CN112526671B

CN112526671B - Low-loss glass ceramic planar optical waveguide and preparation method thereof

Info

Publication number: CN112526671B
Application number: CN202011478621.2A
Authority: CN
Inventors: 张乐; 甄方正; 康健; 陈东顺; 申冰磊; 赵超; 罗泽; 陈浩
Original assignee: Xinyi Xiyi High Tech Material Industry Technology Research Institute Co Ltd
Current assignee: Xinyi Xiyi High Tech Material Industry Technology Research Institute Co Ltd
Priority date: 2020-12-15
Filing date: 2020-12-15
Publication date: 2022-03-11
Anticipated expiration: 2040-12-15
Also published as: CN112526671A

Abstract

A low-loss glass ceramic planar optical waveguide and a preparation method thereof belong to the technical field of planar optical waveguide preparation and application. The prepared glass ceramic planar optical waveguide satisfies the condition that the component is SiO₂–30mol%SnO₂:xEr³⁺Wherein x is more than or equal to 0.3 and less than or equal to 0.5, is prepared by a sol-gel method and a dip coating technology, and SnO₂Er is added into the nanocrystalline³⁺The non-radiative relaxation process is blocked, the loss is reduced, and the propagation loss at 1542nm is as low as 0.6 dB/cm. The preparation method provided by the invention has the advantages of simple process and stable product performance, and is suitable for industrial production.

Description

Low-loss glass ceramic planar optical waveguide and preparation method thereof

Technical Field

The invention provides a low-loss glass ceramic planar optical waveguide and a preparation method thereof, belonging to the technical field of preparation and application of planar optical waveguides.

Background

Glass-ceramics are two-phase materials consisting of glass embedded with nanocrystals. When the nanocrystalline is activated by luminescent ions such as transition metal ions and rare earth ions, the photonic glass ceramic is obtained. The advantages of photonic glass-ceramics over optical glasses and crystals result from their combination of optical properties of the glass with spectral properties of the crystals, which is that glass-ceramics have both advantages over glass, single crystals and sintered transparent ceramics in photonic applications. Therefore, the use of glass-ceramics in photonics, and in particular in integrated optics, is being investigated more and more intensively. Notably, the spectral characteristics of rare earth ions can be tailored and enhanced in photonic glass ceramics depending on their composition and properties. When optically pumped, the optical waveguide inevitably experiences some loss, which results from light refraction and the like, thereby reducing its optical efficiency. Therefore, reducing optical loss is the key to improving the performance of planar optical waveguides.

Disclosure of Invention

1. In order to solve the problems, the invention provides a low-loss glass ceramic planar optical waveguide and a preparation method thereof. The prepared glass ceramic planar optical waveguide satisfies the condition that the component is SiO₂–30mol％SnO₂:xEr³⁺Wherein x is more than or equal to 0.3 and less than or equal to 0.5, is prepared by a sol-gel method and a dip coating technology, and SnO₂Er is added into the nanocrystalline³⁺The non-radiative relaxation process is blocked, the loss is reduced, and the low propagation loss of about 0.4-0.8 dB/cm is shown at 1542 nm. The preparation method provided by the invention has the advantages of simple process and stable product performance, and is suitable for industrial production.

2. The technical scheme of the invention is as follows:

SnCl with purity of more than 99.9 percent is weighed according to stoichiometric ratio₂、Er(NO₃)₃Citric acid and tetraethyl orthosilicate (TEOS) as starting materials. Firstly SnCl₂、Er(NO₃)₃And mixing TEOS and citric acid, wherein the molar ratio of the citric acid to the metal ions is 1 (0.5-1), adding deionized water with the volume fraction of 20-50% of the mixture, and stirring at 200-300 rpm for 10-16 h to obtain the sol. The solution was filtered using a 200nm filter and the collected fractions were used for dip coating. In the commercial SiO₂And dip-coating the glass at the dipping speed of 7-7.5 cm/min to deposit 20-30 deposition layers, and drying at 800-900 ℃ for 20-30 min after dip-coating. And finally, heating for 1-3 h at 900-1100 ℃ to obtain the glass ceramic planar optical waveguide.

The invention has the beneficial effects that:

1. the propagation loss of the glass ceramic planar optical waveguide prepared by the invention at 1542nm is as low as 0.4-0.8 dB/cm.

2. In the process of preparing the glass ceramic planar optical waveguide, the method selects high-purity raw material powder, strictly controls the introduction of impurities, and avoids the influence on the optical performance to the maximum extent.

3. The preparation method of the glass ceramic planar optical waveguide provided by the invention has the advantages of high yield and productivity, simple preparation process and no strict requirements on preparation time arrangement, can effectively improve the yield and reduce the production cost, and is very suitable for industrial production.

Drawings

FIG. 1XRD pattern of a sample prepared according to example 1;

FIG. 2 is a TEM image and a partial magnified view of a sample prepared in example 1;

figure 3 shows the electric field energy distribution at 1542nm for the preparation of a planar optical waveguide configuration of example 1.

Detailed Description

The present invention is further illustrated by the following specific examples, which should not be construed as limiting the scope of the invention.

