CN104150755B - Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof - Google Patents
Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof Download PDFInfo
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- CN104150755B CN104150755B CN201410384473.6A CN201410384473A CN104150755B CN 104150755 B CN104150755 B CN 104150755B CN 201410384473 A CN201410384473 A CN 201410384473A CN 104150755 B CN104150755 B CN 104150755B
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
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Abstract
The invention discloses a quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and a manufacturing method of the quartz crucible, wherein the volume density (bubble volume/total volume*100%) of microbubbles within the depth of 1mm in the surface of the quartz crucible is lower than 0.0005%, the method comprises the steps as follows: introducing hydrogen, nitrogen, helium, argon, or one or more of other inert gases in the melting process of the quartz crucible to replace the residual air in quartz sand particles, and melting and refining the inner surface of the quartz glass crucible again to remove the microbubbles wrapped in a bubble depletion layer and prevent the residual microbubbles from expanding in the high-temperature use process of the crucible. The quartz crucible prepared through the method has the characteristic of resisting the continuous high temperature for a long period of time, and meets the demand of repeated batch charging and the demand of pulling the monocrystalline of a monocrystalline manufacturer.
Description
Technical field
The present invention relates in photovoltaic art or semicon industry, repeatedly for fused silica crucible prepared by the arc process of drawn monocrystalline silicon, and the method that in the vague and general layer of quartz crucible bubble, microbubble content and suppression microbubble expand in quartz crucible use procedure can be reduced.
Background technology
Silicon single crystal, it is widely used in semiconducter device and solar cell, prepares in the prior art mainly through vertical pulling method (Czochralski, Cz method).According to vertical pulling method, the growth of silicon single crystal carries out in crystal lifting furnace, is loaded in quartz crucible, melted initial feed polysilicon by the well heater around quartz crucible.Then crystal seed is immersed in the silicon liquid of melting, then upwards lift and the relative growth rotating silicon single crystal lentamente.In this process of growth, very important role served as by quartz crucible, as carrying container containing, bears the erosion of continuous high temperature and molten silicon liquid again simultaneously.
In current existing technology, rotating mold vacuum method is the main manufacture methods preparing quartz crucible, by quartz sand rotate, the mould inner surface with certain hole is shaping, cools formation after making it melt by the electrode discharge arc heated quartz sand being arranged on mould inside.In preparation process, vacuumize from the outside of mould, thus form this quartz crucible with two-layer composite that inner side is the vague and general layer of bubble (also claiming transparent layer), skin is bubble composite bed (also claiming bubble layer).
According to theory of high packing, certain space (contain air in space) is always there is between quartz sand particle, even if vacuumize in quartz crucible manufacturing processed, also all air cannot be drained, these air exist in the vague and general layer of bubble of quartz crucible with diameter at micron-sized microbubble; Even if simultaneously because silica glass its viscosity under the high temperature of 1700 DEG C is this characteristic of 106dPaS, under the dual function of stickiness and inertia, the quartz sand parcel that surrounding can not melt by the quartz sand that surface portion has melted, be mingled with a large amount of air that contain between quartz sand particle simultaneously, the quartz crucible internal skin formed finally is caused to have very high microbubble content, the diameter of these bubbles at micron order, and concentrates in the internal surface 1mm degree of depth.
In monocrystalline silicon growing process, above-mentioned microbubble slowly can expand and grow up under continuous high temperature environment, merges, has a strong impact on the duration of service of quartz crucible.Especially concentrate on the microbubble of crucible internal skin, once break, quartz chips impurity can be brought in the silicon liquid of melting, the level of response of aggravation quartz crucible and molten silicon liquid, the serious industrial accident that leakage silicon will be caused serious like this.Because quartz crucible is expendable consumed product, monocrystalline silicon growing producer, for cost pressure, urgently wishes that quartz crucible can bear the high temperature of longer time, meets the demand of repeatedly crystal pulling.
Need a kind of to reduce in quartz crucible microbubble content in the vague and general layer of bubble simultaneously, suppress microbubble to expand in quartz crucible use procedure, meet repeatedly feed intake, the quartz crucible preparation method of crystal pulling demand.
