CN115521065A - Samarium-doped chalcogenide glass and preparation method thereof - Google Patents
Samarium-doped chalcogenide glass and preparation method thereof Download PDFInfo
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- CN115521065A CN115521065A CN202110186923.0A CN202110186923A CN115521065A CN 115521065 A CN115521065 A CN 115521065A CN 202110186923 A CN202110186923 A CN 202110186923A CN 115521065 A CN115521065 A CN 115521065A
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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
- C03C3/00—Glass compositions
- C03C3/32—Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
- C03C3/321—Chalcogenide glasses, e.g. containing S, Se, Te
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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Abstract
The invention discloses samarium-doped chalcogenide glass and a preparation method thereof. The samarium-doped sulfur glass comprises the following components (in atomic percentage): s:50% -70%; 20 to 45 percent of Ge; 5 to 15 percent of As; 0.1 to 5 percent of Sm. According to the invention, the rare earth element samarium is added into a common As-Ge-S chalcogenide glass system, and the structural densification generated by the high field intensity and high coordination characteristic of rare earth ions is utilized, so that the transition temperature of the glass is raised, the hardness of the glass is improved, and the infrared window material with better thermal and mechanical properties is obtained, thereby meeting the use requirements of a laser radar.
Description
Technical Field
The invention belongs to the technical field of chalcogenide glass, and relates to samarium-doped chalcogenide glass and a preparation method thereof. The glass is suitable for being used as an infrared window material of laser radar.
Background
Chalcogenide glass refers to glass containing sulfides, and antimonides as main components. Compared with oxide glass, the glass has larger mass and weaker bond energy, has smaller forbidden bandwidth than the oxide glass, is prepared by adopting a quenching process, generally has a wider glass forming area, and has infrared transmission wavelength covering an infrared atmospheric window of 8-12 mu m. Due to the characteristics, in a laser radar system utilizing infrared binocular imaging, chalcogenide glass can be used as a window material of an infrared laser receiving and transmitting structure.
However, one of the problems faced by chalcogenide glass as a structural functional window material is that the chalcogenide glass has low strength and generates a dispersion phenomenon under laser irradiation, which affects the optical signal acquisition quality. According to the invention, rare earth element samarium is added into a common As-Ge-S chalcogenide glass system, and the structural densification generated by the high field intensity and high coordination property of rare earth ions is utilized, so that the transition temperature of the glass is raised, the hardness of the glass is improved, and an infrared window material with better thermal and mechanical properties is obtained, thereby meeting the use requirements of a laser radar.
Disclosure of Invention
The invention mainly aims to provide samarium-doped chalcogenide glass and a preparation method thereof so as to meet the use requirement of a laser radar infrared window material.
The samarium-doped chalcogenide glass is prepared by adopting the following technical scheme:
a samarium-doped chalcogenide glass comprises the following components (the contents are calculated by atomic percent):
S：50%～70％
Ge: 20%～45％
As: 5%～15％
Sm: 0.1%～5％
a preparation method of samarium-doped chalcogenide glass comprises the following steps:
step 1 preparation of glass batch:
and respectively weighing the simple substances of S, ge, as and Sm by using an electronic balance, and mixing to obtain the glass batch.
Wherein the precision of the electronic balance is 0.001 g; the purity of the raw material simple substance is 5N.
Step 2, vacuum sealing:
and (2) placing the glass batch obtained in the step (1) into a quartz ampoule, extracting air from the quartz ampoule by using a vacuum pump, and after reaching a proper vacuum degree, welding and sealing the quartz ampoule by using oxyhydrogen flame.
Preferably: the quartz ampoule is soaked in 50% hydrofluoric acid for 20-40 min.
Preferably, the following components: the vacuum degree in the ampoule is 10 when sealing -2 Pa。
Step 3, glass melting:
and (3) placing the sealed quartz ampoule in the step (2) in a rocking furnace, slowly heating to a melting temperature, starting the rocking furnace to swing, and keeping the temperature for a proper time.
Preferably: the heating rate is not more than 10 ℃/min.
Preferably, the following components: the melting temperature is 850-950 ℃.
Preferably, the following components: the swinging frequency of the swinging furnace is 40-60 times/min.
Preferably: the heat preservation time is 10-20 hours.
