CN105040099A - Single crystal extraction method - Google Patents
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Abstract
The single crystal extraction method is used for shortening the extraction time from the forming of a straight body part to crystal excision from a meltwater, extracting single crystal and improving a rate of finished products. The method comprises a first process, a second process and a third process. The first process forms the straight body part (C2), and the second process is behind the first process. In the final process of forming the straight body part, a lower protruded shape (C3) protruded downwards is formed at the lower end of the crystal, and the third process is configured to cut the lower protruded shape formed in the second process from the silicon meltwater. In the second process, the field density of the horizontal magnetic field is controlled lower than the first process in the range of 800 to 1000 gausses, the crystal extract speed is controlled lower than the first process in the range of 0.2 to 0.5 mm/min, the crystal rotation speed is controlled lower than the first process in the range of 1 to 3 rpm, and the crucible rotation speed is controlled in the range of 0.5 to 5 rpm.
Description
Technical field
The present invention relates to and cultivate according to cutting krousky single crystal growing method (hereinafter referred to as " CZ method ") the monocrystalline extracting method that monocrystalline extracts monocrystalline simultaneously.
Background technology
About the cultivation of silicon single crystal, CZ method is widely used.In the method, as shown in Figure 4, by the heat of the side heater 52 in calciner 55 at quartz glass crucibles 50(hereinafter referred to only crucible 50) in form the fused solution M of silicon.Then, by emission shield 51 by around in the scope of surrounding, make crystal seed P be contacted with the surperficial M1 of fused solution M, crucible 50 rotated, and this crystal seed P is rotated in reverse direction extract upward simultaneously, form monocrystalline C in the lower end of crystal seed P thus.
Specifically, carry out the necking down of the terminal part melting crystal seed P to form neck P1, from neck P1, crystal diameter being expanded and form shoulder C1, also forming the stretched portion C2 by forming product section.
At this, when stretched portion C2 reaches certain length, be necessary to cut off monocrystalline C from fused solution M, if cut off under the state that stretched portion C2 is thick, the bottom of the monocrystalline C then after cutting off produces temperature variation sharply, in monocrystalline, produce gliding dislocations, and monocrystalline rate declines.
Therefore, carried out following operation: after formation stretched portion C2, form the afterbody slowly drawn in by crystal diameter, under the state making the contact surface of monocrystalline C and melting liquid level M1 fully reduce, cut off by monocrystalline C from melting liquid level M1 in the past.
But in the formation process of aforementioned afterbody, activity time is longer, and can not use as product because crystal diameter is less, become the reason that yield rate is low.Therefore, shorten or omit this afterbody formation process and become problem.
For such problem, in Japanese Unexamined Patent Publication 2012-36042 publication, disclose following method: after stretched portion is formed, under the state making the lifting of crucible stop, stop the extraction of silicon single crystal completely, after the growth face entirety of the crystal lower end (solid-liquid interface) by being contacted with fused solution is formed as the lower convex form given prominence to downwards, cut off monocrystalline from fused solution.
That is, utilize following method: although when the extraction of stretched portion C2, the shape of crystal lower end is the epirelief shape outstanding to crystal side, and by stopping extracting, crystal lower end flattens, and afterwards, grows up along direction outstanding downwards.
Whether form the judgement of sufficient convex form in crystal lower end, be monitor the change by the apparent weight (deducting the buoyancy of fused solution from the weight of silicon single crystal) of the monocrystalline cultivated, the change based on weight is carried out.
According to such monocrystalline extracting method, the manufacturing time of monocrystalline can be shortened compared with the afterbody formation process implemented in the past.
But, in monocrystalline extracting method disclosed in Japanese Unexamined Patent Publication 2012-36042 publication, for crystal lower end is formed as lower convex form, need the lifting stopping crucible, and the state stopping crystal extracting is maintained given time, so significantly can not shorten the time compared with the situation of the afterbody formation process implemented in the past.
In addition, because the judgement whether forming suitable convex form in crystal lower end is carried out in the apparent weight change by detecting monocrystalline, if the precision of weight determination is lower, then can not obtain suitable convex form, having the danger producing dislocation in crystal.That is, when the formation of convex form is insufficient, produce temperature variation sharply in crystal bottom, have the danger producing gliding dislocations in monocrystalline, when in extremely sharp-pointed convex state, fused solution overcooling thus there is the danger of dislocation.
