CN106435714A - Polycrystalline silicon solution liquid level distance positioning method - Google Patents

Polycrystalline silicon solution liquid level distance positioning method Download PDF

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Publication number
CN106435714A
CN106435714A CN201510482493.1A CN201510482493A CN106435714A CN 106435714 A CN106435714 A CN 106435714A CN 201510482493 A CN201510482493 A CN 201510482493A CN 106435714 A CN106435714 A CN 106435714A
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seed crystal
lower edge
liquid level
guide shell
distance
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CN201510482493.1A
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Chinese (zh)
Inventor
王保胜
何紫平
孙喜良
郭振宇
马卫康
翟胜涛
苏金玉
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TBEA Xinjiang Sunoasis Co Ltd
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TBEA Xinjiang Sunoasis Co Ltd
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Priority to CN201510482493.1A priority Critical patent/CN106435714A/en
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Abstract

The present invention provides a polycrystalline silicon solution liquid level distance positioning method. According to the present invention, the method comprises: sealing the main furnace chamber and the sub furnace chamber of a single crystal furnace, vacuumizing the main furnace chamber and the sub furnace chamber, and heating polycrystalline silicon in a crucible; before the main furnace chamber and the sub furnace chamber are sealed, the method further comprises: determining the lower edge position of a diversion cylinder; after the polycrystalline silicon in the crucible completely melts, the method further comprises: descending the seed crystal, and controlling the seed crystal descending distance according to the diversion cylinder lower edge position and a preset liquid level distance m, wherein the liquid level distance is the distance between the liquid level of the polycrystalline silicon solution in the crucible and the diversion cylinder lower edge; with the method, the polycrystalline silicon solution liquid level distance can be accurately positioned, such that the positioning of the polycrystalline silicon solution liquid level distance is not dependent on the experience of the operator so as to improve the accuracy and the reliability, such that the crystal pulling is cured; and the method has characteristics of simple operation, strong practicality, and wide application range.

Description

A kind of polysilicon liquid level of solution is away from localization method
Technical field
The present invention relates to the production technical field of solar energy industry silicon single crystal rod and silicon core, tool Body is related to a kind of polysilicon liquid level of solution away from localization method.
Background technology
Semiconductor silicon single crystal is most of to be manufactured using Czochralski method (abbreviation vertical pulling method). During manufacturing single crystal silicon semiconductor silicon rod using vertical pulling method, polysilicon is put into quartz In crucible, heating fusing, after overstabilization, seed crystal is introduced in single crystal growing furnace, and warp Cross the series of processes such as seeding, shouldering, turn shoulder, isometrical, ending and complete a monocrystal silicon The drawing of silicon rod.
Due in monocrystal silicon silicon rod production technology, in crucible polysilicon liquid level of solution with lead The distance between flow cartridge lower edge (i.e. liquid level away from), is the weight determining monocrystal silicon silicon rod quality Want parameter, liquid level away from size directly affect carbon and oxygen element in monocrystal silicon silicon rod Content and technique solidify standardized effective execution, thus affecting the disconnected rib rate of silicon rod.
Therefore, in the stabilization step before production process starts, how to be accurately positioned earthenware In crucible, polysilicon liquid level of solution and the liquid level of guide shell lower edge are given birth to away from just becoming monocrystal silicon silicon rod Important step in production. art.
At present, traditional polysilicon liquid level of solution fully relies on operator away from positioning to be carried out Range estimation, the experience by operator is positioned.Because operator's level differs, It is difficult to ensure that polysilicon liquid level of solution away from positioning accuracy, liquid level away from sometimes excessive sometimes Too small, lead to crystal pulling parameter cannot solidify.
Therefore, need a kind of polysilicon liquid level of solution badly away from targeting scheme, to solve above-mentioned skill Art problem.
Content of the invention
The present invention is directed to above-mentioned deficiency present in prior art, provides a kind of polysilicon molten Liquid liquid level away from localization method, in order to solve polysilicon liquid level of solution away from Position location accuracy difference Problem.
