CN113998896B - High-efficiency synthesis method of chalcogenide glass powder - Google Patents
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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
- C03C12/00—Powdered glass; Bead compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge
- B02C17/163—Stirring means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/1815—Cooling or heating devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/182—Lids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/24—Driving mechanisms
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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
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The application discloses a high-efficiency synthesis method of chalcogenide glass powder, which comprises the steps of crushing and sieving a simple substance raw material in a glove box to obtain the simple substance raw material with the granularity of less than 500 mu m; then weighing the simple substance raw materials and mixing the simple substance raw materials to obtain a raw material mixture; and finally, filling the raw material mixture and the grinding balls into a ball milling tank of a stirring ball mill, and introducing protective gas and liquid nitrogen to perform low-temperature ball milling combination. The synthetic method can shorten the synthetic time of the chalcogenide glass powder from more than 72 hours to less than 12 hours, improve the single-time productivity from less than 4kg to more than 20kg, and can be used for preparing the bulk chalcogenide glass with high optical quality, and the synthesized chalcogenide glass powder has high purity and small granularity.
Description
Technical Field
The invention relates to a glass synthesis method, in particular to a high-efficiency synthesis method of chalcogenide glass powder.
Background
The infrared thermal imaging product has wide application in the fields of power and electricians, metallurgy and petrochemical industry, biological epidemic prevention, fire rescue, rail transit, security night vision and the like. In an infrared thermal imaging system, an infrared lens is a key element of its optical system. Commonly used infrared lens materials are mainly germanium, zinc selenide and chalcogenide glass. Compared with germanium and zinc selenide crystal materials, the amorphous chalcogenide glass material has the advantages of lower preparation and processing cost, low temperature coefficient of refractive index, continuously adjustable refractive index and the like, so chalcogenide glass lenses become necessary optical elements in temperature self-adaptive infrared thermal imaging products in recent years.
At present, the production of chalcogenide glass adopts a vacuum melting-quenching technology, namely, raw materials are sealed in a vacuum quartz ampoule, and then high-temperature melting, quenching and annealing are carried out. Because the raw materials need to be fused and combined in a quartz ampoule, the caliber and the single capacity of the produced chalcogenide glass are both limited by the size of a quartz tube, and the single production period is long (generally more than 5 days), so the technology is not suitable for industrialized large-scale production of chalcogenide glass. In addition, the links of cutting, grinding, polishing and the like of glass in the lens forming process consume a large amount of human resources, and the utilization rate of materials is low (generally not more than 40%); the cold working also produces extra heavy metal waste emission, causing environmental pollution. Therefore, the existing production technology cannot meet the requirements of the civil industry on low-cost and high-efficiency mass production of chalcogenide lenses.
In order to reduce the production cost of chalcogenide glass and improve the production efficiency of chalcogenide glass, researchers try to prepare chalcogenide glass powder by a high-energy ball milling chemical combination method and then obtain bulk chalcogenide glass with high optical quality by a powder hot pressing technology. The method can greatly improve the utilization rate of the material (generally over 90 percent), and obviously reduce the production cost of the chalcogenide glass. Although the powder hot pressing process only takes 2-8 hours, the reported times for high energy ball milling to synthesize chalcogenide glass powders typically exceed 72 hours, resulting in a total time for making chalcogenide glass using this process of more than 3 days. In order to further significantly shorten the preparation time of chalcogenide glass, a faster and more efficient method for synthesizing chalcogenide glass powder is required.
