CN103691948A - Device and method for machining high-density aluminum oxide by plasma - Google Patents
Device and method for machining high-density aluminum oxide by plasma Download PDFInfo
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- CN103691948A CN103691948A CN201310725529.5A CN201310725529A CN103691948A CN 103691948 A CN103691948 A CN 103691948A CN 201310725529 A CN201310725529 A CN 201310725529A CN 103691948 A CN103691948 A CN 103691948A
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Abstract
The invention discloses a device and a method for machining high-density aluminum oxide by plasma, and belongs to the technical field of high-density aluminum oxide for sapphire crystals. The device is characterized in that a radio frequency plasma generator (8) and a plasma torch (10) are arranged below a feed hopper, a high-frequency induction coil (7) is wound outside the plasma torch (10), a deposition platform (12) for receiving materials is arranged below the plasma torch (10), and aluminum oxide powder is fed by the feed hopper, instantly melted in the process of falling in the plasma torch (10), solidified in a directional crystallization manner on the deposition platform (12) to obtain the high-purity high-density aluminum oxide. By the aid of the device and the method, the high-purity aluminum oxide cannot be polluted, parts of impurities in the aluminum oxide can be volatilized under the action of high-temperature plasma, and the aluminum oxide is further purified. Continuous process can be kept, production efficiency is accelerated, and the stable performance of the aluminum oxide can be kept.
Description
Technical field
A device and method for plasma process high density aluminum oxide, belongs to sapphire crystal high density aluminum oxide technical field.
Background technology
Highly dense aluminium oxide is mainly used in sapphire crystal field, and sapphire, because its special nature is widely used, is mainly used in military project window material and LED lighting field.Along with the support of country to energy-conservation industry, LED illumination day by day increases, for the demand of high purity aluminium oxide also rapid growth.Sapphire crystal growth method has a variety of, such as kyropoulos and czochralski method, heat-exchanging method, temperature gradient method etc.In these processes, be mainly that high purity aluminium oxide is placed in crucible and is heated to fusing point, regrow into monocrystalline gained.In order to improve output and to reduce costs, need high purity aluminium oxide raw material to be filled up crucible to greatest extent as far as possible.So the density of high purity aluminium oxide is had to very high requirement.
The method that at present high-purity alumina powder is processed into high density material has two kinds of compressing high-temperature sintering process and oxyhydrogen flame high-temperature melting methods, the former all has larger pollution to product by mould and the kiln furnitures in high temperature sintering in pressing process, the latter has certain purification effect in melting process, but can retain a large amount of protiums.And two kinds of modes are discontinuity and produce, can there is larger fluctuating in the quality between product.Continuous Influence of production to downstream industry is larger, and corresponding product is very different, brings about great losses.And the throughput rate that discontinuity is produced slows down, reduce output.The high density high purity aluminium oxide that above two kinds of methods are produced, all can be on there being larger impact when for growing sapphire monocrystalline in sapphire quality or yield rate.
Summary of the invention
The technical problem to be solved in the present invention is: overcome above-mentioned the deficiencies in the prior art, a kind of continuous production is provided, can improves the device and method of product density a kind of plasma process high density aluminum oxide that can further purify.
For solving the problems of the technologies described above, technical scheme provided by the invention is: the device of this plasma process high density aluminum oxide, it is characterized in that: comprise charging hopper, RF plasma reactor, plasma torch, radio-frequency induction coil, deposition table, stainless steel water cold reactor, described charging hopper below is provided with RF plasma reactor, RF plasma reactor below is provided with plasma torch, plasma torch is around with radio-frequency induction coil, the lower end of plasma torch is fastened in the upper shed of stainless steel water cold reactor, in stainless steel water cold reactor, be provided with the deposition table that multi-directional rotation moving assembly supports, charging hopper, RF plasma reactor, plasma torch, deposition table are on same vertical curve, the material spilling in assurance charging hopper can be fallen in deposition table after RF plasma reactor and plasma torch, and multi-directional rotation moving assembly can carry deposition table and move back and forth in upper and lower, left and right direction.
