CN108977878A - Method based on monocrystalline growth with czochralski silicon - Google Patents
Method based on monocrystalline growth with czochralski silicon Download PDFInfo
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- CN108977878A CN108977878A CN201710402193.7A CN201710402193A CN108977878A CN 108977878 A CN108977878 A CN 108977878A CN 201710402193 A CN201710402193 A CN 201710402193A CN 108977878 A CN108977878 A CN 108977878A
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- seeding
- growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of method based on monocrystalline growth with czochralski silicon, the Modelling of Crystal Growth in CZ-Si Pulling method key steps are as follows: and process preparation → shove charge → evacuates → stops leakage in the roof → and applying argon gas → heating → seeding → shrinking neck → shouldering → turns shoulder → isodiametric growth → ending → cooling → have a power failure → stopping argon gas → stop vacuum pump → tears furnace open.Equipment and simple process of the present invention using monocrystalline growth with czochralski, automatic control easy to accomplish, high production efficiency, easily prepared major diameter single crystal, the impurity concentration being easy to control in monocrystalline can prepare low resistivity single crystal.
Description
Technical field
The present invention relates to single silicon fields, and in particular to a method of based on monocrystalline growth with czochralski silicon.
Background technique
Monocrystalline silicon is a kind of nonmetalloid that comparison is active, is the important component of crystalline material, is in new material
The forward position of development.Its main application is used as semiconductor material and utilizes solar energy power generating, heat supply etc..Since solar energy has
The many advantages such as have cleaning, environmental protection, facilitate, in the late three decades, solar utilization technique research and develop, commercially produce, city
Developing aspect all obtains tremendous development, become the world quickly, one of the new industry of stable development.Monocrystalline silicon can be used for
Production and the deep processing manufacture of diode grade, rectifying device grade, circuit-level and solar battery grade single crystal product article, subsequent production
Product integrated circuit and semiconductor separation part are widely used to every field, also occupy importantly in military avionic equipment
Position.In today that photovoltaic technology and microminiature semiconductor inverter technology develop rapidly, silicon single crystal solar energy produced is utilized
Solar energy directly can be converted into luminous energy by battery, realize the beginning for green energy resource revolution of marching toward.2008 Beijing Olympic Games
It will show using " Green Olympics " as important displaying towards the whole world, the utilization of monocrystalline silicon will be very important one wherein
Ring.Now, external solar photovoltaic power plant has arrived the theoretical stage of ripeness, to practical stage transition, the sun
The utilization of energy silicon single crystal will spread to worldwide, and market demand is self-evident.Monocrystalline silicon growing side in the prior art
Method equipment requirement is high, at high cost, complex process.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, provide a kind of method based on monocrystalline growth with czochralski silicon.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A method of based on monocrystalline growth with czochralski silicon, the method the following steps are included:
Step 1: charging
Material is fitted into crucible；And before charging, particle is pre-placed in crucible bottom；
It stops leakage in the roof Step 2: evacuating
After being closed stove, vacuum pump knob is opened, then open Vacuum ball valve, the control pumpdown time is not less than 40 minutes；
Step 3: material
Check that all data should be at initial value, confirmation water route is unimpeded, hydraulic pressure is required up to technique；Starting adds after filling 5 minutes argon gas
Thermoelectric generator is added to material power peak power no more than 85kw in three times in 1 hour；
Step 4: seeding
Crucible position is placed on seeding crucible position, crystalline substance turns, pot turns to be set as crystal pulling requirement parameter, adjusts according to the seeding temperature of upper heat
Temperature preheats 5 to 10 minutes when then declining seed crystal to liquid level 30mm；When aperture is stablized, start seeding；
Step 5: shouldering；
Step 6: isometrical
During isometrical, crystal diameter variation is paid close attention in real time, if discovery diameter is exceeded, does corresponding cooling or heating adjustment；
Step 7: ending
Start to finish up when the 92% of isodiametric growth to inventory；
Step 8: blowing out.
When further technical solution is seeding in the step four, seeding speed is adjusted according to aperture size, is drawn
The equal casting speed control of Jinping is in 2-6mm/min.
During further technical solution is the seeding, thin neck diameter control is between 3-5mm, when thin neck
When less than 3mm, melt back draws again.
Compared with prior art, the beneficial effects of the present invention are: the present invention uses the equipment and work of monocrystalline growth with czochralski
Skill is simple, automatic control easy to accomplish, high production efficiency, easily prepared major diameter single crystal, and the impurity being easy to control in monocrystalline is dense
Degree, can prepare low resistivity single crystal.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below.
According to one embodiment of present invention, the present embodiment discloses a kind of method based on monocrystalline growth with czochralski silicon, should
Modelling of Crystal Growth in CZ-Si Pulling method key step are as follows: process preparation → shove charge → evacuates → stops leakage in the roof → applying argon gas → heating → seeding →
Shrinking neck → shouldering →, which turns shoulder → isodiametric growth, → ending → cooling → have a power failure → stopping argon gas → stop vacuum pump → tears furnace open.