Disclosure of Invention
Aiming at the problems of long production cycle and low efficiency of synthesizing chalcogenide glass powder by the existing high-energy ball milling chemical combination technology, the invention provides a preparation method of chalcogenide glass powder with short synthesis time and high efficiency.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a high-efficiency synthetic method of chalcogenide glass powder comprises the following steps:
the first step is as follows: crushing and sieving the elementary raw materials in a glove box to obtain the elementary raw materials with the granularity of less than 500 mu m;
the second step is that: calculating the mass of each elementary substance raw material according to the chemical composition and the mass of the chalcogenide glass powder to be synthesized;
the third step: weighing various simple substance raw materials in a glove box, filling the weighed simple substance raw materials into a clean container, mixing to obtain a raw material mixture, and sealing the container by using a cover;
the fourth step: opening a cover of a ball milling tank of the stirring ball mill, filling grinding balls into the ball milling tank, taking out a sealed container filled with the raw material mixture from the glove box, opening the cover of the sealed container, pouring the raw material mixture into the ball milling tank, and covering the cover of the ball milling tank;
the fifth step: continuously introducing shielding gas from a shielding gas inlet on a ball milling tank cover for more than 30 minutes, and discharging air in the ball milling tank through a gas outlet on the ball milling tank cover;
and a sixth step: intermittently introducing liquid nitrogen from a liquid nitrogen inlet on a ball milling pot cover, controlling the temperature in the ball milling pot to be-20 ℃, and monitoring the temperature in the ball milling pot through a thermal resistor;
the seventh step: setting the rotating speed of a ball mill motor, starting the ball mill motor, and driving a stirring rod penetrating through a sealing ring to rotate, so that grinding balls are driven to rotate at a high speed to grind the raw material mixture;
the eighth step: and stopping introducing the liquid nitrogen and the protective gas when the ball mill continuously operates for 8-12 hours, opening a ball valve switch below a discharge port at the bottom of the ball mill tank, and collecting the integrated powder at the discharge port.
Further, the composition of the chalcogenide glass comprises one or two elements of Ge, as and Sb and one or two elements of S, se and Te.
Further, the purity of the elementary substance raw material is not less than 99.999%.
Further, the glove box is filled with dry nitrogen or argon, and the oxygen content of water in the glove box is lower than 0.1ppm.
Furthermore, the lining of the ball milling tank, the grinding balls and the stirring rod are all made of tungsten carbide or zirconium oxide.
Further, the mass ratio of the grinding balls to the raw material mixture (i.e. the ball-to-feed ratio) is 12.
Furthermore, the diameter of the grinding ball is 5-20 mm.
Further, the rotating speed of the stirring rod is 200-400 revolutions per minute.
Further, the pressure of the protective gas is 0.02-0.1 MPa.
Has the beneficial effects that:
compared with the prior art, the high-efficiency synthesis method of chalcogenide glass powder provided by the invention has the following advantages:
1. the synthetic method can shorten the synthetic time of the chalcogenide glass powder from more than 72 hours to within 12 hours in the prior art;
2. the chalcogenide glass powder synthesized by the synthesis method has high purity and small particle size, and can be used for preparing bulk chalcogenide glass with high optical quality;
3. the synthetic method can improve the single-time capacity of the chalcogenide glass powder from below 4kg to above 20 kg.
Drawings
FIG. 1 is a schematic view of the structure of an agitator ball mill according to the present invention.
