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CN-118993537-B - Photosensitive glass, preparation method thereof, reinforced photosensitive glass and application

CN118993537BCN 118993537 BCN118993537 BCN 118993537BCN-118993537-B

Abstract

By controlling the raw material composition of the photosensitive glass, the photosensitive glass containing Ag 2 O can ensure the stability of glass components in the melting process, solve the problem of loss and damage of silver atom Ag 0 generated by the decomposition of Ag 2 O to a noble metal container, and ensure that the optical transmittance of an exposure area in the visible light and near infrared wavelength ranges is extremely low when the photosensitive glass is obtained after radiation treatment and heat treatment, thereby realizing the shielding of optical signals.

Inventors

  • LUO SITE
  • HUANG HAO
  • YIN WEIWEI
  • TIAN QIAN

Assignees

  • 重庆鑫景特种玻璃有限公司

Dates

Publication Date
20260512
Application Date
20240812

Claims (10)

  1. 1. A method for preparing photosensitive glass, comprising: Preparing raw material components, wherein the raw material components comprise, by mass, 50-60% of silica sand, 15-22% of lithium carbonate, 6-10% of aluminum hydroxide, 3-6% of potassium nitrate, 3-6% of sodium nitrate, 3-5% of zirconium oxide, 0.3-0.6% of silver nitrate, 0.05-0.10% of cerium oxide and pentavalent antimony salt, wherein the mass percentage of the pentavalent antimony salt in the composition of the photosensitive glass is 0.3-0.3 wt.8% of sodium antimonate, then the photosensitive glass is mixed and melted in a noble metal container, then formed, and then annealed to obtain base material glass; The substrate glass comprises a first area and a second area, wherein the first area is subjected to masking treatment, and the second area is not subjected to masking treatment, so that the masked substrate glass is obtained; And carrying out radiation treatment and heat treatment on the masked substrate glass to obtain photosensitive glass with a non-exposure area and an exposure area, wherein the non-exposure area corresponds to the first area, and the exposure area corresponds to the second area.
  2. 2. The preparation method according to claim 1, wherein the raw material components comprise the following components in percentage by mass: The content of the silica sand is 53-59 wt percent, and/or, The content of the lithium carbonate is 17-20wt% and/or, The content of the aluminum hydroxide is 8-10 wt wt percent, and/or, The content of the potassium nitrate is 4-6 wt wt percent, and/or, The content of the sodium nitrate is 3.5-5.5 wt percent, and/or, The content of the zirconia is 3-5 wt percent, and/or, The content of the silver nitrate is 0.3-0.5 wt percent, and/or, The content of the cerium oxide is 0.05wt% to 0.10wt%, and/or, The content of the pentavalent antimony salt is 0.3-0.7 wt%.
  3. 3. The preparation method according to claim 1, wherein the raw material components comprise the following components in percentage by mass: the content of the silica sand is 54.00wt% to 58.96 wt%, and/or, The content of the lithium carbonate is 17.43-19.94 wt% and/or, The content of the aluminum hydroxide is 8.22-9.97 wt percent, and/or, The content of the potassium nitrate is 4.07 to 5.97 weight percent and/or, The content of the sodium nitrate is 3.77 to 5.45 wt wt percent and/or, The content of the zirconia is 3.33-4.96 wt percent, and/or, The content of the silver nitrate is 0.32-0.49 wt%, and/or, The content of the cerium oxide is 0.06-0.09 wt percent, and/or, The content of the pentavalent antimony salt is 0.3-0.5 wt%.
  4. 4. The method of claim 1, wherein the pentavalent antimony salt comprises at least one of NaSbO 3 、KSbO 3 、NH 4 SbO 3 and hydrates thereof.
  5. 5. The method according to claim 1, wherein the noble metal container is a container prepared using at least one metal selected from the group consisting of gold, platinum, and rhodium.
  6. 6. The method according to claim 1, wherein the melting temperature is 1400 ℃ to 1650 ℃, the melting time is 6h to 48h, and/or the annealing temperature is 400 ℃ to 500 ℃, and the annealing time is 8h to 24h.
  7. 7. The method according to any one of claims 1 to 6, wherein the radiation treatment comprises ultraviolet irradiation treatment.
  8. 8. The method according to claim 7, wherein the wavelength of the ultraviolet irradiation treatment is 300nm to 320nm, the intensity of the ultraviolet irradiation treatment is 20mw/cm 2 ~360mw/cm 2 , and the time of the ultraviolet irradiation treatment is 5min to 60min.
  9. 9. The method according to any one of claims 1 to 6, wherein the heat treatment includes a nucleation treatment and a crystallization treatment.
  10. 10. The method according to claim 9, wherein the rate of temperature rise of the nucleation treatment is 1 ℃ to 10 ℃ per minute, and/or, The temperature of the nucleation treatment is 430-540 ℃, and/or, The nucleating treatment time is 30 min-360 min, and/or, The temperature rising rate of the crystallization treatment is 1-10 ℃ per minute, and/or, The crystallization treatment temperature is 540-800 ℃, and/or, The crystallization treatment time is 30-240 min.

