CN103014855A - Preparation method and equipment for preparing alpha-Al2O3 single crystal through gamma-Al2O3 - Google Patents
Preparation method and equipment for preparing alpha-Al2O3 single crystal through gamma-Al2O3 Download PDFInfo
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- CN103014855A CN103014855A CN2012105726716A CN201210572671A CN103014855A CN 103014855 A CN103014855 A CN 103014855A CN 2012105726716 A CN2012105726716 A CN 2012105726716A CN 201210572671 A CN201210572671 A CN 201210572671A CN 103014855 A CN103014855 A CN 103014855A
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- raw material
- nozzle
- sintering oven
- oxygen
- al2o3
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Abstract
The invention discloses a preparation method and equipment for preparing an alpha-Al2O3 single crystal through gamma-Al2O3. The equipment comprises a frame, wherein a raw material conveying device, a nozzle, a sintering furnace core and an alpha-Al2O3 crystallization column lifting tray are sequentially which is arranged on the frame from top to bottom, wherein the raw material conveying device comprises a raw material barrel for accommodating gamma-Al2O3, and an oxygen conveying pipe and a hydrogen conveying pipe which are respectively connected with the raw material barrel for accommodating gamma-Al2O3; the nozzle comprises an oxygen nozzle and a hydrogen nozzle which is sleeved on the oxygen nozzle; an inlet of the oxygen nozzle is connected with the gamma-Al2O3 raw material barrel and the oxygen conveying pipe; an inlet of the hydrogen nozzle is connected with the hydrogen conveying pipe; the nozzle stretches into a cavity of the furnace core of the sintering furnace; the alpha-Al2O3 crystallization column can be lifted through the alpha-Al2O3 crystallization column lifting tray, so that the alpha-Al2O3 crystallization column can go in and out of the cavity of the furnace core of the sintering furnace; the bottom of the raw material barrel for accommodating gamma-Al2O3 is provided with a filtering net; and the raw material barrel is provided with a device for allowing the filtering net to generate different vibrations so as to regulate the conveying speed of gamma-Al2O3. The alpha-Al2O3 single crystal prepared by the method and equipment has good color, and the size of the crystal can be adjusted.
Description
Technical field
The present invention relates to α-Al
2O
3The preparation of single crystal relates in particular to a kind of with γ-Al
2O
3Preparation α-Al
2O
3The preparation method of single crystal and equipment thereof.
Background technology
Sapphire is widely used in window material, the high pressure material of substrate material, special optical components and parts, high energy detection and the high power strong laser of substrate material, precision instrument bearing, large-scale integrated circuit SOI and the SOS of high-brightness LED.
But the growth method of growing sapphire crystal mainly contains at present: heat-exchanging method, kyropoulos, the terraced method of resistive heating temperature, falling crucible method.But heat-exchanging method adopts helium to make cooling gas, costs dearly, and can not the axial crystal of direct growth C; The kyropoulos process repeatability is poor, energy consumption is high; The terraced method process repeatability of resistive heating temperature is poor, yield rate is low.Induction heating iridium crucible crystal pulling method has high input, cost is high.Traditional falling crucible method, the thermograde setting range is limited, and the thermograde that provides the growing large-size sapphire crystal required is provided, and causes simultaneously the ability of crystal impurity removal and bubble low, and matter crystal internal defect is more, crystal yield rate only about 50%.
The equipment that is used at present in addition growing sapphire mainly is sintering oven, yet sintering oven of the prior art can not effectively be controlled and make sapphire raw material γ-Al
2O
3And the concentration between oxygen and the hydrogen that is to say to be difficult to control oxygen, hydrogen and γ-Al
2O
3Mass ratio between the powder, and because oxygen and hydrogen are gas, only need to load onto flowrate control valve at their transfer line, just can well control the ratio of combustion of hydrogen and oxygen, this just shows needs control γ-Al
2O
3, the mass ratio between the oxygen, hydrogen key be to control γ-Al well
2O
3The quality of powder.
Summary of the invention
In order to overcome the deficiencies in the prior art, the usefulness γ-Al that the purpose of this invention is to provide a kind of low cost of manufacture, technology controlling and process is simple, yield rate is high, crystal mass is good
2O
3Preparation α-Al
2O
3The preparation method of single crystal.
