CN107746972A - A kind of preparation method of metallic aluminium - Google Patents
A kind of preparation method of metallic aluminium Download PDFInfo
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- CN107746972A CN107746972A CN201710846616.4A CN201710846616A CN107746972A CN 107746972 A CN107746972 A CN 107746972A CN 201710846616 A CN201710846616 A CN 201710846616A CN 107746972 A CN107746972 A CN 107746972A
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- Prior art keywords
- aluminium
- heating
- metallic aluminium
- preparation
- temperature
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 79
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000004411 aluminium Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017083 AlN Inorganic materials 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000007158 vacuum pyrolysis Methods 0.000 abstract description 3
- 238000010792 warming Methods 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 238000004131 Bayer process Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 238000009626 Hall-Héroult process Methods 0.000 description 1
- 229910012725 Li3N-LiCl Inorganic materials 0.000 description 1
- 229910012718 Li3N—LiCl Inorganic materials 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 238000009866 aluminium metallurgy Methods 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001234 light alloy Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/0038—Obtaining aluminium by other processes
- C22B21/0053—Obtaining aluminium by other processes from other aluminium compounds
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of preparation method of metallic aluminium, following steps are specifically included:First in the case where pressure is 7.5~30Pa vacuum condition, aluminium nitride is carried out to the first heating, the second heating, the 3rd heating and the 4th heating successively, 4th is heated to outlet temperature, then material is proceeded by from outlet temperature and cooled for the first time, and it is incubated, then carry out cooling for second, so as to obtain metallic aluminium;The present invention is using aluminium nitride as raw material, utilize vacuum pyrolysis, by controlling vacuum and heating-up temperature, holding temperature and time, improve the direct yield of metallic aluminium, the purity and direct yield of metallic aluminium prepared by the inventive method are higher, and metallic aluminium well-crystallized, easily separated prepared by the present invention, preparation method of the present invention is simple to operate, energy consumption is low, pollution-free, has preferable application prospect.
Description
Technical field
The present invention relates to non-ferrous metal metallurgy technical field, more particularly to a kind of preparation method of metallic aluminium.
Background technology
Aluminium is the second largest metalloid for being only second to iron at present, and has possessed wide application field.According to statistics, the earth's crust
Middle aluminium content is about 8.8%, and unlike other common metals, the time that aluminium is found is not grown.Because aluminium is a kind of
Very active metal, there is tendency with oxygen kickback, one layer of the surface of aluminium often generation is continuous and fine and close in atmosphere
Film, play a part of making aluminium not continue to oxidation, so the aluminium of free state is not present in nature, this is also that aluminium has well
The reason for corrosion stability.
Aluminium has outstanding advantages of small density, thermal conductivity, electric conductivity, good corrosion stability, and and can forms excellent with many metals
Matter aluminium base light-alloy, thus aluminium on modern industrial technology using relatively broad, be mainly used in building, traffic, engineering and cable,
Other fields such as packaging.The application of aluminium mainly has two kinds of forms:Fine aluminium and aluminium alloy.
At present, industrialization aluminium metallurgy technique is generally divided into two steps in the world:First, refined using Bayer process from bauxite
Aluminum oxide.Ore is leached with the sodium hydroxide solution containing aluminium, leachate crystalline deposit goes out aluminium hydroxide, and then obtains oxygen
Change aluminium.Then, primary aluminum is prepared using Hall Heroult process, the aluminum oxide being dissolved in molten cryolitic is electrolysed, extracted
Metallic aluminium.And the refinement aluminium process is present that technological process is various, building equipment investment is big, high energy consumption, has greenhouse gases and perfluor
The shortcomings of discharge of carbide (PFCs).
To avoid above mentioned problem, the extraction research for metallic aluminium starts to turn to using aluminium nitride as raw material.At present, from nitridation
The research that metallic aluminium is extracted in aluminium focuses primarily upon electrolysis and thermal decomposition method.
