CN104514031A - Czochralski monocrystalline silicon doping apparatus and use method thereof - Google Patents
Czochralski monocrystalline silicon doping apparatus and use method thereof Download PDFInfo
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- CN104514031A CN104514031A CN201310651433.9A CN201310651433A CN104514031A CN 104514031 A CN104514031 A CN 104514031A CN 201310651433 A CN201310651433 A CN 201310651433A CN 104514031 A CN104514031 A CN 104514031A
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Abstract
The invention discloses a Czochralski monocrystalline silicon doping apparatus and a use method thereof. The apparatus includes a supporting frame (2), a sliding device (1) nested to a supporting frame sliding rod, a doping container (3) connected with the supporting frame (2) and the sliding device, and connecting ropes or rods (4) used for connection. The invention also discloses the use method of the doping apparatus. The accurate and rapid doping of Czochralski monocrystalline silicon can be realized in the invention.
Description
Technical field
The invention belongs to growing semiconductor crystal field, particularly a kind of adulterating method of czochralski silicon monocrystal and doper, can realize pulling of silicon single crystal and accurately adulterate fast.
Background technology
Pulling of silicon single crystal growth method is also known as cutting krousky (Czochralski) method, and be called for short the primary growth technology that CZ method is current single crystal silicon semiconductor, the materials of electronic components more than 98% all uses silicon single crystal.Wherein account for about 85% by CZ method.Polysilicon is mainly put into quartz crucible by pulling of crystals silicon technology, heating and melting in thermal field of single crystal furnace, and takes suitable doping, utilizes seed crystal and temperature to control a kind of method of lifting crystal growth from melt.Of a great variety due to semiconducter device, purposes otherness is very large, therefore has very large difference to the requirement of silicon single crystal resistivity, and how accurately controlled doping is the difficult point and emphasis that face in single crystal silicon semiconductor production reality.
Adulterating method main is at present divided into two classes, and a class is eutectic method, and another kind of is throw-in play.Eutectic method refers to that hotchpotch is put into crucible together with polycrystal to be melted; Throw-in play refers to after polycrystal dissolves completely, hotchpotch is dropped into fusing by various doper and adulterating method, realizes doping.Eutectic method is that doping agent or hotchpotch are put into single crystal growing furnace, heat fused together with polycrystal.Be in more than 1450 DEG C high-temperature times because material to crystal growing process will have 5 ~ 8 hours, cause doped element steam output large, doping efficiency is low, process temperature simultaneously, air-flow, the othernesses such as the working of a furnace, also monocrystalline resistivity can be caused accurately to control, and resistivity consistence is poor.Throw-in play refers to after polycrystal fusing, uses doper and correlation method to adulterate, better can realize doping, reduce the steam output of doping agent, improve doping accuracy, can also realize supplementing doping etc., in actual production, combine again feeding technique there is very strong production application.
The heavy doping method of patent ZL00122075.6 Modelling of Crystal Growth in CZ-Si Pulling " middle use silicon single crystal umbrella shape doping device, it is single use, silicon single crystal umbrella shape doping device to be made before using at every turn, need strictly to control temperature, melt temperature steady time be long, doping time poor controllability, doping agent easily siphon away when vacuumizing, so production efficiency is lower.The doper doping efficiency used in the patent 201120085198.X doper of middle high resistant czochralski silicon monocrystal " be applicable to gently to mix and " is better, but due to opened upper end, easily kick up when single crystal growing furnace upper chamber vacuumizes for tiny doping agent, cause the poor accuracy that adulterates.Simultaneously because the container holding doping agent is level and smooth not, when container inclination doping agent drops to melt, element dopants easily remains in a reservoir, therefore accuracy of adulterating in actual use is lower, this device support stand is shelved on slide valve sealing-ring simultaneously, easy scald sealing-ring, affects slide valve sealing property.Use silicon single crystal doper in patent 201010132399.0 " the gallium element adulterating method of czochralski silicon monocrystal and doper used " and be mainly applicable to liquid doping agent doping use, fine doping cannot be carried out for solid dopants, accurately control melt temperature afterwards in doping again simultaneously, realize heterogeneous nucleation, container bottom is sealed, otherwise cannot realize secondary to use, in actually operating, difficulty is larger.
Summary of the invention
In order to solve the problem, the invention provides a kind of doper and using method of pulling of silicon single crystal, the accurately doping fast of pulling of crystals silicon growth can be realized.