Described charging hopper is water-cooled charging hopper, and water-cooled charging hopper is that charging hopper is covered with cold water circulating box, and cold water circulating box connects circulating condensing water system, offers powder import on cold water circulating box.Water-cooled charging hopper reduces the wherein temperature of alumina powder at any time, prevents that alumina powder partial melting from affecting blanking speed.
Described RF plasma reactor and the distance between deposition table are 300 ~ 400mm, and RF plasma reactor is covered with cold water circulating box and connects circulating condensing water system.This highly guarantees the best distance of fall of alumina powder, thereby can guarantee best fall time.
Described plasma torch is quartzy material, and plasma torch overcoat has quartzy chuck, between plasma torch and quartzy chuck, is hollow interlayer, and hollow interlayer connects circulating condensing water system.This structure can the withstand high temperatures electric discharge phenomena that effectively isolated radio-frequency induction coil causes again.
Described multi-directional rotation moving assembly comprises pedestal, horizontal mobile mechanism, elevating mechanism and rotating mechanism, horizontal mobile mechanism is to move horizontally power motor to be fixed on and to move horizontally track one end and drive the pedestal wheel of pedestal to move in the horizontal direction by crawler belt, elevating mechanism is the bottom that flexible motor is fixed on expansion link, expansion link passes pedestal and is connected with pedestal gear, rotating mechanism is that the rotary power motor that is fixed on pedestal below rotates by gear driven expansion link, and the top of expansion link is fixed on the bottom surface of deposition table.
Utilize said apparatus to carry out a method for plasma process high density aluminum oxide, it is characterized in that, concrete technology step is:
A, first with the speed of 305 ~ 350L/h, utilize RF plasma reactor to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil after entering in plasma torch and be constantly warming up to 9000 ~ 10000 ℃;
B, alumina powder enter plasma torch by RF plasma reactor by charging hopper continuously with the feed rate of 200 ~ 500g/min, there is moment melting in alumina powder plasma heating through 9000 ~ 10000 ℃ in the process falling, the alumina deposit of melting is on deposition table;
C, deposition table keep the rotating speed of 0 ~ 300r/min when collecting the aloxite (AI2O3) falling, and deposition table all keeps the speed of 10 ~ 50mm/min to move back and forth in the horizontal and vertical directions; Aloxite (AI2O3) drop to and in deposition table, first forms liquid layer, and then completes crystallographic orientation and get final product through spontaneous process of setting.
The distance of fall of described aluminium oxide is 300 ~ 400mm.
Plasma generation gas described in step a is hydrogen and the A gas gaseous mixture of 1.5 ~ 14:100 by volume, and described A gas is the mist of one or more arbitrary proportions in nitrogen, argon gas, helium.
The particle diameter of the alumina powder adopting in step b is 0.1 ~ 500 μ m.
Deposition table described in step c keeps the rotating speed of 200 ~ 300r/min when collecting the aloxite (AI2O3) falling; Described deposition table all keeps in the horizontal and vertical directions the speed of 30 ~ 40mm/min to move back and forth when collecting the aloxite (AI2O3) falling.
In the present invention forms alumina powder plasma by radio-frequency induction coil, because now the temperature of plasma is very high, maximum temperature can reach 10000 ℃, and alumina powder melts the molecule that forms melting in pyroprocess, and then melt granules is deposited in deposition table.Deposition table constantly moves in the several directions of difference, thereby guarantees the shape of finished product, makes the alumina block density of condensation more even.Aluminium oxide molten melt drop drop to and in deposition table, first forms liquid layer, then cooling experience crystallographic orientation process slowly.In process, can realize aluminium oxide is further purified.Most of impurity all can vapor away a part under the high temperature action of plasma, and remaining part is a meeting impurities removal part in crystallographic orientation process, thereby can also purify to product in the non-staining situation of assurance.The purity of final products partly depends on the purity of raw material, and utilizing method in the present invention can obtain purity is more than 99.999% alumina block material.