Summary of the invention
The present invention relates to one repeatedly drawn monocrystalline silicon quartz crucible, it skin (also claiming bubble layer) comprising the vague and general internal layer of bubble (also claiming transparent layer) and be rich in bubble, microbubble volume density in the internal surface 1mm degree of depth of the vague and general layer of this quartz crucible internal layer bubble is lower than 0.0005%, and in outer bubble layer, bubble volume density is 40% ~ 80%.
The invention still further relates to manufacture and above-mentionedly repeatedly drawn monocrystalline silicon can use the method for quartz crucible.
The Graphite Electrodes center adopted in quartz crucible melting process has a diameter to be the aperture of 3 ~ 10mm.
A kind of gas in hydrogen, nitrogen, helium, argon gas or other rare gas elementes or several mixed gas is passed in quartz crucible melting process.
Wherein, when passing into mixed gas, in gas mixture, the content of a certain gas is 1% ~ 99%.
Gas enters into the inner chamber of graphite jig through the centre hole of Graphite Electrodes.
The pressure passing into gas is 0.05 ~ 0.2Mpa, and flow is 0.5 ~ 4m3/h.
Pass into gas to start to be after quartz sand striking forms crucible shape idiosome, open before vacuumizing.
Pass into gas to terminate to be after closedown vacuumizes.
In different steps prepared by quartz crucible, regulate mould speed of rotation, covering heat shading apparatus and die coat Edge Distance suitable for reading, the pressure passing into gas and flow, vacuum pump suction pressure, electrode position and found power, realize can repeatedly drawn monocrystalline silicon use quartz crucible, concrete grammar step is as follows:
(1) in the mould rotated, supply quartz sand raw material and form crucible shape idiosome: mould is installed on turning axle together with die coat, this mould is rotated, to be pressed onto well on the inwall of mould by quartz sand around this turning axle with the speed of 50 ~ 120 revs/min under motor drives; With the moulding stick with certain size radian the quartz sand being pressed in mould inner wall scraped and make required shape.Described mould equipment has the passage that can apply air-breathing/bleed, and these are connected to vacuum pump by the chamber of die coat; Heat-insulation device for quartz crucible is arranged at the top of described mould, described heat-insulation device for quartz crucible can move up and down above mould; Graphite Electrodes group is arranged on movably (axis of electrode group and rotating shaft coaxle) above mould, Graphite Electrodes in described Graphite Electrodes group is that centre has aperture, can found formation stages pass into gas to quartz crucible shape idiosome internal cavities at quartz crucible;
(2) quartz glass crucibles is formed: regulate mould to rotate with the speed of 70 ~ 100 revs/min, covering heat shading apparatus moves to distance die coat edge 15 ~ 50mm suitable for reading, gas from the aperture Graphite Electrodes with pressure for 0.05 ~ 0.2Mpa, flow is 0.5 ~ 4m
3/ h enters quartz crucible shape idiosome internal cavities, open the vacuum pump that is connected with die coat and be that-0.1 ~-0.05MPa bleeds with pressure, apart from mould 5 ~ 20cm starting the arc suitable for reading bottom Graphite Electrodes group, power is that 200 ~ 600kW makes it melt to the heating of quartz crucible shape idiosome.Continue to pass into gas to close after 1 ~ 10 minute, be that-0.03 ~ 0MPa bleeds with pressure again, covering heat shading apparatus moves to distance die coat edge 40 ~ 80mm suitable for reading, in mould following 15cm ~ mould suitable for reading above 10cm position suitable for reading bottom Graphite Electrodes group, power is that 400 ~ 800kW makes its melt-forming to quartz crucible shape idiosome continuation heating, and the time length is 2 ~ 15 minutes;
(3) electric arc melting is utilized to make described quartz glass crucibles internal surface melting process of refinement again: to close vacuum pump, mould rotates with 50 ~ 120 revs/min of speed, covering heat shading apparatus moves to distance die coat edge 10 ~ 50mm suitable for reading, the straight wall portion mid-way of 5mm ~ crucible bottom distance quartz crucible bottom adjustment Graphite Electrodes group, power is 450 ~ 1200kW, the internal surface melting more respectively in the straight wall portion of quartz crucible formed step (2), bottom and R angular distortion portion, the microbubble that internal surface is existed reduces further.Wherein, respectively to make electrode group form the electric arc of the 3rd power P 3 to the melting again of straight wall portion, very first time T1 is continued, with the electric arc of the 4th power P 4 to bottom melting again, continue the second time T2, with the electric arc of the 5th power P 5 to the melting again of R angular distortion portion, continue the 3rd time T3; And meet: T1>T3 and T2>T3, P5>P3 and P4>P3;
(4) naturally cooling, step of coming out of the stove: cut off the electricity supply after keeping 1 ~ 30 minute of above-mentioned (3) step, naturally cooling was come out of the stove after 5 ~ 30 minutes; Obtain microbubble volume density (bubble volume/cumulative volume × 100%) in the internal surface 1mm degree of depth of the vague and general layer of internal layer bubble lower than 0.0008%, especially lower than 0.0005%, the bubble volume density of outer bubble layer is the quartz crucible of the repeatedly drawn monocrystalline silicon use of 40% ~ 80%.