Summary of the invention
The present invention carries out in the previous case, the object of invention is to provide a kind of monocrystalline extracting method, extracting the monocrystalline extracting method of silicon single crystal according to cutting krousky single crystal growing method from crucible, the extraction time to cutting off monocrystalline from fused solution from stretched portion is formed can be shortened, extracting monocrystalline when not producing dislocation, improving yield rate.
For solving foregoing problems, relate to monocrystalline extracting method of the present invention and form silicon melt in crucible, horizontal magnetic field is applied to aforementioned silicon melt, and extract silicon single crystal according to cutting krousky single crystal growing method from aforementioned silicon melt, it is characterized in that, described monocrystalline extracting method comprises the 1st operation, 2nd operation and the 3rd operation, described 1st operation forms stretched portion, described 2nd operation is after aforementioned 1st operation, in the final operation that stretched portion is formed, outstanding lower convex form is formed downwards in crystal lower end, the aforementioned lower convex form formed in aforementioned 2nd operation cuts off from aforementioned silicon melt by described 3rd operation, in aforementioned 2nd operation, crystal extraction rate is located at the scope of 0.2 ~ 0.5mm/min to cultivate crystal, by lower than aforementioned 1st operation for the magneticflux-density of horizontal magnetic field the scope controlled in 800 ~ 1000 Gausses, by lower than aforementioned 1st operation for Crystal Rotation speed the scope controlled at 1 ~ 4rpm, by the scope of crucible rotation speed control at 0.5 ~ 5rpm.
In addition, preferably, in aforementioned 2nd operation, scope crystal extraction rate being located at 0.3 ~ 0.5mm/min to cultivate crystal, by the scope of Crystal Rotation speed control at 1 ~ 3rpm, by the scope of crucible rotation speed control at 0.5 ~ 3rpm.
In addition, the length of the vertical of the lower convex form preferably formed in aforementioned crystal lower end is in the scope of 10 ~ 30mm.
According to the method, in stretched portion forming process, outstanding lower convex form can be formed downwards in crystal lower end at short notice.
Consequently, in indeformable situation, monocrystalline can be cut off from fused solution with the state not producing dislocation, significantly can shorten the extraction time to cutting off monocrystalline from fused solution from stretched portion is formed, improve yield rate.
According to the present invention, extracting the monocrystalline extracting method of silicon single crystal according to cutting krousky single crystal growing method from crucible, the extraction time to cutting off monocrystalline from fused solution from stretched portion is formed can being shortened, monocrystalline can be extracted when not producing dislocation, improve yield rate.
Accompanying drawing explanation
Fig. 1 represents the sectional view implementing to relate to the local structure of the monocrystalline extraction element of monocrystalline extracting method of the present invention.
Fig. 2 is the schema of the flow process representing the monocrystalline extracting method implemented in the monocrystalline extraction element of Fig. 1.
Fig. 3 represents the sectional view according to the length relating to the lower convex form that monocrystalline extracting method of the present invention is formed in crystal lower end in stretched portion forming process.
Fig. 4 is the sectional view for illustration of monocrystalline abstraction process.
Embodiment
Below, based on accompanying drawing, the embodiment relating to monocrystalline extracting method of the present invention is described.Fig. 1 represents the sectional view implementing to relate to the local structure of the monocrystalline extraction element of monocrystalline extracting method of the present invention.
This monocrystalline extraction element 1 possesses body of heater 10, described body of heater 10 is formed with concubine 10b overlappingly above columnar main chamber 10a, described monocrystalline extraction element 1 also possesses carbon pedestal (or graphite base) 2 and quartz glass crucibles 3(hereinafter referred to only crucible 3), described carbon pedestal (or graphite base) 2 can rotate around vertical axis and can arrange up and down in this body of heater 10, and described quartz glass crucibles 3(is hereinafter referred to only crucible 3) kept by aforementioned carbon pedestal 2.
Bottom 3b under aforementioned crucible 3 has stretched portion 3a and is formed at it, together can rotate around vertical axis with the rotation of carbon pedestal 2.