The present invention is to solve above-mentioned technical problem, adopts the following technical scheme that:
The present invention provides a kind of polysilicon liquid level of solution away from localization method, including:Sealing is single The main furnace chamber of brilliant stove and secondary furnace chamber, the main furnace chamber to single crystal growing furnace and secondary furnace chamber evacuation, and Polysilicon in heating crucible, before the main furnace chamber and secondary furnace chamber of sealing single crystal growing furnace, institute Method of stating also includes:
Determine the position of the lower edge of guide shell;
After polysilicon in crucible is completely melt, methods described also includes:
Decline seed crystal, and the position according to the lower edge of guide shell and default liquid level are controlled away from m The distance that seed crystal processed declines;Wherein, liquid level refers to polysilicon liquid level of solution in crucible away from m The distance between with the lower edge of guide shell.
Specifically, the position of the described lower edge determining guide shell, specifically includes:
The lower surface of isolating valve of measurement single crystal growing furnace and the distance between the lower edge of guide shell a, And, the thickness b of the isolating valve of measurement single crystal growing furnace;
The position of the lower edge of described guide shell is:The lower edge of guide shell and isolating valve upper surface Relative distance (a+b).
Specifically, described decline seed crystal, and the position according to the lower edge of guide shell and default Liquid level away from m control seed crystal decline distance, specifically include:
The bottom of control seed crystal declines the distance of (a+b) at the upper surface of isolating valve, with Make the bottom of seed crystal concordant with the lower edge of guide shell;
Seed crystal is controlled to decline the distance away from m for the liquid level.
Specifically, the position of the described lower edge determining guide shell, specifically includes:
The lower surface of isolating valve of measurement single crystal growing furnace and the distance between the lower edge of guide shell a, And, the thickness b of the isolating valve of measurement single crystal growing furnace;
The upper surface of the bottom of seed crystal and isolating valve is leant, and records current seed crystal Brilliant position c, the brilliant position of described seed crystal is between the default initial point above the bottom of seed crystal and seed crystal Distance;
The position of the lower edge of described guide shell is:Pre- above the lower edge of guide shell and seed crystal If the absolute distance between initial point (a+b+c).
Specifically, described decline seed crystal, and the position according to the lower edge of guide shell and default Liquid level away from m control seed crystal decline distance, specifically include:
Decline seed crystal to brilliant position (a+b+c), so that the lower edge of the bottom of seed crystal and guide shell Concordantly;
Decline seed crystal to brilliant position (a+b+c+m).
Further, methods described also includes:
After seed crystal stops declining, rise crucible, when polysilicon liquid level of solution and seed in crucible When brilliant bottom contacts, stop rising crucible.
The present invention passes through, before the main furnace chamber and secondary furnace chamber of sealing single crystal growing furnace, to determine water conservancy diversion The position of the lower edge of cylinder, and after the unmelted polycrystalline silicon in crucible, according under guide shell The position on edge and liquid level decline away from control seed crystal, thus seed crystal bottom when being stopped according to seed crystal Position determine the position of polysilicon liquid level of solution in crucible, realize to liquid level away from carrying out standard Determine position.The method can be accurately positioned polysilicon liquid level of solution away from so that polysilicon is molten Liquid liquid level away from positioning eliminate the reliance on the experience of operator and carry out, improve accuracy and reliability Property, thus solidifying crystal pulling technique;Additionally, the method is simple to operate, practical, fit With in extensive range.
Brief description
Fig. 1 is the structural representation of straight pull type single crystal furnace;
Fig. 2 is polysilicon liquid level of solution provided in an embodiment of the present invention away from localization method flow process Figure.
Specific embodiment
Below in conjunction with the accompanying drawing in the present invention, the technical scheme in the present invention is carried out clearly Chu, complete description are it is clear that described embodiment is the part enforcement of the present invention Example, rather than whole embodiments.Based on the embodiment in the present invention, this area is common The every other enforcement that technical staff is obtained on the premise of not making creative work Example, broadly falls into the scope of protection of the invention.
The present invention passes through to determine the position of the lower edge of guide shell, the lower edge according to guide shell Position and liquid level decline away from control seed crystal, and are determined in crucible according to the position of seed crystal bottom The final particular location of polysilicon liquid level of solution, thus realization is accurately fixed away from carrying out to liquid level Position, poor away from Position location accuracy in order to solve the problems, such as polysilicon liquid level of solution.