Rhamdhani et al. points out that in theory aluminium nitride can be decomposed into aluminium and nitrogen, and point of aluminium nitride at 700 DEG C
Solution voltage is 0.75V, and this decomposition voltage compares AlCl3(l), Al2S3And Al (s)2O3(s) decomposition voltage will at that same temperature
It is low.Therefore from the viewpoint of thermodynamics, electrolysis has good potentiality, available for extracting aluminium from aluminium nitride, but face
It is difficult to find a kind of appropriate electrolyte to dissolve highly stable AlN (s) that subject matter, which is,.Bonomi et al. is to 660 ~ 700
℃(Li3N-LiCl) solubility of electrolyte and AlN molten-salt electrolysis have carried out limited research.Goto et al. uses LiCl-
KCl-Li3N molten salt systems depositing Al N thin film on aluminium base.Yan et al. CaCl at a temperature of 1133k2Carried out in-NaCl melts
The experiment of Direct electrochemical reduction aluminium nitride, finally observes fine aluminium drop on minus plate, but this experimentation there was only 3 ~
5% yield.
Patent 201510334601.0 discloses a kind of preparation side with alumina carbon tropical resources vacuum thermally decomposable metal aluminium
Method.The patent adds carbon in vertical vacuum furnace into aluminum oxide, is then well mixed and obtains mixed material, by mixed material pressure
Bulk is made, aluminium nitride is obtained being passed through nitrogen, pressure is 10 ~ 50Pa, being reduced under conditions of 1300 ~ 1700 DEG C of temperature;Will
The aluminium nitride arrived carries out 20 ~ 60min of pyrolysis under conditions of pressure is 5 ~ 60Pa, temperature is 1850 ~ 2050K, then
Be cooled to room temperature, collected on condenser and obtain the metallic aluminium of well-crystallized, but the patent be prepared metallic aluminium purity with it is straight
Yield is relatively low.
The content of the invention
It is an object of the invention to provide a kind of preparation method of metallic aluminium, the present invention is mainly anti-using vacuum thermal decomposition
Metallic aluminium should be prepared, the purity and direct yield of metallic aluminium prepared by the present invention are all higher.
Technical scheme is as follows:First in the case where pressure is 7.5~30Pa vacuum condition, aluminium nitride is entered successively
Row first heats, the second heating, the 3rd heating and the 4th heating, the 4th is heated to outlet temperature, then by material from terminal temperature
Degree proceeds by cool for the first time, and is incubated, and then carries out second and cools, so as to obtain metallic aluminium.
The preparation method of metallic aluminium, concrete operations are as follows in the present invention:
(1)Pressure be 7.5~30Pa vacuum condition under, aluminium nitride is carried out successively the first heating, second heating, the 3rd plus
Heat and the 4th heating, wherein first is heated to the first temperature as 700 ~ 800 DEG C, second is heated to second temperature as 1100 ~ 1200
DEG C, the 3rd is heated to the 3rd temperature as 1400 ~ 1500 DEG C, and the 4th is heated to outlet temperature as 1650 ~ 1670 DEG C, wherein first adds
The heating rate of heat be 60 ~ 80 DEG C/min, and the heating rate of the second heating is 45 ~ 50 DEG C/min, the 3rd heating rate heated
For 15 ~ 20 DEG C/min, the heating rate of the 4th heating is 10 ~ 15 DEG C/min, and vacuum pyrolysis occurs for aluminium nitride, generates aluminium
Steam and nitrogen;
(2)Then by step(1)Resulting material proceeds by from outlet temperature to cool for the first time, is cooled to 1550 ~ 1650 DEG C simultaneously
Insulation, the time of insulation is 10 ~ 30min;
(3)By step(2)Material after insulation terminates carries out second of cooling, less than 100 DEG C is cooled to, so as to obtain metal
Aluminium.
First cooling produces larger temperature difference, is advantageous to the enrichment of product aluminium, and described first cools and be incubated
Cheng Zhong, aluminium nitride continue to thermally decompose, and the part aluminium steam of generation starts to condense.
The method that second of cooling can use furnace cooling, metal is condensed into by the aluminium steam that pyrolysis generates
Aluminium.
The preparation method of metallic aluminium of the present invention is carried out in vaccum sensitive stove, and metallic aluminium is placed in into vaccum sensitive stove
In crucible, the efficiency of heating surface of vaccum sensitive stove is high, and energy consumption is low, pollution-free.
Advantages of the present invention and technique effect:
(1)The present invention is using aluminium nitride as raw material, using vacuum pyrolysis, by controlling vacuum and heating-up temperature, guarantor
Warm temperature and time, improve the direct yield of metallic aluminium.