The carriage (1) the invention provides a kind of doper and using method of pulling of silicon single crystal, its doper comprises bracing frame (2), being nested with bracing frame litter, the doping container (3) be connected with carriage with bracing frame, for the connection cord that is connected or union lever (4).Support frame as described above is provided with support panel (2-1), be provided with 3 below support panel (2-1) edge to be fixedly linked support bar (2-3) with support panel (2-1), below, support panel (2-1) middle part is provided with the vertical litter (2-2) that 2 have lower limit, vertical litter (2-2) and support panel (2-1) thread connecting mode are fixed, and support panel (2-1) middle part is provided with the first through hole (2-4).Described carriage is provided with hanger bar (1-1), hanger bar (1-1) runs through support panel (2-1) by bracing frame first through hole (2-4), hanger bar (1-1) top is provided with carves type groove, for being fixedly linked use with single crystal furnace seed crystal clamping device, hanger bar (1-1) bottom is provided with the slide block (1-2) be fixedly linked with hanger bar (1-1), slide block (1-2) is provided with second and third through-hole (1-3), use when sliding for vertical with bracing frame litter (2-2), carriage (1) can be slided along vertical litter (2-2) direction.Described doping container (3) comprises separable container upper cover (3-1), in the middle part of container (3-2), container bottom (3-3), container upper cover (3-1) is provided with fourth hole (3-4), it is suitable for reading that container upper cover (3-1) is placed in (3-2) in the middle part of container, and there is better geometrical dimension coupling, in the middle part of container, (3-2) is connected with the vertical litter of bracing frame (2-2) fixed vertical by connection cord or union lever (4), container bottom (3-3) is connected with carriage (1) base slider (1-2) fixed vertical by connection cord or union lever (4) fourth hole (3-4) through container upper cover (3-1).
As preferably, institute's bracing frame (2) and parts thereof, the carriage (1) be nested with vertical litter (2-2) and the material of parts thereof are stainless steel.
As preferably, described doping container (3) and parts thereof adopt high purity quartz material.
As preferably, described connection cord for connecting or union lever (4) adopt high pure metal molybdenum rope or molybdenum rod, stainless steel cable or stainless steel.
The using method of described pulling of silicon single crystal doper is as follows:
1, doper prepare: 1. by hanger bar (1-1) through the first through hole (2-4), vertical litter (2-2) through second and the third through-hole (1-3) of slide block, and is fixedly linked with support panel (2-1); 2. will adulterate container upper cover (3-1) in a reservoir portion (3-2) go up and be fixedly linked with vertical litter (2-2) bottom by connection cord or union lever (4); 3. the container bottom that adulterates (3-3) is fixedly linked with carriage (1) base slider (1-2) by connection cord or union lever (4) fourth hole (3-4) through container upper cover (3-1); 4. said apparatus removing surface is clean, prepare doping and use.
2, the polycrystal raw material required for calculated single crystal growth and doping metering.
3, after thermal field cleans, dropped into by polysilicon in high-purity silica pot, close thermal field and single crystal growing furnace, vacuumize, after checking vacuum leak rate meets production requirement, heating and melting polysilicon, stablizes to melt temperature.
4, single crystal growing furnace flashboard valve gap is utilized to isolate main chamber and concubine; To concubine inflation, unclamp the compact heap of concubine simultaneously; Open concubine door, take off seed crystal, doper hanger bar (1-1) and seed crystal clamping device are fixedly linked, note should carefully cleaning before loading onto this device, guarantee not stain, open doping container upper cover (3-1), and pour ready doping agent into doping container, and build doping container upper cover (3-1), doper is suspended in auxiliary furnace of mono-crystal indoor, height is as the criterion not affect main chamber's concubine middle gate plate valve activity simultaneously.
5, clean concubine, carries out gas washing to concubine and vacuumizes, and opens slide valve and is communicated with concubine and main chamber.
6, decline seed crystal clamping device makes doper steadily decline, after the bracing frame (2) of doper drops to top, main chamber and stops declining, continue decline seed crystal clamping device, make carriage (1) can along the steady slide downward in vertical litter (2-2) direction along with carriage (1) decline, doping container bottom (3-3) synchronously declines, and be separated with (3-2) in the middle part of doping container, doping agent falls in melt gradually, now pay close attention to ullage situation in single crystal growing furnace, guarantee that doping agent all falls into melt, and prevent doping container bottom (3-3) from touching melt.