As shown in figure 1, straight pull type single crystal furnace 1 includes main furnace chamber 11 and secondary furnace chamber 12, It is provided with isolating valve 13 between main furnace chamber 11 and secondary furnace chamber 12, be provided with main furnace chamber 11 Guide shell 14, crucible 15 and heater 16, are equipped with the polysilicon of solid-state in crucible 15 Raw material, heater 16 can form thermal field in main furnace chamber 11, in fusion crucible 15 Polycrystalline silicon raw material, guide shell 14 is used for water conservancy diversion argon.In secondary furnace chamber 12, tungsten wire rope 2 In the presence of balancing weight 3, seed crystal 4 is vertically lifted.
During using straight pull type single crystal furnace 1 drawn monocrystalline silicon silicon rod, polycrystalline silicon raw material is contained in In crucible 15, it is heated to more than the fusing point of polysilicon, now, earthenware using heater 16 Polysilicon in crucible 15 is just molten into liquid.Seed crystal 4 is made to enter by controlling tungsten wire rope 2 In main furnace chamber 11, and after dropping to certain position, rise crucible 15, make many in crucible Crystal silicon solution is just contacted with the bottom of seed crystal 4.At a temperature of 1450 DEG C about, seed Crystalline substance 4 is both non-fusible and does not grow up, and is lifted upwards and rotation seed crystal 4 by slow, and slowly Ground reduces heating power, and seed crystal 4 is gradually long thick, thus obtaining the monocrystal silicon of required diameter Silicon rod.
When starting drawn monocrystalline silicon silicon rod, the position of polysilicon liquid level of solution in crucible 15 (i.e. in crucible the liquid level between the lower edge 141 of polysilicon liquid level of solution and guide shell away from) The product quality of monocrystal silicon silicon rod is had a major impact, therefore, the embodiment of the present invention provides A kind of can be accurately positioned liquid level away from polysilicon liquid level of solution away from localization method.
Below in conjunction with Fig. 1 and Fig. 2, to polysilicon solution liquid provided in an embodiment of the present invention Identity distance localization method is described in detail.As shown in Fig. 2 the method comprises the following steps:
Step 201, determines the position of the lower edge of guide shell.
Specifically, after straight pull type single crystal furnace 1 installs, you can determine guide shell The position of lower edge 141.
The position of the lower edge 141 of guide shell can be relative position or absolute position Put, subsequently by by two embodiments respectively to determine guide shell lower edge relative position and Determine that two kinds of situations of the absolute position of the lower edge of guide shell are described respectively.
Step 202, the main furnace chamber of sealing single crystal growing furnace and secondary furnace chamber, the main stove to single crystal growing furnace Room and secondary furnace chamber evacuation, and the polysilicon in heating crucible.
Specifically, after determining the position of lower edge 141 of guide shell, you can enter and open Heater stage, in the blow-on stage, seals the main furnace chamber 11 of single crystal growing furnace and secondary furnace chamber 12, and right The main furnace chamber 11 of single crystal growing furnace and secondary furnace chamber evacuation 12, to form negative pressure.Detect main furnace chamber 11 and the vacuum of secondary furnace chamber 12, and after vacuum degree measurement is qualified, start with heating Polycrystalline silicon raw material in device 16 radiations heat energy heating crucible 15, so that polycrystalline silicon raw material melts Turn to liquid.In heating process, it is passed through high-purity argon gas into main furnace chamber 11, makes main stove Room 11 keeps certain negative pressure pressure.
Step 203, after the polysilicon in crucible is completely melt, declines seed crystal, and according to The position of the lower edge of guide shell and default liquid level control the distance of seed crystal decline away from m.
Specifically, after polysilicon is completely melt, keeps coarse vacuum in main furnace chamber 11, and make The temperature of polysilicon solution and surface pressure reach and stablize.
When the polycrystalline silicon material in crucible 15 be completely melt and reach stablize after, start control seed Brilliant 4 decline, specifically, the position of the lower edge 141 according to guide shell and default liquid level Control the distance of seed crystal decline away from m.Liquid level refers to polysilicon solution in crucible 15 away from m The distance between lower edge 141 of liquid level and guide shell, generally, liquid level is away from for 15-30mm.