(2)The purity and direct yield of metallic aluminium prepared by the inventive method is higher, and effect preferably can obtained metallic aluminium
Purity reaches more than 98wt%, and direct yield is up to more than 98.5%.
(3)Metallic aluminium well-crystallized, easily separated prepared by the inventive method.
(4)Preparation method provided by the invention is simple to operate, and energy consumption is low, pollution-free.
Brief description of the drawings
Fig. 1 is the pictorial diagram that metallic aluminium is prepared in the embodiment of the present invention 1;
Fig. 2 is the SEM figures that metallic aluminium is prepared in the embodiment of the present invention 1;
Fig. 3 is the XRD that metallic aluminium is prepared in the embodiment of the present invention 1.
Embodiment
The present invention is described in further detail below by embodiment, but the scope of the present invention is not limited in described
Hold.
Embodiment 1:The preparation method of metallic aluminium, concrete operations are as follows:
It is 2 ~ 3cm by 70g bulks volume3Wurtzite-type analyze pure aln raw material and be placed in crucible (volume in vaccum sensitive stove
For 0.5L) in, it is 7.5Pa to control vacuum, is then warming up to 800 DEG C from 30 DEG C with 70 DEG C/min of speed, with 45 DEG C of speed/
Min is warming up to 1200 DEG C from 800 DEG C, and 1500 DEG C are warming up to from 1200 DEG C with 15 DEG C/min of speed, with 15 DEG C/min of speed from
1500 DEG C are warming up to 1650 DEG C, are then cooled to 1600 DEG C, and 30min is incubated under conditions of 1600 DEG C, and insulation again will after terminating
When temperature is down to 90 DEG C, is collected on condensing unit and obtain well-crystallized, segregative metallic aluminium.
Pictorial diagram, SEM figures, the XRD spectrum for the metallic aluminium that the present embodiment is prepared are distinguished as shown in Figure 1, 2, 3, metal
Aluminium purity>98wt.%, metallic aluminium direct yield > 98.5%.
Embodiment 2:The preparation method of metallic aluminium, concrete operations are as follows:
It is 1.5 ~ 2cm by 50g bulks volume3Wurtzite-type analyze pure aln raw material and be placed in crucible in vaccum sensitive stove and (hold
Product is 0.4L) in, it is 10Pa to control vacuum, is then warming up to 700 DEG C from 30 DEG C with 60 DEG C/min of speed, with 50 DEG C of speed/
Min is warming up to 1150 DEG C from 700 DEG C, and 1480 DEG C are warming up to from 1150 DEG C with 20 DEG C/min of speed, with 10 DEG C/min of speed from
1480 DEG C are warming up to 1670 DEG C, are then cooled to 1650 DEG C, and 10min is incubated under conditions of 1650 DEG C, and insulation terminates rear temperature
When being down to 100 DEG C, collected on condensing unit and obtain well-crystallized, segregative metallic aluminium.
The metallic aluminium purity that the present embodiment is prepared>95wt.%, metallic aluminium direct yield > 96%.
Embodiment 3:The preparation method of metallic aluminium, concrete operations are as follows:
It is 3 ~ 5cm by 80g bulks volume3Wurtzite-type analyze pure aln raw material and be placed in crucible (volume in vaccum sensitive stove
For 0.6L) in, it is 15Pa to control vacuum, is then warming up to 750 DEG C from 30 DEG C with 80 DEG C/min of speed, with 47 DEG C/min of speed
1180 DEG C are warming up to from 750 DEG C, 1450 DEG C are warming up to from 1180 DEG C with 17 DEG C/min of speed, with 15 DEG C/min of speed from 1450 DEG C
1670 DEG C are warming up to, is then cooled to 1620 DEG C, is incubated 20min under conditions of being 1620 DEG C in temperature, insulation terminates rear temperature
When being down to 90 DEG C, collected on condensing unit and obtain well-crystallized, segregative metallic aluminium.
The metallic aluminium purity that the present embodiment is prepared>97wt.%, metallic aluminium direct yield > 98%.
