WO2020118999A1 - 一种vb/vgf法晶体生长用石英管及装置 - Google Patents

一种vb/vgf法晶体生长用石英管及装置 Download PDF

Info

Publication number
WO2020118999A1
WO2020118999A1 PCT/CN2019/083281 CN2019083281W WO2020118999A1 WO 2020118999 A1 WO2020118999 A1 WO 2020118999A1 CN 2019083281 W CN2019083281 W CN 2019083281W WO 2020118999 A1 WO2020118999 A1 WO 2020118999A1
Authority
WO
WIPO (PCT)
Prior art keywords
quartz tube
quartz
crystal growth
groove
cap
Prior art date
Application number
PCT/CN2019/083281
Other languages
English (en)
French (fr)
Inventor
邵会民
孙聂枫
孙同年
刘惠生
王书杰
史艳磊
康永
姜剑
付莉杰
张晓丹
Original Assignee
中国电子科技集团公司第十三研究所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 中国电子科技集团公司第十三研究所 filed Critical 中国电子科技集团公司第十三研究所
Priority to JP2020522301A priority Critical patent/JP6913430B2/ja
Publication of WO2020118999A1 publication Critical patent/WO2020118999A1/zh

Links

Images

Classifications

    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt

Definitions

  • the present invention relates to the field of crystal growth technology, and more particularly, to a quartz tube and device for crystal growth using the VB/VGF method.
  • the VB/VGF method is one of the main process technologies for growing high-quality, low-dislocation crystals.
  • the mature VB/VGF crystal growth technology is to put seed crystals, dehydrated boron oxide, and polycrystalline material into a pyrolytic boron nitride (PBN) crucible, and then install the PBN crucible into a quartz tube and install a cap
  • PBN pyrolytic boron nitride
  • the vacuum inside the quartz tube is evacuated to the required vacuum degree, then the quartz tube and the quartz cap are welded to a seal, and finally put into the VGF furnace for pyrolysis.
  • the quartz tube used in it needs to be welded and sealed.
  • the welded and sealed quartz tube can only be used once, resulting in high cost; on the other hand, in the process of crystal growth and heating, often due to heating procedures or put Unsuitable conditions such as the amount of red phosphorous make the pressure difference between the inside and outside of the quartz tube greater than the pressure on the quartz tube and cause the "explosion tube” phenomenon, which results in interruption of crystal growth and damage to the quartz tube, reducing production efficiency and causing cost waste.
  • the utility model patent with application number 201420795278.8 discloses a charging container and melting treatment system for polycrystalline compound synthesis of multiple compounds, including a quartz tube and a quartz cap, the quartz tube is hollow inside, one end is sealed, the other end is opened, and the quartz cap is from The opening can be inserted or pulled out and assembled in a quartz tube; the quartz tube is provided with a plurality of grooves recessed inwards on the outer wall near the seal or/and the opening to achieve accurate positioning of the quartz cap after loading
  • it does not solve the problem of unbalanced pressure in the quartz tube during the crystal growth process, which is still easy to cause the growth process to be interrupted and the efficiency is low.
  • the present invention provides a quartz tube and device for crystal growth using the VB/VGF method, which uses a split quartz
  • the tube structure through the through hole of the connection, realizes the internal and external communication, and cleverly uses the state change of the heated sealant to form the heating liquid seal, thereby realizing the pressure difference between the inside and outside of the quartz tube during the crystal growth process to be adjustable within a certain range, avoiding the pressure difference It causes the quartz tube to explode, and also makes the quartz tube reusable, reducing the cost.
  • a quartz tube for crystal growth by the VB/VGF method includes a quartz tube body and a quartz cap.
  • the key is that a support groove with an opening upward is provided along the circumference of the upper portion of the quartz tube body, and the quartz cap is inserted into the support groove and The through hole provided at the lower end realizes the internal and external communication of the quartz tube.
  • More than one through hole is provided at the lower end of the quartz cap.
  • the supporting groove is a U-shaped groove or a V-shaped groove.
  • the supporting groove is provided with a solid particle sealant which becomes a liquid upon heating to form a seal.
  • the invention also provides a VB/VGF method crystal growth device, which includes a furnace body provided with an evacuation pipe, a heater in the furnace body, a quartz tube limited to the bottom of the furnace body by a support body, and a crucible inside the quartz tube,
  • the quartz tube structure includes a quartz tube body and a quartz cap.
  • the key is that a support groove is provided at the upper part of the quartz tube body along the circumferential direction, and a solid particle sealant is formed in the support groove to become a liquid to form a seal when heated.
  • the quartz cap is inserted into the supporting groove, and the inside and outside of the quartz tube are communicated through the through hole provided at the lower end.