Step 4, quenching glass:
the quartz ampoule was taken out of the rocking furnace, allowed to stand in the coolant for 1 to 3 minutes, and the glass was observed to be formed and separated from the ampoule wall.
Preferably, the following components: the cooling liquid is water, and the temperature is not more than 50 ℃.
Step 5, glass annealing:
and (3) placing the ampoule in an annealing furnace, preserving the heat for 1 hour at a proper temperature, cooling along with the furnace, and taking out the glass from the quartz ampoule to obtain the chalcogenide glass.
Preferably: the annealing temperature is 200-300 ℃.
Detailed Description
In order to make the technical solutions of the present invention more clear and definite for those skilled in the art, the present invention is further described in detail with reference to the following examples, but the embodiments of the present invention are not limited thereto.
Example one
The samarium-doped chalcogenide glass provided by the embodiment comprises the following components (the contents are calculated by atomic percent):
S：50%
Ge: 44.9％
As: 5%
Sm: 0.1%
the preparation method comprises the following steps:
step 1, preparation of glass batch:
s, ge, as and Sm simple substances with the purity of 5N are respectively weighed by an electronic balance with the precision of 0.001 g and then mixed to obtain the glass batch.
Step 2, vacuum sealing:
placing the glass batch obtained in the step 1 into a quartz ampoule, and extracting air from the quartz ampoule by using a vacuum pump until the air content reaches 10 DEG -2 And (4) after the vacuum degree is Pa, welding and sealing the quartz ampoule by adopting oxyhydrogen flame. The quartz ampoule is soaked in 50% hydrofluoric acid for 20 min.
Step 3, glass melting:
and (3) placing the sealed quartz ampoule in the step (2) into a rocking furnace, heating to 950 ℃ at the heating rate of 3 ℃/min, starting the rocking furnace to rock, wherein the rocking frequency is 45 times/min. And keeping the temperature for 10 hours.
Step 4, quenching glass:
the quartz ampoule was taken out of the rocking furnace, left to stand in water at 40 ℃ for 2 minutes, and the glass was observed to be shaped and separated from the ampoule wall.
Step 5, glass annealing:
and (3) placing the ampoule into an annealing furnace, preserving the heat for 1 hour at the temperature of 250 ℃, cooling along with the furnace, and taking out the glass from the quartz ampoule to obtain the required chalcogenide glass.
The sample is subjected to performance test, the microhardness is 2089 Mpa, and the glass transition temperature is 375 ℃.
Example two
The samarium-doped chalcogenide glass provided by the embodiment comprises the following components (the contents are calculated by atomic percent):
S：55%
Ge: 25％
As: 15%
Sm: 5%
the preparation method comprises the following steps:
step 1 preparation of glass batch:
s, ge, as and Sm simple substances with the purity of 5N are respectively weighed by an electronic balance with the precision of 0.001 g and then mixed to obtain the glass batch.
Step 2, vacuum sealing:
putting the glass batch obtained in the step 1 into a quartz ampoule, and extracting air from the quartz ampoule by using a vacuum pump until the air content reaches 10 DEG -2 And (4) after the vacuum degree is Pa, welding and sealing the quartz ampoule by adopting oxyhydrogen flame. The quartz ampoule is immersed in 50% hydrofluoric acid for 30 minutes.
Step 3, melting glass:
and (3) placing the sealed quartz ampoule in the step (2) into a rocking furnace, raising the temperature to 900 ℃ at the heating rate of 10 ℃/min, starting the rocking furnace to rock, wherein the rocking frequency is 60 times/min. And keeping the temperature for 20 hours.
Step 4, quenching glass:
the quartz ampoule was taken out of the rocking furnace, left to stand in water at 20 ℃ for 3 minutes, and the glass was observed to be shaped and separated from the ampoule wall.
Step 5, annealing glass:
and (3) placing the ampoule into an annealing furnace, preserving the heat for 12 hours at the temperature of 300 ℃, cooling along with the furnace, and taking out the glass from the quartz ampoule to obtain the required chalcogenide glass.
The sample is subjected to performance test, the microhardness is 2203Mpa, and the glass transition temperature is 365 ℃.
EXAMPLE III
The samarium-doped chalcogenide glass provided by the embodiment comprises the following components (the contents are calculated by atomic percent):
S：65%
Ge: 35％
As: 4%
Sm: 1%
the preparation method comprises the following steps:
step 1 preparation of glass batch:
s, ge, as and Sm simple substances with the purity of 5N are respectively weighed by an electronic balance with the precision of 0.001 g and then mixed to obtain the glass batch.
