CN113185145B - Laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation and preparation method and application thereof - Google Patents

Laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation and preparation method and application thereof Download PDF

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CN113185145B
CN113185145B CN202110466209.7A CN202110466209A CN113185145B CN 113185145 B CN113185145 B CN 113185145B CN 202110466209 A CN202110466209 A CN 202110466209A CN 113185145 B CN113185145 B CN 113185145B
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glass
neodymium glass
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laser neodymium
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CN113185145A (en
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孔壮
刘辉
贾金升
孙勇
曹振博
赵冉
余刚
孟政
孟凡禹
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China Building Materials Academy CBMA
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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
    • C03C21/005—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 introduce in the glass such metals or metallic ions as Ag, Cu
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
    • H01S3/16—Solid materials
    • H01S3/1601—Solid materials characterised by an active (lasing) ion
    • H01S3/1603—Solid materials characterised by an active (lasing) ion rare earth
    • H01S3/1611—Solid materials characterised by an active (lasing) ion rare earth neodymium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
    • H01S3/16—Solid materials
    • H01S3/17—Solid materials amorphous, e.g. glass

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Abstract

The invention provides laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation and a preparation method and application thereof, wherein the method comprises the following steps: 1) cu+Ion exchange; 2) electric field assisted ion diffusion; 3) cu (copper)+And (4) oxidizing ions. The laser neodymium glass has the reflectivity of 0-1% at 1053nm, and the depth of a copper ion exchange layer is more than 250 mu m.

Description

Laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation and preparation method and application thereof
Technical Field
The invention relates to a solid-state laser, in particular to laser neodymium glass for inhibiting Amplified Spontaneous Emission (ASE), and more particularly relates to laser neodymium glass for inhibiting Amplified Spontaneous Emission and parasitic oscillation, and a preparation method and application thereof.
Background
Laser neodymium glass is special glass containing rare earth luminescent ions, namely neodymium ions, can generate laser or amplify laser energy under the excitation of 'pump light', is a 'heart' of a laser, and amplifies the negligible laser energy to the energy of 'small sun' magnitude.
To achieve higher energy and power, the size and gain of the laser amplifier are required to be increased continuously so that the maximum energy that can be output is increased, and thus the slab laser amplifier is the main source for obtaining high energy output. However, as the transverse dimension of the laser glass is increased, the spontaneous radiation amplification and parasitic oscillation caused by surface Fresnel reflection are enhanced, so that the escape and reduction of the number of reversed particles are caused, and the gain of the neodymium laser glass is reduced. Therefore, suppression and elimination of parasitic oscillation become the key to increase the laser amplification efficiency and achieve high-energy laser output. Parasitic oscillation effect elimination study:
studies have shown that the conditions for parasitic oscillation formation are:
R·eDβ≥1。
wherein R is the residual reflectivity of the boundary; beta is a gain coefficient; d is the long axis diameter of the laser glass sheet.
Therefore, the residual reflectivity R of the boundary must be continuously reduced, or even completely eliminated, to reduce and eliminate parasitic oscillations. A model is established according to the propagation of light between the two layers of media of the laser glass and the edge covering material, a method for measuring the residual reflectivity is provided, and a calculation formula of the residual reflectivity is deduced.
At present, the most effective method for inhibiting and eliminating parasitic oscillation is a hemming method, namely, an absorption medium is matched on the side surface of the laser glass vertical to the optical path direction. The wrapping edges are divided into a soft wrapping edge and a hard wrapping edge, wherein the soft wrapping edge is formed by bonding a wrapping material and laser glass together by adopting an organic bonding agent; the hard edge covering is to directly pour molten glass liquid on the periphery of high-temperature sheet laser glass or coat an absorption layer on the surface of the laser glass by adopting a powder sintering method, and then sinter the laser glass at high temperature. Copper is a transition element, and the electronic structure of copper atom is 3s104s1. Typically, the copper atom has an oxidation state of Cu0，Cu1+，Cu2+。Cu2+The d-orbitals of the ions are partially filled and the wavelength is strongly absorbing at 1053 nm.
In summary, no matter the coating technology or the edge covering process has an inevitable interface, and the expansion coefficient of the coating is different from that of the optical element, the coating is easy to fall off, the service life of the element is influenced, and the application of the method on the laser neodymium glass is limited.
