CN110282975A - A kind of Germanium selenide target and preparation method thereof - Google Patents
A kind of Germanium selenide target and preparation method thereof Download PDFInfo
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- CN110282975A CN110282975A CN201910610004.4A CN201910610004A CN110282975A CN 110282975 A CN110282975 A CN 110282975A CN 201910610004 A CN201910610004 A CN 201910610004A CN 110282975 A CN110282975 A CN 110282975A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- C04B2235/40—Metallic constituents or additives not added as binding phase
Abstract
The present invention relates to photoelectric material production technical fields more particularly to a kind of Germanium selenide target and preparation method thereof.The preparation method includes: A) germanium block is heated to 980~1050 DEG C, after heat preservation, obtain germanium liquid；B) heating selenium block is to 230~250 DEG C, after heat preservation, the fusing of selenium block, and instill in the germanium liquid, obtain mixed smelting liquid；C) the mixed smelting liquid is heated into 30~60min after cooling at 980~1050 DEG C and obtains selenium germanium alloy；D the selenium germanium alloy) is subjected to ball milling, obtained selenium germanium powder obtains Germanium selenide target through vacuum heating-press sintering；Step A), B) and C) carried out under conditions of vacuum.The present invention prepares selenium germanium alloy using vacuum drop method, then obtains selenium germanium powder by ball milling, Germanium selenide target then is prepared with vacuum hot-pressing, the Germanium selenide target consistency prepared is higher, differs smaller with theoretical Se content.
Description
Technical field
The present invention relates to photoelectric material production technical fields more particularly to a kind of Germanium selenide target and preparation method thereof.
Background technique
Germanium selenide is applied to photodetection field in periodic table group IVA, Group VIA compound semiconductor more.Common half
The preparation method of conductor compound target generally uses powder metallurgic method.Each elemental powders of this method needs are uniformly mixed or straight
It connects and is sintered with compound powder.The fusing point of germanium is 938.5 DEG C, and the fusing point of selenium is 221 DEG C, and fusing point difference is too big, therefore such as
Fruit directly uses germanium powder and selenium powder to prepare Germanium selenide target, and it is too low to directly result in sintering temperature, target low density, so needing
Synthesize Germanium selenide powder.
Application No. is 201610793216.7 Chinese patents to disclose a kind of preparation method of Germanium selenide powder, this method
Using germanium powder and selenium powder heating and thermal insulation under vacuum conditions, then crushes and be prepared under protection of argon gas.The preparation method has
Following deficiency: 1. need germanium and selenium to be prepared into powder, remix uniformly, due to the specific surface of powder compare it is larger, it is easy
Oxidation；2. needing to use argon gas protection in the process, energy consumption is bigger；3. process is more complicated, powder processed is needed, briquetting and etc.,
Easily cause pollution.
Summary of the invention
In view of this, adopting the technical problem to be solved in the present invention is that provide a kind of Germanium selenide target and preparation method thereof
The Germanium selenide target consistency prepared with preparation method provided by the invention or device is higher, differs smaller with theoretical Se content.
The present invention provides a kind of preparation methods of Germanium selenide target, comprising the following steps:
A) heating germanium block after heat preservation, obtains germanium liquid to 980~1050 DEG C；
B) heating selenium block is to 230~250 DEG C, after heat preservation, the fusing of selenium block, and instill in the germanium liquid, obtain mixed smelting
Liquid；
C) the mixed smelting liquid is heated into 30~60min after cooling at 980~1050 DEG C and obtains selenium germanium alloy；
D the selenium germanium alloy) is subjected to ball milling, obtained selenium germanium powder obtains Germanium selenide target through vacuum heating-press sintering；
Step A), B) and C) carried out under conditions of vacuum.
Preferably, the molar ratio of the germanium block and selenium block is 1:1.01~1.015.
Preferably, step A) in, the time of the heat preservation is 25~30min.
Preferably, step B) in, the rate of the heating is 10~15 DEG C/min；
The time of the heat preservation is 30~90min.
Preferably, step C) in, it is described to be cooled to natural cooling；The temperature after cooling is room temperature.