Description

Photosensitive glass, preparation method thereof, reinforced photosensitive glass and application Technical Field The application relates to the technical field of glass, in particular to photosensitive glass, a preparation method thereof, reinforced photosensitive glass and application thereof. Background The photosensitive glass can respond to external light stimulus, and under certain illumination conditions, the glass structure and the phase can change, and different mechanical and optical properties are presented. Ag-containing photosensitive glass is the most common type of photosensitive glass, and Ag is typically combined with Ce and Sb ions, sb 3+ can transfer electrons to Ce 4+ to reduce it to Ce 3+ during melting, ce 3+ can transfer electrons to Ag + to reduce it to Ag 0,Ag0 as the growth center of colloidal Ag crystals during further UV exposure, and subsequent heat treatment can lead to precipitation and growth of Ag colloids which can induce precipitation of lithium metasilicate crystals due to the close lattice constants. Based on the reaction chain principle, the products of Fotoform/Fotoceram and Foturan are respectively developed by Corning and Schottky, and micro-region machining of glass can be realized through subsequent etching of the glass, and the glass can be used for MEMS, TGV, microfluidic glass chips and the like. The photosensitive glass containing Ag has many problems in the melting process, such as the adoption of corundum and quartz containers, the great influence on the final glass component in the high-temperature melting process and the easy breakage of the melting container, and the adoption of noble metal containers (particularly platinum, rhodium and other metal containers) in the glass component can erode the containers, and the long-term melting can cause serious loss and damage to the containers (the melting containers comprise a crucible, a kiln, a channel and the like). Therefore, the method ensures the melting stability, maintains the stability of the glass components, reduces and avoids the damage to the container in the melting process, and is a technical problem to be solved urgently. The system photosensitive glass has mainly focused on glass micromachining, but has not been reported in optical applications. In fact, in the UV exposure area, the optical transmittance of the photosensitive glass is obviously reduced along with the precipitation of colloidal Ag crystals and the precipitation of lithium silicate crystals, and the characteristic enables the Ag photosensitive glass ceramics to be applied to shielding of optical signals, and the shielding of the specific area to the optical signals in a certain wavelength range can be realized through the process of combining UV exposure with a specific area of a mask. It should be noted that this section of the disclosure only provides a background related to the present disclosure, and does not necessarily constitute prior art or known technology. Disclosure of Invention The application aims to provide photosensitive glass, which not only can ensure that the glass component of the photosensitive glass containing Ag 2 O is stable in the melting process, and solves the problem that silver atoms Ag 0 generated by the decomposition of Ag 2 O are lost and destroyed to a noble metal container, but also can ensure that the optical transmittance of an exposure area of the photosensitive glass in the visible light and near infrared wavelength ranges is extremely low when the photosensitive glass is obtained after radiation treatment and heat treatment, and can realize shielding of optical signals. In order to achieve the above object, the present application provides the following technical solutions: According to the first aspect, the photosensitive glass comprises, by mass, 50-60% of silica sand, 15-22% of lithium carbonate, 6-10% of aluminum hydroxide, 3-6% of potassium nitrate, 3-6% of sodium nitrate, 3-5% of zirconium oxide, 0.3-0.6% of silver nitrate, 0.05-0.10% of cerium oxide and pentavalent antimony salt, wherein the mass percentage of the pentavalent antimony salt in the composition of the photosensitive glass is 0.3-0.8% of sodium antimonate. As an alternative embodiment, the composition of the photosensitive glass, in terms of the mass percent of the raw material components in the photosensitive glass, comprises the following components: the content of silica sand is 53wt% to 59wt%, preferably the content of silica sand is 54.00wt% to 58.96wt%, and/or, The content of lithium carbonate is 17wt% to 20wt%, preferably the content of lithium carbonate is 17.43wt% to 19.94wt%, and/or, The content of aluminum hydroxide is 8wt% to 10wt%, preferably 8.22wt% to 9.97wt% of aluminum hydroxide, and/or, The content of potassium nitrate is 4 to 6 weight percent, preferably 4.07 to 5.97 weight percent, and/or, The content of sodium nitrate is 3.5wt% to 5.5wt%, preferably 3.77wt% to 5.45wt% and/or, The zirconia content is 3.33w