Description of reference numerals: 1-a ball milling tank cover, 2-a ball milling tank, 3-grinding balls, 4-a raw material mixture, 5-a shielding gas inlet, 6-a gas outlet, 7-a liquid nitrogen inlet, 8-a thermal resistor, 9-a motor, 10-a sealing ring, 11-a stirring rod, 12-a discharge port and 13-a ball valve switch.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1
40kgAs 0.4 Se 0.6 Synthesizing chalcogenide glass powder:
crushing the As and Se elementary substance raw materials with the purity of 99.999 percent in a glove box filled with dry nitrogen and the water oxygen content of which is lower than 0.1ppm, and sieving the crushed raw materials with a 35-mesh sieve to obtain the elementary substance raw materials with the granularity of less than 500 mu m;
according to the chemical composition As of the chalcogenide glass powder to be synthesized 0.4 Se 0.6 And the mass of the simple substance raw materials of As and Se required for calculating 40kg is 15.50kg and 24.50kg respectively;
weighing the obtained simple substance raw materials in a glove box, filling the weighed simple substance raw materials into a clean container for mixing to obtain a raw material mixture 4, and then sealing the container by using a cover;
opening a ball milling tank cover 1 of a stirring type ball mill (shown in figure 1), filling 160kg of zirconia grinding balls 3 with the diameter of 20mm into a ball milling tank 2 with the inner lining made of zirconia, then taking out a sealed container containing raw material mixture 4 from a glove box, opening the cover of the sealed container, pouring the raw material mixture 4 into the ball milling tank 2, and covering the ball milling tank cover 1;
continuously introducing nitrogen with the air pressure of 0.02MPa into a protective gas inlet 5 on the ball milling tank cover 1 for 30 minutes, and discharging the air in the ball milling tank 2 through an air outlet 6 on the ball milling tank cover 1;
introducing liquid nitrogen from a liquid nitrogen inlet 7 on the ball milling tank cover 1 discontinuously, and controlling the temperature in the ball milling tank 2 to be 15-20 ℃ (measured by a thermal resistor 8);
setting the rotation speed of a ball mill motor 9 to be 200 revolutions per minute, starting the ball mill motor 9 to drive a stirring rod 11 to rotate, wherein the stirring rod 11 is made of zirconia, penetrates through a sealing ring 10 on a ball mill tank cover 1 from the inside of a ball mill tank 2 and is connected with the motor 9, so that grinding balls 3 are driven to rotate at a high speed to grind a raw material mixture 4;
and (3) stopping introducing liquid nitrogen and nitrogen when the ball mill continuously operates for 8 hours, opening a ball valve switch 13 below a discharge port 12 at the bottom of the ball mill tank, and collecting the synthesized powder at the discharge port 12.
Performing phase analysis on the obtained powder by using an X-ray diffractometer (XRD, bruker D2); the particle size of the obtained powder was measured with a particle size analyzer (Nano Brook Omni); testing the impurity content in the obtained powder by adopting an inductively coupled plasma spectrometer (ICP, PQ 9000); testing the chemical composition of the obtained powder by adopting a scanning electron microscope (SEM, JEOL JSM-6510) equipped with an energy spectrometer;
the detection result of the powder obtained in this example is: the powder is in an amorphous state; the average particle size of the powder is 8 mu m; the impurity content (Zr is the main impurity) in the powder is about 25ppm; the chemical composition of the powder is As 0.401±0.003 Se 0.599±0.003 。
Example 2
30kg Ge 0.12 As 0.24 S 0.64 Synthesizing chalcogenide glass powder:
crushing Ge with the purity of 99.999 percent, as with the purity of 99.9999 percent and S elementary substance raw materials in a glove box filled with dry argon and with the water oxygen content of less than 0.1ppm, and sieving the raw materials with a 45-mesh sieve to obtain the elementary substance raw materials with the granularity of less than 355 mu m;
according to the chemical composition Ge of the chalcogenide glass powder to be synthesized 0.12 As 0.24 S 0.64 And the mass of the elementary substance raw materials Ge, as and S required for calculating 30kg is 5.54kg, 11.42kg and 13.04kg respectively;
weighing the obtained simple substance raw materials in a glove box, filling the weighed simple substance raw materials into a clean container for mixing to obtain a raw material mixture 4, and then sealing the container by using a cover;
opening a ball milling tank cover 1 of the stirring ball mill, filling 180kg of zirconia grinding balls with the diameter of 10mm into a ball milling tank 2 with the inner lining made of zirconia, taking out a sealed container containing a raw material mixture 4 from a glove box, opening the cover of the sealed container, pouring the raw material mixture 4 into the ball milling tank 2, and covering the ball milling tank cover 1;
continuously introducing nitrogen with the air pressure of 0.06MPa from a protective gas inlet 5 on the ball milling tank cover 1 for 60 minutes, and discharging the air in the ball milling tank 2 through an air outlet 6 on the ball milling tank cover 1;
introducing liquid nitrogen from a liquid nitrogen inlet 7 on the ball milling tank cover 1 discontinuously, and controlling the temperature in the ball milling tank 2 to be-10 to-5 ℃;
setting the rotation speed of a motor 9 of the ball mill to 300 revolutions per minute, starting the motor 9 of the ball mill, driving a stirring rod 11 to rotate, and enabling a zirconium oxide material of the stirring rod 11 to penetrate through a sealing ring 10 on a cover 1 of the ball mill from the inside of a ball milling tank 2 to be connected with the motor 9, so that grinding balls 3 are driven to rotate at a high speed to grind a raw material mixture 4;
and stopping introducing liquid nitrogen and nitrogen when the ball mill continuously operates for 10 hours, opening a ball valve switch 13 below a discharge port 12 at the bottom of the ball mill tank, and collecting the synthesized powder at the discharge port 12.
