percent; wherein, La2O3、Pr2O3And Nb2O5In a molar ratio of 2.5: 1.7: 1.
the preparation process is the same as that of example 1, except that:
s1: the melting temperature is 1300 ℃;
s2: the casting molding temperature is 1100 ℃, and the annealing temperature is 550 ℃;
s3: and (3) heat treatment process: heating the glass at a constant temperature of 575 ℃ for 1.5h, heating to 725 ℃ at a speed of 4 ℃/min, preserving heat for 3h, heating to 860 ℃ at a speed of 12 ℃/min, preserving heat for 2h, cooling to 575 ℃ at a speed of 18 ℃/min, and finally cooling to room temperature at a speed of 9 ℃/min.
Example 3
A PbTe/CdTe double quantum dot codoped borosilicate glass comprises the following raw materials in percentage by mole: SiO 2275％、B2O36％％、Na2O 4％、Al2O30.1％、ZnTe 2.5％、PbO 1.2％、CdO 1％、CaO 5％、ZnO 4％、SrF21％、Mg2B2O50.1％、La2O3+Pr2O3+Nb2O50.1 percent; wherein, La2O3、Pr2O3And Nb2O5In a molar ratio of 6: 1.6: 1.
the preparation process is the same as that of example 1, except that:
s1: the melting temperature is 1350 ℃;
s2: the casting molding temperature is 1200 ℃, and the annealing temperature is 570 ℃;
s3: and (3) heat treatment process: heating the glass at the constant temperature of 600 ℃ for 2h, raising the temperature to 750 ℃ at the speed of 5 ℃/min, preserving the heat for 5h, raising the temperature to 900 ℃ at the speed of 15 ℃/min, preserving the heat for 1-3h, then reducing the temperature to 600 ℃ at the speed of 20 ℃/min, and finally reducing the temperature to the room temperature at the speed of 10 ℃/min.
The borosilicate glasses produced in examples 1 to 3 were subjected to the performance tests, the test results of which are shown in the following table:
Figure BDA0001759769100000061
as can be seen from the above table, the doping rate of the PbTe quantum dots is not less than 6.28%, the doping rate of the CdTe quantum dots is not less than 5.89%, the visible light region and the near and intermediate infrared light regions can be simultaneously covered, and the spectral response range is enlarged.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.

Claims (4)

1. A PbTe/CdTe double quantum dot codoped borosilicate glass is characterized by comprising the following raw materials in mole percentage: SiO 2245-75％、B2O36-12％、Na2O 4-8％、Al2O30.1-3％、ZnTe 2.5-9％、PbO 1.2-2.4％、CdO 1-2％、CaO 5-9％、ZnO 4-6％、SrF21-2％、Mg2B2O50.1-0.6％、La2O3+Pr2O3+Nb2O50.1-1％。
2. The PbTe/CdTe double quantum dot co-doped borosilicate glass according to claim 1, wherein the La is2O3、Pr2O3And Nb2O5The molar ratio of (2-3): (1.5-2): 1.
3. a process for the preparation of PbTe/CdTe dual quantum dot co-doped borosilicate glass according to any of claims 1-2, characterized in that it comprises the following steps:
s1: uniformly mixing the glass raw materials according to the mole percentage, heating to 1250-;
s2: when the temperature of the glass melt is reduced to 1000-1200 ℃, the glass melt is cast on a graphite mold for molding, and then annealing treatment is carried out for 3 hours at the temperature of 550-570 ℃;
s3: and carrying out heat treatment on the annealed glass, and cutting and polishing after the PbTe quantum dots and the CdTe quantum dots are separated out to obtain the PbTe/CdTe double-quantum-dot co-doped borosilicate glass.
4. The process for preparing PbTe/CdTe double quantum dot co-doped borosilicate glass according to claim 3, wherein the heat treatment process comprises the following steps: heating the glass at the constant temperature of 600 ℃ for 1-2h at 550 ℃ and then raising the temperature to 750 ℃ at the rate of 3-5 ℃/min, preserving the heat for 1-5h, raising the temperature to 900 ℃ at the rate of 10-15 ℃/min, preserving the heat for 1-3h, then lowering the temperature to 600 ℃ at the rate of 15-20 ℃/min, and finally lowering the temperature to room temperature at the rate of 8-10 ℃/min.
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CN104310784A (en) * 2014-10-17 2015-01-28 东华大学 Quantum dot LED light emitting glass and preparation method thereof
CN104556678A (en) * 2015-01-19 2015-04-29 华南理工大学 Preparation method of quantum dot doped microcrystalline glass optical fiber
CN104692658A (en) * 2015-02-27 2015-06-10 武汉理工大学 Method for fixing CdS and Se in borosilicate glass
CN105293906A (en) * 2015-12-08 2016-02-03 武汉理工大学 CdTe quantum-dot doped glass and preparation method thereof
CN106865980A (en) * 2017-03-08 2017-06-20 武汉理工大学 A kind of praseodymium doped CdS quantum dot glass and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104310784A (en) * 2014-10-17 2015-01-28 东华大学 Quantum dot LED light emitting glass and preparation method thereof
CN104556678A (en) * 2015-01-19 2015-04-29 华南理工大学 Preparation method of quantum dot doped microcrystalline glass optical fiber
CN104692658A (en) * 2015-02-27 2015-06-10 武汉理工大学 Method for fixing CdS and Se in borosilicate glass
CN105293906A (en) * 2015-12-08 2016-02-03 武汉理工大学 CdTe quantum-dot doped glass and preparation method thereof
CN106865980A (en) * 2017-03-08 2017-06-20 武汉理工大学 A kind of praseodymium doped CdS quantum dot glass and preparation method thereof

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