Preferably, the preparation facilities of the selenium germanium alloy includes:
Cabinet；
The melting pot being set in the cabinet, the germanium block heat in the melting pot；
The quartz funnel being set in the cabinet, the selenium block heat in the quartz funnel；
The quartz funnel is placed in the top of the melting pot, so that described in the melt instillation in the quartz funnel
In melting pot；
First heater, the first heater is for heating the melting pot；
Secondary heating mechanism, the secondary heating mechanism is for heating the quartz funnel.
Preferably, the aperture of the quartz funnel is 0.8~1.2mm.
Preferably, step D) in, the ratio of grinding media to material of the ball milling is 2:1；
The time of the ball milling is 3~6h.
Preferably, step D) in, the temperature of the vacuum heating-press sintering is 550~580 DEG C；The vacuum heating-press sintering
Pressure is 35~55MPa；The time of the vacuum heating-press sintering is 90~120min；The vacuum degree of the vacuum heating-press sintering is small
In 5Pa.
The present invention also provides a kind of Germanium selenide targets of preparation method preparation described above.
The present invention provides a kind of preparation methods of Germanium selenide target, comprising the following steps: A) heating germanium block to 980~
1050 DEG C, after heat preservation, obtain germanium liquid；B) heating selenium block is to 230~250 DEG C, after heat preservation, the fusing of selenium block, and instill the germanium liquid
In, obtain mixed smelting liquid；C the mixed smelting liquid 30~60min) is heated after cooling to obtain at 980~1050 DEG C
Selenium germanium alloy；D the selenium germanium alloy) is subjected to ball milling, obtained selenium germanium powder obtains Germanium selenide target through vacuum heating-press sintering
Material；Step A), B) and C) carried out under conditions of vacuum.The present invention prepares selenium germanium alloy using vacuum drop method, so that germanium block
It is in different temperature and melts respectively with selenium block, wherein selenium block is in low-temperature zone, avoids leading to waving for selenium because vapour pressure is big
Hair amount increases.Selenium germanium powder is obtained by ball milling again, Germanium selenide target then is prepared with vacuum hot-pressing, prepares
Germanium selenide target consistency is higher, differs smaller with theoretical Se content.In addition, preparation method provided by the invention is simple, production
It is high-efficient, impurity will not be introduced, the volatile quantity of selenium is smaller.
The experimental results showed that Se content is close to stoichiometric in Germanium selenide target prepared by the present invention, with theoretical Se content
For difference less than 0.3%, the relative density of Germanium selenide target is greater than 96%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the selenium germanium alloy preparation facilities that one embodiment of the application provides.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of preparation methods of Germanium selenide target, comprising the following steps:
A) heating germanium block after heat preservation, obtains germanium liquid to 980~1050 DEG C；
B) heating selenium block is to 230~250 DEG C, after heat preservation, the fusing of selenium block, and instill in the germanium liquid, obtain mixed smelting
Liquid；
C) the mixed smelting liquid is heated into 30~60min after cooling at 980~1050 DEG C and obtains selenium germanium alloy；
D the selenium germanium alloy) is subjected to ball milling, obtained selenium germanium powder obtains Germanium selenide target through vacuum heating-press sintering；
Step A), B) and C) carried out under conditions of vacuum.
The raw material that preparation method provided by the invention is used is germanium block and selenium block.The present invention is pure to the germanium block and selenium block
Degree has no special limitation.The present invention has no special limitation to the source of the germanium block and selenium block, can be general commercially available.?
In certain embodiments of the present invention, the molar ratio of the germanium block and selenium block is 1:1.01~1.02.In certain embodiments, described
The molar ratio of germanium block and selenium block is 1:1.01,1:1.012 or 1:1.015.
The present invention first heats germanium block to 980~1050 DEG C, after heat preservation, obtains germanium liquid.
The present invention has no special limitation to the rate of heat addition of heating germanium block, using germanium block well known to those skilled in the art
The rate of heat addition.