Wherein, can be preferred, make the vague and general layer thickness of bubble account for whole crucible wall thickness 20% ~ 50%, and bubble layer thickness account for whole crucible wall thickness 50% ~ 80%.
Described first pressure passing into gas is 0.05 ~ 0.2Mpa, and described first flow is 0.5 ~ 4m
3/ h; The described very first time continuing to pass into gas is 1 ~ 10 minute, and continuing heating and continuous second time is 2 ~ 15 minutes; The first described speed of rotation is 50 ~ 120 revs/min, and the second speed of rotation is 70 ~ 100 revs/min, and the 3rd speed of rotation is 50 ~ 120 revs/min; The first described suction pressure is-0.1 ~-0.05MPa, and the second suction pressure is-0.03 ~ 0MPa; The first distance that described covering heat shading apparatus moves to distance die coat edge suitable for reading is 15 ~ 50mm, and second distance is 40 ~ 80mm, and the 3rd distance is 10 ~ 50mm; Described Graphite Electrodes group first location is apart from mould above 5 ~ 20cm suitable for reading bottom electrode group, the second position is at mould following 15cm ~ mould suitable for reading above 10cm suitable for reading bottom electrode group, 3rd position is be positioned at quartz crucible straight wall portion mid-way height bottom electrode group, 4th position is apart from 5 ~ 20cm bottom quartz crucible bottom electrode group, and the 5th position is apart from 10 ~ 30cm bottom quartz crucible bottom electrode group; The first described power is 200 ~ 600kW, and the second power is 400 ~ 800kW, and the 3rd power is 450 ~ 850kW, and the 4th power is 600 ~ 1000kW, and the 5th power is 700 ~ 1200kW;
Melting the 3rd time is 1 ~ 10 minute to described straight wall portion again, and melting the 4th time is 1 ~ 15 minute again in bottom, and melting the 5th time is 1 ~ 5 minute again in R angular distortion portion.
By present method prepare can repeatedly drawn monocrystalline silicon use quartz crucible, reduce the content of microbubble in the vague and general layer of quartz crucible bubble, especially the microbubble content in the vague and general layer of bubble in the internal surface 1mm degree of depth, inhibit the expansion of these residual microbubbles simultaneously, therefore can prevent due to air bubble expansion, break and the vigorous reaction of the silicon liquid caused and crucible and the accidents such as silicon occur to leak, extend duration of service of quartz crucible, meet that monocrystalline producer repeatedly feeds intake, the demand of pulling monocrystal.
Accompanying drawing explanation
Fig. 1 represents that rotating mold vacuum method prepares quartz crucible and assisting building schematic diagram.
Fig. 2 be represent of the present invention can repeatedly drawn monocrystalline silicon use quartz crucible.
Fig. 3 is microbubble situation (amplifying 100 times) in the vague and general layer section of quartz crucible bubble adopting the existing common technology of founding to prepare.
Fig. 4 is microbubble situation (amplifying 100 times) in the vague and general layer section of quartz crucible bubble adopting the inventive method to prepare.
Description of reference numerals: 1 center has a diameter to be the Graphite Electrodes of 3 ~ 10mm aperture, perforate is had and the covering heat shading apparatus that can move up and down above mould in the middle of 2,3 quartz crucible shape idiosomes, 4 moulds with certain hole, 5 die coats that can vacuumize and rotate, the internal layer (transparent layer) that 6 quartz crucible bubbles are vague and general, the top layer (1mm is dark) of the vague and general layer of 7 quartz crucible bubble, 8 quartz crucibles are rich in the skin (bubble layer) of bubble.