Disclosure of Invention
In view of this, the main object of the present invention is to provide a laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation, and a preparation method and an application thereof, which can not only ensure the effective amplification capability of the laser neodymium glass for laser energy, but also effectively suppress the amplified spontaneous emission and parasitic oscillation of the sheet laser neodymium glass, so that the gain performance approaches the theoretical calculation level, and the use requirement of the high power laser device is satisfied.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a preparation method of laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation, which comprises the following steps:
1)Cu+ion exchange: performing ion exchange on a laser neodymium glass raw material by using cuprous chloride and zinc chloride as molten salts to obtain a laser neodymium glass substrate;
2) electric field assisted ion diffusion: manufacturing copper metal films on the two surfaces of the laser neodymium glass substrate obtained in the step 1); then heating the glass substrate to 400-500 ℃, applying direct current bias on two sides of the glass substrate by taking the copper-plated surface as an electrode, and keeping the current density passing through the glass substrate to be 0.2-4 mA/cm2Carrying out electric field assisted ion diffusion, and maintaining exchange for 1-12h to obtain a laser neodymium glass intermediate;
3)Cu+ion oxidation: introducing oxygen mixed gas into the laser neodymium glass intermediate prepared in the step 2) at the rate of 0.1-2L/min, and continuously introducing the oxygen mixed gas for 10-60 min to remove air; after the exhaust is finished, the temperature is raised to the reaction temperature of 400-500 ℃ at the heating rate of 0.1-5 ℃/min, the temperature is kept for 24-72 h, after the temperature is kept, the power is cut off, the gas flow is kept unchanged, and after the temperature is reduced to the room temperature, the laser neodymium glass is obtained.
Further, in the preparation method of the laser neodymium glass for inhibiting amplified spontaneous emission and parasitic oscillation, the molten salt in the step 1) is a mixed solution of cuprous chloride and zinc chloride, wherein the mass ratio of the cuprous chloride to the zinc chloride is 100: 0.1-5.
Further, in the preparation method of the laser neodymium glass for inhibiting amplified spontaneous emission and parasitic oscillation, the exchange temperature of the ion exchange in the step 1) is 400-.
Further, in the preparation method of the laser neodymium glass for inhibiting amplified spontaneous emission and parasitic oscillation, in the step 2), the copper metal film is prepared by adopting a magnetron sputtering method; the thickness of the copper metal film is 50-100nm, and the copper metal film is used as an electrode for electric field assisted ion exchange.
Further, in the preparation method of the laser neodymium glass for inhibiting amplified spontaneous emission and parasitic oscillation, in the step 2), the temperature rise rate is 0.1-5 ℃/min.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures. The invention provides laser neodymium glass for inhibiting amplified spontaneous emission and parasitic oscillation, which comprises a laser neodymium glass substrate, wherein divalent copper ions are introduced into the side surface area of the laser neodymium glass substrate, and the exchange depth of the divalent copper ions is more than 250 mu m.
Further, the aforementioned laser neodymium glass suppressing amplified spontaneous emission and parasitic oscillation, wherein a reflectance of the laser neodymium glass at 1053nm is 0 to 1%.
Further, the laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation, wherein when the optical pumping energy density is 30J/cm, is described3The laser gain coefficient of the laser neodymium glass is 3X10-2cm-1-5X 10-2cm-1。
Further, the laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation is prepared by the method.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures. The laser amplifier comprises a glass window, wherein the glass window is made of the laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation.
By the technical scheme, the laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation and the preparation method and the application thereof provided by the invention at least have the following advantages:
1. the laser neodymium glass has the reflectivity of 0-1% at 1053nm, and the depth of a copper ion exchange layer is more than 250 mu m.
2. The invention selects Cu with different depths2+The ionic absorption glass can effectively control the heat effect and the laser absorption capacity of the absorption glass, and achieve the balance of ASE inhibition effect and long-time stable operation.
3. According to the invention, because copper ions are diffused into the glass from outside to inside without interface reflection, stress is not generated in the temperature alternation process, and the service life and the reliability are improved (through secondary ion mass spectrometry, the copper ions are diffused into the glass from outside to inside, the refractive index gradient of the glass is determined, no interface reflection is generated, and no stress is generated).
4. The invention adopts the electric field to assist and enlarge the ion exchange depth, reduces the molten salt corrosion time, improves the optical performance of the sample and inhibits the effect of amplified spontaneous radiation.
5. The technical operation process of the invention is safe and reliable, is suitable for batch application of inhibiting amplified spontaneous emission of the laser neodymium glass, and is easy to realize performance consistency among products.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Drawings
FIG. 1 is a secondary ion mass spectrum of example 1 of the present invention.
FIG. 2 is a reflectance chart of example 1 of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to a laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation, a method for preparing the same, and embodiments, structures, features and effects thereof according to the present invention. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The following materials or reagents, unless otherwise specified, are all commercially available.
