CN107779614A - A kind of method that atmospheric area melting prepares high purity indium - Google Patents
A kind of method that atmospheric area melting prepares high purity indium Download PDFInfo
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- CN107779614A CN107779614A CN201710994910.XA CN201710994910A CN107779614A CN 107779614 A CN107779614 A CN 107779614A CN 201710994910 A CN201710994910 A CN 201710994910A CN 107779614 A CN107779614 A CN 107779614A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
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Abstract
The invention discloses a kind of method that atmospheric area melting prepares high purity indium.（1）With the smart indium of industry（99.99%）For raw material, high vacuum is substituted with high-purity argon gas or other inert gases；（2）Accurately melting zone is controlled to move using the numerical control kind of drive；（3）Energy consumption is reduced with the high contact heating of heat transfer efficiency；（4）Multi-stove bodies, more molten bath smelting devices are designed, improves zone refining yield；（5）Using smelting device of the present invention as operating unit, expanded production by parallel connection, reduce production cost, improved production efficiency and equipment automatization is horizontal, adapt to the needs of industrialized production.
Description
Technical field
The present invention relates to the method that a kind of melting of contact heating atmospheric area prepares high purity indium.
Background technology
Indium（In）It is silvery white and slightly nattier blue metal, plasticity is strong, there is ductility, can be pressed into piece, be mainly used in
Manufacture the fields such as ITO, semiconductor, electric light source, low-melting alloy, bearing metal.Wherein, electronics, information industry usually require pure
Spend 5N（99.999%）High purity indium above.The purification mode of high purity indium mainly includes sublimed method, zone melting method, vacuum distillation
Method, extraction and electrorefining etc..Wherein, zone refining is by the long and narrow metal charge ingot of local heating, makes material ingot shape into one
Or the melting zone of multiple isolation（Abbreviation melting zone）.Mechanical device is used to make melting zone with several millimeters per hour of speed along assigned direction
It is slowly mobile, using the difference of impurity equilibrium concentration between solid phase and liquid phase, make impurity segregation into solid phase or liquid phase.To be terrible
To the metal material of high-purity, this process generally requires to repeat 15-20 times, and final impurity enriched is middle in the both ends of material ingot
Part is required high pure metal.
At present, zone refining prepares the problem of high pure metal indium is primarily present three aspects, first, generally using high vacuum ring
Border carries out zone refining, and corresponding equipment requirement and production cost are very high；Second, mode of heating is usually coil（It is non-contact
Formula）Heating, energy efficiency is low, and has certain electromagnetic radiation；Third, equipment capacity is relatively low, area's melting apparatus material ingot per treatment
Measure limited and very long the time required to completion zone refining.These problems have impact on zone refining method in high purity indium preparation
Using.The present invention proposes a kind of method that atmospheric area melting of more material ingots, more melting zones prepares high purity indium, and is added using contact
Heat improves energy utilization efficiency, can significantly improve the production efficiency of area smelting refinement indium, reduces equipment and production cost, just
In industrialized production.This method has no report at present.
The content of the invention
It is an object of the present invention to provide the method that a kind of melting of contact heating atmospheric area prepares high purity indium, overcome
Existing zone refining prepares problem present in high purity indium technique.It is mainly characterized by：（1）With high-purity argon gas or other inertia
Gas instead high vacuum；（2）Accurately melting zone is controlled to move using the numerical control kind of drive；（3）Added with the contact that heat transfer efficiency is high
Heat drop low energy consumption；（4）Multi-stove bodies, more molten bath smelting devices are designed, improves zone refining yield；（5）With smelting device of the present invention
For operating unit, expanded production by parallel connection, adapt to the needs of large-scale production, reduce production cost, improve zone refining technique
Practicality and stability.
Concretely comprise the following steps：
1. by industrial electrolysis essence indium 4N（99.99%）After melting sources, pour into the quartz boat that length is 300~2000 mm, casting
Into elongated indium ingot.
2. opening the hermatic door of smelting device side, one or more quartz boats are placed on copper heat-transfer foundation support specific bit
Put, and keep being in close contact with copper-based seat.
3. heater is made up of electric heating sheets and graphite flake, wherein graphite flake thickness is 10~20 mm, electric heating sheets
Graphite flake side is fixed on, away from the mm of bottom 8~20；Heater is fixed on the crossbearer of numerical control mobile device, and is ensured molten
The graphite flake bottom of heater and indium ingot surface good contact during refining.