In the present invention, germanium block is heated to 980~1050 DEG C.In certain embodiments of the present invention, germanium block is heated to 1050
DEG C, 1000 DEG C or 980 DEG C.
In certain embodiments of the present invention, the time of the heat preservation is 25~30min.In certain embodiments, described
The time of heat preservation is 25min or 30min.
In certain embodiments of the present invention, the germanium block heats in melting pot obtains germanium liquid.
After obtaining germanium liquid, selenium block is heated to 230~250 DEG C, and after heat preservation, selenium block melts, and instills in the germanium liquid, obtains
Mixed smelting liquid.
In the present invention, selenium block is heated to 230~250 DEG C.In certain embodiments of the present invention, the selenium block is heated to
230 DEG C, 240 DEG C or 250 DEG C.
In certain embodiments of the present invention, the rate of heat addition for heating selenium block is 10~15 DEG C/min.In some embodiments
In, the rate of heat addition is 15 DEG C/min, 12 DEG C/min or 10 DEG C/min.
In certain embodiments of the present invention, after selenium block is heated to 230~250 DEG C, the time of heat preservation is 30~90min.
In certain embodiments, the time of the heat preservation is 60min, 90min or 30min.After the heat preservation, selenium block can melt completely
Change, and instill in the germanium liquid, obtains mixed smelting liquid.
In certain embodiments of the present invention, the selenium block heats in quartz funnel obtains selenium liquid, and selenium liquid passes through quartz
Funnel instills in the melting pot, obtains mixed smelting liquid.
The mixed smelting liquid is heated into 30~60min after cooling at 980~1050 DEG C and obtains selenium germanium alloy.
Temperature after the heating temperature of the mixed smelting liquid is heated with germanium block is identical, is 980~1050 DEG C.In the present invention
Some embodiments in, the heating temperature of the mixed smelting liquid is 1050 DEG C, 1000 DEG C or 980 DEG C.The mixed smelting liquid
Heating time be 30~60min.In certain embodiments of the present invention, the heating time of the mixed smelting liquid be 40min,
30min or 50min.
In certain embodiments of the present invention, described to be cooled to natural cooling, the temperature after cooling is room temperature.
In the present invention, step A), B) and C) carried out under conditions of vacuum.Specifically, it is preferred that are as follows: start in step A)
Before, system is vacuumized, so that the vacuum degree of system is less than 3Pa.In certain embodiments, the vacuum degree of the system is 2Pa
Or 2.5Pa.
In certain embodiments of the present invention, the preparation facilities of the selenium germanium alloy is that vacuum drips device.It preferably includes:
Cabinet；
The melting pot being set in the cabinet, the germanium block heat in the melting pot；
The quartz funnel being set in the cabinet, the selenium block heat in the quartz funnel；
The quartz funnel is placed in the top of the melting pot, so that described in the melt instillation in the quartz funnel
In melting pot；
First heater, the first heater is for heating the melting pot；
Secondary heating mechanism, the secondary heating mechanism is for heating the quartz funnel.
The preparation facilities of the selenium germanium alloy is as shown in Figure 1.Fig. 1 is the selenium germanium alloy that one embodiment of the present of invention provides
The structural schematic diagram of preparation facilities.Wherein, 1 is cabinet, and 1-1 is case body, and 1-2 is case lid, and 2 be melting pot, and 3 be quartz leakage
Bucket, 4 be first heater, and 5 be secondary heating mechanism.
In certain embodiments of the present invention, the cabinet is preferably to be made up of the quartz plate of 3~5mm thickness of welding.
The cabinet is preferably cube shaped.In one embodiment of the invention, the cabinet 1 is cuboid, including case body 1-1
With case lid 1-2, as shown in Figure 1.
In certain embodiments of the present invention, the case body and case lid are sealed by vacuum flange.The present invention is to institute
The type for stating vacuum flange has no special limitation, can be general commercially available.