Performing phase analysis on the obtained powder by using an X-ray diffractometer (XRD, bruker D2); the particle size of the obtained powder was measured with a particle size analyzer (Nano Brook Omni); testing the impurity content in the obtained powder by adopting an inductively coupled plasma spectrometer (ICP, PQ 9000); the chemical composition of the obtained powder was tested by scanning electron microscopy (SEM, JEOL JSM-6510) equipped with an energy spectrometer.
The detection result of the powder obtained in this example is: the powder is in an amorphous state; the average particle size of the powder is 5 mu m; the impurity content (Zr is the main impurity) in the powder is about 42ppm; the chemical composition of the powder is Ge 0.122±0.003 As 0.241± 0.003 S 0.637±0.003 。
Example 3
20kg Ge 0.20 As 0.20 Se 0.45 Te 0.15 Synthesizing chalcogenide glass powder:
crushing Ge, as, se and Te elementary substance raw materials with the purity of 99.999 percent in a glove box filled with dry argon and with the water oxygen content lower than 0.1ppm, and sieving the crushed raw materials with a sieve of 60 meshes to obtain the elementary substance raw materials with the granularity of less than 250 mu m;
according to the chemical composition Ge of the chalcogenide glass powder to be synthesized 0.20 As 0.20 Se 0.45 Te 0.15 And the mass of the elementary substance raw materials Ge, as, se and Te required for calculating 20kg is respectively 3.45kg, 3.56kg, 8.44kg and 4.55kg;
weighing the obtained simple substance raw materials in a glove box, filling the weighed simple substance raw materials into a clean container for mixing to obtain a raw material mixture 4, and then sealing the container by using a cover;
opening a ball milling tank cover 1 of the stirring ball mill, filling 80kg of tungsten carbide grinding balls with the diameter of 5mm into a ball milling tank 2 with the inner lining made of tungsten carbide, taking out a sealed container containing a raw material mixture 4 from a glove box, opening the cover of the sealed container, pouring the raw material mixture 4 into the ball milling tank 2, and covering the ball milling tank cover 1;
continuously introducing nitrogen with the air pressure of 0.1MPa into the ball milling tank cover 1 from a protective gas inlet 5 for 45 minutes, and discharging the air in the ball milling tank 2 through an air outlet 6 on the ball milling tank cover 1;
introducing liquid nitrogen from a liquid nitrogen inlet 7 on the ball milling tank cover 1 discontinuously, and controlling the temperature in the ball milling tank 2 to be-20 to-10 ℃;
setting the rotation speed of a ball mill motor 9 to 400 revolutions per minute, starting the ball mill motor 9 to drive a stirring rod to rotate, wherein the stirring rod 11 made of tungsten carbide penetrates through a sealing ring 10 on a ball mill tank cover 1 from the inside of a ball mill tank 2 to be connected with the motor 9, so that grinding balls 3 are driven to rotate at a high speed to grind a raw material mixture 4;
and stopping introducing liquid nitrogen and nitrogen when the ball mill continuously operates for 12 hours, opening a ball valve switch 13 below a discharge port 12 at the bottom of the ball mill tank, and collecting the synthesized powder at the discharge port 12.