4. closing the hermatic door of smelting device side, tighten screw and check air-tightness；Sealing starts to change after meeting the requirements
Gas；Vavuum pump pumping is opened, valve is closed when to pressure being 0.06~0.1Pa；Then open valve and be passed through high-purity argon gas（>
99.9995%）, keep pressure（0.1~0.15 MPa）5~10 minutes；It is final to keep high after repeating above-mentioned ventilation operation three times
Pure argon pressure is 0.1~0.15 MPa, prepares start region melting.
5. starting temperature controller, it is 150~300 to control heater temperature oC, after observation melting zone width meets the requirements, according to
Setting program start region melting.Heater is at the uniform velocity moved from left to right with 5~50 mm/h speed, is added during to low order end
Thermal is with crossbearer lifting；After all heaters all shift to indium ingot low order end lifting, crossbearer return to origin, restart area
Domain melting.Operation 10~20 times more than being repeated under programme-control；In the process, it is 0.1~0.15 MPa to keep ar pressure.
6. closing temperature controller power supply, heater returns to initial position under programme-control, in lifting state.Keep argon gas
Air pressure is 0.1~0.15 MPa, and room temperature is cooled to indium ingot.
7. indium metal is taken out, the high surface portion of impurity content is removed in glove box, according to impurity in indium ingot length side
The upward regularity of distribution, the higher two end portions of impurity content are sliced off, remaining high pure metal indium is packed.
The atmospheric area method of smelting of the present invention has that equipment is low with production cost, energy utilization efficiency is high, is easily achieved
The features such as multi-stove bodies, more melting zones are refined, can improve production efficiency and equipment automatization is horizontal, be adapted to industrial applications.
Brief description of the drawings
Fig. 1 is contact heating double-furnace-body double of the present invention, double melting zone high purity indium zone refining equipment schematic diagrams.Wherein：A-area
Molten beginning state, the 1st group of calandria decline contact indium ingot, and the 2nd group is in lifting position；B-area was melting between the departure date, two groups of heating
Device is in decline state, and 2 melting zones are respectively formed in the diverse location of 2 indium ingots.
Fig. 2 is the beam lifting control unit schematic diagram of the fixed heater of the present invention.
Marked in figure：1- hermatic doors；2- quartz boats；3- indium ingots；4- graphite flakes；5- vacuum chambers；6- electric heating sheets；7- copper
Exchange heat pedestal；8- crossbearers；9- crawler belts；10- stepper motors.
Embodiment
Embodiment 1：（Single body of heater, single melting zone are refined）
Zone refining method according to the present invention carries out high purity indium refinement, and its specific implementation step is：
1. the purity that industrial electrolysis is obtained is 4N（99.99%）Indium metal fusing after, pour into length be 1000 mm quartz
In boat, elongated indium ingot is cast.
2. opening sealing vacuum box goalkeeper's quartz boat is placed on atmospheric area smelting equipment correspondence position, keep close with copper-based seat
Contact.
3. heater is made up of electric heating sheets and graphite flake, wherein graphite flake thickness is 10 mm, and electric heating sheets are fixed on
Graphite flake side, away from the mm of bottom 10.Heater is fixed on the crossbearer of mobile controller, and is ensured in fusion process
The graphite flake bottom of heater and indium ingot surface good contact.
4. closing vacuum box hermetic door, tighten screw and check air-tightness.Sealing starts to take a breath after meeting the requirements.Open
Vavuum pump is evacuated, and valve is closed when to pressure being 0.07Pa；Then open valve and be passed through high-purity argon gas（>99.9995%）, keep
Pressure（0.12 MPa）8 minutes.After repeating above-mentioned ventilation operation three times, it is 0.12 MPa to keep high-purity argon gas pressure, is prepared out
Beginning zone refining.
5. starting temperature controller, it is 200 to control heater temperature oC, after observation melting zone width meets the requirements, according to setting
Program start region melting.Heater is at the uniform velocity moved from left to right with 30 mm/h speed, to stepper motor band during low order end
Dynamic crawler belt, which rotates, makes crossbearer lifting, is then back to starting point, restarts zone refining.Operation 16 more than being repeated under programme-control
It is secondary.In the process, it is 0.12 MPa to keep ar pressure.
6. closing temperature controller power supply, heater returns to initial position under programme-control, in lifting state.Keep argon gas
Air pressure is cooled to room temperature for 0.12MPa to indium ingot.