In addition, in the below of carbon pedestal 2, be provided with rotary driving part 14 and lifting driving part 15, described rotary driving part 14 is rotation motors etc. that this carbon pedestal 2 is rotated around vertical axis, and described lifting driving part 15 makes carbon pedestal 2 lifting moving.
In addition, rotary driving part 14 is connected with rotary actuation control part 14a, lifting driving part 15 is connected with lifting drive control part 15a.
In addition, monocrystalline extraction element 1 possesses well heater 4 and extraction mechanism 9, described well heater 4 is by resistive heating, by the raw semiconductor filled in crucible 3 (raw material polysilicon) melting to form silicon melt M(hereinafter referred to only fused solution M), described extraction mechanism 9 rolls wire rod 6, extracts by the monocrystalline C cultivated.The end of the wire rod 6 had in aforementioned extraction mechanism 9 is provided with crystal seed P.
In addition, side heater 4 is connected with the heater-driven control part 4a controlling delivery, in extraction mechanism 9, is connected with the rotary actuation control part 5a of the control carrying out its rotary actuation.
In addition, in this monocrystalline extraction element 1, have in the arranged outside of body of heater 2 and apply magnetic field solenoid 8.When applying set electric current to this applying magnetic field solenoid 8, apply the horizontal magnetic field of given strength relative to the silicon melt M in crucible 3.In applying magnetic field with on solenoid 8, be connected with the solenoid controlled portion 8a carrying out its action control.
That is, in the present embodiment, implementing applying magnetic field in fused solution M to cultivate the MCZ method (magnetic control vertical pulling method) of monocrystalline, controlling the convection current of silicon melt M thus, realize the stable of single crystallization.
In addition, being formed at above the fused solution M in crucible 3, the emission shield 7 of the surrounding surrounding monocrystalline C is configured with.The upper and lower of this emission shield 7 forms opening, cover relative to the monocrystalline C in cultivating, from the unnecessary radiant heat of side heater 4 and fused solution M etc., and by the air-flow rectification in stove.In addition, the gap between the lower end of emission shield 7 and melting liquid level is controlled as, and the characteristic of the hope of the monocrystalline that correspondence will be cultivated, maintains set distance.
In addition, this monocrystalline extraction element 1 possesses the computer 11 with storing device 11a and operation control device 11b, and rotary actuation control part 14a, lifting drive control part 15a, solenoid controlled portion 8a, rotary actuation control part 9a are connected to operation control device 11b.
Such as, in the monocrystalline extraction element 1 formed like this, when cultivating the monocrystalline C of diameter 300mm, as described belowly to extract.That is, first load raw material polysilicon (such as 350kg) to crucible 3, start crystal based on the program stored in the storing device 11a of computer 11 and cultivate operation.
First, be set as set atmosphere surrounding (being mainly the atmosphere surrounding of argon gas) in body of heater 10, fill in the raw material polysilicon in crucible 3 and be melted by the heating of side heater 4, become fused solution M.And then crucible 3 carries out spinning movement with set speed of rotation (rpm) on set height location.
Then, in applying magnetic field solenoid 8, flow through set electric current, start to apply horizontal magnetic field with the magneticflux-density (such as 3000 Gausses) be set in the scope of 1000 ~ 4000 Gausses in fused solution M.
In addition, wire rod 6 is lowered, and crystal seed P is contacted with fused solution M, carries out the necking down of the terminal part melting crystal seed P, starts the step S1 forming neck P1(Fig. 2).
When forming neck P1, the delivery of counter-lateral quadrents well heater 4, extraction rate, applying magneticstrength etc. being adjusted extraction conditions as parameter, starting to rotate crystal seed P with set speed of rotation along the direction contrary with the sense of rotation of crucible 3.
Then, crystal diameter is gently expanded forms shoulder C1, is transferred to the 1st operation (the step S2 of Fig. 2) of the stretched portion C2 formed forming product section.
In the formation of stretched portion C2, such as, extraction rate is controlled in the scope of 0.6 ~ 0.8mm/min, and Crystal Rotation speed is controlled in the scope of 5 ~ 8rpm, and crucible rotation speed is controlled in the scope of 0.5 ~ 1rpm.By carrying out monocrystalline extraction under such imposing a condition, the silicon single crystal can cultivating diameter 300mm extracts.In addition, the crystal lower end shape during extraction of stretched portion C2 is in the epirelief shape outstanding to crystal side.