As shown in fig. 1, the present invention provides a method for preparing laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation, comprising the following steps:
1)Cu+ion exchange: performing ion exchange on a laser neodymium glass raw material by using cuprous chloride and zinc chloride as molten salts to obtain a laser neodymium glass substrate;
2) electric field assisted ion diffusion: manufacturing copper metal films on the two surfaces of the laser neodymium glass substrate obtained in the step 1); then heating the glass substrate to 400-500 ℃, applying direct current bias on two sides of the glass substrate by taking the copper-plated surface as an electrode, and keeping the current density passing through the glass substrate to be 0.2-4 mA/cm2Carrying out electric field assisted ion diffusion, and maintaining exchange for 1-12h to obtain a laser neodymium glass intermediate; under the action of DC bias voltage, ions on the glass surface formed by the first ion exchange are further pushed into the glass substrate, and the diffusion time is determined according to the required diffusion depth;
3)Cu+ion oxidation: due to Cu2+Strong absorption at 1053nm, therefore Cu needs to be added+Ion oxidation to Cu2+Ions; and (3) introducing oxygen mixed gas into the laser neodymium glass intermediate prepared in the step 2) at the speed of 0.1-2L/min, and continuously introducing the oxygen mixed gas for 10-60 min to remove air. After the exhaust is finished, the temperature is raised to the reaction temperature of 400-500 ℃ at the heating rate of 0.1-5 ℃/min, the temperature is kept for 24-72 h, after the temperature is kept, the power is cut off, the gas flow is kept unchanged, and after the temperature is reduced to the room temperature, the sample is obtained.
In specific implementation, the exchange temperature is designed to be 400-+-Na+In the ion exchange process, a proper amount of ZnCl is added into the molten salt2Can form stable complex Na2ZnCl4The exchange speed of ions can be accelerated; excess ZnCl2The exchange speed of the ions is reduced. At a suitable temperature andunder the condition of time, the glass surface is seriously corroded due to the excessively high and excessively high ion exchange speed. Therefore, the molten salt in the step 1) is selected to be a mixed solution of cuprous chloride and zinc chloride, wherein the mass ratio of the cuprous chloride to the zinc chloride is 100: 0.1-5; preferably 100: 2; the exchange temperature of the ion exchange is 400-; preferably, the exchange temperature of the ion exchange is 480 ℃, the temperature rising rate is 3 ℃/min, and the exchange time is 6 h. The ion exchange temperature is determined according to the selected molten salt composition and the glass substrate, and the ion exchange time is determined according to the design requirements. The temperature and the time influence the diffusion depth of ions, and the parameters are too small, so that the diffusion depth of the ions is shallow; the parameters are too high, the glass corrosion is serious, the depth change of ion diffusion is not large, and resources are wasted.
In specific implementation, considering that the thickness, the reaction temperature, the reaction time and the heating rate of copper influence the depth of ion diffusion, the parameters are too small, and the depth of ion diffusion is shallow; the parameters are too high, the depth change of ion diffusion is not large, and resources are wasted. In the step 2), the copper metal film can be prepared by adopting a magnetron sputtering or atomic force deposition (ALD) method; the thickness of the copper metal film is 50-100nm, preferably 80nm, and the copper metal film is used as an electrode for electric field auxiliary ion exchange; the temperature is raised to 480 ℃, and the current density passing through the glass substrate is 2mA/cm2The exchange time was maintained for 8 h. The rate of temperature rise is 3 ℃/min.
In specific implementation, the temperature rise rate, the temperature and the time influence the oxidation degree of copper ions, the parameters are too small, the copper ions are not completely oxidized, and the performance is poor; the parameters are too large, the glass is seriously corroded, the oxidation degree is not changed greatly, and resources are wasted. In the step 3), the heating rate is 3 ℃/min, the reaction temperature is 480 ℃, and the heat preservation time is 48 h.
The invention also provides laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation, which comprises a laser neodymium glass substrate, wherein divalent copper ions are introduced into the side surface area of the laser neodymium glass substrate, and the exchange depth of the divalent copper ions is more than 250 mu m; the reflectivity of the laser neodymium glass at 1053nm is 0-1%; when the optical pumping energy density is 30J/cm3The laser gain coefficient of the laser neodymium glass is 3X10-2cm-1-5X 10-2cm-1。
The invention also provides a laser amplifier which comprises a glass window, wherein the glass window is made of the laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation.
The present invention will be described in further detail with reference to specific examples.