For the preparation of dopant material, keep being uniformly distributed of doped chemical most important, this just requires will stop the formation of liquid layer in this process, and solidification process is more favourable rapidly.
In device of the present invention, also can adopt radio-frequency generator to generate plasma.
Plasma torch is with water cooling equipment, and is placed in quartzy chuck, and quartzy chuck can completely cut off the electric discharge phenomena that radio-frequency induction coil causes.Plasma-generating gas is imported in plasma torch, and radio-frequency induction coil produces high frequency strain magnetic field, makes gas ionization, thereby produces plasma.The selection of gas is not strict especially, anyly can produce isoionic gas and can use.In the preparation of high purity aluminium oxide, alumina powder enters reactor by water-cooled charging hopper.Because plasma has very high temperature, alumina particle will melt fast, and partial impurities can vapor away.The liquid oxidatively al deposition of fusing is in deposition table, and deposition table is made by aluminium oxide or other exotic materials, and the directional solidification process of liquid layer experience then forming obtains alumina block material.The distance of this process and deposition table and flame passes is closely related, main by the distance between RF plasma reactor and deposition table.If hypertelorism does not have enough mobility when dropping to deposition table, the aluminium oxide of melting solidifies within the very short time, is unfavorable for the discharge of impurity and keeps the high density of alumina block and be uniformly distributed; If hypotelorism is affected by the temperature in plasma torch easily, the aluminium oxide long volatilization that is also unfavorable for impurity hardening time; Only in distance of the present invention, can keep under deposition table is in than the environment of higher temperatures, being conducive to the preservation of liquid layer, not only guarantee to be further purified alumina block material but also can allow aluminium oxide solidify in the best time; In process, aluminium oxide first exists with the form of liquid, and in solidification process, impurity tends to concentrate in late curing top layer, the oxide block that just can obtain being further purified by simple mechanical grinding after solidifying completely.
In the present invention, keep deposition table in lasting motion, by slewing rate, move horizontally the adjusting of frequency and amplitude, vertical rate travel and amplitude, the position that keeps deposition table to accept aloxite (AI2O3) is constantly changing; Make the aluminium oxide first receiving have time enough to solidify, and keep at the volley the even density of alumina block.And can consciously mould the shape of alumina block.
Compared with prior art, the beneficial effect that the device and method of a kind of plasma process high density aluminum oxide of the present invention has is: apparatus and method of the present invention not only do not have to pollute the partial impurities volatilization that can also make under the action of plasma of high temperature in aluminium oxide to high purity aluminium oxide is further purified aluminium oxide.Apparatus and method working environment of the present invention is clean and tidy, pollution-free, can keep technique to carry out continuously, has not only accelerated the stable performance that production efficiency can also keep product.Being melted in the very short time in dropping process of aluminium oxide completes, and almost eliminated the melting time, accelerated greatly the efficiency of aluminium oxide processing.The forming process controllability of alumina block is good, can keep shape and the even density of alumina block, and can consciously mould the shape of alumina block.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of device of plasma process high density aluminum oxide.
Wherein: 1, powder import; 2, funnel recirculated water entrance; 3, funnel circulating water outlet; 4, water-cooled charging hopper; 5, transmitter recirculated water entrance; 6, transmitter circulating water outlet; 7, radio-frequency induction coil; 8, RF plasma reactor; 9, quartzy chuck; 10, plasma torch; 11, alumina block; 12, deposition table; 13, thermal insulation board; 14, stainless steel water cold reactor; 15, pedestal; 16, expansion link; 17, rotary power motor; 18, move horizontally power motor; 19, pedestal wheel; 20, flexible motor; 21, move horizontally track.
The specific embodiment
Fig. 1 is the most preferred embodiment of the device of plasma process high density aluminum oxide of the present invention, below in conjunction with accompanying drawing 1 and specific embodiment, the device and method of a kind of plasma process high density aluminum oxide of the present invention is described further.Wherein embodiment 1 is most preferred embodiment.