  • More than one through hole is provided at the lower end of the quartz cap.
  • the supporting groove is a U-shaped groove or a V-shaped groove.
  • a quartz tube for crystal growth of the VB/VGF method which includes a quartz tube body and a quartz cap.
  • the key design is that a supporting groove with an opening upward in the circumferential direction is provided on the upper part of the quartz tube body, and the quartz cap is inserted In the support groove, there is a freedom of movement up and down in the support groove.
  • the lower end of the quartz cap is provided with a through-hole structure. With the aid of the through-hole structure, the quartz tube communicates inside and outside.
  • the VB/VGF method crystal growth device includes a furnace body with a vacuum pipe, a quartz tube and a crucible.
  • the furnace body is provided with a heater for heating the quartz tube and the atmosphere temperature in the furnace.
  • the quartz tube is limited to
  • the quartz tube structure includes a quartz tube body and a quartz cap.
  • the crucible is set inside the quartz tube.
  • the key is that the upper part of the quartz tube body is provided with an opening upwardly along the circumferential direction, and the support groove is provided with a liquid formed by heating A sealed solid particle sealant.
  • the quartz cap is inserted into the support groove and has freedom of movement up and down in the support groove.
  • the lower end of the quartz cap is provided with a through-hole structure. With the aid of the through-hole structure, the quartz tube communicates inside and outside.
  • the quartz tube is isolated inside and outside Then, the temperature is increased to heat the polycrystalline material to melt the top of the seed crystal, and the crystal growth process is started for crystal growth. After the crystal growth is completed, annealing is performed to obtain the crystal. After the solid particle sealant is melted and sealed, during the reheating process, when the vapor pressure of the red phosphorus in the quartz tube is greater than the pressure of the quartz tube, the quartz cap can move upward until it bears the top surface of the furnace body, forming a pressure relief to prevent the quartz tube from bursting When the pressure in the quartz tube is low, the quartz cap drops again to maintain the pressure required for crystal growth.
  • the beneficial effects of the present invention are: (1)
  • the quartz tube for crystal growth provided by the VB/VGF method of the present invention has a simple and practical structure, does not require welding to seal the tube, and the pressure difference between the inside and outside of the quartz tube during the crystal growth process can be automatically adjusted within a certain range.
  • the quartz tube can be used repeatedly and save costs; (3) By setting solid particle sealant in the support groove and cleverly forming a seal with the change of its heating state, polycrystalline material is avoided Loss causes mismatch; (4) The device for VB/VGF method compound single crystal growth can directly realize the uniform vacuuming in the furnace body and the quartz tube, and then the quartz tube is sealed by the change of the heating state of the sealant to ensure the crystal growth pressure.
  • FIG. 1 is a schematic structural view of a quartz tube for crystal growth of the VB/VGF method of the present invention
  • FIG. 2 is a schematic structural view of a VB/VGF method crystal growth apparatus of the present invention.
  • a quartz tube for crystal growth by the VB/VGF method includes a quartz tube body 8 and a quartz cap 10, and an upper supporting groove 9 is provided in the upper part of the quartz tube body 8 along the circumferential direction, and the quartz cap 10 is inserted into the supporting groove 9 , And through the through hole 12 provided at the lower end to achieve internal and external communication of the quartz tube.
  • the quartz tube structure includes a quartz tube body 8 and a quartz cap 10.
  • the upper part of the quartz tube body 8 is circumferentially provided with an opening upward.
  • the support groove 9 and the quartz cap 10 are inserted into the support groove 9.
  • the quartz cap 10 has a degree of freedom of movement up and down in the support groove 9.
  • the lower end of the quartz cap is provided with a through hole 12 structure.
  • the supporting groove 9 can be provided on the outer surface or the inner surface of the quartz tube body 8, when the outer surface, the inner diameter of the quartz cap 10 is larger than the outer diameter of the quartz tube body 8; when the inner surface, the outer diameter of the quartz cap 10 is smaller than the quartz tube body 8 Inner diameter.
  • the support groove 9 is provided on the outer surface of the quartz tube body 8 to facilitate production.
  • the through hole 12 at the lower end of the quartz cap 10 is provided with more than one, preferably 2, 4, 6, 8, etc., which are arranged symmetrically and uniformly to ensure the uniform pressure in all directions during the vacuuming process.