After controlling seed crystal 4 to stop declining, seed crystal 4 is kept to toast two, three points in this position Clock, makes the temperature close to polysilicon solution for the temperature of seed crystal 4, to reduce to seed crystal 4 Thermal shock.
Step 204, after seed crystal stops declining, rises crucible, when in crucible, polysilicon is molten When liquid liquid level is contacted with the bottom of seed crystal, stop rising crucible.
Specifically, seed crystal 4 stops declining and after of short duration baking, controls on crucible 15 Rise, when in crucible 15, polysilicon liquid level of solution is contacted just with the bottom of seed crystal 4, Stop rising crucible 15.Now, under polysilicon liquid level of solution and guide shell in crucible 15 Along the liquid level between 141 away from as m.
Can be seen that the present invention by above-mentioned steps 201-204 to pass through in sealing single crystal growing furnace Main furnace chamber and secondary furnace chamber before, determine the position of the lower edge of guide shell, and in crucible Unmelted polycrystalline silicon after, the position of the lower edge according to guide shell and liquid level are away from controlling under seed crystal Fall, thus the position of seed crystal bottom determines polysilicon solution in crucible when being stopped according to seed crystal The position of liquid level, realizes to liquid level away from being accurately positioned.The method can be accurately positioned Polysilicon liquid level of solution away from so that polysilicon liquid level of solution away from positioning eliminate the reliance on operation The experience of member is carried out, and improves accuracy and reliability, thus solidifying crystal pulling technique;Additionally, The method is simple to operate, practical, applied widely.
Below by way of two embodiments, relative to the lower edge by determining guide shell respectively Position and absolute position both schemes are described in detail.
Embodiment 1
Embodiment 1 is the scheme of the relative position of lower edge determining guide shell, in embodiment In 1, the position of the lower edge of guide shell is relative position, i.e. the lower edge of guide shell and isolating valve Relative distance between upper surface.
As shown in figure 1, by the lower surface of isolating valve 13 and the guide shell that measure single crystal growing furnace The distance between lower edge 141 a and the thickness b of isolating valve 13 of single crystal growing furnace lead to determine The relative position of the lower edge 141 of flow cartridge.The position of the lower edge 141 of described guide shell is: The lower edge 141 of guide shell and the relative distance (a+b) of isolating valve 13 upper surface.
It should be noted that due to carry out every batch monocrystal silicon silicon rod draw after the completion of, It is required for tearing stove open, reinstalled crucible 15, guide shell 14 etc. again before next time produces and set Standby, therefore, before carrying out every batch monocrystal silicon silicon rod drawing, it is required for measuring monocrystalline The lower surface of isolating valve 13 of stove and the distance between the lower edge 141 of guide shell a.And it is single The thickness b of the isolating valve 13 of brilliant stove generally will not change, therefore, isolating valve 13 Thickness b only need to measure once, when subsequently carrying out every batch monocrystal silicon silicon rod and drawing, directly Connect using this data.
The main furnace chamber 11 of sealing single crystal growing furnace and secondary furnace chamber 12, the main furnace chamber 11 to single crystal growing furnace With secondary furnace chamber 12 evacuation, and the polysilicon in heating crucible 15, make unmelted polycrystalline silicon For liquid.
Due to pre-test be guide shell the phase with isolating valve 13 upper surface for the lower edge 141 To position (i.e. relative distance), therefore, after the polysilicon in crucible 15 is completely melt, The stroke of seed crystal 4 decline is controlled away from m according to this relative distance and liquid level.Specifically, first First, control the bottom of seed crystal 4 decline at the upper surface of isolating valve 13 (a+b) away from From so that the bottom of seed crystal 4 concordant with the lower edge 141 of guide shell that is to say, that logical Cross control tungsten wire rope 2, so that the bottom of seed crystal 4 is located at the upper surface of isolating valve 13, and The distance of (a+b) is begun to decline at this, now, the bottom of seed crystal 4 and guide shell Lower edge 141 is concordant.Then, continue to control seed crystal 4 decline liquid level to stop after the distance of m Only decline.