Example 1
Mixing solid fused salt (100g of cuprous chloride and 2g of zinc chloride) in a crucible in proportion, putting the mixture into an oven, putting a laser neodymium glass raw material into the oven, heating to 480 ℃ at the speed of 3 ℃/min, completely melting the fused salt in the crucible, putting the laser neodymium glass into the crucible containing the fused salt, carrying out ion exchange for 6h, carefully clamping a glass sheet after the exchange is finished, putting the glass sheet into a glassware, closing a heating switch of the oven, slowly returning the temperature to the room temperature, dissolving the fused salt on the surface of the glass sheet by using deionized water, drying the water on the surface of the glass sheet by using nitrogen, and using a sample for later use; by magnetron sputtering (parameter: vacuum degree of 1.2X 10)-1pa, plating copper (the thickness of copper ions is 80nm) on two sides of the glass at the plating temperature of 80 ℃, the plating power of 0.75 kilowatt and the plating time of 160s, wherein the copper is used as an electrode for electric field assisted ion exchange, and the copper wire is used as a lead. Placing the copper-plated neodymium glass in an oven, heating to 480 ℃ at the speed of 3 ℃/min, applying direct current bias voltage on two sides of the glass substrate by taking the copper-plated surface as an electrode, and keeping the current density of 2mA/cm passing through the glass substrate2Carrying out electric field assisted ion diffusion, reacting for 8h, turning off a power supply after the reaction is finished, turning off a heating furnace, slowly returning the temperature to the room temperature, and taking out a neodymium laser glass sample for later use; and (3) placing the neodymium laser glass sample in a tubular furnace, introducing oxygen with the flow rate of 0.1L/min, and continuously introducing the oxygen for 60min to remove impurity gases such as air in a hearth. After the exhaust is finished, the temperature is increased to 480 ℃ at the speed of 3 ℃/min, the heat preservation is carried out for 48h, after the heat preservation is finished, the power supply is turned off, the gas flow is kept unchanged, after the temperature of the hearth is reduced to the room temperature, the laser neodymium glass sample is obtained, and the laser neodymium glass sample can be used as the laser neodymium glass sampleGlass window of laser amplifier.
The thickness of the laser neodymium glass sample of the embodiment is tested by a secondary ion mass spectrometer, and the copper ion exchange depth reaches 350 μm, as shown in fig. 1.
And (3) testing the absorption value of the laser neodymium glass sample by using an ultraviolet visible infrared spectrophotometer, wherein the reflectivity of the laser neodymium glass sample at 1053nm is 0.1%, as shown in figure 2, namely the reflectivity of a glass window of the laser amplifier at 1053nm is 0.1%. Since Cu2+The absorption characteristic is presented near 1053nm wave band, and the parasitic oscillation light and ASE light which are scattered or reflected inside can be well absorbed, so the effects of restraining parasitic oscillation and reducing ASE in the system can be achieved. The larger the reflectivity of the interface is, the more easily parasitic oscillation is generated, so that the more difficult the parasitic oscillation is to be eliminated, and the laser amplifier gain is ultimately affected. The gain coefficient of the laser neodymium glass sample of the embodiment is tested when the optical pumping energy density is 30J/cm3The laser gain coefficient is 5X10-2cm-1(ii) a The laser gain coefficient of the untreated laser neodymium glass raw material is 2X10-2cm-1。
Example 2
Mixing solid molten salt in a crucible according to a ratio (100g of cuprous chloride and 0.1g of zinc chloride), putting the mixture into an oven, putting a laser neodymium glass raw material into the oven, heating to 400 ℃ at the speed of 0.1 ℃/min, completely melting the molten salt in the crucible, putting the laser neodymium glass into the crucible containing the molten salt, reacting for 0.5h, carefully taking out a glass sheet after the exchange is finished, putting the glass sheet into a glass utensil, closing a heating switch of the oven, slowly returning the temperature to the room temperature, dissolving the molten salt on the surface of the glass sheet with deionized water, drying the water on the surface of the glass with nitrogen, and using a sample; by magnetron sputtering (parameter: vacuum degree of 1.2X 10)- 1pa, plating copper (the thickness of copper ions is 50nm) on two sides of the glass at the plating temperature of 80 ℃, the plating power of 0.75 kilowatt and the plating time of 100s, wherein the copper is used as an electrode for electric field assisted ion exchange, and the copper wire is used as a lead. Putting the copper-plated neodymium glass in an oven, heating to 400 ℃ at the speed of 0.1 ℃/min, and taking the copper-plated surface as an electrode-on-glassApplying DC bias voltage to two sides of the glass substrate to maintain the current density of 0.2mA/cm passing through the glass substrate2Carrying out electric field assisted ion diffusion, reacting for 1h, turning off a power supply after the reaction is finished, turning off a heating furnace, slowly returning the temperature to the room temperature, and taking out a sample for later use; and (3) placing the neodymium laser glass in a tubular furnace, introducing oxygen with the flow rate of 0.1L/min, and continuously introducing the oxygen for 10min to remove impurity gases in a hearth. After the exhaust is finished, the temperature is raised to 400 ℃ at the speed of 0.1 ℃/min, the temperature is kept for 24h, after the temperature is kept, the power supply is turned off, the gas flow is kept unchanged, and after the temperature of the hearth is reduced to the room temperature, the laser neodymium glass sample is obtained and can be used as a glass window of a laser amplifier.
The thickness of the sample was measured by a secondary ion mass spectrometer, and the exchange depth of copper ions reached 250 μm.