Specific embodiment
This invention exploits a kind of can repeatedly drawn monocrystalline silicon use quartz crucible and manufacture method, adopt mechanical means as known in the art, by increasing Graphite Electrodes centre hole, hydrogen is passed in quartz crucible melting process, nitrogen, helium, a kind of gas in argon gas or other rare gas elementes or several mixed gas, different power is adopted in the different steps of founding, to quartz glass crucibles internal surface melting process of refinement again, to form in bubble vague and general layer in the internal surface 1mm degree of depth microbubble volume density lower than 0.0005%, and these residual microbubbles can be suppressed to expand in crucible applied at elevated temperature process.
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but not as a limitation of the invention.
Embodiment 1
Cut-off footpath is the Graphite Electrodes of 20mm, and the hole that diameter is 3mm is opened at center, installs, for subsequent use.
Regulate second depressurized valve to make gas outlet pressure be 0.06Mpa, adjust flux meter Valve controlling flow is 0.8m
3/ h, connects hydrogen, for subsequent use.10 inches of moulds and die coat for subsequent use.
Mould rotates with the speed of 110 revs/min, and after being used by quartz sand shaping jig shaping in a mold, quartz sand organizer enters specified location together with die coat.
Regulate mould to rotate with the speed of 100 revs/min, covering heat shading apparatus moves to distance die coat edge 15mm suitable for reading, and gas is 0.06Mpa from the aperture Graphite Electrodes with pressure, and flow is 0.8m
3/ h enters quartz crucible shape idiosome internal cavities, the vacuum pump that unlatching is connected with die coat is also bled for-0.07MPa with pressure, apart from the mould above 5cm starting the arc suitable for reading bottom Graphite Electrodes group, power is that 220kW makes it melt to the heating of quartz crucible shape idiosome.Continue to pass into gas to close after 1.5 minutes, bleed for-0.01MPa with pressure again, covering heat shading apparatus moves to distance die coat edge 40mm suitable for reading, the bottom of Graphite Electrodes group is in mould above 10cm position suitable for reading, power is that 450kW makes its melt-forming to quartz crucible shape idiosome continuation heating, and the time length is 2 minutes.
Close vacuum pump, mould rotates with 95 revs/min of speed, and covering heat shading apparatus moves to distance die coat edge 15mm suitable for reading, regulates Graphite Electrodes group to make to be positioned at the straight wall portion mid-way of quartz crucible bottom it, power be 500kW to the melting again of straight wall portion, continue 2 minutes; Regulate Graphite Electrodes group make bottom its apart from 5cm bottom quartz crucible, power be 600kW to bottom melting again, continue 1.5 minutes; Regulate Graphite Electrodes group to make it apart from 10cm bottom quartz crucible, power be 700kW to the melting again of R angular distortion portion, continue 1 minute; Cut off the electricity supply, naturally cooling 5 minutes, comes out of the stove.
Embodiment 2
Cut-off footpath is the Graphite Electrodes of 40mm, and electrode centers opens the hole that diameter is 5mm, installs, for subsequent use.
Regulate reducing valve to make gas outlet pressure be 0.1Mpa, adjust flux meter Valve controlling flow is 1.2m
3/ h, connects nitrogen and helium mix gas (wherein nitrogen accounts for 20%, and helium accounts for 80%), for subsequent use.20 inches of moulds and die coat for subsequent use.
Mould rotates with the speed of 90 revs/min, and after being used by quartz sand shaping jig shaping in a mold, quartz sand organizer enters specified location together with die coat.
Regulate mould to rotate with the speed of 85 revs/min, covering heat shading apparatus moves to distance die coat edge 25mm suitable for reading, and gas is 0.1Mpa from the aperture Graphite Electrodes with pressure, and flow is 1.2m
3/ h enters quartz crucible shape idiosome internal cavities, the vacuum pump that unlatching is connected with die coat is also bled for-0.08MPa with pressure, apart from the mould above 8cm starting the arc suitable for reading bottom Graphite Electrodes group, power is that 400kW makes it melt to the heating of quartz crucible shape idiosome.Continue to pass into gas to close after 3 minutes, bleed for-0.015MPa with pressure again, covering heat shading apparatus moves to distance die coat edge 50mm suitable for reading, the bottom of Graphite Electrodes group is in mould following 5cm position suitable for reading, power is that 650kW makes its melt-forming to quartz crucible shape idiosome continuation heating, and the time length is 4 minutes.