  • the supporting groove 9 is a U-shaped groove or a V-shaped groove, that is, the longitudinal section of the quartz tube body 9, the supporting groove 9 may be a U-shaped groove or a V-shaped groove, preferably a U-shaped groove, and the flatness of the bottom surface of the U-shaped groove is high , Which is conducive to stable contact between the quartz cap 10 and the support groove 9.
  • the supporting groove 9 is provided with a solid particle sealant that becomes a liquid upon heating to form a seal.
  • the solid particle sealant changes from a solid state to a liquid to form a liquid seal upon heating, realizing insulation between the inside and the outside of the quartz tube, and the through hole 12 cooperates
  • the solid particle sealant realizes that the quartz tube can be evacuated uniformly with the furnace body, and then the quartz tube is self-sealed by heating, thereby ensuring crystal growth.
  • a leaking groove 13 is provided below the supporting groove 9 to prevent the solid particle sealant in the supporting groove 9 from overflowing when melted by heat.
  • the quartz tube for crystal growth of the VB/VGF method of the present embodiment is used in a single crystal growth furnace for VB/VGF method compounds.
  • a device for crystal growth by VB/VGF method includes a furnace body 1 provided with an evacuation pipe 14, a heater 2 in the furnace body 1, a quartz tube limited to the bottom of the furnace body 1 by the support body 3 and the inside of the quartz tube
  • the crucible 7, the quartz tube structure includes a quartz tube body 8 and a quartz cap 10, the upper part of the quartz tube body 8 is provided with a supporting groove 9 which is open upwards along the circumferential direction, and the supporting groove 9 is provided with a solid which becomes a liquid by heating to form a sealed solid
  • the quartz cap 10 is inserted into the support groove 9, and the inside and outside of the quartz tube are communicated through the through hole 12 provided at the lower end.
  • the device structure includes a furnace body 1, a quartz tube and a crucible 7 provided with a vacuum pipe 14, and a heater is provided in the furnace body 1 3.
  • the quartz tube Used to heat the quartz tube and the atmosphere temperature in the furnace; the quartz tube is limited to the bottom of the furnace body 1 by the support 3, the structure of the quartz tube includes a quartz tube body 8 and a quartz cap 10, and the crucible 7 is set in the quartz tube Inside the body 8, creatively, the upper part of the quartz tube body 8 is provided with a supporting groove 9 which is open upwards in the circumferential direction.
  • the supporting groove 9 is provided with a solid particle sealant which becomes a liquid by heating to form a seal, and the quartz cap 10 is inserted into the supporting groove 9, In addition, the support groove 9 has a degree of freedom to move up and down.
  • the lower end of the quartz cap 10 is provided with a through-hole 12 structure. With the aid of the through-hole 12 structure, the quartz tube communicates inside and outside.
  • the supporting groove 9 is a U-shaped groove or a V-shaped groove.
  • Quartz tube Place the filled quartz tube in the furnace body 1 and evacuate through the vacuum pipe 14 to make the furnace body 1 and the quartz tube reach the set vacuum degree.
  • the heating will melt all the solid particle sealant to form a seal.
  • Quartz tube is isolated inside and outside, and then the temperature is raised to heat the polycrystalline material 6, and the top of the seed crystal 4 is melted, and the crystal growth process is started to perform crystal growth. After the crystal growth is completed, the crystal is obtained by annealing. After the solid particle sealant is melted and sealed, in the reheating process, when the vapor pressure of the red phosphorus in the quartz tube is greater than the pressure of the quartz tube, the quartz cap 10 can move upward.
  • the furnace body 1 is provided with a furnace body
  • the upper insulation board 11 and the quartz cap 10 move upward when the upper displacement plate is against the upper insulation board 11 of the furnace body.
  • the upward movement of the quartz cap 10 forms a pressure relief, thereby preventing the quartz tube from bursting.
  • the quartz cap 10 drops again Thereby maintaining the pressure required for crystal growth.
  • the invention is used to protect the structure of the quartz tube and device for crystal growth of the VB/VGF method. It is not for the temperature and pressure control of crystal growth.
  • the temperature and pressure control involved can be realized by the existing furnace body. Have technology.
  • the VB/VGF method quartz tube for crystal growth provided by the present invention has a simple and practical structure, and can be used repeatedly, avoiding accidental damage during the crystal growth process, improving the success rate, and reducing the cost; VB/VGF method The device for crystal growth cleverly uses the state change of the solid particle sealant to form a uniform vacuum in the furnace body and the quartz tube, and then self-sealing.