And (3) testing the absorption value of the laser neodymium glass sample by using an ultraviolet visible infrared spectrophotometer, wherein the reflectivity of the laser neodymium glass sample at 1053nm is 0.9%, namely the reflectivity of a glass window of the laser amplifier at 1053nm is 0.9%. Since Cu2+The absorption characteristic is presented near 1053nm wave band, and the parasitic oscillation light and ASE light which are scattered or reflected internally can be well absorbed, so the parasitic oscillation can be restrained, and the ASE in the system can be reduced. The larger the reflectivity of the interface is, the more easily parasitic oscillation is generated, so that the more difficult the parasitic oscillation is to be eliminated, and the laser amplifier gain is ultimately affected. The gain coefficient of the laser neodymium glass sample of the embodiment is tested when the optical pumping energy density is 30J/cm3The laser gain coefficient is 3X10-2cm-1(ii) a The laser gain coefficient of the untreated laser neodymium glass raw material is 2X10-2cm-1。
Example 3
Mixing solid molten salt in proportion (100g cuprous chloride and 5g zinc chloride) in a crucible, placing the crucible in an oven, simultaneously placing laser neodymium glass raw material in the oven, heating to 500 ℃ at the speed of 5 ℃/min, completely melting the molten salt in the crucible, placing the laser neodymium glass in the crucible containing the molten salt, reacting for 8h, carefully taking out a glass sheet after the exchange is finished, and placing the glass sheet in the crucibleIn a glass vessel, closing a heating switch of an oven, slowly returning the temperature to room temperature, dissolving molten salt on the surface of a glass sheet by using deionized water, drying water on the surface of the glass by using nitrogen, and using a sample for later use; by magnetron sputtering (parameter: vacuum degree of 1.2X 10)-1pa, plating copper (the thickness of copper ions is 100nm) on two sides of the glass at the plating temperature of 80 ℃, the plating power of 0.75 kilowatt and the plating time of 200s, wherein the copper is used as an electrode for electric field assisted ion exchange, and the copper wire is used as a lead. Placing the copper-plated neodymium glass in an oven, heating to 500 deg.C at a rate of 5 deg.C/min, applying DC bias voltage on two sides of the glass substrate with the copper-plated surface as electrode, and maintaining the current density of 4mA/cm passing through the glass substrate2Carrying out electric field assisted ion diffusion, reacting for 12h, turning off a power supply after the reaction is finished, turning off a heating furnace, slowly returning the temperature to the room temperature, and taking out a sample for later use; and (3) placing the neodymium laser glass in a tubular furnace, introducing oxygen with the flow rate of 2L/min, and continuously introducing the oxygen for 60min to remove impurity gases in a hearth. After the exhaust is finished, the temperature is raised to 500 ℃ at the speed of 5 ℃/min, the temperature is kept for 72h, after the temperature is kept, the power supply is turned off, the gas flow is kept unchanged, and after the temperature of the hearth is reduced to the room temperature, the laser neodymium glass sample is obtained and can be used as a glass window of a laser amplifier.
The thickness of the sample was measured by using a secondary ion mass spectrometer, and the copper ion exchange depth reached 280 μm.
And (3) testing the absorption value of the laser neodymium glass sample by using an ultraviolet visible infrared spectrophotometer, wherein the reflectivity of the laser neodymium glass sample at 1053nm is 0.8%, namely the reflectivity of a glass window of the laser amplifier at 1053nm is 0.8%. Since Cu2+The absorption characteristic is presented near 1053nm wave band, and the parasitic oscillation light and ASE light which are scattered or reflected internally can be well absorbed, so the parasitic oscillation can be restrained, and the ASE in the system can be reduced. The larger the reflectivity of the interface is, the more easily parasitic oscillation is generated, so that the more difficult the parasitic oscillation is to be eliminated, and the laser amplifier gain is ultimately affected. The gain coefficient of the laser neodymium glass sample of the embodiment is tested when the optical pumping energy density is 30J/cm3The gain coefficient of the laser is 3.5X10-2cm-1(ii) a The laser gain coefficient of the untreated laser neodymium glass raw material is 2X10-2cm-1。
Example 4
Mixing solid molten salt (100g of cuprous chloride and 2g of zinc chloride) in a crucible in proportion, putting the mixture into an oven, putting a laser neodymium glass raw material into the oven, heating to 460 ℃ at the speed of 3 ℃/min, completely melting the molten salt in the crucible, putting the laser neodymium glass into the crucible containing the molten salt, carrying out ion exchange for 5 hours, carefully clamping a glass sheet after the exchange is finished, putting the glass sheet into a glass utensil, closing a heating switch of the oven, slowly returning the temperature to the room temperature, dissolving the molten salt on the surface of the glass sheet with deionized water, drying the water on the surface of the glass sheet with nitrogen, and using a sample for later use; by magnetron sputtering (parameter: vacuum degree of 1.2X 10)-1pa, plating copper (the thickness of copper ions is 70nm) on two sides of the glass at the plating temperature of 80 ℃, the plating power of 0.75 kilowatt and the plating time of 140s, wherein the copper is used as an electrode for electric field assisted ion exchange, and the copper wire is used as a lead. Placing the copper-plated neodymium glass in an oven, heating to 460 ℃ at the speed of 3 ℃/min, applying direct current bias on two sides of the glass substrate by taking the copper-plated surface as an electrode, and keeping the current density of 2mA/cm passing through the glass substrate2Carrying out electric field assisted ion diffusion, reacting for 6h, turning off a power supply after the reaction is finished, turning off a heating furnace, slowly returning the temperature to the room temperature, and taking out a neodymium laser glass sample for later use; and (3) placing the neodymium laser glass sample in a tubular furnace, introducing oxygen with the flow rate of 0.1L/min, and continuously introducing the oxygen for 60min to remove impurity gases such as air in a hearth. After the exhaust is finished, the temperature is raised to 460 ℃ at the speed of 3 ℃/min, the heat preservation is carried out for 40h, after the heat preservation is finished, the power supply is turned off, the gas flow is kept unchanged, and after the temperature of the hearth is reduced to the room temperature, the laser neodymium glass sample is obtained and can be used as a glass window of a laser amplifier.