Close vacuum pump, mould rotates with 80 revs/min of speed, and covering heat shading apparatus moves to distance die coat edge 30mm suitable for reading, regulates Graphite Electrodes group to make to be positioned at the straight wall portion mid-way of quartz crucible bottom it, power be 650kW to the melting again of straight wall portion, continue 3 minutes; Regulate Graphite Electrodes group to make apart from 8cm bottom quartz crucible bottom it, power be 700kW to bottom melting again, continue 2 minutes; Regulate Graphite Electrodes group to make apart from 13cm bottom quartz crucible bottom it, power be 800kW to the melting again of R angular distortion portion, continue 1 minute; Cut off the electricity supply, naturally cooling 10 minutes, comes out of the stove.
Embodiment 3
Cut-off footpath is the Graphite Electrodes of 55mm, and electrode centers opens the hole that diameter is 8mm, installs, for subsequent use.
Regulate reducing valve to make gas outlet pressure be 0.18Mpa, adjust flux meter Valve controlling flow is 2.5m
3/ h, connects argon gas, for subsequent use.28 inches of moulds and die coat for subsequent use.
Mould rotates with the speed of 75 revs/min, and after being used by quartz sand shaping jig shaping in a mold, quartz sand organizer enters specified location together with die coat.
Regulate mould to rotate with the speed of 70 revs/min, covering heat shading apparatus moves to distance die coat edge 40mm suitable for reading, and gas is 0.18Mpa from the aperture Graphite Electrodes with pressure, and flow is 2.5m
3/ h enters quartz crucible shape idiosome internal cavities, the vacuum pump that unlatching is connected with die coat is also bled for-0.09MPa with pressure, apart from the mould above 13cm starting the arc suitable for reading bottom Graphite Electrodes group, power is that 550kW makes it melt to the heating of quartz crucible shape idiosome.Continue to pass into gas to close after 5 minutes, bleed for-0.02MPa with pressure again, covering heat shading apparatus moves to distance die coat edge 60mm suitable for reading, the bottom of Graphite Electrodes group is in mould following 10cm position suitable for reading, power is that 800kW makes its melt-forming to quartz crucible shape idiosome continuation heating, and the time length is 7 minutes.
Close vacuum pump, mould rotates with 68 revs/min of speed, and covering heat shading apparatus moves to distance die coat edge 40mm suitable for reading, regulates Graphite Electrodes group to make to be positioned at the straight wall portion mid-way of quartz crucible bottom it, power be 820kW to the melting again of straight wall portion, continue 3 minutes; Regulate Graphite Electrodes group to make apart from 15cm bottom quartz crucible bottom it, power be 880kW to bottom melting again, continue 4 minutes; Regulate Graphite Electrodes group to make apart from 18cm bottom quartz crucible bottom it, power be 960kW to the melting again of R angular distortion portion, continue 2 minutes; Cut off the electricity supply, naturally cooling 15 minutes, comes out of the stove.
Although the present invention discloses as above with preferred embodiment, the present invention is not defined in this.Any those skilled in the art, without departing from the spirit and scope of the present invention, all can do various variation and amendment, and therefore, protection scope of the present invention should be as the criterion with claim limited range.
