CN107858534A - A kind of processing sapphire crystallization furnace tungsten calandria simultaneously reclaims the method and apparatus of metal molybdenum - Google Patents
A kind of processing sapphire crystallization furnace tungsten calandria simultaneously reclaims the method and apparatus of metal molybdenum Download PDFInfo
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- CN107858534A CN107858534A CN201711178301.3A CN201711178301A CN107858534A CN 107858534 A CN107858534 A CN 107858534A CN 201711178301 A CN201711178301 A CN 201711178301A CN 107858534 A CN107858534 A CN 107858534A
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- tungsten
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- calandria
- molybdenum
- sedimentary
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- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 65
- 239000010937 tungsten Substances 0.000 title claims abstract description 65
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 64
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 37
- 239000011733 molybdenum Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 23
- 239000010980 sapphire Substances 0.000 title claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 22
- 239000002184 metal Substances 0.000 title claims abstract description 22
- 238000002425 crystallisation Methods 0.000 title claims abstract description 20
- 230000008025 crystallization Effects 0.000 title claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 229910015221 MoCl5 Inorganic materials 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims abstract description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 25
- 239000000460 chlorine Substances 0.000 claims description 25
- 229910052801 chlorine Inorganic materials 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000004809 Teflon Substances 0.000 claims description 8
- 229920006362 Teflon® Polymers 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 241000370738 Chlorion Species 0.000 claims description 4
- 150000004767 nitrides Chemical class 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 2
- 238000000053 physical method Methods 0.000 claims description 2
- 238000001311 chemical methods and process Methods 0.000 claims 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract 1
- QXYJCZRRLLQGCR-UHFFFAOYSA-N molybdenum(IV) oxide Inorganic materials O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 abstract 1
- 230000008929 regeneration Effects 0.000 abstract 1
- 238000011069 regeneration method Methods 0.000 abstract 1
- 235000016768 molybdenum Nutrition 0.000 description 20
- 239000007789 gas Substances 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 101100230509 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) hat-1 gene Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 150000003657 tungsten Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
Abstract
The invention provides a kind of processing sapphire crystallization furnace tungsten calandria and the method and apparatus of metal molybdenum is reclaimed, using a reactor assembly system, processing surface deposited the sapphire crystallization furnace tungsten calandria of Mo layer.Go to reduce the thickness of deposition molybdenum layer using ultrasonic wave, recycle chemical method to remove remaining molybdenum layer.Chemical method refers to react raw MoCl with molybdenum atom using chlorine gas selecting5Volatile molecules, so as to remove the Mo layer on tungsten bar surface, regeneration tungsten calandria surface is reached, has extended the service life of tungsten calandria.Meanwhile volatility MoCl5Molecule is by alkali liquor absorption, by generating MoO2Afterwards, being reduced property gas reduction is into molybdenum atom.The present invention can both extend the service life of tungsten bar calandria, can recycle infusibility non-ferrous metal molybdenum again.
Description
Technical field
The present invention relates to a kind of extension method of service life of sapphire crystallization furnace tungsten bar calandria and metal molybdenum again
The method of recovery.
Background technology
Sapphire, also known as corundum, it is a kind of oxide being made up of aluminium element and oxygen element.Its hardness is very big, optics
Light transmittance is excellent.It has been applied to the screen of the electronic equipments such as personal consumption electronic product, such as mobile phone, Ipad, while it is
Microelectronics and the particularly important base material of photoelectronic industry, may serve as the base material of LED.With personal consumption electricity
The growth of sub- product demand and the needs for saving the energy, the demand of sapphire material are increasing.
The growing method of sapphire monocrystal has a lot, main to include bubble hair tonic, czochralski method, reverse mould method and heat exchange
Method.No matter any method, it is required for polycrystalline alpha-alumina crystals or alumina powder melting sources, forms the molten of aluminum oxide
Melt body.This process is general to use resistance heating or the method for inductive heating.Sapphire crystallization furnace interior, there is birdcage shape
Tungsten bar calandria, it is crucible inside tungsten bar calandria, and the outside thermal insulation board for having molybdenum matter.At high temperature, tungsten has with materials such as molybdenums
Certain volatility, forms a kind of mixed volatilization thing, and main component is molybdenum element.This volatile matter can be deposited on tungsten bar calandria
Surface, and the lamination that more sinks is thicker, and the diameter difference maximum of upper and lower tungsten bar can be more than 2 millimeters.This volatile matter influences length
Brilliant process has two aspects:First, volatile matter can enter Crystallization nonferrous layer, be commonly called as " peeling " phenomenon, influence the matter of crystal
Amount.Second, according to Ohm's law, the diameter of resistance is thicker, and resistance value can decline.The temperature field point of crystal growth can so be changed
Cloth, crystalline heterogeneity is caused, can also influence crystal mass.Therefore, the volatile matter being immersed on birdcage shape tungsten bar calandria
Layer is, it is necessary to a kind of effective processing method, the service life of increase tungsten bar calandria.Production cost so can be not only reduced,
The metallics volatilized can be reclaimed.