Embodiment 4:The preparation method of metallic aluminium, concrete operations are as follows:
It is 2.5 ~ 4cm by 100g bulks volume3Wurtzite-type analyze pure aln raw material and be placed in crucible in vaccum sensitive stove and (hold
Product is 0.7L) in, it is 30Pa to control vacuum, is then warming up to 720 DEG C from 30 DEG C with 70 DEG C/min of speed, with 45 DEG C of speed/
Min is warming up to 1100 DEG C from 720 DEG C, and 1400 DEG C are warming up to from 1100 DEG C with 15 DEG C/min of speed, with 12 DEG C/min of speed from
1400 DEG C are warming up to 1660 DEG C, are then cooled to 1550 DEG C, are incubated 25min under conditions of being 1550 DEG C in temperature, insulation terminates
When temperature is down to 90 DEG C afterwards, is collected on condensing unit and obtain well-crystallized, segregative metallic aluminium.
The metallic aluminium purity that the present embodiment is prepared>96wt.%, metallic aluminium direct yield > 97%.
Claims (5)
1. a kind of preparation method of metallic aluminium, it is characterised in that specifically include following steps:
(1)Pressure be 7.5~30Pa vacuum condition under, aluminium nitride is carried out successively the first heating, second heating, the 3rd plus
Heat and the 4th heating, wherein first is heated to the first temperature as 700 ~ 800 DEG C, second is heated to second temperature as 1100 ~ 1200
DEG C, the 3rd is heated to the 3rd temperature as 1400 ~ 1500 DEG C, and the 4th is heated to outlet temperature as 1650 ~ 1670 DEG C;
(2)Then by step(1)Resulting material proceeds by from outlet temperature to cool for the first time, is cooled to 1550 ~ 1650 DEG C simultaneously
Insulation, the time of insulation is 10 ~ 30min;
(3)By step(2)Material after insulation terminates carries out second of cooling, less than 100 DEG C is cooled to, so as to obtain metal
Aluminium.
2. the preparation method of metallic aluminium according to claim 1, it is characterised in that:It is described first heating heating rate be
60~80℃/min。
3. the preparation method of metallic aluminium according to claim 1, it is characterised in that:It is described second heating heating rate be
45~50℃/min。
4. the preparation method of metallic aluminium according to claim 1, it is characterised in that:It is described 3rd heating heating rate be
15~20℃/min。
5. the preparation method of metallic aluminium according to claim 1, it is characterised in that:It is described 4th heating heating rate be
10~15℃/min。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109852799A (en) * | 2019-04-11 | 2019-06-07 | 昆明理工大学 | A kind of bauxite prepares metallic aluminium and the method for SiC |
CN109913665A (en) * | 2019-04-11 | 2019-06-21 | 昆明理工大学 | A kind of method that bauxite vacuum distillation prepares metallic aluminium |
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US4430120A (en) * | 1981-07-24 | 1984-02-07 | Moshe Fruchter | Process for the manufacture of pure metallic aluminum from aluminum ores and other aluminum-bearing materials |
CN104745816A (en) * | 2015-03-24 | 2015-07-01 | 昆明理工大学 | Method for preparing metallic aluminum by means of chlorination reduction of aluminum nitride |
CN104988335A (en) * | 2015-06-17 | 2015-10-21 | 昆明理工大学 | Method of preparing metallic aluminium by alumina carbothermal nitridation vacuum thermal decomposition |
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2017
- 2017-09-19 CN CN201710846616.4A patent/CN107746972A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US4430120A (en) * | 1981-07-24 | 1984-02-07 | Moshe Fruchter | Process for the manufacture of pure metallic aluminum from aluminum ores and other aluminum-bearing materials |
CN104745816A (en) * | 2015-03-24 | 2015-07-01 | 昆明理工大学 | Method for preparing metallic aluminum by means of chlorination reduction of aluminum nitride |
CN104988335A (en) * | 2015-06-17 | 2015-10-21 | 昆明理工大学 | Method of preparing metallic aluminium by alumina carbothermal nitridation vacuum thermal decomposition |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109852799A (en) * | 2019-04-11 | 2019-06-07 | 昆明理工大学 | A kind of bauxite prepares metallic aluminium and the method for SiC |
CN109913665A (en) * | 2019-04-11 | 2019-06-21 | 昆明理工大学 | A kind of method that bauxite vacuum distillation prepares metallic aluminium |
CN109913665B (en) * | 2019-04-11 | 2020-03-10 | 昆明理工大学 | Method for preparing metal aluminum by bauxite vacuum distillation |
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