Landscapes

  • 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)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)

Abstract

本发明提供一种VB/VGF法晶体生长用石英管及装置，涉及化合物晶体生长技术领域，采用的技术方案是：一种VB/VGF法晶体生长用石英管，包括石英管体和石英帽，关键在于，所述石英管体上部沿周向设置开口向上的支撑槽，所述石英帽插入支撑槽内，并借助设置在下端的通孔实现石英管内外连通。有益效果是：本VB/VGF法晶体生长用石英管结构简单实用，不用焊接封管，避免了压差造成的"炸管"，可重复实用，节省成本；VB/VGF法晶体生长用装置可直接实现炉体内、石英管内统一抽真空，后续借助密封剂受热状态变化使石英管密封，保证了晶体生长压力。

Description

一种VB/VGF法晶体生长用石英管及装置 技术领域
本发明涉及晶体生长技术领域，更具体地说，是涉及一种VB/VGF法晶体生长用石英管及装置。
背景技术
VB/VGF方法是生长高质量、低位错晶体的主要工艺技术之一。目前，成熟的VB/VGF法晶体生长技术是将籽晶、脱水氧化硼、多晶料装入热解氮化硼(PBN)坩埚中，再将PBN坩埚装到石英管中并装上封帽，通过抽真空，将石英管内真空抽到所需真空度,再将石英管和石英帽焊接到一块密封，最后放入VGF炉中进行热解。其中所采用的石英管，需要焊接密封，然而，焊接密封的石英管，一方面只能一次性使用，造成成本高；另一方面，在晶体生长升温过程中，经常出现由于升温程序或放入红磷量等条件不合适使得石英管内外压差大于石英管所承受的压力而发生“炸管”现象，造成晶体生长中断、石英管损毁，降低了生产效率，还造成成本浪费。
申请号为201420795278.8的实用新型专利公开了一种多元化合物多晶合成的装料容器及熔化处理系统，包括石英管和石英封帽，石英管内部中空，一端封口、另一端开口，石英封帽从所述开口可插入或拔出的装配在石英管内；所述石英管在靠近封口或/和开口的外壁上设有向内凹陷的多个凹槽，实现了装料后石英封帽的准确定位，但并未解决晶体生长过程中石英管压力不平衡问题，仍然容易造成生长过程中断，效率低。
发明内容
为解决现有晶体生长用石英管在生长过程中易“炸管”损毁、一次性使用成本高的技术问题，本发明提供一种VB/VGF法晶体生长用石英管及装置，采用分体式石英管结构，借助连接处的通孔实现内外连通，并巧妙借助受热密封剂的状态变化形成加热液封，从而实现了晶体生长过程中石英管内外压差在一定范围可调，避免了由于压差导致石英管炸管，还使得石英管可重复利用，降低了成本。
本发明采用的技术方案是：
一种VB/VGF法晶体生长用石英管，包括石英管体和石英帽，关键在于，所述石英管体上部沿周向设置开口向上的支撑槽，所述石英帽插入支撑槽内，并借助设置在下端的通孔实现石英管内外连通。
所述石英帽下端的通孔设有一个以上。
所述支撑槽为U型槽或V型槽。
所述支撑槽内设有受热变为液态形成密封的固体颗粒密封剂。
所述支撑槽下方设有接漏槽。
本发明还提供一种VB/VGF法晶体生长用装置，包括设有抽真空管道的炉体、炉体内的加热器、借助支撑体限位在炉体底部的石英管及石英管内部的坩埚，石英管结构中包括石英管体和石英帽，关键在于，所述石英管体上部沿周向设置开口向上的支撑槽，支撑槽内设有受热变为液态形成密封的固体颗粒密封剂，所述石英帽插入支撑槽内，并借助设置在下端的通孔实现石英管内外连通。
所述石英帽下端的通孔设有一个以上。
所述支撑槽为U型槽或V型槽。