After seed crystal 4 stops declining, rise crucible 15, when polysilicon solution in crucible 15 When liquid level is contacted with the bottom of seed crystal 4, stop rising crucible 15, now, crucible 15 Liquid level between interior polysilicon liquid level of solution and the lower edge 141 of guide shell is away from as m.
Embodiment 2
Embodiment 2 is the scheme of the absolute position of lower edge determining guide shell, in embodiment In 2, a certain position of the top of seed crystal is set to default initial point, the lower edge of guide shell Position is absolute position, that is, between the default initial point above the lower edge of guide shell and seed crystal Absolute distance.
As shown in figure 1, by the lower surface of isolating valve 13 and the guide shell that measure single crystal growing furnace The distance between lower edge 141 a, the thickness b of the isolating valve 13 of single crystal growing furnace and work as seed crystal When the upper surface of 4 bottom and isolating valve 13 leans, the brilliant position c of seed crystal 4 to determine and to lead The absolute position of the lower edge 141 of flow cartridge.The brilliant position of seed crystal 4 refers to, the bottom of seed crystal 4 The distance between with default initial point.The position of the lower edge 141 of described guide shell is:Water conservancy diversion Absolute distance (a+b+c) between the default initial point of the lower edge 141 of cylinder and seed crystal 4 top.
It should be noted that because the length of seed crystal 4 differs, therefore, carrying out every batch Before secondary monocrystal silicon silicon rod draws, it is required for measuring the bottom when seed crystal 4 and isolating valve 13 Upper surface seed crystal 4 when leaning brilliant position c.
The main furnace chamber 11 of sealing single crystal growing furnace and secondary furnace chamber 12, the main furnace chamber 11 to single crystal growing furnace With secondary furnace chamber 12 evacuation, and the polysilicon in heating crucible 15, make unmelted polycrystalline silicon For liquid.
Due to pre-test be absolute between the lower edge 141 of guide shell and default initial point Distance (i.e. absolute distance), therefore, after the polysilicon in crucible 15 is completely melt, can With the position of the directly lower edge 141 according to guide shell, seed crystal 4 is dropped to brilliant position (a+b+c), so that the bottom of seed crystal 4 is concordant with the lower edge 141 of guide shell, that is, pass through Control tungsten wire rope 2, make the bottom of seed crystal 4 be in brilliant position (a+b+c) place, now, seed Brilliant 4 bottom is concordant with the lower edge 141 of guide shell.Then, continue to control under seed crystal 4 It is down to brilliant position (a+b+c+m), that is, continue to control seed crystal 4 decline liquid level to stop after m Decline.
After seed crystal 4 stops declining, rise crucible 15, when polysilicon solution in crucible 15 When liquid level is contacted with the bottom of seed crystal 4, stop rising crucible 15, now, crucible 15 Liquid level between interior polysilicon liquid level of solution and the lower edge 141 of guide shell is away from as m.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present And the illustrative embodiments adopting, but the invention is not limited in this.For ability For those of ordinary skill in domain, in the situation without departing from spirit and substance of the present invention Under, various modifications and improvement can be made, these modifications and improvement are also considered as the present invention's Protection domain.

Claims (6)

1. a kind of polysilicon liquid level of solution is away from localization method, including:The master of sealing single crystal growing furnace Furnace chamber and secondary furnace chamber, the main furnace chamber to single crystal growing furnace and secondary furnace chamber evacuation, and heating crucible Interior polysilicon it is characterised in that before the main furnace chamber and secondary furnace chamber of sealing single crystal growing furnace, Methods described also includes:
Determine the position of the lower edge of guide shell;
After polysilicon in crucible is completely melt, methods described also includes:
Decline seed crystal, and the position according to the lower edge of guide shell and default liquid level are controlled away from m The distance that seed crystal processed declines;Wherein, liquid level refers to polysilicon liquid level of solution in crucible away from m The distance between with the lower edge of guide shell.
2. the method for claim 1 is it is characterised in that described determination guide shell Lower edge position, specifically include:
The lower surface of isolating valve of measurement single crystal growing furnace and the distance between the lower edge of guide shell a, And, the thickness b of the isolating valve of measurement single crystal growing furnace;
The position of the lower edge of described guide shell is:The lower edge of guide shell and isolating valve upper surface Relative distance (a+b).