A further object of the present invention provides a kind ofly can effectively regulate γ-Al
2O
3Transfer rate, and then control γ-Al
2O
3Powder, oxygen is the mass ratio between the hydrogen very easily, the α-Al of generation
2O
3Usefulness γ-Al that crystal mass is good, yield rate is high
2O
3Make α-Al
2O
3The sintering oven of single crystal.
For achieving the above object, technical scheme of the present invention is: a kind of with γ-Al
2O
3Preparation α-Al
2O
3The preparation method of single crystal may further comprise the steps:
1) with the γ-Al of purity 〉=99.99%
2O
3In the charging feedstock bucket;
2) pass into oxygen for the oxygen conveying pipe that is connected with Raw material pail, oxygen is with γ-Al
2O
3Bring in the nozzle of sintering oven, pass into hydrogen for simultaneously the nozzle of sintering oven;
3) light from hydrogen, oxygen and the γ-Al of the nozzle ejection of sintering oven
2O
3Mixture, make this mixture at the combustion chamber internal combustion of sintering oven, γ-Al
2O
3Fusing;
4) with being provided with α-Al
2O
3The crystallization post of crystal seed makes the γ-Al of melted state
2O
3Crystallization conversion becomes α-Al on this crystallization post
2O
3, this Tc≤2050 ℃ namely make α-Al
2O
3Single crystal.
The temperature of the mixture burns in the described step 3) 〉=2050 ℃.
A kind of with γ-Al
2O
3Preparation α-Al
2O
3The sintering oven of single crystal comprises frame, from top to bottom sequentially is provided with lower device on this frame:
Raw material conveying device, affiliated raw material conveying device comprises splendid attire γ-Al
2O
3Raw material pail, and with splendid attire γ-Al
2O
3The Raw material pail oxygen conveying pipe and the hydrogen delivery tube that connect respectively;
Nozzle, described nozzle comprise oxygen nozzle and the hydrogen shower nozzle that is set on the oxygen nozzle, the import of oxygen nozzle and γ-Al
2O
3Raw material pail be connected with oxygen conveying pipe, the import of hydrogen shower nozzle is connected with hydrogen delivery tube;
The combustion chamber of sintering oven;
And α-Al
2O
3The lifting tray of crystallization post;
Described nozzle extends in the cavity of combustion chamber of sintering oven, α-Al
2O
3The lifting tray liftable α-Al of crystallization post
2O
3The crystallization post makes α-Al
2O
3The cavity of the combustion chamber of crystallization post turnover sintering oven, described splendid attire γ-Al
2O
3Raw material pail bottom be provided with filter screen, and this Raw material pail is provided with and makes filter screen produce different vibrations to regulate γ-Al
2O
3The device of transfer rate.
The described vibrative device of filter screen that makes is the described γ-Al that impacts that is arranged on the frame
2O
3The lever construction of Raw material pail, the top that is positioned at Raw material pail is held in impacting of lever construction, the cam that the other end of lever construction and is arranged on the camshaft on the frame cooperates, when the other end of lever construction cooperates with the cam base circle of this camshaft, the end that impacts of lever construction impacts described Raw material pail, when the other end of lever construction cooperated with other parts of the cam of this camshaft, impacting of lever construction held away from described Raw material pail, and this camshaft is by the variable-frequency motor drive of the rotating speed that can change camshaft.
Described lever construction is provided with the elevating lever for the height of the fulcrum of adjustment (adjusting) lever structure.Described elevating lever can the adjustment (adjusting) lever structure the height of fulcrum, and then the adjustment (adjusting) lever structure impacts γ-Al
2O
3The dynamics of Raw material pail, realize regulating the Oscillation Amplitude of filter screen.
Slip is provided with the combustion chamber of isolation sintering oven and operator's heat insulation protective shield on the frame of described sintering oven.
The combustion chamber of described sintering oven is provided with vision slit.