The content of the invention
It is an object of the invention to provide a kind of volatile matter that can be removed and be deposited on sapphire crystallization furnace tungsten bar calandria
Layer so that the diameter of tungsten bar calandria is homogeneous, increases tungsten calandria service life, while reclaim the processing of metal molybdenum in volatile matter
Sapphire crystallization furnace tungsten calandria and the method for reclaiming metal molybdenum.
In order to solve above-mentioned technical problem, the object of the present invention is achieved like this：
（1）Design and make a gas reactor, this reactor includes two sealing lids, and a lid installs ultrasonic wave
Generator, another installation gas introducing system and pressure gauge.Inside reactor has Teflon liner, and reactor bottom carries
The vapor-liquid outlet of one sealing, the diameter of Teflon liner are more than the size of birdcage shape tungsten calandria, and tungsten calandria can be with whole
Body enters inside reactor, but copper-based seat must be removed；
（2）When the volatilization nitride layer being deposited on tungsten bar is thicker, the thickness of volatilization nitride layer is reduced first with physical method；By tungsten
Rod calandria enters in the aqueous solution, while adds ultrasonic wave above tungsten bar；In the presence of ultrasonic wave, a part of loose deposition
Layer can come off because of vibration, and the thickness of volatile matter sedimentary diminishes；Further enter from vapor-liquid outlet withdrawal liquid and cast
Row chemical treatment；
（3）After reactor with tungsten bar calandria is dried, the operation that chemical method removes sedimentary is carried out；Replacing carries gas
The closure of body pressure gauge, chlorine is passed through to inside reactor, is sealed after air is discharged.The reactor of this sealing is heated,
And temperature is controlled 200 ~ 250oBetween C；Following chemical reaction occurs for inside reactor：
2Mo (s) + 5Cl2(g)2MoCl5 (g)
The molybdenum layer metal on tungsten bar surface, changes into gaseous MoCl5Molecule, with unnecessary chlorine outflow reactor, and by
Outside alkali liquor absorption, tungsten under this reaction temperature, not with chlorine reaction；
（4）In alkalescence absorbs groove, chlorine is eventually converted into chlorion or hypochlorite ion；Adjust the pH of solution so that
MoCl5Molecule changes into Mo (OH)2Or Mo (OH)3Precipitation, after filtering further thermal conversion into molybdenum oxide, finally by and also
Reduced oxide is reclaimed metal molybdenum by originality gas.
Another object of the present invention is to provide a kind of processing sapphire crystallization furnace tungsten calandria for realizing the above method simultaneously
Reclaim the device of metal molybdenum.What this purpose of the present invention was realized in：It includes reactor, the lid with excusing from death wave producer
Son 3, the closure 4 with gas gauge and the tungsten bar 7 with molybdenum sedimentary being arranged in reactor, reactor is by reacting
Device box hat 1 and Teflon liner 2 form, and reactor lower end is provided with vapor-liquid outlet 6, when the closure with excusing from death wave producer
Physical is formed when on reactor reduces deposit thickness device, and deposited layers of material chip 9 is provided with device, and band is super
The closure connection excusing from death wave producer of raw wave producer；The group when the closure with gas gauge is arranged on reactor
Sedimentary device is removed into chemical method, closure connection gas introducing system and pressure gauge with gas gauge, gas-liquid row
Outlet connects closed lye tank (vat) 12, and digital pH meter 13 is provided with closed lye tank (vat) 12, and external computer connects digital pH meter
13 and thermocouple 14, in the coupled reaction device of thermocouple 14.
The present invention also has so some technical characteristics：
1st, described chemical method removes the external equipment that the connection of sedimentary device produces chlorine molecule；
2nd, described Physical reduces deposit thickness device and chemical method removes in sedimentary device and is provided with water liquid, heat
Water liquid in the contact reactor of galvanic couple 14；
3rd, the heating-up temperature of the described tungsten bar calandria with molybdenum sedimentary is 200 ~ 250oC；
4th, the diameter of described reactor Teflon liner is more than the tungsten bar with molybdenum sedimentary.
Brief description of the drawings
Fig. 1-3 is the structure chart of gas reactor and the structural representation of two kinds of closures；
Fig. 4 is the structural representation that Physical reduces deposit thickness device；
Fig. 5 is the structural representation that chemical method removes sedimentary device.