Specifically describe method of the present embodiment based on monocrystalline growth with czochralski silicon, this method specific steps are as follows:
Step 1 prepares: wearing mask, disposable glove.Furnace chamber, vacuum pipe and graphite are cleaned with dust catcher and brush special
Device.If peep-hole is fuzzy or has dirt, should clean out.Replace plastic glove, with high pure paper and dehydrated alcohol wiping furnace chamber,
Telltale hole is surveyed in sweet seal.Graphite device is reviewed and validate without sparking, not damaged, then according to get on, get off, in elder generation after it is outer suitable
Sequence successively installs graphite device, and the junction of electrode will pad graphite paper, and quartz socket tube is placed on two electrodes, and each device is wanted
Ask installation steady, firm.It after installing graphite crucible, opens crucible and turns, see whether there is or not rotation bias, touch situations such as other graphite devices,
If influencing crystal pulling, should adjust in time.
Step 2, charging: charging pronucleus is to polycrystalline, crucible, it is ensured that is consistent with the requirement of work order.Put on when charging mask,
Nylon gloves, then disposable glove is worn, and pay attention to preventing material from scratching.Size matching when charging, aniseed can be broken and refill.Crucible bottom needs
A little particles are put, especially big block is then put, median size and particle can put portion, and sharp bulk material tip cannot be directed at quartz
Crucible.It is safe that material will be placed, and prevent material when material from dropping out, influence crystal pulling.Insulation cover in inspection, each sealing ring whether there is or not silicon slag,
It is sopped up with dust catcher.Time each sealing ring of alcohol wipe is used again.Seed crystal non-oxidation and damage are carefully confirmed before being closed secondary furnace chamber,
Confirm that seed crystal is fixed by seedholder, confirms that seedholder and flexible axle are not damaged also without serious aging.It is closed secondary furnace chamber
When, it should be specifically noted that slowly push secondary furnace chamber, and with high-purity gloves it is hand steered live seed crystal, in order to avoid seed crystal collision furnace wall.
Step 3, evacuation are stopped leakage in the roof: after being closed stove, opening vacuum pump knob, then open Vacuum ball valve.If vacuumized
It is undesirable, it can be slightly evacuated after applying argon gas again.Vacuum requirement is to be extracted into 4 pas hereinafter, then successively closing vacuum sphere in 40 minutes
Valve, vacuum pump knob start to hunt leak, and leak detection requires 5 minutes leak rates to be no more than 1 pa.
Step 4, material: check that all data should be at initial value, confirmation water route is unimpeded, hydraulic pressure is required up to technique.Fill 5
Start heating power supply after minute argon gas, is added to material power peak power in 1 hour in three times no more than 85kw.In material mistake
It should be noted that situation should open crucible early and turn, and adjust crucible in time according to the material position in furnace if material is declined in observation furnace in journey
Position, to prevent abnormal conditions.It when materialization is complete, need to cool down in time, in order to avoid melt temperature is excessively high, cause to splash silicon.
Step 5, seeding: crucible position is placed on seeding crucible position, crystalline substance turns, pot turns to be set as crystal pulling requirement parameter, according to upper furnace
Secondary seeding temperature adjusts temperature.Then decline seed crystal to liquid level 30mm or so preheating 5 to 10 minutes.Seed crystal contacts liquid level one
Secondary decline should not be too many, if seed crystal aperture or fusing occurs at once, illustrates that liquid level temperature is higher；If seed crystallization and long
It cannot melt long, show that liquid level temperature is lower；According to circumstances adjust melt temperature.It should the welding at original thin seed crystal when seeding
It opens and draws, try not seed crystal to return and have seeding at original thick seed crystal.When aperture is stablized it is suitable when, start seeding, according to aperture
Size adjusts seeding speed, and seeding average pull rate is preferably in 2-6mm/min.Thin neck diameter should be between 3-5mm, and such as thin neck is less than
3mm wants melt back to draw again.Thin neck length requirement is in 150mm, and when seeding is to 130mm that temperature is stabilized, pulling rate not go up downward
It saves excessive, guides to 150mm and start shouldering.
Step 6, shouldering: by pulling rate to 0.4mm/min or so, if seeding temperature is lower, shouldering is too fast, can properly increase crystalline substance
When lifting shoulder, according to growing state, appropriate adjustment temperature and pulling rate, shouldering will be smoothly.
Step 7 turns shoulder: turning shoulder pulling rate should not be too large, and be usually no more than 2.5mm/min.Meter Changqing is carried out when just turning shoulder
Zero.When diameter control is lived, pulling rate is slowly reduced, follow-up crucible is raised to technique requirement.It is diametrically stable to live to press aperture signal (1/3),
Automatic control can be thrown.2 × V crystalline substance liter in V crucible Φ monocrystal rod/Φ crucible.