Step 2, vacuum sealing:
placing the glass batch obtained in the step 1 into a quartz ampoule, and extracting air from the quartz ampoule by using a vacuum pump until the air content reaches 10 DEG -2 And (4) after the vacuum degree is Pa, welding and sealing the quartz ampoule by adopting oxyhydrogen flame. The quartz ampoule was immersed in 50% hydrofluoric acid for 40 minutes.
Step 3, melting glass:
and (3) placing the sealed quartz ampoule in the step (2) into a rocking furnace, raising the temperature to 850 ℃ at the heating rate of 1 ℃/min, starting the rocking furnace to rock, wherein the rocking frequency is 45 times/min. And keeping the temperature for 10 hours.
Step 4, quenching glass:
the quartz ampoule was taken out of the rocking furnace, left to stand in water at 40 ℃ for 1 minute, and the glass was observed to be shaped and separated from the ampoule wall.
Step 5, glass annealing:
and (3) placing the ampoule into an annealing furnace, preserving heat for 5 hours at the temperature of 200 ℃, cooling along with the furnace, and taking the glass out of the quartz ampoule to obtain the required chalcogenide glass.
The sample was subjected to a property test having a microhardness of 2175MPa and a glass transition temperature of 370 ℃.
Claims (9)
1. The samarium-doped chalcogenide glass is characterized by comprising the following components in atomic percentage: s: 50-70 percent of Ge, 20-45 percent of Ge, 5-15 percent of As and 1-10 percent of Sm.
2. A preparation method of samarium-doped chalcogenide glass is characterized by comprising the following steps: the method comprises the following steps: step 1 preparation of glass batch: weighing the simple substances of S, ge, as and Sm respectively by an electronic balance, and mixing to obtain a glass batch; step 2, vacuum sealing: placing the glass batch obtained in the step 1 into a quartz ampoule, extracting air from the quartz ampoule by using a vacuum pump, and after reaching a proper vacuum degree, welding and sealing the quartz ampoule by using oxyhydrogen flame; step 3, melting glass: placing the quartz ampoule sealed in the step (2) in a rocking furnace, slowly heating to a melting temperature, starting the rocking furnace to swing, and keeping the temperature for a proper time; step 4, quenching glass; taking the quartz ampoule out of the rocking furnace, standing in cooling liquid for 1-3 minutes, and observing glass forming and separating from the ampoule wall; step 5, annealing glass: and (3) placing the ampoule in an annealing furnace, preserving the heat for 1-12 hours at a proper temperature, cooling along with the furnace, and taking the glass out of the quartz ampoule to obtain the chalcogenide glass.
3. The method for preparing a light rare earth doped silicon aluminum alloy according to claim 2, wherein the elemental purity selected in step 1 is 5N.
4. The method for preparing a light rare earth-doped Si-Al alloy according to claim 2, wherein the quartz ampoule used in step 2 is soaked in 50% hydrofluoric acid for 20-40 min.
5. The method for preparing a light rare earth-doped Si-Al alloy according to claim 2, wherein the temperature rise rate of the rocking furnace used in the step 3 is not more than 10 ℃/min.
6. The method for preparing a light rare earth doped silicon aluminum alloy according to claim 2, wherein the melting temperature adopted in the step 3 is 850-950 ℃, and the holding time is 10-20 hours.
7. The method for preparing a light rare earth doped silicon aluminum alloy according to claim 2, wherein the swing frequency of the swing furnace adopted in the step 3 is 40-60 times/min.
8. The method for preparing a light rare earth doped silicon aluminum alloy according to claim 2, wherein the cooling liquid adopted in the step 4 is water, and the temperature is not more than 50 ℃.
9. The method for preparing a light rare earth doped silicon aluminum alloy according to claim 2, wherein the annealing temperature adopted in the step 4 is 200-300 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110186923.0A CN115521065A (en) | 2021-02-23 | 2021-02-23 | Samarium-doped chalcogenide glass and preparation method thereof |
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| CN202110186923.0A CN115521065A (en) | 2021-02-23 | 2021-02-23 | Samarium-doped chalcogenide glass and preparation method thereof |
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- 2021-02-23 CN CN202110186923.0A patent/CN115521065A/en active Pending
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