Along with the formation in the stretched portion of silicon single crystal C, the carbon pedestal 2 of storage crucible 3 is mobile by rising, maintains the position of emission shield 7 that melting liquid level M1 fixes relative to position and side heater 4.
In addition, suppress the natural convection of fused solution M by applying magnetic field, the magneticflux-density in described magnetic field is set at the scope of 1000 ~ 4000 Gausses, is more preferably set at 2000 ~ 3000 Gausses.
Then, when stretched portion C2 is formed into set length, be transferred to the final operation that stretched portion is formed, i.e. the 2nd operation (the step S3 of Fig. 2).In addition, the transfer to the 2nd operation is preferably carried out in the moment that the curing degree of crystal is 0.7 ~ 0.85.If in the scope of such curing degree, then fully can guarantee the remaining molten liquid after crystal extraction, so raw material can be added again (recharging) to remaining molten liquid, again extract crystal.In addition, when not making decrease in yield, crystal can be pulled away from while guaranteeing crystal to be pulled away from required sufficient remaining molten liquid.
Then, in the 2nd operation, crystal extraction rate continues the cultivation of monocrystalline in the scope of 0.2 ~ 0.5mm/min, more preferably crystal extraction rate continues the cultivation of monocrystalline in the scope of 0.3 ~ 0.5mm/min, the magneticflux-density of horizontal magnetic field is the scope of 800 ~ 1000 Gausses, Crystal Rotation speed is the scope of 1 ~ 4rpm, more preferably drops to the scope of 1 ~ 3rpm.And then crucible rotation speed changes to the scope of 0.5 ~ 5rpm, more preferably change to the scope of 0.5 ~ 3rpm.
At this, when being transferred to the 2nd operation from the 1st operation, if only the magneticflux-density of horizontal magnetic field to be set in lower the scope of 800 ~ 1000 Gausses, then fused solution M is unstable, easy generation crystal modification, but due to the value of adjustment crystal extraction rate, Crystal Rotation speed and crucible rotation speed, control in certain scope, so can not crystal modification be there is.
By setting the value of each parameter in this wise, as shown in Figure 3, the lower end shape (epirelief shape when extracting from aforementioned stretched portion C2) of monocrystalline C is changing into the lower convex form to fused solution M side depression.Specifically, in the shape of the bowl-type of not rocking in interface.
Then, as shown in Figure 3, at short notice, formed in crystal lower end with the length of more than 10mm below 30mm lower convex form C3 outstanding downwards.In addition, the length h of the vertical of aforementioned lower convex form C3 be (negative direction) of the point of contact Pt of germ nucleus axle CA when the height of melting liquid level M1 being set to 0 and solid-liquid interface highly.At this, the length h of aforementioned lower convex form C3 less than 10mm when, the shape of crystal lower end close to smooth, so become greatly with the contact area of fused solution M, become be easy to produce dislocation.The length of aforementioned lower convex form C3 more than 30mm when, fused solution M overcooling, have before cutting off crystal from fused solution M produce dislocation danger.
Then, when crystal lower end forms aforementioned lower convex form C3, be transferred to the 3rd operation (the step S4 of Fig. 2).In the 3rd operation, the contact area of aforementioned lower convex form C3 and fused solution M slowly reduces, and is cut off by monocrystalline C and fused solution M by forming lower convex form C3 fully.
Basis described above relates to embodiments of the present invention, in the stretched portion forming process of monocrystalline, formed in the 2nd operation of outstanding lower convex form downwards in crystal lower end, with the cultivation that crystal extraction rate is 0.2 ~ 0.5mm/min continuation monocrystalline, distinguish the scope of magneticflux-density in 800 ~ 1000 Gausses in level of control magnetic field simultaneously, Crystal Rotation speed is in the scope of 1 ~ 3rpm, and crucible rotation speed is in the scope of 0.5 ~ 5rpm.Thus, crystal is necking down at short notice, forms outstanding lower convex form downwards.
Consequently, in indeformable situation, monocrystalline can be cut off from fused solution with the state of dislocation-free, significantly shorten the extraction time to cutting off monocrystalline from fused solution from stretched portion is formed, can yield rate be improved.