7, after doping agent all falls into melt, rising seed crystal clamping device, now carriage (1) and doping container bottom (3-3) go up to original height, and lift and stop after whole doper continues to rise to the height not affecting slide valve activity.
8, cover slide valve, again the isolation of main chamber's concubine, and be inflated to normal pressure in concubine, open concubine door, after the cooling some time, take off doper, reinstall seed crystal, vacuumize after clean concubine, be communicated with major-minor room, enter normal single crystal growing link.
9, be put in clean dried place after this device carefully being cleaned, take again when next time uses.
10, this device also can use in charging technology again, and namely charging technology material terminates rear repeating step 4 ~ 9 and can realize doping again.
Advantage of the present invention: doper is simple, it is convenient to realize; Energy available protecting dopant dosage, realizes accurately adulterating; Production efficiency is high, is conducive to reducing production cost.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described:
Fig. 1 describes to obtain doper structure iron in the present invention;
Fig. 2 is each parts diagram of carriage in the Fig. 1 described in the present invention;
Fig. 3 is each parts diagram of Fig. 1 bracing frame described in the present invention.
Fig. 4 is that the Fig. 1 described in the present invention adulterates container each parts diagram.
Fig. 5 is that the doper that describes in the present invention and single crystal growing furnace assemble and illustrate.
Fig. 6 is the diagram that the doper described in the present invention realizes adulterating in single crystal growing furnace.
Fig. 7 is the cylindrical hollow type distressed structure of the doper described in the present invention.
Fig. 8 is the hollow sphere distressed structure of the doper described in the present invention.
Fig. 9 is the taper of the doper doping container bottom described in the present invention or spherical distressed structure.
Embodiment
Embodiment 1
The doper that the present invention relates to install 1. by hanger bar (1-1) through the first through hole (2-4), vertical litter (2-2) through second and the third through-hole (1-3) of slide block (1-2), and is fixedly linked with support panel (2-1); 2. the container upper cover (3-1) that will adulterate is placed on (3-2) in the middle part of container and goes up and be fixedly linked with vertical litter (2-2) bottom by connection cord or union lever (4); 3. the fourth hole (3-4) that the container bottom that adulterates (3-3) passes doping container upper cover (3-1) by connection cord or union lever (4) is fixedly linked with carriage base slider (1-2); 4. said apparatus removing surface is clean, prepare doping and use.
Embodiment 2
The column stainless steel that the hanger bar (1-1) of described carriage is diameter 10mm, length is 200m, be provided with and carve type groove, for being fixedly linked use with single crystal furnace seed crystal clamping device, hanger bar (1-1) bottom is provided with the slide block (1-2) be fixedly linked with hanger bar (1-1), slide block (1-2) is high 10mm, the piece of stainless steel of diameter 80mm, slide block (1-2) is provided with second and third through-hole (1-3), and through-hole diameter is 8.5mm; Support frame as described above (1) is provided with support panel (2-1), plate thickness is 10mm, be provided with 3 below support panel (2-1) edge to be fixedly linked support bar (2-3) with support panel (2-1), it is the stainless steel of diameter 8mm, below, support panel (2-1) middle part is provided with the vertical litter (2-2) that 2 have lower limit, it is diameter 8mm body of stainless steel, vertical litter (2-2) and support panel thread connecting mode are fixed, support panel (2-1) middle part is provided with the first through hole (2-4), and this through-hole diameter is 11mm; It is 4mm that described doping container (3) comprises (3-2) wall thickness in the middle part of quartz cover plate that separable container upper cover (3-1) thickness is 5mm, container, the quartzy vertebra platform of the hollow of height 110mm, the high purity quartz cone end of container bottom (3-3) for being mutually 60 °, container upper cover (3-1) is provided with fourth hole (3-4), and its diameter is 5mm; The wireline that described connection cord or union lever (4) are diameter 3mm.
Embodiment 3
CG3000 type single crystal growing furnace, 14 cun of thermal fields, drop into polysilicon 20kg, manufacture order stove silicon single crystal, head target resistivity is the N-type of 35 Ω .cm, and doping agent is 3 inches of silicon single crystal of phosphoric.Use doping agent is mother alloy (the silicon single crystal material of high-concentration dopant), and is 10g according to calculating the dopant dose needed.