With reference to accompanying drawing 1: the device of plasma process high density aluminum oxide of the present invention comprises water-cooled charging hopper 4, RF plasma reactor 8, plasma torch 10, radio-frequency induction coil 7, deposition table 12, stainless steel water cold reactor 14, water-cooled charging hopper 4 belows are provided with RF plasma reactor 8, RF plasma reactor 8 belows are provided with plasma torch 10, plasma torch 10 is around with radio-frequency induction coil 7, the lower end of plasma torch 10 is fastened in the upper shed of stainless steel water cold reactor 14, in stainless steel water cold reactor 14, be provided with the deposition table 12 that multi-directional rotation moving assembly supports, water-cooled charging hopper 4, RF plasma reactor 8, plasma torch 10, deposition table 12 are on same vertical curve, and the material spilling in assurance water-cooled charging hopper 4 can be fallen in deposition table 12 after RF plasma reactor 8 and plasma torch 10.
Multi-directional rotation moving assembly comprises pedestal 15, horizontal mobile mechanism, elevating mechanism and rotating mechanism, horizontal mobile mechanism is to move horizontally power motor 18 to be fixed on and to move horizontally track 21 one end and drive the pedestal wheel 19 of pedestal 15 to move in the horizontal direction by crawler belt, elevating mechanism is the bottom that flexible motor 20 is fixed on expansion link 16, expansion link 16 passes pedestal 15 and is connected with pedestal 15 gears, rotating mechanism is that the rotary power motor 17 that is fixed on pedestal 15 belows rotates by gear driven expansion link 16, the top of expansion link 16 is fixed on the bottom surface of deposition table 12.
Between pedestal 15 and stainless steel water cold reactor 14, be provided with thermal insulation board 13, completely cut off the high temperature in stainless steel water cold reactor 14, prevent from affecting the service behaviour of pedestal 15, horizontal mobile mechanism, elevating mechanism and rotating mechanism.
Water-cooled charging hopper 4 is covered with cold water circulating box for funnel, and cold water circulating box connects circulating condensing water system, offers powder import on cold water circulating box.Distance between RF plasma reactor 8 and deposition table 12 is 300 ~ 400mm, and RF plasma reactor 8 is covered with cold water circulating box and connects circulating condensing water system.Plasma torch 10 is quartzy material, and plasma torch 10 overcoats have quartzy chuck 9, between plasma torch 10 and quartzy chuck 9, is hollow interlayer, and hollow interlayer connects circulating condensing water system.Deposition table 12 can move in all directions under the effect of multi-directional rotation moving assembly, can be accepted aluminium oxide at different parts, guarantees cool time, again can be continuously shaped.
Stainless steel water cold reactor 14 is outer to be provided with chuck and to connect circulating condensing water system.
The present invention is connected structure longitudinally by the global design of device.Directly water-cooled charging hopper 4 is placed in to the top of device, after once feeding in raw material toward 4 li of water-cooled charging hoppers, can utilizes charging hopper to control blanking speed, and keep speed homogeneous.Alumina powder can fall and also pass through successively RF plasma reactor 8 and the plasma torch 10 of device under the effect of self gravitation, without additionally providing power to process continuously.Can guarantee to increase to greatest extent processing speed.
Distance between RF plasma reactor 8 and deposition table 12 is controlled at 300 ~ 400mm, meets the density that aluminium oxide melting and cooling time guarantee alumina block.This is highly actual is that alumina material fall time is controlled is the most critical place that whole device can practical function.
Embodiment 1
A, to take nitrogen and hydrogen volume be plasma-generating gas than the mist of 97:3, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 10000 ℃.
B, particle diameter be at the alumina powder of 0.3 ~ 50 μ m, detects its impurity content to be by glow discharge mass spectrometry: silicon 11ppm, iron 5 ppm, sodium 10 ppm, manganese 5 ppm, zinc 6 ppm, copper 5 ppm, calcium 6 ppm, magnesium 4 ppm; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 400g/min, there is moment melting in alumina powder plasma heating through 10000 ℃ in the process falling, the alumina deposit of melting is on deposition table 12.