Claims (8)
1. a manufacture method for repeatedly drawn monocrystalline silicon quartz crucible, wherein said quartz crucible comprises the vague and general transparent inner layer of bubble and is rich in the skin of bubble, and described manufacture method comprises the steps:
The first step, in the mould rotated, supply the step that quartz sand raw material forms crucible shape idiosome, it is specifically divided into:
1) mould is built into the passage having and can apply air-breathing/bleed, makes dies cavity be connected to vacuum pump by these passages through the chamber of die coat;
2) mould is installed on turning axle together with die coat, this mould is rotated with the first speed of rotation around this turning axle, to be pressed onto well on the inwall of mould by quartz sand under motor drives;
3) with the moulding stick with certain size radian the quartz sand being pressed in mould inner wall scraped and make required shape;
4) covering heat shading apparatus of quartz crucible is arranged at the top of described mould, described covering heat shading apparatus can move up and down above mould;
5) Graphite Electrodes group is arranged on above mould movably, makes the axis of described electrode group and described rotating shaft coaxle;
Wherein, centered by each Graphite Electrodes of described Graphite Electrodes group, have aperture, formation stages can be founded at quartz crucible and pass into gas to quartz crucible shape idiosome internal cavities;
Second step, quartz glass crucibles forming step, it is specifically divided into:
1) described mould is rotated with the second speed of rotation, and make described covering heat shading apparatus move to first distance at distance die coat edge suitable for reading;
2) gas is entered the internal cavities of quartz crucible shape idiosome with the first pressure, first flow from the aperture Graphite Electrodes;
3) open the vacuum pump be connected with die coat and bleed with the first suction pressure;
4) make Graphite Electrodes group be positioned at the first location starting the arc, the electric arc forming the first power makes it melt to the heating of quartz crucible shape idiosome;
5) close after continuing to pass into gas very first time T1;
6) then bleed with the second suction pressure, make described covering heat shading apparatus move to the second distance place at distance die coat edge suitable for reading;
7) make Graphite Electrodes group be positioned at the second position again, the electric arc forming the second power continues heating to quartz crucible shape idiosome makes its melt-forming, continues the second time T2;
3rd step, utilize electric arc melting to make the step of described quartz glass crucibles internal surface melting process of refinement again, it is specifically divided into:
1) vacuum pump is closed;
2) described mould is rotated with the 3rd speed of rotation, make covering heat shading apparatus move to the 3rd distance at distance die coat edge suitable for reading;
3) by above-mentioned second step quartz glass crucibles forming step form quartz crucible internal surface be divided into straight wall portion, bottom and R angular distortion portion virtually, and respectively melting is again carried out to various piece, reduce further with the microbubble making the internal surface of its each several part exist; It is specifically subdivided into:
3.1) straight wall portion melting step again: Graphite Electrodes group is placed in the 3rd position, the electric arc of the 3rd power P 3 formed to make electrode group, to the melting again of straight wall portion, continues the 3rd time T3;
3.2) bottom melting step again: Graphite Electrodes group is placed in the 4th position, the electric arc of the 4th power P 4 formed to make electrode group, to bottom melting again, continues the 4th time T4;
3.3) R angular distortion portion melting step again: Graphite Electrodes group is placed in the 5th position, the electric arc of the 5th power P 5 formed to make electrode group, to the melting again of R angular distortion portion, continues the 5th time T5;
Wherein, described 3rd time, the 4th time and the 5th time meet: T3>T5 and T4>T5, and described 3rd power, the 4th power and the 5th power meet: P5>P3 and P4>P3;
4th step, naturally cooling is come out of the stove step: it is specifically divided into:
1) the 3rd step continues to cut off the electricity supply after 1 ~ 30 minute, and naturally cooling was come out of the stove after 5 ~ 30 minutes;
2) bubble volume density obtaining outer bubble layer is 40% ~ 80%, the vague and general layer bubble volume density of internal layer bubble lower than 0.0008% quartz glass crucibles; Wherein:
Described first pressure passing into gas is 0.05 ~ 0.2Mpa, and described first flow is 0.5 ~ 4m
3/ h;
The described very first time continuing to pass into gas is 1 ~ 10 minute, and continuing heating and continuous second time is 2 ~ 15 minutes;
The first described speed of rotation is 50 ~ 120 revs/min, and the second speed of rotation is 70 ~ 100 revs/min, and the 3rd speed of rotation is 50 ~ 120 revs/min;
The first described suction pressure is-0.1 ~-0.05MPa, and the second suction pressure is-0.03 ~ 0MPa;
The first distance that described covering heat shading apparatus moves to distance die coat edge suitable for reading is 15 ~ 50mm, and second distance is 40 ~ 80mm, and the 3rd distance is 10 ~ 50mm;
Described Graphite Electrodes group first location is apart from mould above 5 ~ 20cm suitable for reading bottom electrode group, the second position is at mould following 15cm ~ mould suitable for reading above 10cm suitable for reading bottom electrode group, 3rd position is be positioned at quartz crucible straight wall portion mid-way height bottom electrode group, 4th position is apart from 5 ~ 20cm bottom quartz crucible bottom electrode group, and the 5th position is apart from 10 ~ 30cm bottom quartz crucible bottom electrode group;
The first described power is 200 ~ 600kW, and the second power is 400 ~ 800kW, and the 3rd power is 450 ~ 850kW, and the 4th power is 600 ~ 1000kW, and the 5th power is 700 ~ 1200kW;
Melting the 3rd time is 1 ~ 10 minute to described straight wall portion again, and melting the 4th time is 1 ~ 15 minute again in bottom, and melting the 5th time is 1 ~ 5 minute again in R angular distortion portion.