The present invention adopts above technical scheme, utilizes lever construction that the frame at sintering oven arranges and at γ-Al
2O
3Raw material pail bottom filter screen is set, the end that impacts of lever construction impacts sintering oven γ-Al
2O
3Raw material pail, thereby cause filter screen vibration, make the γ-Al in the filter screen
2O
3Powder enters oxygen conveying pipe and oxygen mix, owing to driven by variable-frequency motor at the camshaft of the other end of lever, and the rotating speed that the rotating speed of regulating variable-frequency motor just can the adjustment cam axle, and then adjustment cam axle drive lever impacts γ-Al
2O
3The frequency of Raw material pail, make the filter screen of Raw material pail produce different vibrations, and then achieve effective control γ-Al
2O
3The influx of powder when participating in oxygen and combustion of hydrogen, controlled γ-Al well
2O
3The influx of powder when participating in oxygen and combustion of hydrogen, also just realized γ-Al
2O
3During burning and the concentration of oxygen and hydrogen can adjust and control α-Al that method of the present invention and sintering oven are made
2O
3Single crystal is of good quality, the big or small controllable adjustable of crystalline size.
Description of drawings
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments:
Fig. 1 is the perspective view of sintering oven of the present invention;
Fig. 2 is the connection diagram of analysing and observe of the raw material conveying device of sintering oven of the present invention and nozzle arrangements.
Embodiment
Shown in one of Fig. 1-2, a kind of with γ-Al
2O
3Preparation α-Al
2O
3The preparation method of single crystal may further comprise the steps:
1) with the γ-Al of purity 〉=99.99%
2O
3In the charging feedstock bucket 21;
2) pass into oxygen for the oxygen conveying pipe 22 that is connected with Raw material pail 21, oxygen is with γ-Al
2O
3Bring in the nozzle 3 of sintering oven, pass into hydrogen for simultaneously the nozzle 3 of sintering oven;
3) light from hydrogen, oxygen and the γ-Al of nozzle 3 ejections of sintering oven
2O
3Mixture, make this mixture at combustion chamber 4 internal combustion of sintering oven, γ-Al
2O
3Fusing;
4) with being provided with α-Al
2O
3The crystallization post 5 of crystal seed makes the γ-Al of melted state
2O
3Crystallization conversion becomes α-Al on this crystallization post 5
2O
3, this Tc≤2050 ℃ namely make α-Al
2O
3Single crystal.
The temperature of the mixture burns in the described step 3) 〉=2050 ℃.
A kind of with γ-Al
2O
3Preparation α-Al
2O
3The sintering oven of single crystal comprises frame 1, from top to bottom sequentially is provided with lower device on this frame 1:
Raw material conveying device 2, affiliated raw material conveying device 2 comprises splendid attire γ-Al
2O
3Raw material pail 21, and with splendid attire γ-Al
2O
3Raw material pail 21 oxygen conveying pipe 22 and the hydrogen delivery tube 23 that connect respectively;
Nozzle 3, described nozzle 3 comprise oxygen nozzle 31 and the hydrogen shower nozzle 32 that is set on the oxygen nozzle 31, import 33 and the γ-Al of oxygen nozzle 31
2O
3 Raw material pail 21 are connected connection with oxygen conveying pipe, the import 34 of hydrogen shower nozzle 32 is connected with hydrogen delivery tube 23;
The combustion chamber 4 of sintering oven;
And α-Al
2O
3The lifting tray 6 of crystallization post 5;
Described nozzle 3 extends in the cavity of combustion chamber 4 of sintering oven, α-Al
2O
3The lifting tray 6 liftable α-Al of crystallization post 5
2O
3Crystallization post 5 makes α-Al
2O
3The cavity of the combustion chamber 4 of crystallization post 5 turnover sintering ovens, described splendid attire γ-Al
2O
3 Raw material pail 21 bottoms be provided with filter screen 7, and this Raw material pail 21 is provided with and makes filter screen 7 produce different vibrations to regulate γ-Al
2O
3The device 8 of transfer rate.
The described filter screen 7 vibrative devices 8 that make are for being arranged on the described γ-Al that impacts on the frame 1
2O
3The lever construction of Raw material pail 21, lever construction 8 impact the top that end 81 is positioned at Raw material pail 21, the cam 91 that the other end 82 and of lever construction 8 is arranged on the camshaft 9 on the frame 1 cooperates, when the other end 82 of lever construction 8 cooperates with cam 91 basic circles of this camshaft 9, the end 81 that impacts of lever construction 8 impacts described Raw material pail 21, when the other end 82 of lever construction 8 cooperates with the cam of this camshaft 9 91 other parts, impacting of lever construction 8 holds 81 away from described Raw material pail 21, and this camshaft 9 is by variable-frequency motor (not shown in FIG.) drive of the rotating speed that can change camshaft 9.