3. method as claimed in claim 2 is it is characterised in that described decline seed crystal, And the position according to the lower edge of guide shell and default liquid level away from m control that seed crystal declines away from From specifically including:
The bottom of control seed crystal declines the distance of (a+b) at the upper surface of isolating valve, with Make the bottom of seed crystal concordant with the lower edge of guide shell;
Seed crystal is controlled to decline the distance away from m for the liquid level.
4. the method for claim 1 is it is characterised in that described determination guide shell Lower edge position, specifically include:
The lower surface of isolating valve of measurement single crystal growing furnace and the distance between the lower edge of guide shell a, And, the thickness b of the isolating valve of measurement single crystal growing furnace;
The upper surface of the bottom of seed crystal and isolating valve is leant, and records current seed crystal Brilliant position c, the brilliant position of described seed crystal is between the default initial point above the bottom of seed crystal and seed crystal Distance;
The position of the lower edge of described guide shell is:Pre- above the lower edge of guide shell and seed crystal If the absolute distance between initial point (a+b+c).
5. method as claimed in claim 4 is it is characterised in that described decline seed crystal, And the position according to the lower edge of guide shell and default liquid level away from m control that seed crystal declines away from From specifically including:
Decline seed crystal to brilliant position (a+b+c), so that the lower edge of the bottom of seed crystal and guide shell Concordantly;
Decline seed crystal to brilliant position (a+b+c+m).
6. the method as described in any one of claim 1-5 is it is characterised in that described side Method also includes:
After seed crystal stops declining, rise crucible, when polysilicon liquid level of solution and seed in crucible When brilliant bottom contacts, stop rising crucible.
CN201510482493.1A 2015-08-07 2015-08-07 Polycrystalline silicon solution liquid level distance positioning method Pending CN106435714A (en)

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CN107523869A (en) * 2017-09-21 2017-12-29 浙江晶盛机电股份有限公司 A kind of single crystal growing furnace can lift water cooling heat shield arrangement
CN109576780A (en) * 2018-12-28 2019-04-05 宁夏隆基硅材料有限公司 A kind of seed crystal welding process and equipment
CN110284185A (en) * 2019-07-26 2019-09-27 内蒙古中环协鑫光伏材料有限公司 A kind of pulling of crystals liquid level protection device and control method
CN110552059A (en) * 2019-09-19 2019-12-10 宁夏隆基硅材料有限公司 Liquid gap positioning device and method and single crystal furnace
CN111826710A (en) * 2019-04-23 2020-10-27 上海新昇半导体科技有限公司 Method and device for controlling safe lifting of silicon melt crucible
CN113566722A (en) * 2021-06-23 2021-10-29 浙江晶阳机电股份有限公司 Device and method for automatically measuring distance between liquid ports
CN113913922A (en) * 2021-10-28 2022-01-11 双良硅材料(包头)有限公司 Method for setting liquid gap of single crystal furnace

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CN107523869A (en) * 2017-09-21 2017-12-29 浙江晶盛机电股份有限公司 A kind of single crystal growing furnace can lift water cooling heat shield arrangement
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CN111826710A (en) * 2019-04-23 2020-10-27 上海新昇半导体科技有限公司 Method and device for controlling safe lifting of silicon melt crucible
CN110284185A (en) * 2019-07-26 2019-09-27 内蒙古中环协鑫光伏材料有限公司 A kind of pulling of crystals liquid level protection device and control method
CN110552059A (en) * 2019-09-19 2019-12-10 宁夏隆基硅材料有限公司 Liquid gap positioning device and method and single crystal furnace
CN113566722A (en) * 2021-06-23 2021-10-29 浙江晶阳机电股份有限公司 Device and method for automatically measuring distance between liquid ports
CN113913922A (en) * 2021-10-28 2022-01-11 双良硅材料(包头)有限公司 Method for setting liquid gap of single crystal furnace
CN113913922B (en) * 2021-10-28 2023-01-10 双良硅材料(包头)有限公司 Method for setting liquid gap of single crystal furnace

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