Embodiment
The present invention is described further with reference to the accompanying drawings and detailed description：
Embodiment 1
With reference to Fig. 1-5, the present embodiment takes out birdcage shape tungsten bar calandria, the copper bottom of removal calandria from sapphire crystallization furnace
Seat.Several points are respectively selected in the upper and lower part of tungsten bar calandria, the diameter of tungsten bar is determined with slide measure.If that puts up and down is straight
Footpath differs by more than 1 millimeter, illustrates the thicker of sedimentary, and this tungsten bar calandria needs two steps of physics and chemistry to carry out again
It is raw.First, tungsten bar calandria is loaded into reactor 1, injects certain water liquid 8, liquid level is higher than the height of calandria.So
Afterwards, using the sealing lid 3 for being connected to ultrasonic generator, reactor assembly is sealed, and implement ultrasound using ultrasonic generator 5
Ripple vibration washing.After certain time, the tungsten bar calandria 7 with molybdenum sedimentary is taken out, continues to be measured with slide measure, and
Diameter difference above and below record.If diameter difference diminishes, illustrate that the thickness of deposit layer diminishes.Repeat above-mentioned operation, it is known that straight
One constant of footpath difference convergence.Now, the pH value for adjusting solution reaches acid, repeats an aforesaid operations.Then, reaction is passed through
Sealing vapor-liquid outlet 6 below device collects solution and sedimentary chip.In next step, carry out the elution of deionized water and dry behaviour
Make.The closure 4 with gas gauge is changed, chlorine molecule 11, flow constant (20 are imported to the inside of reactor
Ml/min), outlet is sealed after discharging the air in reactor using chlorine.Then, heating response device is overall, keeping temperature
200 ~ 250oIn the range of C.Inside reactor, chlorine are chemically reacted under this temperature range with metal molybdenum, and generation is waved
The MoCl of hair property5Gas molecule 10.In this temperature range, tungsten does not react with chlorine.After reacting a period of time,
Continue to discharge product molecule mixture with chlorine.The chlorine and MoCl of discharge5Molecule is inhaled by the alkali lye in closed lye tank (vat) 12
Receive, generate chlorion and Mo (OH)2Precipitate molecules.Filter to isolate Mo (OH)2Precipitation, the oxide mixing of molybdenum is generated after heating
Thing, recycle reducibility gas that oxide is reduced into recovery metal molybdenum.After being repeated several times such operate, there is no heavy in alkali lye
Precipitation goes out, and illustrates do not have MoCl in gaseous emission5Molecule.Stopping is passed through chlorine, and stops heating response device.Utilize nitrogen
Empty residual chlorine qi leel in reactor.Reactor is opened, tungsten bar calandria is eluted with deionized water, is taken out after drying.Group
After loading onto copper pedestal, it is reloaded into sapphire crystallization furnace and is continuing with.Due to eliminating the sedimentary on tungsten bar surface to greatest extent,
The diameter difference very little of upper and lower tungsten bar, the distribution of resistance of calandria both add heating rod service life than more uniform, cause production again
Raw temperature field is advantageous to the growth course of sapphire crystal than more uniform, improves the yields of crystal generation.Closed lye tank (vat)
Digital pH meter 13 is provided with 12, external computer connects digital pH meter 13 and thermocouple 14, the contact reactor of thermocouple 14
Interior water liquid.
Embodiment 2
Tungsten bar calandria, the copper pedestal of removal calandria are taken out from sapphire crystallization furnace.On the top of tungsten bar calandria with
Portion respectively selects several points, and the diameter of tungsten bar is determined with slide measure.If the diameter difference put up and down is less than 1 millimeter, illustrate now
The thickness of sedimentary is smaller.In this case, it is convenient to omit ultrasonic wave reduces the process of deposit thickness, directly utilizes chemistry side
Method removes the sedimentary on tungsten bar surface, and reclaims refractory metal molybdenum.The tungsten bar calandria of birdcage shape is integrally fitted into reactor,
Utilize the seal cap sealing reactor with gas gauge.Chlorine is imported to the inside of reactor, is discharged and reacted using chlorine
Outlet is sealed after air in device.Then, heating response device is overall, maintains the temperature at 200 ~ 250oIn the range of C.In reactor
Portion, chlorine chemically react under this temperature range with metal molybdenum, generate volatile MoCl5Molecule.When reacting one section
Between after, continue with chlorine discharge product molecule mixture.The chlorine and MoCl of discharge5Molecule is by alkali liquor absorption.Adjust alkali lye
PH value, generate chlorion and Mo (OH)2Precipitate molecules.Filter to isolate Mo (OH)2Precipitation, the oxide of molybdenum is generated after heating
Mixture, recycle reducibility gas that oxide is reduced into recovery metal molybdenum.After being repeated several times such operate, do not exist in alkali lye
There is Precipitation, illustrate there is no MoCl in gaseous emission5Molecule.Stopping is passed through chlorine, and stops heating response device.Utilize
Residual chlorine qi leel in nitrogen purge reactor.Reactor is opened, tungsten bar calandria is eluted with deionized water, is taken after drying
Go out.In assembling after copper pedestal, it is reloaded into sapphire crystallization furnace and is continuing with.