所述支撑槽下方设有接漏槽。
上述技术方案中，首先提供一种VB/VGF法晶体生长用石英管，包括石英管体和石英帽，关键设计在于，石英管体上部沿周向设置开口向上的支撑槽，所述石英帽插入支撑槽内，并在支撑槽内具有上下移动自由度，石英帽的下端设有通孔结构，借助通孔结构，石英管内外连通。
VB/VGF法晶体生长用装置，包括设有抽真空管道的炉体、石英管及坩埚，炉体内设有加热器，用于加热石英管及炉内气氛温度，石英管借助支撑体限位在炉体底部，石英管结构中包括石英管体和石英帽，坩埚设置在石英管内部，关键在于，石英管体上部沿周向设置开口向上的支撑槽，支撑槽内设有受热变为液态形成密封的固体颗粒密封剂，所述石英帽插入支撑槽内，并在支撑槽内具有上下移动自由度，石英帽的下端设有通孔结构，借助通孔结构，石英管内外连通。
使用本装置进行晶体生长时，首先将籽晶、脱水氧化硼和多晶料依次放入坩埚，并将坩埚放入石英管，再根据生长工艺所需压力、温度及理想气体状态方程PV＝MRT/m计算出石英管空间所需的红磷量，称量计算好的红磷并放置到石英管内。向石英管体的支撑槽内填入液封剂，再将石英帽插入支撑槽内，装料完毕。将装好料的石英管置于炉体中，通过抽真空管道抽真空，使得炉体内及石英管内达到设定真空度，加热使固体颗粒密封剂全部融化，形成密封，此时石英管内外隔绝,再升高温度加热多晶料、使籽晶顶部熔化，开始晶体生长程序进行晶体生长，晶体生长完成后，进行退火即得到晶体。固体颗粒密封剂融化密封后，再加热过程中，石英管内红磷受热产生的蒸气压大于石英管承受压力时，石英帽可向上移动直至顶住炉体上顶面，形成泄压避免石英管炸裂，石英管内压力低时石英帽又下降从而 维持晶体生长所需压力。
本发明的有益效果是：(1)本发明提供的VB/VGF法晶体生长用石英管结构简单实用，不用焊接封管，晶体生长过程中石英管内外压差，在一定范围内可自动调节，避免了压差造成的“炸管”；(2)石英管可重复实用，节省成本；(3)通过在支撑槽设置固体颗粒密封剂并巧妙借助其受热状态变化形成密封，避免了多晶料损失而造成不配比；(4)VB/VGF法化合物单晶生长用装置可直接实现炉体内、石英管内统一抽真空，后续借助密封剂受热状态变化使石英管密封，从而保证其晶体生长压力。
附图说明
图1为本发明的VB/VGF法晶体生长用石英管的结构示意图；
图2为本发明的VB/VGF法晶体生长用装置的结构示意图；
图中，1、炉体，2、加热器，3、支撑体，4、籽晶，5、氧化硼，6、多晶料，7、坩埚，8、石英管体，9、支撑槽，10、石英帽，11、炉体上部保温板，12、通孔，13、接漏槽，14为抽真空管道。
具体实施方式
以下以具体实施例详细说明本发明所提供的一种VB/VGF法晶体生长用石英管及装置的结构及使用方法，但不以任何形式限制本发明的保护范围，所属领域技术人员根据技术方案所进行的改善修改或者类似替换，均应包含在本发明的保护范围之内。
实施例1
一种VB/VGF法晶体生长用石英管，包括石英管体8和石英帽10，所述石英管体8上部沿周向设置开口向上的支撑槽9，所述石英帽10插入支撑槽9内，并借助设置在下端的通孔12实现石英管内外连通。
本实施例提供一种VB/VGF法晶体晶生长用石英管，参见附图1所示，石英管结构中包括石英管体8和石英帽10，石英管体8上部沿周向设置开口向上的支撑槽9，石英帽10插入支撑槽9内，石英帽10在支撑槽9内具有上下移动自由度，石英帽的下端设有通孔12结构，借助通孔12结构，石英管内外实现气压连通。其中，支撑槽9可设置于石英管体8外表面或内表面，设置在外表面时，石英帽10内径大于石英管体8外径；设置在内表面时，石英帽10外径小于石英管体8内径，本实施例中，支撑槽9设置于石英管体8外表面，便于生产制作。
