CN101844229B - Preparation method and production equipment of high-purity antimony particles - Google Patents
Preparation method and production equipment of high-purity antimony particles Download PDFInfo
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- CN101844229B CN101844229B CN2010101312661A CN201010131266A CN101844229B CN 101844229 B CN101844229 B CN 101844229B CN 2010101312661 A CN2010101312661 A CN 2010101312661A CN 201010131266 A CN201010131266 A CN 201010131266A CN 101844229 B CN101844229 B CN 101844229B
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 126
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 239000002245 particle Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 133
- 239000010453 quartz Substances 0.000 claims abstract description 131
- 239000000463 material Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 77
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- 239000003708 ampul Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 10
- 230000008676 import Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 238000012216 screening Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 abstract description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052793 cadmium Inorganic materials 0.000 abstract description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 229910052738 indium Inorganic materials 0.000 abstract description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 229910000838 Al alloy Inorganic materials 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 239000011449 brick Substances 0.000 description 6
- 239000006260 foam Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of high-purity antimony particles, which comprises the following steps of: heating, charging materials, dropping materials and treating antimony particles. The invention also discloses production equipment of high-purity antimony particles, which comprises a vertical resistance furnace, a quartz outer sleeve, a quartz conical hopper and a quartz cooling recycling container, wherein the vertical resistance furnace is electrically connected with electric control equipment; the middle part of the quartz outer sleeve is sleeved in the vertical resistance furnace, and the top end of the quartz outer sleeve is sealed; the quartz conical hopper is nested in the quartz outer sleeve and provided with small holes at the bottom; and the quartz cooling recycling container is positioned below the vertical resistance furnace. Chemical reagents are not used by the invention in the production process, products can not be polluted, the equipment can be operated simply and easily, and the production efficiency is high; 99.999% and 99.9999% of antimony particles produced by the method and the equipment meet the GB10117-88 high-purity antimony particle standard and can be used for partially replacing imported products; and the method and the equipment not only can be used for producing high-purity antimony particles but also can be used for producing granular products of high-purity lead, high-purity tin, high-purity zinc, high-purity cadmium, high-purity indium and the like.
Description
Technical field
The present invention relates to a kind of preparation method and production equipment of high-purity antimony particles, belong to the high pure metal production field.
Background technology
High-purity antimony particles is mainly used in the doped chemical and the multialkali photocathode of semi-conducting material, is semicon industry, scientific research, the indispensable raw material of military project.
The device of original production high pure metal pelletized product is: a quartzy tapered funnel is fixed on the support; Put into tapered funnel to material to be granulated; Tapered funnel below put into one fill with pure water beaker; Heat quartzy tapered funnel with hydrogen lamp, make material melting splash into from funnel that condensation forms granular the pure water; The shortcoming of this method is not protect gas shiled, and material is prone to oxidation, and particle diameter is wayward; Pure water in the beaker is the formation temperature gradient not, and the material of fusing splashes into pure water moment chilling and splits, and is difficult for the granular of formation rule; And this device production efficiency is low, and inconvenience is worked continuously.
Summary of the invention
In view of above situation, the object of the invention provides a kind of preparation method of high-purity antimony particles.
The present invention seeks to realize through the enforcement following technical proposals:
A kind of preparation method of high-purity antimony particles mainly may further comprise the steps:
1) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, the quartzy scope that cools back the following 300mm in receptacle top of heating;
2) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 700～750 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; The first amount of expecting that adds earlier at least 50 grams, every then interval 5min 50-300g that feeds in raw material;
3) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle;
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process;
4) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into.