In addition, according to the crystal relating to monocrystalline extracting method of the present invention and manufacture, can as such as FR(focusing ring) crystal use.
Embodiment
Be further detailed relating to monocrystalline extracting method of the present invention based on embodiment.In the present embodiment, use the monocrystalline extraction element represented in the foregoing embodiment to carry out monocrystalline extraction, the crystal extracted is verified.
Specifically, after the 1st operation forming stretched portion, in final operation i.e. the 2nd operation (during curing degree 0.77) that stretched portion is formed, implement embodiment 1 ~ 8, the comparative example 1 ~ 13 distinguished according to each condition of magneticflux-density, crystal extraction rate, Crystal Rotation speed, crucible rotation speed.Then, for the crystal be extracted, judge extraction when can carry out dislocation-free, whether there is the length of distortion, lower convex form.The diameter of the monocrystalline cultivated is 390mm, loads the silicon crystal raw material of 350kg in crucible.
In addition, the condition of the 1st operation is set to, and magneticflux-density is 3000 Gausses, and crystal extraction rate is 0.6 ~ 0.8mm/min, and Crystal Rotation speed is 6rpm, and crucible rotation speed is 0.5rpm.
Represent condition and the evaluation result of embodiment 1 ~ 8, comparative example 1 ~ 13 in Table 1.In addition, in the result of table 1, zero represent condition can obtain dislocation-free and without distortion monocrystalline, realize the significantly shortening of monocrystalline extraction time compared with the past, the condition that △ represents can obtain dislocation-free and without distortion monocrystalline, but need to expend time in extraction, the condition of × expression can produce dislocation or distortion.
Table 1
| Magneticstrength (Gauss) | Crystal Rotation (rpm) | Crucible rotation (rpm) | Extraction rate (mm/min) | Stand-by time (hr) | Dislocation | Distortion | Lower convexity | Result | |
| Comparative example 1 | 500 | 2 | 0.5 | 0.5 | - | Have | Have | - | × |
| Comparative example 2 | 700 | 2 | 0.5 | 0.5 | - | Have | Have | - | × |
| Embodiment 1 | 800 | 2 | 0.5 | 0.5 | - | Nothing | Nothing | Convex under 21mm | ○ |
| Comparative example 3 | 1000 | 0.5 | 0.5 | 0.5 | - | Have | Have | - | × |
| Embodiment 2 | 1000 | 1 | 0.5 | 0.5 | - | Nothing | Nothing | Convex under 15mm | ○ |
| Comparative example 4 | 1000 | 2 | 0.3 | 0.5 | - | Have | Nothing | Convex under 5mm | × |
| Comparative example 5 | 1000 | 2 | 0.5 | 0.1 | - | Nothing | Nothing | Convex under 19mm | △ |
| Embodiment 3 | 1000 | 2 | 0.5 | 0.2 | - | Nothing | Nothing | Convex under 17mm | ○ |
| Embodiment 4 | 1000 | 2 | 0.5 | 0.5 | - | Nothing | Nothing | Convex under 13mm | ○ |
| Comparative example 6 | 1000 | 2 | 0.5 | 0.6 | - | Have | Have | - | × |
| Embodiment 5 | 1000 | 2 | 0.5 | 0.4 | - | Nothing | Nothing | Convex under 15mm | ○ |
| Embodiment 6 | 1000 | 2 | 3 | 0.5 | - | Nothing | Nothing | Convex under 15mm | ○ |
| Embodiment 7 | 1000 | 2 | 5 | 0.5 | - | Nothing | Nothing | Convex under 18mm | ○ |
| Comparative example 7 | 1000 | 2 | 7 | 0.5 | - | Have | Have | - | × |
| Embodiment 8 | 1000 | 3 | 0.5 | 0.5 | - | Nothing | Nothing | Convex under 10mm | ○ |
| Comparative example 8 | 1000 | 5 | 0.5 | 0.5 | - | Have | Have | - | × |
| Comparative example 9 | 1100 | 2 | 0.5 | 0.5 | - | Have | Nothing | Convex under 6mm | × |
| Comparative example 10 | 2000 | 2 | 0.5 | 0.5 | - | Have | Nothing | Epirelief | × |
| Comparative example 11 | 3000 | 2 | 0.5 | 0 | 1 | Have | Nothing | Epirelief | × |
| Comparative example 12 | 3000 | 2 | 0.5 | 0 | 2 | Nothing | Nothing | Smooth | △ |
| Comparative example 13 | 3000 | 2 | 0.5 | 0.5 | - | Have | Nothing | Epirelief | × |
In embodiment 1 ~ 8, expend time in as less than about 24 hours to cutting off crystal from fused solution from stretched portion is formed.