In an embodiment of the present invention, the preparation facilities further includes vacuum pump, for providing vacuum ring to the cabinet
Border.The present invention has no special limitation to the connection type of the vacuum pump and cabinet, can provide vacuum environment to cabinet and be
It can.In some embodiment of the invention, be provided with vacuum orifice on the case lid of the cabinet, the vacuum orifice with it is described
Vacuum pump is connected.The present invention has no special limitation to the type of the vacuum pump, can be general commercially available.
When starting operation, case lid is opened, germanium block is placed in melting pot, selenium block is placed in quartz funnel, closed
Closed box lid covers upper vacuum flange between case body and case lid, vacuumizes.
The preparation facilities of the selenium germanium alloy further includes melting pot 2.Melting pot is set in the cabinet, the germanium
Block heats in the melting pot.The present invention has no special limitation, Neng Gourong to the type and size of the melting pot
Receive required mixed smelting liquid.
The preparation facilities of the selenium germanium alloy further includes quartz funnel 3.Quartz funnel is set in the cabinet, the selenium
Block heats in the quartz funnel.The present invention has no special limitation to the size of the quartz funnel, in certain of the invention
In a little embodiments, the aperture of the quartz funnel is 0.8~1.2mm.In certain embodiments, the aperture of the quartz funnel is
0.8mm, 1mm or 1.2mm.
In the present invention, the quartz funnel is placed in the top of the melting pot, so that the fusing in the quartz funnel
Drop enters in the melting pot.
The present invention has no special limitation to the size of the cabinet, in certain embodiments of the present invention, the melt
The vertical distance of crucible and quartz funnel is 50~70cm.In certain embodiments, the melting pot and quartz funnel is perpendicular
Straight distance is 65cm.
The preparation facilities of the selenium germanium alloy further includes first heater.The first heater is described for heating
Melting pot.The present invention has no special limitation to the installation site of the first heater, can heat the melt earthenware
Crucible.In certain embodiments of the present invention, the outer wall on the cabinet top is arranged in the first heater.The present invention
Special limitation is had no to the structure of the first heater, it, can using heating device well known to those skilled in the art
The melting pot is heated to required temperature.In certain embodiments of the present invention, the first heater is city
The high-temperature heater sold is specifically as follows the high-temperature heater of highly dense Pood Electronics Equipment Co., Ltd production.
The preparation facilities of the selenium germanium alloy further includes secondary heating mechanism.The secondary heating mechanism is described for heating
Quartz funnel.The present invention has no special limitation to the installation site of the secondary heating mechanism, can heat the quartz leakage
Bucket.In certain embodiments of the present invention, the outer wall of the lower box is arranged in the secondary heating mechanism.The present invention
Special limitation is had no to the structure of the secondary heating mechanism, it, can using heating device well known to those skilled in the art
The quartz funnel is heated to required temperature.In certain embodiments of the present invention, the secondary heating mechanism is city
The low-temperature heat furnace sold is specifically as follows the low-temperature heat furnace of highly dense Pood Electronics Equipment Co., Ltd production.
In specific operation, the germanium block in first heater heating melting pot is first passed through to 980~1050 DEG C, is kept the temperature
Afterwards, germanium liquid is obtained；Again by the selenium block in secondary heating mechanism heated quartz funnel to 230~250 DEG C, after heat preservation, selenium block is molten
Change, and instilled in melting pot by quartz funnel, mixed smelting liquid is obtained in the melting pot；Add finally by second
The mixed smelting liquid is heated at 980~1050 DEG C 30~60min after cooling and obtains selenium germanium alloy by thermal.The present invention
Selenium germanium alloy is prepared using vacuum drippage device, so that germanium block and selenium block are in different temperature respectively and melt, wherein
Selenium block is in low-temperature zone, avoids causing the volatile quantity of selenium to increase because vapour pressure is big.
After obtaining selenium germanium alloy, the selenium germanium alloy is subjected to ball milling, obtained selenium germanium powder is obtained through vacuum heating-press sintering
To Germanium selenide target.
The present invention has no special limitation to the method for the ball milling, using ball grinding method well known to those skilled in the art
?.In certain embodiments of the present invention, the ratio of grinding media to material of the ball milling is 2~3:1.In certain embodiments, the ball milling
Ratio of grinding media to material be 2:1.