As optimal way, select quartzy tapered funnel aperture according to antimony grain diameter, the relation in antimony grain diameter and funnel aperture is following:
Antimony grain diameter is Φ 0.5～1.5mm, and selecting the aperture is the funnel of Φ 0.3mm,
Antimony grain diameter is Φ 0.5～2.5mm, and selecting the aperture is the funnel of Φ 0.5mm,
Antimony grain diameter is Φ 1.0～3.0mm, and selecting the aperture is the funnel of Φ 0.8mm,
Antimony grain diameter is Φ 1.0～3.5mm, and selecting the aperture is the funnel of Φ 1.0mm,
Antimony grain diameter is Φ 1.5～4.5mm, and selecting the aperture is the funnel of Φ 1.2mm,
Antimony grain diameter is Φ 2.0～4.5mm, and selecting the aperture is the funnel of Φ 1.5mm.
As optimal way, confirm each feeding quantity according to antimony grain diameter, the relation of each feeding quantity and antimony grain diameter is:
Antimony grain diameter is Φ 0.5～1.5mm, and each feeding quantity is 300 grams,
Antimony grain diameter is Φ 0.5～2.5mm, and each feeding quantity is 250 grams,
Antimony grain diameter is Φ 1.0～2.5mm, and each feeding quantity is 200 grams,
Antimony grain diameter is Φ 1.0～3.5mm, and each feeding quantity is 150 grams,
Antimony grain diameter is Φ 1.5～4.5mm, and each feeding quantity is 100 grams,
Antimony grain diameter is Φ 2.0～4.5mm, and each feeding quantity is 50 grams.
As optimal way, before intensification, need the quartzy outer tube of cleaning, quartzy tapered funnel, quartz to cool back receptacle.
As optimal way, described inert gas is an argon gas.
Another object of the present invention provides a kind of production equipment with the method for preparing high-purity antimony particles, and this goal of the invention realizes through implementing following technical proposals:
A kind of production equipment of high-purity antimony particles comprises that the vertical resistance furnace, the centre that are electrically connected with control panel are set on the quartzy outer tube of vertical resistance furnace inside and end sealing, are nested in that the inner bottom of quartzy outer tube has the quartzy conical hopper of aperture, the quartz that is positioned at vertical resistance furnace below cools back receptacle;
Wherein
Said quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, and quartz ampoule puts outward and is provided with inert gas import.
As optimal way, said quartzy outer tube top seals with quartz crucible.
As optimal way, said vertical resistance furnace set inside has the thermocouple that is electrically connected with control panel.
As optimal way, said quartz cools back receptacle and is provided with water inlet and delivery port.
As optimal way, the hole diameter of said quartzy conical hopper bottom is 0.3-1.5mm.
Table 1 is to produce 99.999% the antimony grain and the comparison of GB GB10117-88 high purity antimony with the inventive method:
Table 1
Table 2 is to produce 99.9999% the antimony grain and the comparison of GB GB10117-88 high purity antimony with the inventive method:
Table 2
Can find out that from above form the high-purity antimony particles of preparing with the inventive method satisfies even is higher than GB GB10117-88 high purity antimony standard.
The present invention does not use any chemical reagent in process of production; Product there is not contamination; And equipment is simple to operation; Production efficiency is high, and 99.999% and 99.9999% antimony grain through above equipment and explained hereafter satisfies GB GB10117-88 high purity antimony section standard, and the diameter that the present invention prepares is used to make the alkali photocathode is that the average yield rate of high-purity antimony particles of 8mg ± 1mg and 27.5mg ± 2.5mg can reach 25%～35%; The diameter that is used for the semi-conducting material doping is that the high-purity antimony particles yield rate of Φ 1.0～Φ 3.0mm can reach 75%～85%; But part substituting import one product, this equipment and technology not only can be produced high-purity antimony particles, can also produce high purity lead, high purity tin, high purity zinc, high purity cadmium, high purity indium equigranular product.
Description of drawings
Fig. 1 is the structure drawing of device of present device.
Wherein 1 is that control panel, 2 is that thermocouple, 3 is that vertical resistance furnace, 4 is that argon gas import, 5 is that silica crucible, 6 is that quartzy outer tube, 7 is that quartzy conical hopper, 8 is that gap, 10 is that water inlet, 11 is a grate for quartz cools back receptacle, 9.