On the other hand, arrange in the comparative example 12 of stand-by time after stretched portion is formed, expend time in as less than about 25.5 hours to cutting off crystal from fused solution from stretched portion is formed.
The result of this embodiment is, in final operation i.e. the 2nd operation that stretched portion is formed, condition in embodiment 1 ~ 8, namely, the magneticflux-density of horizontal magnetic field is in the scope of 800 ~ 1000 Gausses, crystal extraction rate is at 0.2 ~ 0.5mm/min(more preferably 0.3 ~ 0.5mm/min) scope, Crystal Rotation speed is at 1 ~ 4rpm(more preferably 1 ~ 3rpm) scope, crucible rotation speed is at 0.5 ~ 5rpm(more preferably 0.5 ~ 3rpm) scope, the outstanding lower convex form of the length of more than 10mm below 30mm is formed at short notice downwards in crystal lower end, can shorten from stretched portion is formed to the extraction time cutting off crystal from fused solution.
Further, confirm the lower convex form that can form the length of more than 10mm below 30mm in crystal lower end, obtain dislocation-free and without the monocrystalline of distortion.
Claims (3)
1. a monocrystalline extracting method, described monocrystalline extracting method forms silicon melt in crucible, applies horizontal magnetic field to described silicon melt, and extracts silicon single crystal according to cutting krousky single crystal growing method from described silicon melt, it is characterized in that,
Comprise the 1st operation, the 2nd operation and the 3rd operation,
Described 1st operation forms stretched portion,
Described 2nd operation, after described 1st operation, in the final operation that stretched portion is formed, forms outstanding lower convex form downwards in crystal lower end,
The described lower convex form formed in described 2nd operation cuts off from described silicon melt by described 3rd operation,
In described 2nd operation,
Crystal extraction rate is located at the scope of 0.2 ~ 0.5mm/min to cultivate crystal,
By lower than described 1st operation for the magneticflux-density of horizontal magnetic field the scope controlled in 800 ~ 1000 Gausses,
By lower than described 1st operation for Crystal Rotation speed the scope controlled at 1 ~ 4rpm,
By the scope of crucible rotation speed control at 0.5 ~ 5rpm.
2. monocrystalline extracting method as claimed in claim 1, is characterized in that,
In described 2nd operation,
Crystal extraction rate is located at the scope of 0.3 ~ 0.5mm/min to cultivate crystal,
By the scope of Crystal Rotation speed control at 1 ~ 3rpm,
By the scope of crucible rotation speed control at 0.5 ~ 3rpm.
3. monocrystalline extracting method as claimed in claim 1 or 2, is characterized in that,
The length of the vertical of the lower convex form formed in described crystal lower end is in the scope of 10 ~ 30mm.
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| JP2014-087151 | 2014-04-21 | ||
| JP2014087151A JP2015205793A (en) | 2014-04-21 | 2014-04-21 | Method for drawing up single crystal |
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| CN109763167A (en) * | 2019-03-15 | 2019-05-17 | 靳俊改 | A kind of single crystal silicon semiconductor pulling machine |
| CN110249080A (en) * | 2016-12-20 | 2019-09-17 | 胜高股份有限公司 | The manufacturing method of monocrystalline silicon |
| CN115233297A (en) * | 2022-07-25 | 2022-10-25 | 北京麦竹吉科技有限公司 | Czochralski single crystal pulling method without ending and silicon single crystal |
| CN115233298A (en) * | 2022-07-25 | 2022-10-25 | 北京麦竹吉科技有限公司 | Re-immersion type non-ending Czochralski method and silicon single crystal |
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| CN111379030A (en) * | 2020-05-03 | 2020-07-07 | 朱雪玉 | Novel semiconductor crystal bar arrangement forming die |
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