2. manufacture method according to claim 1, wherein in the quartz glass crucibles internal surface 1mm degree of depth bubble volume density lower than 0.0005%.
3. manufacture method according to claim 1, is characterized in that: make the vague and general layer thickness of bubble account for whole crucible wall thickness 20% ~ 50%, and bubble layer thickness accounts for whole crucible wall thickness 50% ~ 80%.
4. manufacture method according to claim 1, is characterized in that: Graphite Electrodes center has a diameter to be the aperture of 3 ~ 10mm, and gas thus aperture enters.
5. manufacture method according to claim 1, is characterized in that: the gas passed into is a kind of gas in hydrogen, nitrogen, helium, argon gas or other rare gas elementes or several mixed gas.
6. manufacture method according to claim 5, is characterized in that: in the gas mixture passed into, the content of a certain gas is 1 ~ 99%.
7. a repeatedly drawn monocrystalline silicon quartz crucible, it is characterized in that: manufactured by any one manufacture method in the claims 1 ~ 6, the bubble volume density of the outer bubble layer of this quartz glass crucibles is 40% ~ 80%, the vague and general layer bubble volume density of internal layer bubble lower than 0.0008% quartz glass crucibles.
8. quartz crucible according to claim 7, is characterized in that: in the quartz glass crucibles internal surface 1mm degree of depth, bubble volume density is lower than 0.0005%.
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| CN201410384473.6A CN104150755B (en) | 2014-08-07 | 2014-08-07 | Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof |
| PCT/CN2014/090685 WO2016041242A1 (en) | 2014-08-07 | 2014-11-10 | Quartz crucible used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method therefor |
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| CN201410384473.6A CN104150755B (en) | 2014-08-07 | 2014-08-07 | Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104150755B (en) * | 2014-08-07 | 2015-06-17 | 南通路博石英材料有限公司 | Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof |
| CN106544726A (en) * | 2016-11-30 | 2017-03-29 | 江苏恒合科技有限公司 | A kind of crystal pulling, charging, material, the method for separating the continuous drawing silicon single crystal rod that impurity is synchronously carried out |
| CN107287652A (en) * | 2017-05-29 | 2017-10-24 | 德令哈晶辉石英材料有限公司 | A kind of silica crucible for suppressing melting silicon liquid level vibration and preparation method thereof |
| CN109112613B (en) * | 2017-06-22 | 2021-03-12 | 内蒙古欧晶科技股份有限公司 | Preparation process of quartz crucible |
| CN108642560A (en) * | 2018-05-21 | 2018-10-12 | 宁晋晶兴电子材料有限公司 | A kind of preparation method of large scale silica crucible |
| CN113735421A (en) * | 2020-05-28 | 2021-12-03 | 隆基绿能科技股份有限公司 | Quartz crucible manufacturing method and forming device |
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| CN115745382A (en) * | 2022-12-22 | 2023-03-07 | 宁夏鑫晶新材料科技有限公司 | Quartz crucible preparation process for improving microbubbles on transparent layer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624258A (en) * | 2008-07-10 | 2010-01-13 | 日本超精石英株式会社 | Method for manufacturing quartz glass crucibles |
| CN102180589A (en) * | 2009-12-30 | 2011-09-14 | 圣戈班石英有限公司 | Silica crucible |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5377930B2 (en) * | 2008-10-31 | 2013-12-25 | 株式会社Ｓｕｍｃｏ | Method for producing quartz glass crucible for pulling silicon single crystal |
| US9376761B2 (en) * | 2012-01-13 | 2016-06-28 | Shin-Etsu Quartz Products Co., Ltd. | Single-crystal silicon pulling silica container and method for producing the same |
| CN104150755B (en) * | 2014-08-07 | 2015-06-17 | 南通路博石英材料有限公司 | Quartz crucible capable of being used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method thereof |
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| CN101624258A (en) * | 2008-07-10 | 2010-01-13 | 日本超精石英株式会社 | Method for manufacturing quartz glass crucibles |
| CN102180589A (en) * | 2009-12-30 | 2011-09-14 | 圣戈班石英有限公司 | Silica crucible |
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