CN113200686A - High temperature heat treatment method for optical element - Google Patents
High temperature heat treatment method for optical element Download PDFInfo
- Publication number
- CN113200686A CN113200686A CN202110507050.9A CN202110507050A CN113200686A CN 113200686 A CN113200686 A CN 113200686A CN 202110507050 A CN202110507050 A CN 202110507050A CN 113200686 A CN113200686 A CN 113200686A
- Authority
- CN
- China
- Prior art keywords
- optical element
- salt bath
- heat treatment
- temperature heat
- metal
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
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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
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
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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
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/007—Other surface treatment of glass not in the form of fibres or filaments by thermal treatment
-
- 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
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0095—Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
Abstract
The invention discloses a high-temperature heat treatment method of an optical element, which comprises the following steps: s1, soaking the optical element in the mixed chemical solution; s2, carrying out heat treatment on the optical element after surface treatment at the temperature of 200-300 ℃, wherein the preheating time is controlled to be 5-10 minutes; s3, performing salt bath on the preheated optical element, and heating the salt bath to the reaction temperature of 300-500 ℃; s4: continuously adding silicon dioxide into the salt bath of the step S2 until the mass of the silicon dioxide is 3-5% of the mass of the salt bath; s5: treating in the salt bath of the step S3 for 3-10 h. The strength of the optical glass is improved.
Description
Technical Field
The invention relates to the technical field of optical element production, in particular to a high-temperature heat treatment method of an optical element.
Background
The optical glass element can change the propagation direction of light and can change the relative spectral distribution of ultraviolet, visible or infrared light. Optical glass in the narrow sense means colorless optical glass; the optical glass in a broad sense also includes colored optical glass, laser glass, quartz optical glass, radiation-resistant glass, ultraviolet infrared optical glass, fiber optical glass, acousto-optic glass, magneto-optic glass and photochromic glass. The optical glass can be used for manufacturing lenses, prisms, reflectors, windows and the like in optical instruments. Components made of optical glass are critical elements in optical instruments.
The optical glass element is a finished product and is required to have precise size, good smoothness and certain optical specificity, but the general thin-wall special-shaped optical glass element has the defects of high brittleness, low strength, fragility, unsafe use and easy waste.
Disclosure of Invention
The invention aims to provide a high-temperature heat treatment method of an optical element, which improves the strength of optical glass.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for high temperature heat treatment of an optical element comprising the steps of:
s1, soaking the optical element in the mixed chemical solution;
s2, carrying out heat treatment on the optical element after surface treatment at the temperature of 200-300 ℃, wherein the preheating time is controlled to be 5-10 minutes;
s3, performing salt bath on the preheated optical element, and heating the salt bath to the reaction temperature of 300-500 ℃;
s4: continuously adding silicon dioxide into the salt bath of the step S2 until the mass of the silicon dioxide is 3-5% of the mass of the salt bath;
s5: treating in the salt bath of the step S3 for 3-10 h.
Further, the temperature of the surface treatment in step S1 is decreased at a rate of 2-4 deg.C/min until the temperature is decreased to 160-180 deg.C.
Further, the salt bath of step S2 includes a nitrate salt and a metal compound; the mass fraction of the nitrate is not less than 60 percent and is in a molten state; the metal compound is melted in the nitrate, and the metal compound and the nitrate contain the same metal elements; the mass fraction of the metal element in the molecular formula corresponding to the metal compound is larger than that in the molecular formula corresponding to the nitrate.
Further, the metal compounds include metal peroxides, metal carbonates, and metal silicates.
Further, in step S4, the shaking treatment is performed during the salt bath process, and the shaking treatment is performed sequentially every 20-30 min.
Further, the optical element is placed in a special cup body, the cup body is arranged in a salt bath device, the cup body rotates every 20-30min, the cup body rotates forwards for 2-3s and then rotates backwards for 2-3s, and the operation is repeated for 3-5 times.
The invention has the beneficial effects that:
1) the treatment method is simple, the formula is reasonable, the defects of corrosion, scratch, fuzzing and the like of the surface of the optical glass can be avoided, the ion exchange speed can be increased, and the surface quality and the strength of the optical glass element can be improved.
2) The optical glass element has high surface smoothness, and the optical characteristics of surface processing precision, light transmittance, color and the like are kept intact.
Detailed Description
Example 1
The invention relates to a high-temperature heat treatment method of an optical element, which comprises the following steps:
s1, soaking the optical element in the mixed chemical solution; the temperature of the surface treatment is decreased at a rate of 2-4 deg.C/min until the temperature is decreased to 160-180 deg.C.
S2, carrying out heat treatment on the optical element after surface treatment at the temperature of 200-300 ℃, wherein the preheating time is controlled to be 5-10 minutes; the salt bath comprises a nitrate salt and a metal compound; the mass fraction of the nitrate is not less than 60 percent and is in a molten state; the metal compound is melted in the nitrate, and the metal compound and the nitrate contain the same metal elements; the mass fraction of the metal element in the molecular formula corresponding to the metal compound is larger than that in the molecular formula corresponding to the nitrate. The metal compounds include metal peroxides, metal carbonates and metal silicates. The mass fraction of the metal compound is preferably greater than 0.1% and less than 10%, so that the metal compound can be completely dissolved in the corresponding nitrate.
The metal element is selected from the first main group metal elements in the periodic table, such as Li, Na, K, Rb, Cs, etc., and the metal element may also Be selected from the second main group elements, such as Be, Mg, Ca, Sr, Ba, etc.