The specific embodiment
Following non-limiting examples is used to explain the present invention
Embodiment 1 preparation diameter is the antimony grain of Φ 0.5～1.5mm
As shown in Figure 1; Vertical resistance furnace is electrically connected with control panel; Control panel 1 is a thyristor controlled thermoregulator; Vertical resistance furnace set inside has the thermocouple 2 that is electrically connected with control panel, realizes the furnace temperature thermostatic control according to thermocouple 2 feedback data by the thermoregulator control silicon controlled angle of flow.The single hop resistance furnace that vertical resistance furnace 3 is made up of aluminium oxide boiler tube, foam and oxidize aluminium insulating brick, resistance wire, aluminium alloy furnace shell; Vertical resistance furnace is cylinder height 500mm, body of heater external diameter 250mm, burner hearth internal diameter diameter 80mm; Vertical resistance furnace is placed on the grate 11; Quartzy outer tube 6 is quartz ampoules of an external diameter 60mm, length 750mm, and it is inner that quartzy outer tube is set on vertical resistance furnace, is being provided with argon gas import 4 apart from quartzy overcoat pipe end 50mm place; Quartzy outer sleeve upper prevents that with quartz crucible 5 sealings of a Φ 90mm argon gas from overflowing.Quartzy outer tube nested inside has quartzy conical hopper; Quartzy tapered funnel 7 is quartz ampoules that an external diameter 45mm, length 350mm, tapered end have Φ 0.3mm aperture; Quartz cools back the quartz ampoule that receptacle 8 is an external diameter 120mm, length 800mm back cover; Be positioned at vertical resistance furnace below; Quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, has gap 9, cools back apart from quartz that the 20mm place has water inlet 10 bottom the receptacle cooling back receptacle upper opening 20mm place apart from quartz.
Use the said equipment to prepare the high-purity antimony particles of diameter as Φ 0.5～1.5mm, step is following:
1) quartzy outer tube, quartzy tapered funnel clean in elder generation before intensification, quartz cools back receptacle makes it reach high-purity production requirement.
2) selecting the aperture is the funnel of Φ 0.3mm, assembles, debugged equipment by accompanying drawing,
3) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, with the quartzy scope that cools back the following 300mm in receptacle top of hydrogen lamp heating;
4) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 700 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; Begin to add the first amount of expecting of at least 50 grams, every then interval 5min 300g that feeds in raw material;
5) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle.
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process.
6) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into;
As shown in Figure 1; Vertical resistance furnace is electrically connected with control panel; Control panel 1 is a thyristor controlled thermoregulator; Vertical resistance furnace set inside has the thermocouple 2 that is electrically connected with control panel, realizes the furnace temperature thermostatic control according to thermocouple 2 feedback data by the thermoregulator control silicon controlled angle of flow.The single hop resistance furnace that vertical resistance furnace 3 is made up of aluminium oxide boiler tube, foam and oxidize aluminium insulating brick, resistance wire, aluminium alloy furnace shell; Vertical resistance furnace is cylinder height 500mm, body of heater external diameter 250mm, burner hearth internal diameter diameter 80mm; Vertical resistance furnace is placed on the grate 11; Quartzy outer tube 6 is quartz ampoules of an external diameter 60mm, length 750mm, and it is inner that quartzy outer tube is set on vertical resistance furnace, is being provided with argon gas import 4 apart from quartzy overcoat pipe end 50mm place; Quartzy outer sleeve upper prevents that with quartz crucible 5 sealings of a Φ 90mm argon gas from overflowing.Quartzy outer tube nested inside has quartzy conical hopper; Quartzy tapered funnel 7 is quartz ampoules that an external diameter 45mm, length 350mm, tapered end have Φ 0.5mm aperture; Quartz cools back the quartz ampoule that receptacle 8 is an external diameter 120mm, length 800mm back cover; Be positioned at vertical resistance furnace below; Quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, has gap 9, cools back apart from quartz that the 20mm place has water inlet 10 bottom the receptacle cooling back receptacle upper opening 20mm place apart from quartz.