Described lever construction 8 is provided with the elevating lever 84 for the height of the fulcrum 83 of adjustment (adjusting) lever structure 8.Described elevating lever 84 can adjustment (adjusting) lever structure 8 the height of fulcrum 83, and then adjustment (adjusting) lever structure 8 impacts γ-Al
2O
3The dynamics of Raw material pail 21, realize regulating the Oscillation Amplitude of filter screen 7.
Slide on the frame 1 of described sintering oven and be provided with the combustion chamber 4 of isolation sintering oven and operator's heat insulation protective shield 10.
The combustion chamber 4 of described sintering oven is provided with vision slit 41.
Claims (7)
1. one kind with γ-Al
2O
3Preparation α-Al
2O
3The preparation method of single crystal is characterized in that: it may further comprise the steps:
1) with the γ-Al of purity 〉=99.99%
2O
3In the charging feedstock bucket;
2) pass into oxygen for the oxygen conveying pipe that is connected with Raw material pail, oxygen is with γ-Al
2O
3Bring in the nozzle of sintering oven, pass into hydrogen for simultaneously the nozzle of sintering oven;
3) light from hydrogen, oxygen and the γ-Al of the nozzle ejection of sintering oven
2O
3Mixture, make this mixture at the combustion chamber internal combustion of sintering oven, γ-Al
2O
3Fusing;
4) with being provided with α-Al
2O
3The crystallization post of crystal seed makes the γ-Al of melted state
2O
3Crystallization conversion becomes α-Al on this crystallization post
2O
3, this Tc≤2050 ℃ namely make α-Al
2O
3Single crystal.
2. according to claim 1 a kind of with γ-Al
2O
3Preparation α-Al
2O
3The preparation method of single crystal is characterized in that: the temperature of the mixture burns in the described step 3) 〉=2050 ℃.
3. one kind is used for realizing claim 1 or the 2 described γ-Al of using
2O
3Preparation α-Al
2O
3The preparation method's of single crystal sintering oven comprises frame, from top to bottom sequentially is provided with lower device on this frame:
Raw material conveying device, affiliated raw material conveying device comprises splendid attire γ-Al
2O
3Raw material pail, and with splendid attire γ-Al
2O
3The Raw material pail oxygen conveying pipe and the hydrogen delivery tube that connect respectively;
Nozzle, described nozzle comprise oxygen nozzle and the hydrogen shower nozzle that is set on the oxygen nozzle, the import of oxygen nozzle and γ-Al
2O
3Raw material pail be connected with oxygen conveying pipe, the import of hydrogen shower nozzle is connected with hydrogen delivery tube;
The combustion chamber of sintering oven;
And α-Al
2O
3The lifting tray of crystallization post;
Described nozzle extends in the cavity of combustion chamber of sintering oven, α-Al
2O
3The lifting tray liftable α-Al of crystallization post
2O
3The crystallization post makes α-Al
2O
3The cavity of the combustion chamber of crystallization post turnover sintering oven is characterized in that: described splendid attire γ-Al
2O
3Raw material pail bottom be provided with filter screen, and this Raw material pail is provided with and makes filter screen produce different vibrations to regulate γ-Al
2O
3The device of transfer rate.
4. sintering oven according to claim 3, it is characterized in that: the described vibrative device of filter screen that makes is the described γ-Al that impacts that is arranged on the frame
2O
3The lever construction of Raw material pail, the top that is positioned at Raw material pail is held in impacting of lever construction, the cam that the other end of lever construction and is arranged on the camshaft on the frame cooperates, when the other end of lever construction cooperates with the cam base circle of this camshaft, the end that impacts of lever construction impacts described Raw material pail, when the other end of lever construction cooperated with other parts of the cam of this camshaft, impacting of lever construction held away from described Raw material pail, and this camshaft is by the variable-frequency motor drive of the rotating speed that can change camshaft.
5. sintering oven according to claim 4, it is characterized in that: described lever construction is provided with the elevating lever for the height of the fulcrum of adjustment (adjusting) lever structure.
6. sintering oven according to claim 3 is characterized in that: the combustion chamber that is provided with the isolation sintering oven and operator's heat insulation protective shield slide on the frame of described sintering oven.
7. sintering oven according to claim 3, it is characterized in that: the combustion chamber of described sintering oven is provided with vision slit.
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Application publication date: 20130403 |