In certain embodiments of the present invention, the time of the ball milling is 3~6h.In certain embodiments, the ball milling
Time be 5h, 6h or 3h.
In certain embodiments of the present invention, the ball milling carries out in tumbling ball mill.
In certain embodiments of the present invention, the temperature of the vacuum heating-press sintering is 550~580 DEG C；The Vacuum Heat
The pressure of pressure sintering is 35~55MPa；The time of the vacuum heating-press sintering is 90~120min；The vacuum heating-press sintering
Vacuum degree is less than 5Pa.
In certain embodiments, the temperature of the vacuum heating-press sintering is 580 DEG C, 560 DEG C or 550 DEG C；The Vacuum Heat
The pressure of pressure sintering is 35MPa, 55MPa or 50MPa；The time of the vacuum heating-press sintering is 120min or 100min；It is described
The vacuum degree of vacuum heating-press sintering is 4.5Pa, 4Pa or 3Pa.
In certain embodiments of the present invention, the vacuum heating-press sintering carries out in hot pressing furnace.Specifically, it is preferred that are as follows:
Selenium germanium powder after ball milling is fitted into graphite jig, is subsequently placed in hot pressing furnace and carries out vacuum heating-press sintering.
The present invention also provides a kind of Germanium selenide targets of preparation method preparation described above.Selenizing provided by the invention
Germanium target consistency is higher, differs smaller with theoretical Se content.
The experimental results showed that Se content is close to stoichiometric in Germanium selenide target prepared by the present invention, with theoretical Se content
For difference less than 0.3%, the relative density of Germanium selenide target is greater than 96%.
The present invention provides a kind of preparation methods of Germanium selenide target, comprising the following steps: A) heating germanium block to 980~
1050 DEG C, after heat preservation, obtain germanium liquid；B) heating selenium block is to 230~250 DEG C, after heat preservation, the fusing of selenium block, and instill the germanium liquid
In, obtain mixed smelting liquid；C the mixed smelting liquid 30~60min) is heated after cooling to obtain at 980~1050 DEG C
Selenium germanium alloy；D the selenium germanium alloy) is subjected to ball milling, obtained selenium germanium powder obtains Germanium selenide target through vacuum heating-press sintering
Material；Step A), B) and C) carried out under conditions of vacuum.The present invention prepares selenium germanium alloy using vacuum drop method, so that germanium block
It is in different temperature and melts respectively with selenium block, wherein selenium block is in low-temperature zone, avoids leading to waving for selenium because vapour pressure is big
Hair amount increases.Selenium germanium powder is obtained by ball milling again, Germanium selenide target then is prepared with vacuum hot-pressing, prepares
Germanium selenide target consistency is higher, differs smaller with theoretical Se content.In addition, preparation method provided by the invention is simple, production
It is high-efficient, impurity will not be introduced, the volatile quantity of selenium is smaller.
The experimental results showed that Se content is close to stoichiometric in Germanium selenide target prepared by the present invention, with theoretical Se content
For difference less than 0.3%, the relative density of Germanium selenide target is greater than 96%.
In order to further illustrate the present invention, below with reference to embodiment to a kind of Germanium selenide target provided by the invention and its system
Preparation Method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Raw material used in following embodiment is general commercially available.
Embodiment 1
Selenium germanium alloy is prepared using preparation facilities as shown in Figure 1:
The cabinet of cuboid: vacuum orifice, the vacuum orifice and vacuum pump are provided on the case lid of the cabinet
It is connected；
The melting pot being set in the cabinet, the germanium block heat in the melting pot；
The quartz funnel (aperture of the quartz funnel is 0.8mm) being set in the cabinet, the selenium block is described
It is heated in quartz funnel；
The quartz funnel is placed in the top of the melting pot, so that described in the melt instillation in the quartz funnel
In melting pot；The vertical distance of the melting pot and quartz funnel is 65cm.