Use the said equipment to prepare the high-purity antimony particles of diameter as Φ 0.5～2.5mm, step is following:
1) quartzy outer tube, quartzy tapered funnel clean in elder generation before intensification, quartz cools back receptacle makes it reach high-purity production requirement.
2) selecting the aperture is the funnel of Φ 0.5mm, assembles, debugged equipment by accompanying drawing,
3) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, with the quartzy scope that cools back the following 300mm in receptacle top of hydrogen lamp heating;
4) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 750 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; Begin to add the first amount of expecting of at least 50 grams, every then interval 5min 250g that feeds in raw material;
5) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle.
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process.
6) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into;
As shown in Figure 1; Vertical resistance furnace is electrically connected with control panel; Control panel 1 is a thyristor controlled thermoregulator; Vertical resistance furnace set inside has the thermocouple 2 that is electrically connected with control panel, realizes the furnace temperature thermostatic control according to thermocouple 2 feedback data by the thermoregulator control silicon controlled angle of flow.The single hop resistance furnace that vertical resistance furnace 3 is made up of aluminium oxide boiler tube, foam and oxidize aluminium insulating brick, resistance wire, aluminium alloy furnace shell; Vertical resistance furnace is cylinder height 500mm, body of heater external diameter 250mm, burner hearth internal diameter diameter 80mm; Vertical resistance furnace is placed on the grate 11; Quartzy outer tube 6 is quartz ampoules of an external diameter 60mm, length 750mm, and it is inner that quartzy outer tube is set on vertical resistance furnace, is being provided with argon gas import 4 apart from quartzy overcoat pipe end 50mm place; Quartzy outer sleeve upper prevents that with quartz crucible 5 sealings of a Φ 90mm argon gas from overflowing.Quartzy outer tube nested inside has quartzy conical hopper; Quartzy tapered funnel 7 is quartz ampoules that an external diameter 45mm, length 350mm, tapered end have Φ 0.8mm aperture; Quartz cools back the quartz ampoule that receptacle 8 is an external diameter 120mm, length 800mm back cover; Be positioned at vertical resistance furnace below; Quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, has gap 9, cools back apart from quartz that the 20mm place has water inlet 10 bottom the receptacle cooling back receptacle upper opening 20mm place apart from quartz.
Use the said equipment to prepare the high-purity antimony particles of diameter as Φ 1.0～3.0mm, step is following:
1) quartzy outer tube, quartzy tapered funnel clean in elder generation before intensification, quartz cools back receptacle makes it reach high-purity production requirement.
2) selecting the aperture is the funnel of Φ 0.8mm, assembles, debugged equipment by accompanying drawing,
3) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, with the quartzy scope that cools back the following 300mm in receptacle top of hydrogen lamp heating;
4) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 730 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; Begin to add the first amount of expecting of at least 50 grams, every then interval 5min 150g that feeds in raw material;
5) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle.
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process.
6) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into;
Embodiment 4 preparation diameters are the antimony grain of Φ 1.0～3.5mm
As shown in Figure 1; Vertical resistance furnace is electrically connected with control panel; Control panel 1 is a thyristor controlled thermoregulator; Vertical resistance furnace set inside has the thermocouple 2 that is electrically connected with control panel, realizes the furnace temperature thermostatic control according to thermocouple 2 feedback data by the thermoregulator control silicon controlled angle of flow.The single hop resistance furnace that vertical resistance furnace 3 is made up of aluminium oxide boiler tube, foam and oxidize aluminium insulating brick, resistance wire, aluminium alloy furnace shell; Vertical resistance furnace is cylinder height 500mm, body of heater external diameter 250mm, burner hearth internal diameter diameter 80mm; Vertical resistance furnace is placed on the grate 11; Quartzy outer tube 6 is quartz ampoules of an external diameter 60mm, length 750mm, and it is inner that quartzy outer tube is set on vertical resistance furnace, is being provided with argon gas import 4 apart from quartzy overcoat pipe end 50mm place; Quartzy outer sleeve upper prevents that with quartz crucible 5 sealings of a Φ 90mm argon gas from overflowing.Quartzy outer tube nested inside has quartzy conical hopper; Quartzy tapered funnel 7 is quartz ampoules that an external diameter 45mm, length 350mm, tapered end have Φ 1.0mm aperture; Quartz cools back the quartz ampoule that receptacle 8 is an external diameter 120mm, length 800mm back cover; Be positioned at vertical resistance furnace below; Quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, has gap 9, cools back apart from quartz that the 20mm place has water inlet 10 bottom the receptacle cooling back receptacle upper opening 20mm place apart from quartz.
Use the said equipment to prepare the high-purity antimony particles of diameter as Φ 1.0～3.5mm, step is following:
1) quartzy outer tube, quartzy tapered funnel clean in elder generation before intensification, quartz cools back receptacle makes it reach high-purity production requirement.
2) selecting the aperture is the funnel of Φ 1.0mm, assembles, debugged equipment by accompanying drawing,
3) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, with the quartzy scope that cools back the following 300mm in receptacle top of hydrogen lamp heating;
4) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 720 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; Begin to add the first amount of expecting of at least 50 grams, every then interval 5min 150g that feeds in raw material;
5) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle.
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process.
6) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into;
As shown in Figure 1; Vertical resistance furnace is electrically connected with control panel; Control panel 1 is a thyristor controlled thermoregulator; Vertical resistance furnace set inside has the thermocouple 2 that is electrically connected with control panel, realizes the furnace temperature thermostatic control according to thermocouple 2 feedback data by the thermoregulator control silicon controlled angle of flow.The single hop resistance furnace that vertical resistance furnace 3 is made up of aluminium oxide boiler tube, foam and oxidize aluminium insulating brick, resistance wire, aluminium alloy furnace shell; Vertical resistance furnace is cylinder height 500mm, body of heater external diameter 250mm, burner hearth internal diameter diameter 80mm; Vertical resistance furnace is placed on the grate 11; Quartzy outer tube 6 is quartz ampoules of an external diameter 60mm, length 750mm, and it is inner that quartzy outer tube is set on vertical resistance furnace, is being provided with argon gas import 4 apart from quartzy overcoat pipe end 50mm place; Quartzy outer sleeve upper prevents that with quartz crucible 5 sealings of a Φ 90mm argon gas from overflowing.Quartzy outer tube nested inside has quartzy conical hopper; Quartzy tapered funnel 7 is quartz ampoules that an external diameter 45mm, length 350mm, tapered end have Φ 1.2mm aperture; Quartz cools back the quartz ampoule that receptacle 8 is an external diameter 120mm, length 800mm back cover; Be positioned at vertical resistance furnace below; Quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, has gap 9, cools back apart from quartz that the 20mm place has water inlet 10 bottom the receptacle cooling back receptacle upper opening 20mm place apart from quartz.
Use the said equipment to prepare the high-purity antimony particles of diameter as Φ 1.5～4.5mm, step is following:
1) quartzy outer tube, quartzy tapered funnel clean in elder generation before intensification, quartz cools back receptacle makes it reach high-purity production requirement.
2) selecting the aperture is the funnel of Φ 1.2mm, assembles, debugged equipment by accompanying drawing,
3) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, with the quartzy scope that cools back the following 300mm in receptacle top of hydrogen lamp heating;
4) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 710 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; Begin to add the first amount of expecting of at least 50 grams, every then interval 5min 100g that feeds in raw material;
5) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle.
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process.
6) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into;
As shown in Figure 1; Vertical resistance furnace is electrically connected with control panel; Control panel 1 is a thyristor controlled thermoregulator; Vertical resistance furnace set inside has the thermocouple 2 that is electrically connected with control panel, realizes the furnace temperature thermostatic control according to thermocouple 2 feedback data by the thermoregulator control silicon controlled angle of flow.The single hop resistance furnace that vertical resistance furnace 3 is made up of aluminium oxide boiler tube, foam and oxidize aluminium insulating brick, resistance wire, aluminium alloy furnace shell; Vertical resistance furnace is cylinder height 500mm, body of heater external diameter 250mm, burner hearth internal diameter diameter 80mm; Vertical resistance furnace is placed on the grate 11; Quartzy outer tube 6 is quartz ampoules of an external diameter 60mm, length 750mm, and it is inner that quartzy outer tube is set on vertical resistance furnace, is being provided with argon gas import 4 apart from quartzy overcoat pipe end 50mm place; Quartzy outer sleeve upper prevents that with quartz crucible 5 sealings of a Φ 90mm argon gas from overflowing.Quartzy outer tube nested inside has quartzy conical hopper; Quartzy tapered funnel 7 is quartz ampoules that an external diameter 45mm, length 350mm, tapered end have Φ 1.5mm aperture; Quartz cools back the quartz ampoule that receptacle 8 is an external diameter 120mm, length 800mm back cover; Be positioned at vertical resistance furnace below; Quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, has gap 9, cools back apart from quartz that the 20mm place has water inlet 10 bottom the receptacle cooling back receptacle upper opening 20mm place apart from quartz.
Use the said equipment to prepare the high-purity antimony particles of diameter as Φ 2.0～4.5mm, step is following:
1) quartzy outer tube, quartzy tapered funnel clean in elder generation before intensification, quartz cools back receptacle makes it reach high-purity production requirement.
2) selecting the aperture is the funnel of Φ 1.5mm, assembles, debugged equipment by accompanying drawing,
3) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, with the quartzy scope that cools back the following 300mm in receptacle top of hydrogen lamp heating;
4) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 740 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; Begin to add the first amount of expecting of at least 50 grams, every then interval 5min 50g that feeds in raw material;
5) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle.
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process.
6) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into.
Claims (9)
1. the preparation method of a high-purity antimony particles is characterized in that this method mainly may further comprise the steps:
1) heating
Vertical resistance furnace is heated up; Feed inert gas simultaneously; Make the inner air pressure of quartzy outer tube at 1 more than the standard atmospheric pressure, quartz is cooled back annotate pure water in the receptacle to flooding quartzy outer tube lower end, the quartzy scope that cools back the following 300mm in receptacle top of heating;
2) reinforced
Treat that vertical resistance furnace is warming up to pure water temperature that 700～750 ℃, quartz cool back following 300mm place, receptacle top when being higher than 95 ℃; Add high purity antimony material to the quartzy tapered funnel from quartzy outer tube top; The first amount of expecting that adds earlier at least 50 grams, every then interval 5min 50-300g that feeds in raw material;
3) tear drop
Beginning to splash into quartz after the fusing of antimony material cools back in the receptacle;
In the tear drop process, when the quartzy pure water temperature that cools back following 300mm place, receptacle top reaches more than 95 ℃, stop to heat quartz and cool back receptacle, restart to heat quartz when the pure water temperature that quartz cools back following 300mm place, receptacle top is lower than 90 ℃ and cool back receptacle;
When the temperature of the antimony material upper surface in the container was higher than 35 ℃, from water filling port adding pure water, the overfall discharge from the top of high temperature pure water of container bottom, when the temperature of the antimony material upper surface in the container was lower than 25 °, the benefit that stops pure water being gone in the tear drop process;
4) the antimony grain is handled
The antimony grain that quartz cools back in the receptacle is for use through cleaning, screening, dried with splashing into.