The salt bath of the invention can also contain diatomite, alumina, pyroantimonate and the like, additives which are not melted in the salt bath adsorb small ions released by ion exchange of glass in the salt bath in a physical and chemical reaction mode, the interference of the small ions on the normal ion exchange reaction is reduced, the reaction rate of the large ion exchange small ions in the salt bath in one direction is increased, the service life of the salt bath is prolonged or the strengthening capability of the salt bath is improved in the inherent effective ion range in the salt bath, but the absolute quantity of the effective ions in the salt bath cannot be improved, and the essential change of the salt bath and the ion exchange cannot be generated.
And S3, performing salt bath on the preheated optical element, and heating the salt bath to the reaction temperature of 300-500 ℃.
S4: continuously adding silicon dioxide into the salt bath of the step S2 until the mass of the silicon dioxide is 3-5% of the mass of the salt bath; in step S4, the shaking treatment is carried out in the salt bath process, and the shaking treatment is carried out sequentially every 20-30 min. The optical element is placed in a special cup body, the cup body is arranged in a salt bath device, the cup body rotates every 20-30min, the cup body rotates forwards for 2-3s and then rotates backwards for 2-3s, and the operation is repeated for 3-5 times.
S5: treating in the salt bath of the step S3 for 3-10 h.
The cleaned optical glass element is placed in the salt bath for ion exchange, so that the network quality of the raw material glass is improved, the higher intrinsic strength of the glass is realized, and the impact resistance and the compressive stress storage capacity of the raw material glass are improved. The salt bath provided by the invention can provide more effective metal ions, so that the strength of the glass after being strengthened is improved, the service life of the salt bath is prolonged, and the resource waste and the environmental pollution are reduced.
While the invention has been described with reference to a preferred embodiment, 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 spirit and scope of the invention.
Claims (7)
1. A method for high temperature heat treatment of an optical element, comprising: the method comprises the following steps:
s1, soaking the optical element in the mixed chemical solution;
s2, carrying out heat treatment on the optical element after surface treatment at the temperature of 200-300 ℃, wherein the preheating time is controlled to be 5-10 minutes;
s3, performing salt bath on the preheated optical element, and heating the salt bath to the reaction temperature of 300-500 ℃;
s4: continuously adding silicon dioxide into the salt bath of the step S2 until the mass of the silicon dioxide is 3-5% of the mass of the salt bath;
s5: treating in the salt bath of the step S3 for 3-10 h.
2. A high temperature heat treatment method for an optical element according to claim 1, characterized in that: the temperature of the surface treatment in step S1 is decreased at a rate of 2-4 deg.C/min until the temperature is decreased to 160-180 deg.C.
3. A high temperature heat treatment method for an optical element according to claim 1, characterized in that: the salt bath of step S2 includes a nitrate and a metal compound; the mass fraction of the nitrate is not less than 60 percent and is in a molten state; the metal compound is melted in the nitrate, and the metal compound and the nitrate contain the same metal elements; the mass fraction of the metal element in the molecular formula corresponding to the metal compound is larger than that in the molecular formula corresponding to the nitrate.
4. A high temperature heat treatment method for an optical element according to claim 1, characterized in that: the metal compounds include metal peroxides, metal carbonates and metal silicates.
5. A high temperature heat treatment method for an optical element according to claim 1, characterized in that: in the step S4, the shaking treatment is performed in the salt bath process, and the shaking treatment is performed sequentially every 20-30 min.
6. A high-temperature heat treatment method for an optical element according to claim 5, characterized in that: and placing the optical element in a special cup body, wherein the cup body is arranged in a salt bath device, rotating the cup body every 20-30min, positively rotating for 2-3s, and then reversely rotating for 2-3s, and repeating for 3-5 times.
7. A high temperature heat treatment method for an optical element according to claim 1, characterized in that: the mixed chemical solution of step S1 oxidizes the etching solution or hydrofluoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110507050.9A CN113200686A (en) | 2021-05-10 | 2021-05-10 | High temperature heat treatment method for optical element |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110507050.9A CN113200686A (en) | 2021-05-10 | 2021-05-10 | High temperature heat treatment method for optical element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113200686A true CN113200686A (en) | 2021-08-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110507050.9A Pending CN113200686A (en) | 2021-05-10 | 2021-05-10 | High temperature heat treatment method for optical element |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044448A (en) * | 1990-02-27 | 1990-08-08 | 中国科学院光电技术研究所 | Surface strengthening method for optical glass elements and high-strength products thereof |
| CN109206021A (en) * | 2017-06-29 | 2019-01-15 | 深圳市东丽华科技有限公司 | For glass reinforced salt bath and preparation method thereof, strengthened glass and base glass |
| CN110981219A (en) * | 2019-12-11 | 2020-04-10 | 深圳市力沣实业有限公司 | Salt bath impurity ion purification method |
-
2021
- 2021-05-10 CN CN202110507050.9A patent/CN113200686A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044448A (en) * | 1990-02-27 | 1990-08-08 | 中国科学院光电技术研究所 | Surface strengthening method for optical glass elements and high-strength products thereof |
| CN109206021A (en) * | 2017-06-29 | 2019-01-15 | 深圳市东丽华科技有限公司 | For glass reinforced salt bath and preparation method thereof, strengthened glass and base glass |
| CN110981219A (en) * | 2019-12-11 | 2020-04-10 | 深圳市力沣实业有限公司 | Salt bath impurity ion purification method |
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Application publication date: 20210803 |