First heater (i.e. high-temperature heater), the first heater is for heating the melting pot；It is described
The outer wall on the cabinet top is arranged in first heater；
Secondary heating mechanism (i.e. low-temperature heat furnace), the secondary heating mechanism is for heating the quartz funnel；It is described
The outer wall of the lower box is arranged in secondary heating mechanism.
Specific operation:
Case lid is opened, germanium block is placed in melting pot, selenium block is placed in quartz funnel, case lid is closed, in case
Vacuum flange is put between body and case lid, the vacuum degree vacuumized is 2Pa.The molar ratio of germanium block and selenium block is 1:1.01.
First heater is opened, heating temperature keeps the temperature 25min, obtain germanium liquid to 1050 DEG C；It is then turned on the second heating
Device is heated to 230 DEG C with 15 DEG C/min, keeps the temperature 60min, the fusing of selenium block, and instill in the germanium liquid, obtains mixed smelting
Liquid.
Secondary heating mechanism is closed, the mixed smelting liquid is heated 60min at 1050 DEG C by first heater, then
It closes first heater and obtains selenium germanium alloy by the mixed smelting liquid with furnace cooled to room temperature.
The selenium germanium alloy is subjected to ball milling (ratio of grinding media to material of ball milling is 2:1), the time of ball milling is 5h, obtains selenium germanium powder
End；
The selenium germanium powder is fitted into graphite jig, is subsequently placed in hot pressing furnace and carries out vacuum heating-press sintering, obtain selenium
Change germanium target.The temperature of vacuum heating-press sintering is 580 DEG C, and the pressure of the vacuum heating-press sintering is 35MPa, the vacuum hotpressing
The time of sintering is 120min, and the vacuum degree of the vacuum heating-press sintering is 4.5Pa.
Using the Se content in titration test Germanium selenide target, using the density of drainage test Germanium selenide target.
The experimental results showed that the Se content in the present embodiment in Germanium selenide target is 52.10wt%, with theoretical Se content
(52.09wt%) difference 0.02%；The relative density of Germanium selenide target is 97.2%.
Embodiment 2
Selenium germanium alloy is prepared using preparation facilities as shown in Figure 1, difference from Example 1 is: the quartz leakage
The aperture of bucket is 1mm.
Specific operation:
Case lid is opened, germanium block is placed in melting pot, selenium block is placed in quartz funnel, case lid is closed, in case
Vacuum flange is put between body and case lid, the vacuum degree vacuumized is 2.5Pa.The molar ratio of germanium block and selenium block is 1:1.012.
First heater is opened, heating temperature keeps the temperature 30min, obtain germanium liquid to 1000 DEG C；It is then turned on the second heating
Device is heated to 240 DEG C with 12 DEG C/min, keeps the temperature 90min, the fusing of selenium block, and instill in the germanium liquid, obtains mixed smelting
Liquid.
Secondary heating mechanism is closed, the mixed smelting liquid is heated 30min at 1000 DEG C by first heater, then
It closes first heater and obtains selenium germanium alloy by the mixed smelting liquid with furnace cooled to room temperature.
The selenium germanium alloy is subjected to ball milling (ratio of grinding media to material of ball milling is 2:1), the time of ball milling is 6h, obtains selenium germanium powder
End；
The selenium germanium powder is fitted into graphite jig, is subsequently placed in hot pressing furnace and carries out vacuum heating-press sintering, obtain selenium
Change germanium target.The temperature of vacuum heating-press sintering is 560 DEG C, and the pressure of the vacuum heating-press sintering is 55MPa, the vacuum hotpressing
The time of sintering is 100min, and the vacuum degree of the vacuum heating-press sintering is 4Pa.
Using the Se content in titration test Germanium selenide target, using the density of drainage test Germanium selenide target.
The experimental results showed that the Se content in the present embodiment in Germanium selenide target is 51.95wt%, with theoretical Se content phase
Poor 0.27%；The relative density of Germanium selenide target is 96.8%.
Embodiment 3
Selenium germanium alloy is prepared using preparation facilities as shown in Figure 1, difference from Example 1 is: the quartz leakage
The aperture of bucket is 1.2mm.