7. opening sealing vacuum box goalkeeper indium metal to take out, the high surface portion of impurity content, root are removed in glove box
According to the regularity of distribution of the impurity on indium ingot length direction, the higher two end portions of impurity content are sliced off, by remaining high pure metal
Indium packs.
Described above, only embodiments of the invention are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow conversion that bright specification and accompanying drawing content are made, or directly or indirectly it is used in other related skills
Art field, all should similarly it be included within the scope of the present invention.
Embodiment 2：（Double-furnace-body double, double melting zones）
Zone refining method according to the present invention has carried out the refinement of high purity indium, and its specific implementation step is：
1. the purity that industrial electrolysis is obtained is 4N（99.99%）Indium metal fusing after, pour into two 1000 mm of length stone
In Ying Zhou, elongated indium ingot is cast.
2. opening sealing vacuum box two quartz boats of goalkeeper is placed on atmospheric area smelting equipment correspondence position, keep and copper-based seat
It is in close contact.
3. graphite heating device is made up of 4 groups of electric heating sheets and graphite flake, wherein graphite flake thickness is 10 mm, electrical heating
Piece is fixed on graphite flake side, away from the mm of bottom 10.2 crossbearers that heater is separately fixed at mobile controller correspond to position
Put, and ensure graphite flake bottom and indium ingot surface good contact.
4. closing vacuum box hermetic door, tighten screw and check air-tightness.Sealing starts to take a breath after meeting the requirements.Open
Vavuum pump is evacuated, and valve is closed when to pressure being 0.07Pa；Then open valve and be passed through high-purity argon gas（>99.9995%）, keep
Pressure（0.12 MPa）8 minutes.After repeating above-mentioned ventilation operation three times, it is 0.12 MPa to keep high-purity argon gas pressure, is prepared out
Beginning zone refining.
5. starting temperature controller, 4 heater temperature of control are 200 oC, the 1st group of heater decline contact indium first
Ingot left end, after observation melting zone width meets the requirements, according to setting program start region melting.2nd group of heater is located at the 1st group
Behind heater, now programme-control is in lifting state（Such as Fig. 1 a）.Two groups of heaters are with the mutually synchronized of 30 mm/h
Degree at the uniform velocity moves from left to right, automatic when reaching indium ingot left position to the 2nd group of heater to decline contact indium ingot.Hereafter, two
Group heater continues at the uniform velocity to move from left to right with 30 mm/h identical speed, forms double-furnace-body double, double melting zones smelt（Such as figure
1b）.Its automatic lifting when the 1st group of heater reaches indium ingot low order end, and continue to move right with 30 mm/h speed；
Its automatic lifting when the 2nd group of heater reaches indium ingot low order end, is then returned initially together with first group of heater
Position, restart zone refining.Operation 15 times more than being repeated under programme-control.In the process, holding ar pressure is
0.12 MPa。
6. closing temperature controller power supply, two groups of heaters return to initial position under programme-control, in lifting state.Keep
Ar pressure is cooled to room temperature for 0.12MPa to indium ingot.
7. opening sealing vacuum box goalkeeper indium metal to take out, the high surface portion of impurity content is removed in glove box, according to
The regularity of distribution of the impurity on indium ingot length direction, slices off the higher two end portions of impurity content, by remaining high pure metal indium
Pack.
Described above, only embodiments of the invention are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow conversion that bright specification and accompanying drawing content are made, or directly or indirectly it is used in other related skills
Art field, all should similarly it be included within the scope of the present invention.