Concrete operation method is as follows:
1, doper prepare: 1. by hanger bar (1-1) through the first through hole (2-4), vertical litter (2-2) through second and the third through-hole (1-3) of slide block, and is fixedly linked with support panel (2-1); 2. will adulterate container upper cover (3-1) in a reservoir portion (3-2) go up and be fixedly linked with vertical litter (2-2) bottom by connection cord or union lever (4); 3. the container bottom that adulterates (3-3) is fixedly linked with carriage (1) base slider (1-2) by connection cord or union lever (4) fourth hole (3-4) through container upper cover; 4. said apparatus removing surface is clean, prepare doping and use.
2, the polycrystal raw material required for calculated single crystal growth and doping metering, take 20Kg polysilicon and 10g doping agent.
3, after thermal field cleans, dropped into by polysilicon in high-purity silica pot, close thermal field and single crystal growing furnace, vacuumize, after checking vacuum leak rate meets production requirement, heating and melting polysilicon, stablizes to melt temperature.
4, single crystal growing furnace flashboard valve gap is utilized to isolate main chamber and concubine; To concubine inflation, unclamp the compact heap of concubine simultaneously; Open concubine door, take off seed crystal, doper hanger bar (1-1) and seed crystal clamping device are fixedly linked, note should carefully cleaning before loading onto this device, guarantee not stain, open doping container upper cover (3-1), pour ready doping agent into doping container, and build doping container upper cover (3-1), doper is suspended in auxiliary furnace of mono-crystal indoor simultaneously, height is as the criterion not affect main chamber's concubine middle gate plate valve activity, as shown in Figure 5.
5, clean concubine, carries out gas washing to concubine and vacuumizes, and opens slide valve and is communicated with concubine and main chamber
6, decline seed crystal clamping device makes doper steadily decline, after the bracing frame (2) of doper drops to top, main chamber and stops declining, continue decline seed crystal clamping device, make carriage (1) can along the steady slide downward in vertical litter (2-2) direction along with carriage (1) decline, doping container bottom (3-3) synchronously declines, and be separated with (3-2) in the middle part of doping container, doping agent falls in melt gradually, now pay close attention to ullage situation in single crystal growing furnace, guarantee that doping agent all falls into melt, and prevent doping container bottom (3-3) from touching melt, realize doping as shown in Figure 6.
7, after doping agent all falls into melt, rising seed crystal clamping device, now carriage (1) and doping container bottom (3-3) go up to original height, and lift and stop after whole doper continues to rise to the height not affecting slide valve activity.
8, cover slide valve, again the isolation of main chamber's concubine, and be inflated to normal pressure in concubine, open concubine door, after the cooling some time, take off doper, reinstall seed crystal, vacuumize after clean concubine, be communicated with major-minor room, enter normal single crystal growing link.
9, be put in clean dried place after this device carefully being cleaned, take again when next time uses.
10, after seeding, shouldering, turn shoulder, isodiametric growth, ending operation, realize single crystal growing, get head print and carry out resistivity measurement after thermal treatment process, center resistivity is 35.2 Ω .cm, and doping accurately.
Embodiment 4
In the middle part of the doping container that the present invention relates to shape can as required and complete processing adjustment, Fig. 7 is cylindrical hollow type, and Fig. 8 is hollow sphere; Also can need to be adjusted to taper or spherical according to processing bottom doper, as shown in Figure 9.
Obvious the present invention does not limit and above-mentioned embodiment, and those skilled in the art principle according to the present invention can have many distortion.