The thickness of the sample was measured by a secondary ion mass spectrometer, and the copper ion exchange depth reached 320 μm.
And testing the absorption value of the laser neodymium glass sample by adopting an ultraviolet visible infrared spectrophotometer, wherein the laser neodymium glass sample is prepared from neodymium, iron, zinc and zincThe reflectivity of the sample at 1053nm is 0.2%, i.e. the reflectivity of the glass window of the laser amplifier at 1053nm is 0.2%. Since Cu2+The absorption characteristic is presented near 1053nm wave band, and the parasitic oscillation light and ASE light which are scattered or reflected internally can be well absorbed, so the parasitic oscillation can be restrained, and the ASE in the system can be reduced. The larger the reflectivity of the interface is, the more easily parasitic oscillation is generated, so that the more difficult the parasitic oscillation is to be eliminated, and the laser amplifier gain is ultimately affected. The gain coefficient of the laser neodymium glass sample of the embodiment is tested when the optical pumping energy density is 30J/cm3The laser gain coefficient was 4.6X10-2cm-1(ii) a The laser gain coefficient of the untreated laser neodymium glass raw material is 2X10-2cm-1。
Example 5
Mixing solid molten salt (100g of cuprous chloride and 1.8g of zinc chloride) in a crucible in proportion, putting the mixture into an oven, putting a laser neodymium glass raw material into the oven, heating to 450 ℃ at the speed of 3 ℃/min, completely melting the molten salt in the crucible, putting the laser neodymium glass into the crucible containing the molten salt, carrying out ion exchange for 4h, carefully clamping out a glass sheet after the exchange is finished, putting the glass sheet into a glass vessel, closing a heating switch of the oven, slowly returning the temperature to the room temperature, dissolving the molten salt on the surface of the glass sheet with deionized water, drying the water on the surface of the glass sheet with nitrogen, and preparing a sample for later use; by magnetron sputtering (parameter: vacuum degree of 1.2X 10)-1pa, plating copper (the thickness of copper ions is 60nm) on two sides of the glass at the plating temperature of 80 ℃, the plating power of 0.75 kilowatt and the plating time of 120s, wherein the copper is used as an electrode for electric field assisted ion exchange, and the copper wire is used as a lead. Placing the copper-plated neodymium glass in an oven, heating to 450 deg.C at a rate of 3 deg.C/min, applying DC bias voltage to two sides of the glass substrate with the copper-plated surface as electrode, and maintaining the current density of 2mA/cm passing through the glass substrate2Carrying out electric field assisted ion diffusion, reacting for 4h, turning off a power supply after the reaction is finished, turning off a heating furnace, slowly returning the temperature to the room temperature, and taking out a neodymium laser glass sample for later use; placing the neodymium laser glass sample in a tubular furnace, introducing oxygen with the flow rate of 0.1L/min, and continuously introducing air for 60min to remove air and the like in a hearthAn impurity gas. After the exhaust is finished, the temperature is increased to 450 ℃ at the speed of 3 ℃/min, the temperature is kept for 40h, after the temperature is kept, the power supply is turned off, the gas flow is kept unchanged, and after the temperature of the hearth is reduced to the room temperature, the laser neodymium glass sample is obtained and can be used as a glass window of a laser amplifier.
The thickness of the sample was measured by a secondary ion mass spectrometer, and the copper ion exchange depth reached 290 μm.