C, deposition table 12 keep the rotating speed of 175r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 30mm/min to move back and forth in the horizontal and vertical directions, it is 340 ~ 360mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 2ppm, iron 0.4 ppm, sodium 0.2 ppm, manganese 1 ppm, zinc 1 ppm, copper 1 ppm, calcium 1 ppm, magnesium 1 ppm.The density of gained alumina block is 3.72g/cm
3.
Embodiment 2
A, to take helium and hydrogen volume be plasma-generating gas than the mist of 90:10, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 10000 ℃.
B, particle diameter be at the alumina powder of 0.5 ~ 50 μ m, detects its impurity content to be by glow discharge mass spectrometry: silicon 30 ppm, iron 20 ppm, sodium 40 ppm, manganese 10 ppm, zinc 11 ppm, copper 9 ppm, calcium 13 ppm, magnesium 9 ppm; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 350g/min, there is moment melting in alumina powder plasma heating through 10000 ℃ in the process falling, the alumina deposit of melting is on deposition table 12.
C, deposition table 12 keep the rotating speed of 150r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 30mm/min to move back and forth in the horizontal and vertical directions, it is 320 ~ 360mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 2.3 ppm, iron 1.9 ppm, sodium 1 ppm, manganese 1.6 ppm, zinc 1 ppm, copper 1 ppm, calcium 1.2 ppm, magnesium 1 ppm.The density of gained alumina block is 3.70g/cm
3.
Embodiment 3
A, to take argon gas and hydrogen volume be plasma-generating gas than the mist of 93:7, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 10000 ℃;
The alumina powder of b, use embodiment 1; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 450g/min, there is moment melting in alumina powder plasma heating through 10000 ℃ in the process falling, the alumina deposit of melting is on deposition table 12;
C, deposition table 12 keep the rotating speed of 225r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 35mm/min to move back and forth in the horizontal and vertical directions, it is 340 ~ 370mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 2.2ppm, iron 0.4 ppm, sodium 0.2 ppm, manganese 0.9 ppm, zinc 1 ppm, copper 1 ppm, calcium 1 ppm, magnesium 1.1 ppm.The density of gained alumina block is 3.70g/cm
3.
Embodiment 4
A, to take nitrogen, helium and hydrogen volume be plasma-generating gas than the mist of 90:8.5:1.5, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 10000 ℃;
B, particle diameter be at the alumina powder of 100 ~ 500 μ m, detects its impurity content to be by glow discharge mass spectrometry: silicon 40ppm, iron 20 ppm, sodium 38 ppm, manganese 10 ppm, zinc 18 ppm, copper 8 ppm, calcium 12 ppm, magnesium 9 ppm; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 220g/min, there is moment melting in alumina powder plasma heating through 10000 ℃ in the process falling, the alumina deposit of melting is on deposition table 12;
C, deposition table 12 keep the rotating speed of 100r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 10mm/min to move back and forth in the horizontal and vertical directions, it is 360 ~ 400mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 2.2ppm, iron 1.9 ppm, sodium 0.8ppm, manganese 0.5ppm, zinc 0.9 ppm, copper 0.5 ppm, calcium 0.8 ppm, magnesium 1 ppm.The density of gained alumina block is 3.8g/cm
3.