Claims (4)
1. a kind of method that atmospheric area melting prepares high purity indium, it is characterised in that concretely comprise the following steps：
（1）After industrial electrolysis essence indium 4N melting sources, pour into the quartz boat that length is 300~2000 mm, cast elongated
Indium ingot；
（2）The hermatic door of smelting device side is opened, one or more quartz boats are placed in copper heat-transfer foundation support specified location,
And keep being in close contact with copper-based seat；
（3）Heater is made up of electric heating sheets and graphite flake, and wherein graphite flake thickness is 10~20 mm, and electric heating sheets are fixed
In graphite flake side, away from the mm of bottom 8~20；Heater is fixed on the crossbearer of numerical control mobile device, and is ensured in melting
The graphite flake bottom of heater and indium ingot surface good contact in journey；
（4）The hermatic door of smelting device side is closed, screw is tightened and checks air-tightness；Sealing starts to take a breath after meeting the requirements；
Vavuum pump pumping is opened, valve is closed when to pressure being 0.06~0.1Pa；Then open valve and be passed through purity>99.9995%
Argon gas, it is 0.1~0.15 MPa to keep 5~10 minutes pressure；After repeating above-mentioned ventilation operation three times, purity is finally kept>
99.9995% ar pressure is 0.1~0.15 MPa, prepares start region melting；
（5）Start temperature controller, it is 150~300 to control heater temperature oC, after observation melting zone width meets the requirements, according to setting
Determine program start region melting；Heater is at the uniform velocity moved from left to right with 5~50 mm/h speed, is heated during to low order end
Device is with crossbearer lifting；After all heaters all shift to indium ingot low order end lifting, crossbearer return to origin, restart region
Melting；Operation 10~20 times more than being repeated under programme-control；In the process, it is 0.1~0.15 MPa to keep ar pressure；
（6）Temperature controller power supply is closed, heater returns to initial position under programme-control, in lifting state；Keep argon gas gas
Press as 0.1~0.15 MPa, room temperature is cooled to indium ingot；
（7）Indium metal is taken out, the high surface portion of impurity content is removed in glove box, according to impurity on indium ingot length direction
The regularity of distribution, slice off the higher two end portions of impurity content, remaining high pure metal indium packed.
2. the method that atmospheric area melting according to claim 1 prepares high purity indium, it is characterised in that zone melting device
Using contact thermal source.
3. the method that atmospheric area melting according to claim 1 prepares high purity indium, it is characterised in that zone melting device
Designed using multi-stove bodies, more melting zones.
4. the method that atmospheric area melting according to claim 1 prepares high purity indium, it is characterised in that smelting of the present invention can be used
Refining device is operating unit, is expanded production by parallel connection, adapts to the needs of large-scale production.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710994910.XA CN107779614A (en) | 2017-10-23 | 2017-10-23 | A kind of method that atmospheric area melting prepares high purity indium |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710994910.XA CN107779614A (en) | 2017-10-23 | 2017-10-23 | A kind of method that atmospheric area melting prepares high purity indium |
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| CN107779614A true CN107779614A (en) | 2018-03-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257648A (en) * | 2019-07-05 | 2019-09-20 | 上海大学 | A kind of device and preparation method thereof preparing super high purity indium |
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| CN2157817Y (en) * | 1993-07-22 | 1994-03-02 | 施颖 | Zone-melting purification apparatus for high efficient compound |
| CN102051668A (en) * | 2010-11-04 | 2011-05-11 | 西北工业大学 | 10<5> K/cm temperature gradient directional solidification device and directional solidification method |
| CN102965518A (en) * | 2012-11-23 | 2013-03-13 | 桂林理工大学 | High-purity metal refining method for limiting molten zone by utilizing electromagnetic shielding |
| CN202913039U (en) * | 2012-11-23 | 2013-05-01 | 桂林理工大学 | Multi-melting-zone high-frequency heating zone melting device |
| CN103114264A (en) * | 2012-12-28 | 2013-05-22 | 中国神华能源股份有限公司 | Copper-indium alloy target for sputtering and preparation method thereof |
| CN106244830A (en) * | 2016-08-31 | 2016-12-21 | 武汉源脉科技股份有限公司 | A kind of zone melting method prepares super high purity indium |
-
2017
- 2017-10-23 CN CN201710994910.XA patent/CN107779614A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2157817Y (en) * | 1993-07-22 | 1994-03-02 | 施颖 | Zone-melting purification apparatus for high efficient compound |
| CN102051668A (en) * | 2010-11-04 | 2011-05-11 | 西北工业大学 | 10<5> K/cm temperature gradient directional solidification device and directional solidification method |
| CN102965518A (en) * | 2012-11-23 | 2013-03-13 | 桂林理工大学 | High-purity metal refining method for limiting molten zone by utilizing electromagnetic shielding |
| CN202913039U (en) * | 2012-11-23 | 2013-05-01 | 桂林理工大学 | Multi-melting-zone high-frequency heating zone melting device |
| CN103114264A (en) * | 2012-12-28 | 2013-05-22 | 中国神华能源股份有限公司 | Copper-indium alloy target for sputtering and preparation method thereof |
| CN106244830A (en) * | 2016-08-31 | 2016-12-21 | 武汉源脉科技股份有限公司 | A kind of zone melting method prepares super high purity indium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257648A (en) * | 2019-07-05 | 2019-09-20 | 上海大学 | A kind of device and preparation method thereof preparing super high purity indium |
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