Claims (5)
1. a doper for pulling of silicon single crystal, comprising: bracing frame (2), the carriage (1) be nested with bracing frame litter, the doping container (3) be connected with carriage with bracing frame, for the connection cord that is connected or union lever (4), it is characterized in that: support frame as described above is provided with support panel (2.1), be provided with 3 below support panel (2.1) edge to be fixedly linked support bar (2-3) with support panel (2.1), below, support panel (2.1) middle part is provided with the vertical litter (2-2) that 2 have lower limit, vertical litter (2-2) and support panel (2.1) are fixed with thread connecting mode, and support panel (2-1) middle part is provided with the first through hole (2-4), described carriage (1) is provided with hanger bar (1-1), hanger bar (1-1) runs through support panel (2-1) by bracing frame through hole (2-4), hanger bar (1-1) top is provided with carves type groove, for being fixedly linked use with single crystal furnace seed crystal clamping device, hanger bar (1-1) bottom is provided with the slide block (1-2) be fixedly linked with hanger bar (1-1), slide block (1-2) is provided with second and third through-hole (1-3), use when sliding for vertical with bracing frame litter (2-2), carriage (1) can be slided along vertical litter (2-2) direction, when slide block (1-2) touches vertical litter (2-2) end lower limit, slide block stops gliding, described doping container (3) comprises separable container upper cover (3-1), in the middle part of container (3-2), container bottom (3-3), container upper cover (3-1) is provided with fourth hole (3-4), it is suitable for reading that container upper cover (3-1) is placed in (3-2) in the middle part of container, in the middle part of container, (3-2) is connected with the vertical litter of bracing frame (2-2) fixed vertical by connection cord or union lever (4), container bottom (3-3) is connected with carriage (1) bottom fixed vertical through container upper cover (3-1) fourth hole (3-4) by connection cord or union lever (4).
2. the doper of pulling of silicon single crystal as claimed in claim 1, it is characterized in that: bracing frame (2) and parts thereof, the carriage (1) be nested with vertical litter (2-2) and parts thereof are stainless steel.
3. the doper of pulling of silicon single crystal as claimed in claim 1, is characterized in that: described doping container (3) and parts thereof adopt high purity quartz material.
4. the doper of pulling of silicon single crystal as claimed in claim 1, is characterized in that: adopt high pure metal molybdenum rope or molybdenum rod, stainless steel cable or stainless steel for the connection cord that connects or union lever (4).
5. a using method for pulling of silicon single crystal doper, is characterized in that following steps:
(1) doper prepare: 1. by hanger bar (1-1) through the first through hole (2-4), vertical litter (2-2) through second and the third through-hole (1-3) of slide block, and is fixedly linked with support panel (2-1); 2. the container upper cover (3-1) that will adulterate is placed in (3-2) in the middle part of container and goes up and be fixedly linked with vertical litter (2-2) bottom by connection cord or union lever (4); 3. the container bottom that adulterates (3-3) is fixedly linked with carriage (1) base slider by connection cord or union lever (4) fourth hole (3-4) through container upper cover (3-1); 4. apparatus surface is cleaned out, prepare doping and use;
(2) polycrystal raw material required for calculated single crystal growth and dopant dose;
(3) after thermal field cleans, dropped into by polysilicon in high-purity silica pot, close thermal field and single crystal growing furnace, vacuumize, after checking vacuum leak rate meets production requirement, heating and melting polysilicon, stablizes to melt temperature;
(4) single crystal growing furnace flashboard valve gap is utilized to isolate main chamber and concubine; To concubine inflation, unclamp the compact heap of concubine simultaneously; Open concubine door, take off seed crystal, doper hanger bar (1-1) and seed crystal clamping device are fixedly linked, open doping container upper cover (3-1), and pour ready doping agent into doping container, and build doping container upper cover (3-1), doper is suspended in auxiliary furnace of mono-crystal indoor, height is as the criterion not affect main chamber's concubine middle gate plate valve activity simultaneously;
(5) clean concubine, carries out gas washing to concubine and vacuumizes, and opens slide valve and is communicated with concubine and main chamber;
(6) decline seed crystal clamping device makes doper steadily decline, after the bracing frame (2) of doper drops to top, main chamber and stops declining, continue decline seed crystal clamping device, make carriage (1) can along the steady slide downward in vertical litter (2-2) direction along with carriage (1) decline, doping container bottom (3-3) synchronously declines, and be separated with (3-2) in the middle part of doping container, doping agent falls in melt gradually, now pay close attention to ullage situation in single crystal growing furnace, guarantee that doping agent all falls into melt, and prevent doping container bottom (3-3) from touching melt,
(7) after doping agent all falls into melt, rising seed crystal clamping device, now carriage (1) and doping container bottom (3-3) go up to original height, and lift and stop after whole doper continues to rise to the height not affecting slide valve activity;
(8) cover slide valve, again the isolation of main chamber's concubine, and be inflated to normal pressure in concubine, open concubine door, after cooling, take off doper, reinstall seed crystal, vacuumize after clean concubine, be communicated with major-minor room, enter normal single crystal growing link;
(9) be put in clean dried place after carefully being cleaned by doper device, take again when next time uses.
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