所述石英帽10下端的通孔12设有一个以上，优选2个、4个、6个、8个等，对称均布设置，以保证抽真空过程中各个方向压力一致。
所述支撑槽9为U型槽或V型槽，即石英管体9的纵切面看，支撑槽9可为U型槽或V型槽，优选U型槽，U型槽底面平整度较高，有利于石英帽10与支撑槽9的接触稳定。
所述支撑槽9内设有受热变为液态形成密封的固体颗粒密封剂，在使用过程中，固体颗粒密封剂受热由固态变为液态形成液封，实现石英管内外的隔绝，通孔12配合固体颗粒密封剂，实现了石英管可与炉体统一抽真空、而后通过加热实现石英管的自密封，从而保证晶体生长。
所述支撑槽9下方设有接漏槽13，以防支撑槽9内的固体颗粒密封剂受热融化时溢出。
本实施例的VB/VGF法晶体晶生长用石英管在使用时，是在VB/VGF法化合物单晶生长炉中使用。
实施例2
一种VB/VGF法晶体生长用装置，包括设有抽真空管道14的炉体1、炉体1内的加热器2、借助支撑体3限位在炉体1底部的石英管及石英管内部的坩埚7，石英管结构中包括石英管体8和石英帽10，所述石英管体8上部沿周向设置开口向上的支撑槽9，支撑槽9内设有受热变为液态形成密封的固体颗粒密封剂，所述石英帽10插入支撑槽9内，并借助设置在下端的通孔12实现石英管内外连通。
本实施例提供的VB/VGF法晶体生长用装置，参见附图2所示，装置结构中包括设有抽真空管道14的炉体1、石英管及坩埚7，炉体1内设有加热器3，用于加热石英管及炉内气氛温度；石英管借助支撑体3限位在炉体1内的底部，石英管的结构中包括石英管体8和石英帽10，坩埚7设置在石英管体8内部，创造性的，石英管体8上部沿周向设置开口向上的支撑槽9，支撑槽9内设有受热变为液态形成密封的固体颗粒密封剂，石英帽10插入支撑槽9内，并在支撑槽9内具有上下移动自由度，石英帽10的下端设有通孔12结构，借助通孔12结构，石英管内外连通。
所述所石英帽10下端的通孔12设有一个以上。
所述支撑槽9为U型槽或V型槽。
所述支撑槽9下方设有接漏槽13。
使用本装置进行晶体生长时，首先将籽晶4、脱水氧化硼5和多晶料6依次放入坩埚7，坩埚7直径为2英寸～12英寸，并将坩埚7放入石英管，再根据生长工艺所需压力、温度及理想气体状态方程PV＝MRT/m计算出石英管空间所需的红磷量，称量计算好的红磷并 放置到石英管内。将石英帽10插入支撑槽9内，再将固体颗粒密封剂填入支撑槽9内的剩余空间，固体颗粒密封剂优选氧化硼颗粒，装料完毕。将装好料的石英管置于炉体1中，通过抽真空管道14抽真空，使得炉体1内及石英管内达到设定真空度，加热使固体颗粒密封剂全部融化，形成密封，此时石英管内外隔绝,再升高温度加热多晶料6、并使籽晶4顶部熔化，开始晶体生长程序进行晶体生长，晶体生长完成后，进行退火即得到晶体。固体颗粒密封剂融化密封后，在再加热过程中，石英管内红磷受热产生的蒸气压大于石英管承受压力时，石英帽10可向上移动，本实施例中，炉体1内设有炉体上部保温板11，石英帽10向上移动时最大位移为顶住炉体上部保温板11，石英帽10的上移形成泄压，从而避免了石英管炸裂，石英管内压力低时石英帽10又下降从而维持晶体生长所需压力。本发明用于保护VB/VGF法晶体生长用石英管及装置的结构构造，并非对晶体生长中的温度、压力控制等，所涉及的温度、压力控制以现有炉体均可实现，为现有技术。
综上可见，本发明提供的VB/VGF法晶体生长用石英管结构简单实用，且可重复使用，避免了晶体生长过程中的意外损坏，提高了成功率，还降低了成本；VB/VGF法晶体生长用装置巧妙借助固体颗粒密封剂状态变化形成炉体内、石英管内统一抽真空，后续自密封。