Performing phase analysis on the obtained powder by using an X-ray diffractometer (XRD, bruker D2); the particle size of the obtained powder was measured with a particle size analyzer (Nano Brook Omni); testing the impurity content in the obtained powder by adopting an inductively coupled plasma spectrometer (ICP, PQ 9000); the chemical composition of the obtained powder was tested by scanning electron microscopy (SEM, JEOL JSM-6510) equipped with an energy spectrometer.
The detection result of the powder obtained in this example is: the powder is in an amorphous state; the average particle size of the powder is 3 mu m; the impurity content (the main impurity is Zr) in the powder is about 19ppm; the chemical composition of the powder is Ge 0.203±0.003 As 0.198± 0.003 Se 0.447±0.003 Te 0.152±0.003 。
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (9)
1. The efficient synthesis method of the chalcogenide glass powder is characterized by comprising the following steps:
the first step is as follows: crushing and sieving the elementary raw materials in a glove box to obtain the elementary raw materials with the granularity of less than 500 mu m;
the second step: calculating the mass of each simple substance raw material according to the chemical composition and the mass of the chalcogenide glass powder to be synthesized;
the third step: weighing various simple substance raw materials in a glove box, filling the weighed simple substance raw materials into a clean container, mixing to obtain a raw material mixture (4), and sealing the container by using a cover;
the fourth step: opening a ball milling tank cover (1) of the stirring ball mill, filling grinding balls (3) into the ball milling tank (2), then taking out a sealed container containing the raw material mixture (4) from a glove box, opening the cover of the sealed container, pouring the raw material mixture (4) into the ball milling tank (2), and covering the ball milling tank cover (1);
the fifth step: continuously introducing shielding gas from a shielding gas inlet (5) on the ball milling tank cover (1) for more than 30 minutes, and discharging air in the ball milling tank (2) through a gas outlet (6) on the ball milling tank cover (1);
and a sixth step: introducing liquid nitrogen from a liquid nitrogen inlet (7) on a ball milling tank cover (1) discontinuously, controlling the temperature in the ball milling tank (2) to be-20 to 20 ℃, and monitoring the temperature in the ball milling tank through a thermal resistor (8);
the seventh step: setting the rotating speed of a ball mill motor (9), starting the ball mill motor (9), and driving a stirring rod (11) penetrating through a sealing ring (10) to rotate, so that a grinding ball (3) is driven to rotate at a high speed to grind the raw material mixture (4);
the eighth step: and (3) stopping introducing the liquid nitrogen and the protective gas when the ball mill continuously operates for 8 to 12 hours, opening a ball valve switch (13) below a discharge port (12) at the bottom of the ball mill tank, and collecting the synthesized powder at the discharge port (12).
2. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the components of the chalcogenide glass comprise one or two elements of Ge, as and Sb and one or two elements of S, se and Te.
3. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the purity of the simple substance raw material is not less than 99.999%.
4. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the glove box is filled with dry nitrogen or argon, and the oxygen content of water in the glove box is lower than 0.1ppm.
5. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the lining of the ball milling tank (2), the grinding balls (3) and the stirring rod (11) are all made of tungsten carbide or zirconium oxide.
6. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the mass ratio of the grinding ball (3) to the raw material mixture (4) is 12 to 1.
7. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the diameter of the grinding ball (3) is 5-20 mm.
8. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the rotating speed of the stirring rod (11) is 200 to 400 revolutions per minute.
9. The efficient synthesis method of chalcogenide glass powder according to claim 1, characterized in that: the pressure of the protective gas is 0.02 to 0.1MPa.
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