A, to take nitrogen, helium, argon gas and hydrogen volume be plasma-generating gas than the mist of 80:3:3:14, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 9500 ℃;
B, particle diameter be at the alumina powder of 0.1 ~ 20 μ m, detects its impurity content to be by glow discharge mass spectrometry: silicon 10ppm, iron 3ppm, sodium 8 ppm, manganese 4.5 ppm, zinc 4 ppm, copper 3 ppm, calcium 6 ppm, magnesium 2 ppm; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 500g/min, there is moment melting in alumina powder plasma heating through 9500 ℃ in the process falling, the alumina deposit of melting is on deposition table 12;
C, deposition table 12 keep the rotating speed of 300r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 50mm/min to move back and forth in the horizontal and vertical directions, it is 300 ~ 330mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 1.8ppm, iron 0.3 ppm, sodium 0.2 ppm, manganese 0.6 ppm, zinc 0.4 ppm, copper 0.5ppm, calcium 0.6ppm, magnesium 0.3 ppm.The density of gained alumina block is 3.67g/cm
3.
Embodiment 6
A, to take nitrogen and hydrogen volume be plasma-generating gas than the mist of 95:5, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 9000 ℃;
The alumina powder of b, employing embodiment 2; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 200g/min, there is moment melting in alumina powder plasma heating through 9000 ℃ in the process falling, the alumina deposit of melting is on deposition table 12;
C, deposition table 12 are not rotated when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 50mm/min to move back and forth in the horizontal and vertical directions, it is 330 ~ 355mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 2.1ppm, iron 0.4 ppm, sodium 0.2 ppm, manganese 1.1 ppm, zinc 1 ppm, copper 1 ppm, calcium 1.1 ppm, magnesium 1 ppm.The density of gained alumina block is 3.65g/cm
3.
Comparative example 1
A, to take nitrogen and hydrogen volume be plasma-generating gas than the mist of 97:3, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 7000 ℃.
B, employing embodiment 1 alumina powder used; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 400g/min, alumina powder is through the most of melting of plasma heating of 7000 ℃ in the process falling, and alumina deposit is on deposition table 12.
C, deposition table 12 keep the rotating speed of 175r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 30mm/min to move back and forth in the horizontal and vertical directions, it is 340 ~ 360mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 10ppm, iron 4.9 ppm, sodium 9.3 ppm, manganese 4.8 ppm, zinc 5.9 ppm, copper 5 ppm, calcium 5.8 ppm, magnesium 4 ppm; The density of gained alumina block is 3.4g/cm
3.
Comparative example 2
A, to take nitrogen and hydrogen volume be plasma-generating gas than the mist of 97:3, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 10000 ℃.
B, employing embodiment 1 alumina powder used; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 600g/min, alumina powder is through the most of melting of plasma heating of 10000 ℃ in the process falling, and alumina deposit is on deposition table 12.
C, deposition table 12 keep the rotating speed of 175r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 30mm/min to move back and forth in the horizontal and vertical directions, it is 340 ~ 360mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 10ppm, iron 4.5 ppm, sodium 9.1 ppm, manganese 4.6 ppm, zinc 5.6 ppm, copper 4.7 ppm, calcium 5.7 ppm, magnesium 3.8 ppm; The density of gained alumina block is 3.4g/cm
3.
Comparative example 3
The process conditions that adopt the same raw material of embodiment 1, difference is that feeds of alumina speed is 100g/min.The density of gained alumina block is 3.7g/cm
3, impurity content is: silicon 2ppm, iron 0.4 ppm, sodium 0.2 ppm, manganese 1 ppm, zinc 1 ppm, copper 1 ppm, calcium 1 ppm, magnesium 1 ppm.Product quality and embodiment are suitable, but production efficiency reduces greatly, waste tool of production resource.
Comparative example 4
A, to take nitrogen and hydrogen volume be plasma-generating gas than the mist of 97:3, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 10000 ℃.
B, employing embodiment 1 alumina powder used; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 400g/min, alumina powder is through the most of melting of plasma heating of 10000 ℃ in the process falling, and alumina deposit is on deposition table 12.
C, deposition table 12 keep the rotating speed of 400r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 50mm/min to move back and forth in the horizontal and vertical directions, it is 340 ~ 360mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 8ppm, iron 3.9 ppm, sodium 7.9 ppm, manganese 3.8 ppm, zinc 4.3 ppm, copper 4.1 ppm, calcium 3.2 ppm, magnesium 2.8 ppm; The density of gained alumina block is 3.65g/cm
3.On most of impurity is timely, move just to pile up and be capped.