Claims (9)

  1. 一种VB/VGF法晶体生长用石英管，包括石英管体(8)和石英帽(10)，其特征在于，所述石英管体(8)上部沿周向设置开口向上的支撑槽(9)，所述石英帽(10)插入支撑槽(9)内，并借助设置在下端的通孔(12)实现石英管内外连通。
  2. 根据权利要求1所述的石英管，其特征在于，所述石英帽(10)下端的通孔(12)设有一个以上。
  3. 根据权利要求1所述的石英管，其特征在于，所述支撑槽(9)为U型槽或V型槽。
  4. 根据权利要求1-3任一所述的石英管，其特征在于，所述支撑槽(9)内设有受热变为液态形成密封的固体颗粒密封剂。
  5. 根据权利要求1-3任一所述的石英管，其特征在于，所述支撑槽(9)下方设有接漏槽(13)。
  6. 一种VB/VGF法晶体生长用装置，包括设有抽真空管道(14)的炉体(1)、炉体(1)内的加热器(2)、借助支撑体(3)限位在炉体(1)底部的石英管及石英管内部的坩埚(7)，石英管结构中包括石英管体(8)和石英帽(10)，其特征在于，所述石英管体(8)上部沿周向设置开口向上的支撑槽(9)，支撑槽(9)内设有受热变为液态形成密封的固体颗粒密封剂，所述石英帽(10)插入支撑槽(9)内，并借助设置在下端的通孔(12)实现石英管内外连通。
  7. 根据权利要求6所述的装置，其特征在于，所述石英帽(10)下端的通孔(12)设有一个以上。
  8. 根据权利要求6所述的装置，其特征在于，所述支撑槽(9)为U型槽或V型槽。
  9. 根据权利要求6-8任一所述的装置，其特征在于，所述支撑槽(9)下方设有接漏槽(13)。
PCT/CN2019/083281 2018-12-14 2019-04-18 一种vb/vgf法晶体生长用石英管及装置 WO2020118999A1 (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2020522301A JP6913430B2 (ja) 2018-12-14 2019-04-18 Ｖｂ／ｖｇｆ法による結晶成長用石英管及び装置

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201811532469.4 2018-12-14
CN201811532469.4A CN109402723A (zh) 2018-12-14 2018-12-14 一种vb/vgf法晶体生长用石英管及装置

Publications (1)

Publication Number Publication Date
WO2020118999A1 true WO2020118999A1 (zh) 2020-06-18

Family

ID=65459228

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2019/083281 WO2020118999A1 (zh) 2018-12-14 2019-04-18 一种vb/vgf法晶体生长用石英管及装置

Country Status (3)

Country Link
JP (1) JP6913430B2 (zh)
CN (1) CN109402723A (zh)
WO (1) WO2020118999A1 (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114318497A (zh) * 2022-01-25 2022-04-12 洛阳市自动化研究所有限公司 一种用于制备合金晶棒的区熔炉
CN115771996A (zh) * 2022-11-18 2023-03-10 云南中科鑫圆晶体材料有限公司 Vgf晶体生长用超大直径石英管的真空封焊方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109402723A (zh) * 2018-12-14 2019-03-01 中国电子科技集团公司第十三研究所 一种vb/vgf法晶体生长用石英管及装置
CN111962139A (zh) * 2020-09-17 2020-11-20 广东先导先进材料股份有限公司 Vgf工艺制备砷化镓晶体的方法
CN113481604B (zh) * 2021-07-09 2023-03-28 武汉拓材科技有限公司 一种高纯碲化镓多晶合成生产装置