2. the preparation method of high-purity antimony particles according to claim 1, it is characterized in that: select quartzy tapered funnel aperture according to antimony grain diameter, the relation in antimony grain diameter and funnel aperture is following:
Antimony grain diameter is Φ 0.5～1.5mm, and selecting the aperture is the funnel of Φ 0.3mm,
Antimony grain diameter is Φ 0.5～2.5mm, and selecting the aperture is the funnel of Φ 0.5mm,
Antimony grain diameter is Φ 1.0～3.0mm, and selecting the aperture is the funnel of Φ 0.8mm,
Antimony grain diameter is Φ 1.0～3.5mm, and selecting the aperture is the funnel of Φ 1.0mm,
Antimony grain diameter is Φ 1.5～4.5mm, and selecting the aperture is the funnel of Φ 1.2mm,
Antimony grain diameter is Φ 2.0～4.5mm, and selecting the aperture is the funnel of Φ 1.5mm.
3. the preparation method of high-purity antimony particles according to claim 1 is characterized in that: confirm each feeding quantity according to antimony grain diameter, the relation of each feeding quantity and antimony grain diameter is:
Antimony grain diameter is Φ 0.5～1.5mm, and each feeding quantity is 300 grams,
Antimony grain diameter is Φ 0.5～2.5mm, and each feeding quantity is 250 grams,
Antimony grain diameter is Φ 1.0～2.5mm, and each feeding quantity is 200 grams,
Antimony grain diameter is Φ 1.0～3.5mm, and each feeding quantity is 150 grams,
Antimony grain diameter is Φ 1.5～4.5mm, and each feeding quantity is 100 grams,
Antimony grain diameter is Φ 2.0～4.5mm, and each feeding quantity is 50 grams.
4. according to the preparation method of any described high-purity antimony particles of claim 1 to 3, it is characterized in that: the quartzy outer tube of needs cleaning, quartzy tapered funnel, quartz cool back receptacle before intensification.
5. according to the preparation method of any described high-purity antimony particles of claim 1 to 3, it is characterized in that: described inert gas is an argon gas.
6. the production equipment of a high-purity antimony particles is characterized in that: comprise that the vertical resistance furnace, the centre that are electrically connected with control panel are set on the quartzy outer tube of vertical resistance furnace inside and end sealing, are nested in that the inner bottom of quartzy outer tube has the quartzy conical hopper of aperture, the quartz that is positioned at vertical resistance furnace below cools back receptacle;
Wherein
Said quartzy outer tube lower end is stretched into quartz ampoule and is cooled back receptacle inside, and quartz ampoule puts outward and is provided with inert gas import, and
said quartz cools back receptacle and is provided with water inlet and delivery port.
7. the production equipment of high-purity antimony particles according to claim 6, it is characterized in that: said quartzy outer tube top seals with quartz crucible.
8. the production equipment of high-purity antimony particles according to claim 6, it is characterized in that: said vertical resistance furnace set inside has the thermocouple that is electrically connected with control panel.
9. the production equipment of high-purity antimony particles according to claim 6 is characterized in that: the hole diameter of said quartzy conical hopper bottom is 0.3-1.5mm.
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| CN106802083A (en) * | 2015-11-25 | 2017-06-06 | 衡阳恒荣高纯半导体材料有限公司 | A kind of antimony reduction furnace |
| CN109434123B (en) * | 2018-10-26 | 2022-03-22 | 锡矿山闪星锑业有限责任公司 | Device and method for preparing antimony beads |
| CN110303164A (en) * | 2019-06-26 | 2019-10-08 | 有研光电新材料有限责任公司 | The preparation facilities and preparation method of spherical germanium particle |
| CN111482615A (en) * | 2020-05-19 | 2020-08-04 | 郑州机械研究所有限公司 | Bottom leakage casting ultrasonic auxiliary system and bottom leakage casting system |
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