Specific operation:
Case lid is opened, germanium block is placed in melting pot, selenium block is placed in quartz funnel, case lid is closed, in case
Vacuum flange is put between body and case lid, the vacuum degree vacuumized is 2Pa.The molar ratio of germanium block and selenium block is 1:1.015.
First heater is opened, heating temperature keeps the temperature 30min, obtain germanium liquid to 980 DEG C；It is then turned on the second heating
Device is heated to 250 DEG C with 10 DEG C/min, keeps the temperature 30min, the fusing of selenium block, and instill in the germanium liquid, obtains mixed smelting
Liquid.
Secondary heating mechanism is closed, the mixed smelting liquid is heated 50min at 980 DEG C by first heater, then
It closes first heater and obtains selenium germanium alloy by the mixed smelting liquid with furnace cooled to room temperature.
The selenium germanium alloy is subjected to ball milling (ratio of grinding media to material of ball milling is 2:1), the time of ball milling is 3h, obtains selenium germanium powder
End；
The selenium germanium powder is fitted into graphite jig, is subsequently placed in hot pressing furnace and carries out vacuum heating-press sintering, obtain selenium
Change germanium target.The temperature of vacuum heating-press sintering is 550 DEG C, and the pressure of the vacuum heating-press sintering is 50MPa, the vacuum hotpressing
The time of sintering is 100min, and the vacuum degree of the vacuum heating-press sintering is 3Pa.
Using the Se content in titration test Germanium selenide target, using the density of drainage test Germanium selenide target.
The experimental results showed that the Se content in the present embodiment in Germanium selenide target is 52.13wt%, with theoretical Se content phase
Poor 0.08%；The relative density of Germanium selenide target is 96.5%.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of preparation method of Germanium selenide target, which comprises the following steps:
A) heating germanium block after heat preservation, obtains germanium liquid to 980~1050 DEG C；
B) heating selenium block is to 230~250 DEG C, after heat preservation, the fusing of selenium block, and instill in the germanium liquid, obtain mixed smelting liquid；
C) the mixed smelting liquid is heated into 30~60min after cooling at 980~1050 DEG C and obtains selenium germanium alloy；
D the selenium germanium alloy) is subjected to ball milling, obtained selenium germanium powder obtains Germanium selenide target through vacuum heating-press sintering；
Step A), B) and C) carried out under conditions of vacuum.
2. preparation method according to claim 1, which is characterized in that the molar ratio of the germanium block and selenium block be 1:1.01~
1.015。
3. preparation method according to claim 1, which is characterized in that step A) in, time of the heat preservation is 25~
30min。
4. preparation method according to claim 1, which is characterized in that step B) in, the rate of the heating is 10~15
℃/min；
The time of the heat preservation is 30~90min.
5. preparation method according to claim 1, which is characterized in that step C) in, it is described to be cooled to natural cooling；It is described
Temperature after cooling is room temperature.
6. preparation method according to claim 1, which is characterized in that the preparation facilities of the selenium germanium alloy includes:
Cabinet；
The melting pot being set in the cabinet, the germanium block heat in the melting pot；
The quartz funnel being set in the cabinet, the selenium block heat in the quartz funnel；
The quartz funnel is placed in the top of the melting pot, so that the melt in the quartz funnel instills the melt
In crucible；
First heater, the first heater is for heating the melting pot；
Secondary heating mechanism, the secondary heating mechanism is for heating the quartz funnel.
7. preparation method according to claim 6, which is characterized in that the aperture of the quartz funnel is 0.8~1.2mm.
8. preparation method according to claim 1, which is characterized in that step D) in, the ratio of grinding media to material of the ball milling is 2:1；
The time of the ball milling is 3~6h.
9. preparation method according to claim 1, which is characterized in that step D) in, the temperature of the vacuum heating-press sintering
It is 550~580 DEG C；The pressure of the vacuum heating-press sintering is 35~55MPa；The time of the vacuum heating-press sintering be 90~
120min；The vacuum degree of the vacuum heating-press sintering is less than 5Pa.
10. the Germanium selenide target of preparation method preparation described in any one of claim 1 to 9.
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