Step 8, isometrical: the equal diameter control stage can also human assistance if diameter deviation is larger or temperature fluctuation is larger
The adjustment of lifting/lowering temperature.Generally do not adjust pot with than.Crystal diameter variation should be paid close attention to during isometrical often, if discovery diameter is super
Mark should adjust accordingly in time.Monitoring single crystal growing furnace situation: such as fall rib, crystallization (especially close to tail portion), vibration.Other exceptions
Situation, such as gas leakage, sparking, crucible split, power off, cutting off the water, stopping the supple of gas or steam and mechanically or electrically device failure, to make corresponding processing in time.
Abnormal conditions are recorded faithfully on crystal pulling original record.
Step 9, ending: start to finish up when 92 or so of isodiametric growth to inventory.Stay crucible material that should control in inventory
5 within.In epilog, ending situation should be observed constantly, and preventing the generations of abnormal conditions, (such as crystal is long thick suddenly, liquid level
Crystallization etc.) charged material weight/π r2The electrical path lengths such as × 2.33.
Step 10, blowing out: when ending terminates, lifting crystal, and crystal tail end is made to be detached from melt, gives that brilliant to rise 2mm/min left
It is right.By crucible potential drop down to liquid level apart from 30 centimeters of crystal or so, closes crucible and rise with crucible with than reducing crucible turn and brilliant turn, moving back simultaneously
Continental Europe is automatic out, restores each data initial value and starts to cool down.Cooling in three times, has dropped pass heating power supply in 30 minutes.3 is small after power failure
When, stop argon gas and carry out hot inspection, closes vacuum pump after heat leak detection.Furnace is torn open after 1.5 hours.
Claims (3)
1. a kind of method based on monocrystalline growth with czochralski silicon, it is characterised in that: the method the following steps are included:
Step 1: charging
Material is fitted into crucible；And before charging, particle is pre-placed in crucible bottom；
It stops leakage in the roof Step 2: evacuating
After being closed stove, vacuum pump knob is opened, then open Vacuum ball valve, the control pumpdown time is not less than 40 minutes；
Step 3: material
Check that all data should be at initial value, confirmation water route is unimpeded, hydraulic pressure is required up to technique；Starting adds after filling 5 minutes argon gas
Thermoelectric generator is added to material power peak power no more than 85kw in three times in 1 hour；
Step 4: seeding
Crucible position is placed on seeding crucible position, crystalline substance turns, pot turns to be set as crystal pulling requirement parameter, adjusts according to the seeding temperature of upper heat
Temperature preheats 5 to 10 minutes when then declining seed crystal to liquid level 30mm；When aperture is stablized, start seeding；
Step 5: shouldering；
Step 6: isometrical
During isometrical, crystal diameter variation is paid close attention in real time, if discovery diameter is exceeded, does corresponding cooling or heating adjustment；
Step 7: ending
Start to finish up when the 92% of isodiametric growth to inventory；
Step 8: blowing out.
2. the method according to claim 1 based on monocrystalline growth with czochralski silicon, it is characterised in that in the step four
When seeding, seeding speed is adjusted according to aperture size, seeding average pull rate is controlled in 2-6mm/min.
3. the method according to claim 2 based on monocrystalline growth with czochralski silicon, it is characterised in that the seeding process
In, thin neck diameter control is between 3-5mm, and when thin neck is less than 3mm, melt back draws again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710402193.7A CN108977878A (en) | 2017-06-01 | 2017-06-01 | Method based on monocrystalline growth with czochralski silicon |
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| CN201710402193.7A CN108977878A (en) | 2017-06-01 | 2017-06-01 | Method based on monocrystalline growth with czochralski silicon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111304743A (en) * | 2019-10-30 | 2020-06-19 | 弘元新材料(包头)有限公司 | Process for pulling single crystal furnace automatic system |
| CN112301426A (en) * | 2019-08-02 | 2021-02-02 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
| CN114351247A (en) * | 2022-01-12 | 2022-04-15 | 苏州天准科技股份有限公司 | Crystal pulling shaking monitoring method, storage medium, terminal and crystal pulling equipment |
| CN114387251A (en) * | 2022-01-12 | 2022-04-22 | 苏州天准科技股份有限公司 | Method for monitoring a saturation point, storage medium, terminal and crystal pulling installation |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112301426A (en) * | 2019-08-02 | 2021-02-02 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
| CN112301426B (en) * | 2019-08-02 | 2022-08-12 | 宁夏隆基硅材料有限公司 | Method for manufacturing silicon single crystal rod |
| CN111304743A (en) * | 2019-10-30 | 2020-06-19 | 弘元新材料(包头)有限公司 | Process for pulling single crystal furnace automatic system |
| CN114351247A (en) * | 2022-01-12 | 2022-04-15 | 苏州天准科技股份有限公司 | Crystal pulling shaking monitoring method, storage medium, terminal and crystal pulling equipment |
| CN114387251A (en) * | 2022-01-12 | 2022-04-22 | 苏州天准科技股份有限公司 | Method for monitoring a saturation point, storage medium, terminal and crystal pulling installation |
| CN114387251B (en) * | 2022-01-12 | 2022-09-30 | 苏州天准科技股份有限公司 | Method for monitoring a saturation point, storage medium, terminal and crystal pulling apparatus |
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