And (3) testing the absorption value of the laser neodymium glass sample by using an ultraviolet visible infrared spectrophotometer, wherein the reflectivity of the laser neodymium glass sample at 1053nm is 0.2%, namely the reflectivity of a glass window of the laser amplifier at 1053nm is 0.2%. Since Cu2+The absorption characteristic is presented near 1053nm wave band, and the parasitic oscillation light and ASE light which are scattered or reflected internally can be well absorbed, so the parasitic oscillation can be restrained, and the ASE in the system can be reduced. The larger the reflectivity of the interface is, the more easily parasitic oscillation is generated, so that the more difficult the parasitic oscillation is to be eliminated, and the laser amplifier gain is ultimately affected. The gain coefficient of the laser neodymium glass sample of the embodiment is tested when the optical pumping energy density is 30J/cm3The laser gain coefficient was 4.4X10-2cm-1(ii) a The laser gain coefficient of the untreated laser neodymium glass raw material is 2X10-2cm-1。
Comparative example 1
Mixing solid molten salt in a crucible according to a ratio (100g of cuprous chloride and 2g of zinc chloride), putting the mixture into an oven, putting a laser neodymium glass raw material into the oven, heating to 480 ℃ at the speed of 3 ℃/min, completely melting the molten salt in the crucible, putting the laser neodymium glass into the crucible containing the molten salt, carrying out ion exchange for 6h, carefully clamping out a glass sheet after the exchange is finished, putting the glass sheet into a glass utensil, closing a heating switch of the oven, slowly returning the temperature to the room temperature, dissolving the molten salt on the surface of the glass sheet with deionized water, drying the water on the surface of the glass sheet with nitrogen, and preparing a sample for later use; and (3) placing the neodymium laser glass in a tubular furnace, introducing oxygen with the flow rate of 0.1L/min, and continuously introducing the oxygen for 60min to remove impurity gases in a hearth. And after the exhaust is finished, heating to 480 ℃ at the speed of 3 ℃/min, preserving the heat for 48h, after the heat preservation is finished, turning off the power supply, maintaining the gas flow unchanged, and obtaining the laser neodymium glass sample after the temperature of the hearth is reduced to the room temperature.
The thickness of the sample was measured by a secondary ion mass spectrometer, and the exchange depth of copper ions reached 180 μm.
The absorption value of a sample is tested by adopting an ultraviolet visible infrared spectrophotometer, the reflectivity of a neodymium glass sample at 1053nm is 3.2%, even if the neodymium glass is used as a glass window of a laser amplifier, the reflectivity of the glass window of the laser amplifier at 1053nm is 3.2%, and the effect is poor. Since Cu2+The absorption characteristic is presented near 1053nm wave band, and the parasitic oscillation light and ASE light which are scattered or reflected internally can be well absorbed, so the parasitic oscillation can be restrained, and the ASE in the system can be reduced. The larger the reflectivity of the interface is, the more easily parasitic oscillation is generated, so that the more difficult the parasitic oscillation is to be eliminated, and the laser amplifier gain is ultimately affected. The gain coefficient of the laser neodymium glass sample of the comparative example is tested when the optical pumping energy density is 30J/cm3The laser gain coefficient is 2.6X10-2cm-1(ii) a The laser gain coefficient of the untreated laser neodymium glass raw material is 2X10- 2cm-1。
Comparative example 2
Mixing solid molten salt in a crucible according to a ratio (100g of cuprous chloride and 2g of zinc chloride), putting the mixture into an oven, putting a laser neodymium glass raw material into the oven, heating to 480 ℃ at the speed of 3 ℃/min, completely melting the molten salt in the crucible, putting the laser neodymium glass into the crucible, carrying out ion exchange for 6h, carefully clamping a glass sheet after the exchange is finished, putting the glass sheet into a glassware, closing a heating switch of the oven, slowly returning the temperature to room temperature, dissolving the molten salt on the surface of the glass sheet with deionized water, drying the water on the surface of the glass sheet with nitrogen, and using a sample for later use; by magnetron sputtering (parameter: vacuum degree of 1.2X 10)-1pa, plating copper (the thickness of copper ions is 80nm) on two sides of the glass at the plating temperature of 80 ℃, the plating power of 0.75 kilowatt and the plating time of 160s, wherein the copper is used as an electrode for electric field assisted ion exchange, and the copper wire is used as a lead. Putting the copper-plated neodymium glass in a baking ovenIn the box, the temperature is raised to 480 ℃ at the speed of 3 ℃/min, direct current bias is applied to two sides of the glass substrate by taking the copper-plated surface as an electrode, and the current density passing through the glass substrate is kept to be 2mA/cm2And (3) carrying out electric field assisted ion diffusion, reacting for 8h, turning off a power supply after the reaction is finished, turning off the heating furnace, and slowly returning the temperature to the room temperature to obtain the laser neodymium glass sample.
The thickness of the sample was measured by using a secondary ion mass spectrometer, and the copper ion exchange depth reached 240 μm.