Claims (6)
- A kind of 1. method for handling sapphire crystallization furnace tungsten calandria and reclaiming metal molybdenum, it is characterised in that it includes following step Suddenly：（1）Design and make a gas reactor, this reactor includes two sealing lids, and a lid installs ultrasonic wave Generator, another installation gas introducing system and pressure gauge；Inside reactor has Teflon liner, and reactor bottom carries The vapor-liquid outlet of one sealing, the diameter of Teflon liner are more than the size of birdcage shape tungsten calandria, and tungsten calandria can be with whole Body enters inside reactor, but copper-based seat must be removed；（2）When the volatilization nitride layer being deposited on tungsten bar is thicker, the thickness of volatilization nitride layer is reduced first with physical method；By tungsten Rod calandria enters in the aqueous solution, while adds ultrasonic wave above tungsten bar；In the presence of ultrasonic wave, a part of loose deposition Layer can come off because of vibration, and the thickness of volatile matter sedimentary diminishes；Further enter from vapor-liquid outlet withdrawal liquid and cast Row chemical treatment；（3）After reactor with tungsten bar calandria is dried, the operation that chemical method removes sedimentary is carried out；Replacing carries gas The closure of body pressure gauge, chlorine is passed through to inside reactor, is sealed after air is discharged；The reactor of this sealing is heated, and controls temperature 200 ~ 250oBetween C；Following chemistry occurs for inside reactor Reaction：2Mo (s) + 5Cl2(g)2MoCl5 (g)The molybdenum layer metal on tungsten bar surface, changes into gaseous MoCl5Molecule, with unnecessary chlorine outflow reactor, and it is outer The alkali liquor absorption in portion, tungsten under this reaction temperature, not with chlorine reaction；（4）In alkalescence absorbs groove, chlorine is eventually converted into chlorion or hypochlorite ion；Adjust the pH of solution so that MoCl5Molecule changes into Mo (OH)2Or Mo (OH)3Precipitation, after filtering further thermal conversion into molybdenum oxide, finally by and also Reduced oxide is reclaimed metal molybdenum by originality gas.
- 2. a kind of processing sapphire crystallization furnace tungsten calandria simultaneously reclaims the device of metal molybdenum, it is characterised in that it include reactor, Lid, the closure with gas gauge and the tungsten with molybdenum sedimentary being arranged in reactor with excusing from death wave producer Rod, reactor are made up of reactor box hat and Teflon liner, and reactor lower end is provided with vapor-liquid outlet, when band excusing from death ripple hair The closure of raw device forms Physical when being arranged on reactor reduce deposit thickness device, and sedimentary thing is provided with device Matter chip, the closure connection excusing from death wave producer with excusing from death wave producer；When the closure with gas gauge is arranged on Constitutional chemistry method removes sedimentary device when on reactor, closure connection gas introducing system and pressure with gas gauge Power table, vapor-liquid outlet connect closed lye tank (vat), and digital pH meter is provided with closed lye tank (vat), and external computer connection is digital PH meter and thermocouple, in thermocouple coupled reaction device.
- 3. a kind of processing sapphire crystallization furnace tungsten calandria according to claim 2 simultaneously reclaims the device of metal molybdenum, it is special Sign is that described chemical method removes the external equipment that the connection of sedimentary device produces chlorine molecule.
- 4. a kind of processing sapphire crystallization furnace tungsten calandria according to claim 3 simultaneously reclaims the device of metal molybdenum, it is special Sign is that described Physical reduces deposit thickness device and chemical method removes in sedimentary device and is provided with water liquid, heat Water liquid in galvanic contact reactor.
- 5. a kind of processing sapphire crystallization furnace tungsten calandria according to claim 4 simultaneously reclaims the device of metal molybdenum, it is special Sign is that the heating-up temperature of the described tungsten bar calandria with molybdenum sedimentary is 200 ~ 250oC。
- 6. a kind of processing sapphire crystallization furnace tungsten calandria according to claim 5 simultaneously reclaims the device of metal molybdenum, it is special Sign is that the diameter of described reactor Teflon liner is more than the tungsten bar with molybdenum sedimentary.
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| CN201711178301.3A CN107858534A (en) | 2017-11-23 | 2017-11-23 | A kind of processing sapphire crystallization furnace tungsten calandria simultaneously reclaims the method and apparatus of metal molybdenum |
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| CN201711178301.3A CN107858534A (en) | 2017-11-23 | 2017-11-23 | A kind of processing sapphire crystallization furnace tungsten calandria simultaneously reclaims the method and apparatus of metal molybdenum |
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| CN102912430A (en) * | 2012-11-15 | 2013-02-06 | 上海中电振华晶体技术有限公司 | Sapphire crystal growth equipment and method |
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