Example 1: SiO 2₂–30mol％SnO₂:0.5Er³⁺

SnCl with purity of more than 99.9 percent is weighed according to stoichiometric ratio₂、Er(NO₃)₃Citric acid and tetraethyl orthosilicate (TEOS) as starting materials. Firstly SnCl₂、Er(NO₃)₃TEOS and citric acid are mixed, the molar ratio of the citric acid to the metal ions is 1:0.5, deionized water with the volume fraction of 50% of the mixture is added, and the mixture is stirred for 16 hours at 200rpm, so that sol is obtained. The solution was filtered using a 200nm filter and the collected fractions were used for dip coating. In the commercial SiO₂Dipping on glass, wherein the dipping speed is 7cm/min, and 30 deposition layers are deposited in total, and drying is carried out for 20min at 900 ℃ after dipping. Finally heating for 3h at 900 ℃ to obtain the glass ceramic planar optical waveguide.

Example 2: SiO 2₂–30mol％SnO₂:0.4Er³⁺

SnCl with purity of more than 99.9 percent is weighed according to stoichiometric ratio₂、Er(NO₃)₃Citric acid and tetraethyl orthosilicate (TEOS) as starting materials. Firstly SnCl₂、Er(NO₃)₃TEOS and citric acid are mixed, the molar ratio of the citric acid to the metal ions is 1:1, deionized water with the volume fraction of 20% of the mixture is added, and the mixture is stirred at 300rpm for 10 hours to obtain sol. The solution was filtered using a 200nm filter and the collected fractions were used for dip coating. In the commercial SiO₂Dipping on glass, wherein the dipping speed is 7.5cm/min, co-depositing 20 deposition layers, and drying at 800 ℃ for 30min after dipping. Finally heating at 1100 deg.C for 1h to obtain the glass ceramic planar optical waveguide.

Example 3: SiO 2₂–30mol％SnO₂:0.3Er³⁺

SnCl with purity of more than 99.9 percent is weighed according to stoichiometric ratio₂、Er(NO₃)₃Citric acid and tetraethyl orthosilicate (TEOS) as starting materials. Firstly SnCl₂、Er(NO₃)₃TEOS and citric acid are mixed, the molar ratio of the citric acid to the metal ions is 1:0.75, then deionized water with the volume fraction of 40% of the mixture is added, and stirring is carried out at 280rpm for 12 hours, so as to obtain the sol. The solution was filtered using a 200nm filter and the collected fractions were used for dip coating. In the commercial SiO₂Dip-coating on glass at a speed of 7cm/min to deposit 25 deposition layers, and drying at 850 deg.C for 26 min. Finally heating for 2h at 1000 ℃ to obtain the glass ceramic planar optical waveguide.

By way of example in example 1, the XRD pattern of FIG. 1 shows that by comparison with standard cards, at SnO₂The peak has good consistency, which indicates that SiO is successfully synthesized₂–30mol％SnO₂:0.5Er³⁺. The TEM image of FIG. 2(a) shows that dark spots in the image are in SiO₂SnO in matrix₂Nanocrystals, which are light gray in color. The grains are uniformly distributed and have a size less than 10 nm. SnO in FIG. 2(b)₂The interplanar distance of the nanocrystals was 0.32nm, corresponding to the rutile crystal structure. From the electric field energy distribution of fig. 3, its confinement at 1542nm can be calculated to be 82%. The propagation loss was measured by scanning a fiber optic probe and photodetector along the propagation fringes to detect the intensity of light scattered from the waveguide surface, and the propagation loss for each example is shown in the following table:

examples	Propagation loss
		1	0.6dB/cm
2	0.4dB/cm
		3	0.8dB/cm

Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the above embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the present invention.

Claims

1. A preparation method of a low-loss glass ceramic planar optical waveguide is characterized in that the prepared glass ceramic planar optical waveguide satisfies the following components:

SiO₂–30mol%SnO₂:xEr³⁺

wherein x is more than or equal to 0.3 and less than or equal to 0.5; the coating is prepared by a sol-gel method and a dip coating technology, and comprises the following specific steps:

SnCl with purity of more than 99.9 percent is weighed according to stoichiometric ratio₂、Er(NO₃)₃Citric acid and TEOS as raw materials; firstly SnCl₂、Er(NO₃)₃、TEMixing OS and citric acid, wherein the molar ratio of the citric acid to metal ions is 1 (0.5-1), adding deionized water with the volume fraction of 20-50% of the mixture, and stirring at 200-300 rpm for 10-16 h to obtain sol; filtering the solution with a 200nm filter, and collecting the filtrate for dip coating; in SiO₂Dip-coating the glass at the dipping speed of 7-7.5 cm/min to deposit 20-30 deposition layers, and drying at 800-900 ℃ for 20-30 min after dip-coating; and finally, heating for 1-3 h at 900-1100 ℃ to obtain the glass ceramic planar optical waveguide.

2. The low-loss glass ceramic planar optical waveguide is characterized by being prepared by the preparation method of claim 1, and the propagation loss of the prepared glass ceramic planar optical waveguide at 1542nm is as low as 0.5-0.8 dB/cm.