The absorption value of a sample is tested by adopting an ultraviolet visible infrared spectrophotometer, the reflectivity of the neodymium glass sample at 1053nm is 40%, even if the neodymium glass is used as a glass window of a laser amplifier, the reflectivity of the glass window of the laser amplifier at 1053nm is 40%, and the effect is poor. Because of Cu2+The absorption characteristic is presented near 1053nm wave band, and the parasitic oscillation light and ASE light which are scattered or reflected internally can be well absorbed, so the parasitic oscillation can be restrained, and the ASE in the system can be reduced. The larger the reflectivity of the interface is, the more easily parasitic oscillation is generated, so that the more difficult the parasitic oscillation is to be eliminated, and the laser amplifier gain is ultimately affected. The gain coefficient of the laser neodymium glass sample of the comparative example is tested when the optical pumping energy density is 30J/cm3The laser gain coefficient was 2.1X10-2cm-1(ii) a The laser gain coefficient of the untreated laser neodymium glass raw material is 2X10- 2cm-1。
The above-mentioned "reflectance" is expressed by the formula R.eDβThe residual reflectivity R of the boundary in more than or equal to 1, and beta is a gain coefficient; d is the long axis diameter of the laser glass sheet.
The laser neodymium glass raw materials used in examples 1 to 5 and comparative examples 1 to 2 were the same, and the major axis diameter D was 10 cm. However, the preparation method of the laser neodymium glass is not limited to the use of the laser neodymium glass raw material with the major axis diameter D of 10cm, and the laser neodymium glass raw material with the major axis diameter D of 50cm to 100cm can also be used.
Comparing example 1 with comparative examples 1-2, it can be seen that since comparative example 1 has no step of electric field assisted ion diffusion compared to example 1, and comparisonExample 2 No Cu in comparison to example 1+The ion oxidation step, the depth, reflectivity and laser gain coefficient of the sample prepared in comparative example 1 or 2 could not reach the optimum values. Therefore, only example 1, which completed three steps simultaneously, could obtain an optimal sample; in contrast, the comparison of examples 1 to 5 shows that the different processes are essentially to adjust the thickness of the ion exchange and the content of the divalent copper. The deeper the thickness, the more the content of divalent copper, the lower the reflectivity of the sample, and the higher the laser gain coefficient, thereby suppressing amplified spontaneous emission and parasitic oscillation, resulting in better sample performance.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The recitation of numerical ranges herein includes all numbers subsumed within that range and includes any two numbers subsumed within that range. Different values of the same index appearing in all embodiments of the invention can be combined arbitrarily to form a range value.
The features of the invention claimed and/or described in the specification may be combined, and are not limited to the combinations set forth in the claims by the recitations therein. The technical solutions obtained by combining the technical features in the claims and/or the specification also belong to the scope of the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.

Claims (6)

1. A preparation method of laser neodymium glass for inhibiting amplified spontaneous radiation and parasitic oscillation is characterized by comprising the following steps:
1）Cu+ion exchange: performing ion exchange on a laser neodymium glass raw material by using cuprous chloride and zinc chloride as molten salts to obtain a laser neodymium glass substrate;
2) electric field assistanceIon diffusion: manufacturing copper metal films on the two surfaces of the laser neodymium glass substrate obtained in the step 1); then heating the glass substrate to 400-500 ℃, applying direct current bias on two sides of the glass substrate by taking the copper-plated surface as an electrode, and keeping the current density passing through the glass substrate to be 0.2-4 mA/cm2Carrying out electric field assisted ion diffusion, and maintaining exchange for 1-12h to obtain a laser neodymium glass intermediate;
3）Cu+ion oxidation: introducing oxygen mixed gas into the laser neodymium glass intermediate prepared in the step 2) at the rate of 0.1-2L/min, and continuously introducing the oxygen mixed gas for 10-60 min to remove air; after the exhaust is finished, the temperature is increased to the reaction temperature of 400-500 ℃ at the temperature rising rate of 0.1-5 ℃, the temperature is kept for 24-72 h, after the temperature is kept, the power is cut off, the gas flow is kept unchanged, and after the temperature is reduced to the room temperature, the laser neodymium glass is obtained.
2. The method for preparing laser neodymium glass for inhibiting amplified spontaneous emission and parasitic oscillation according to claim 1, wherein the molten salt in the step 1) is a mixed solution of cuprous chloride and zinc chloride, and the mass ratio of the cuprous chloride to the zinc chloride is 100 to (0.1-5).
3. The method for preparing laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation as claimed in claim 1, wherein the ion exchange in step 1) has an exchange temperature of 400-.
4. The method for preparing laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation according to claim 1, wherein in the step 2), the copper metal film is prepared by a magnetron sputtering method.
5. The method of manufacturing a laser neodymium glass suppressing amplified spontaneous emission and parasitic oscillation according to claim 4, wherein the thickness of the copper metal film is 50 to 100 nm.
6. The method for preparing laser neodymium glass for suppressing amplified spontaneous emission and parasitic oscillation according to claim 1, wherein in the step 2), the temperature rise rate is 0.1-5 ℃/min.
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CN101880127A (en) * 2010-05-26 2010-11-10 中国科学院上海光学精密机械研究所 Phosphate laser neodymium glass with enhanced surface ion modification and preparation method thereof
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