Comparative example 4
A, to take nitrogen and hydrogen volume be plasma-generating gas than the mist of 97:3, utilize RF plasma reactor 8 to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil 7 after entering in plasma torch 10 and be constantly warming up to 10000 ℃.
B, employing embodiment 1 alumina powder used; This alumina powder is entered to plasma torch 10 by RF plasma reactor 8 by water-cooled charging hopper 4 continuously with the feed rate of 400g/min, alumina powder is through the most of melting of plasma heating of 10000 ℃ in the process falling, and alumina deposit is on deposition table 12.
C, deposition table 12 keep the rotating speed of 175r/min when collecting the aloxite (AI2O3) falling, and deposition table 12 all keeps the speed of 30mm/min to move back and forth in the horizontal and vertical directions, it is 450 ~ 480mm that deposition table 12 mobile range in the vertical direction keeps the distance of fall of aluminium oxide; Aloxite (AI2O3) drop to and in deposition table 12, first forms liquid layer, and then through the process of setting of crystallographic orientation and get final product.Impurity content by glow discharge mass spectrometry testing product is: silicon 8.1ppm, iron 3.7ppm, sodium 7.9 ppm, manganese 3.7ppm, zinc 4.1 ppm, copper 4.1 ppm, calcium 3.2 ppm, magnesium 2.7ppm; The density of gained alumina block is 3.65g/cm
3.On most of impurity is timely, move just to pile up and be capped.
Comparative example 6
With the compressing high-temperature sintering process Processing Example 1 of traditional handicraft alumina powder used, the impurity content by glow discharge mass spectrometry testing product is: silicon 11.2ppm, iron 5 ppm, sodium 10 ppm, manganese 5 ppm, zinc 6 .1ppm, copper 5 ppm, calcium 6 .3ppm, magnesium 4 ppm; The density of gained alumina block is 3.5g/cm
3.
From embodiment 1 ~ 6 and comparative example 6 contrasts, can find out the method for the present invention of utilizing, the alumina block volume density of producing is large, and in process, has effectively eliminated most of impurity.From embodiment 1 and comparative example 1 contrast, can not find out when plasma reaches temperature of the present invention and can not carry out good removal of impurities to aluminium oxide, can affect the density of alumina block yet.From 2,3 contrasts of embodiment 1 and comparative example, can find out, the excessive or too small production that all can affect alumina block of alumina feeding speed, causes product quality to decline or reduces productive rate.From 4 contrasts of embodiment 1 and comparative example, can find out that movement rate in deposition table can cause partial impurities to take out when excessive.From 5 contrasts of embodiment 1 and comparative example, can find out that aluminium oxide distance of fall crosses the aluminium oxide just being fallen can cause lower liquid aluminium oxide not solidify when near time and cover, cannot complete equally impurity and discharge.
The above, be only preferred embodiment of the present invention, is not the present invention to be done to the restriction of other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (9)
1. the device of a plasma process high density aluminum oxide, it is characterized in that: comprise charging hopper, RF plasma reactor (8), plasma torch (10), radio-frequency induction coil (7), deposition table (12), stainless steel water cold reactor (14), described charging hopper below is provided with RF plasma reactor (8), RF plasma reactor (8) below is provided with plasma torch (10), plasma torch (10) is around with radio-frequency induction coil (7), the lower end of plasma torch (10) is fastened in the upper shed of stainless steel water cold reactor (14), in stainless steel water cold reactor (14), be provided with the deposition table (12) that multi-directional rotation moving assembly supports, charging hopper, RF plasma reactor (8), plasma torch (10), deposition table (12) are on same vertical curve, guarantee that the material spilling in charging hopper can be fallen deposition table (12) after RF plasma reactor (8) and plasma torch (10) upper, multi-directional rotation moving assembly can carry deposition table (12) and move back and forth in upper and lower, left and right direction.
2. the device of a kind of plasma process high density aluminum oxide according to claim 1, it is characterized in that: described charging hopper is water-cooled charging hopper (4), water-cooled charging hopper (4) is covered with cold water circulating box for charging hopper, cold water circulating box connects circulating condensing water system, offers powder import on cold water circulating box.
3. the device of a kind of plasma process high density aluminum oxide according to claim 1, it is characterized in that: the distance between described RF plasma reactor (8) and deposition table (12) is 300 ~ 400mm, RF plasma reactor (8) is covered with cold water circulating box and connects circulating condensing water system.
4. the device of a kind of plasma process high density aluminum oxide according to claim 1, it is characterized in that: described plasma torch (10) is quartzy material, plasma torch (10) overcoat has quartzy chuck (9), between plasma torch (10) and quartzy chuck (9), be hollow interlayer, hollow interlayer connects circulating condensing water system.
5. the device of a kind of plasma process high density aluminum oxide according to claim 1, it is characterized in that: described multi-directional rotation moving assembly comprises pedestal (15), horizontal mobile mechanism, elevating mechanism and rotating mechanism, horizontal mobile mechanism is fixed on to move horizontally track (21) one end and drives the pedestal of pedestal (15) to take turns (19) by crawler belt and moves in the horizontal direction for moving horizontally power motor (18), elevating mechanism is the bottom that flexible motor (20) is fixed on expansion link (16), expansion link (16) passes pedestal (15) and is connected with pedestal gear, rotating mechanism is for the rotary power motor (17) that is fixed on pedestal (15) below is by gear driven expansion link (16) rotation, the top of expansion link (16) is fixed on the bottom surface of deposition table (12).
6. utilize device described in claim 1 ~ 5 any one to carry out a method for plasma process high density aluminum oxide, it is characterized in that, concrete technology step is:
A, first with the speed of 305 ~ 350L/h, utilize RF plasma reactor (8) to launch plasma-generating gas, ionization occurs under the effect of the high frequency magnetic field that plasma-generating gas is sent at radio-frequency induction coil (7) after entering in plasma torch (10) and be constantly warming up to 9000 ~ 10000 ℃;
B, alumina powder enter plasma torch (10) by RF plasma reactor (8) by charging hopper continuously with the feed rate of 200 ~ 500g/min, there is moment melting in alumina powder plasma heating through 9000 ~ 10000 ℃ in the process falling, the alumina deposit of melting is on deposition table (12);
C, deposition table (12) keep the rotating speed of 0 ~ 300r/min when collecting the aloxite (AI2O3) falling, and deposition table (12) all keeps the speed of 10 ~ 50mm/min to move back and forth in the horizontal and vertical directions; Aloxite (AI2O3) drop in deposition table (12) and first forms liquid layer, and then completes crystallographic orientation and get final product through spontaneous process of setting.
7. a kind of method of carrying out plasma process high density aluminum oxide according to claim 6, it is characterized in that: the plasma generation gas described in step a is hydrogen and the A gas gaseous mixture of 1.5 ~ 14:100 by volume, and described A gas is the mist of one or more arbitrary proportions in nitrogen, argon gas, helium.
8. a kind of method of carrying out plasma process high density aluminum oxide according to claim 6, is characterized in that: the particle diameter of the alumina powder adopting in step b is 0.1 ~ 500 μ m.
9. a kind of method of carrying out plasma process high density aluminum oxide according to claim 6, is characterized in that: the deposition table described in step c (12) keeps the rotating speed of 200 ~ 300r/min when collecting the aloxite (AI2O3) falling; Described deposition table (12) all keeps in the horizontal and vertical directions the speed of 30 ~ 40mm/min to move back and forth when collecting the aloxite (AI2O3) falling.
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| CN112126985A (en) * | 2020-07-10 | 2020-12-25 | 新疆三锐佰德新材料有限公司 | Method and device for physically purifying high-purity aluminum oxide material for sapphire |
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