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6011298A (ja) * 1983-06-24 1985-01-21 Furukawa Electric Co Ltd:The 高解離圧化合物単結晶の製造法及び装置
CN103420345A (zh) * 2012-05-22 2013-12-04 广东先导稀材股份有限公司 石墨坩埚、加热炉以及碲化镉的制备方法
CN205077175U (zh) * 2015-11-03 2016-03-09 大庆佳昌晶能信息材料有限公司 一种vgf法单晶生长装置
CN107059132A (zh) * 2017-03-29 2017-08-18 磐石创新（北京）电子装备有限公司 一种碲锌镉单晶的新型单晶炉及生长工艺
CN108060454A (zh) * 2017-12-15 2018-05-22 广东先导先进材料股份有限公司 一种vgf法制备砷化镓晶体的装置及方法
CN207512313U (zh) * 2017-11-30 2018-06-19 广东天鼎思科新材料有限公司 一种磷化铟单晶受控生长装置
CN109402723A (zh) * 2018-12-14 2019-03-01 中国电子科技集团公司第十三研究所 一种vb/vgf法晶体生长用石英管及装置
CN209260248U (zh) * 2018-12-14 2019-08-16 中国电子科技集团公司第十三研究所 一种vb/vgf法晶体生长用石英管及装置

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6011298A (ja) * 1983-06-24 1985-01-21 Furukawa Electric Co Ltd:The 高解離圧化合物単結晶の製造法及び装置
CN103420345A (zh) * 2012-05-22 2013-12-04 广东先导稀材股份有限公司 石墨坩埚、加热炉以及碲化镉的制备方法
CN205077175U (zh) * 2015-11-03 2016-03-09 大庆佳昌晶能信息材料有限公司 一种vgf法单晶生长装置
CN107059132A (zh) * 2017-03-29 2017-08-18 磐石创新（北京）电子装备有限公司 一种碲锌镉单晶的新型单晶炉及生长工艺
CN207512313U (zh) * 2017-11-30 2018-06-19 广东天鼎思科新材料有限公司 一种磷化铟单晶受控生长装置
CN108060454A (zh) * 2017-12-15 2018-05-22 广东先导先进材料股份有限公司 一种vgf法制备砷化镓晶体的装置及方法
CN109402723A (zh) * 2018-12-14 2019-03-01 中国电子科技集团公司第十三研究所 一种vb/vgf法晶体生长用石英管及装置
CN209260248U (zh) * 2018-12-14 2019-08-16 中国电子科技集团公司第十三研究所 一种vb/vgf法晶体生长用石英管及装置

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114318497A (zh) * 2022-01-25 2022-04-12 洛阳市自动化研究所有限公司 一种用于制备合金晶棒的区熔炉
CN115771996A (zh) * 2022-11-18 2023-03-10 云南中科鑫圆晶体材料有限公司 Vgf晶体生长用超大直径石英管的真空封焊方法
CN115771996B (zh) * 2022-11-18 2024-03-22 云南中科鑫圆晶体材料有限公司 Vgf晶体生长用超大直径石英管的真空封焊方法

Also Published As

Publication number Publication date
JP2021510139A (ja) 2021-04-15
JP6913430B2 (ja) 2021-08-04
CN109402723A (zh) 2019-03-01

Similar Documents

Publication Publication Date Title
WO2020118999A1 (zh) 一种vb/vgf法晶体生长用石英管及装置
CN109252220A (zh) 一种vgf/vb砷化镓单晶炉结构及生长方法
CN103849928A (zh) 一种多片式导模法蓝宝石晶片生长工艺
TWI723579B (zh) 大尺寸高純度碳化矽單晶、基材及其製備方法和製備用裝置
CN201756596U (zh) 多瓣石墨坩埚
CN207512313U (zh) 一种磷化铟单晶受控生长装置
CN103938270A (zh) 镓重掺杂低位错锗单晶的生长方法
CN202989351U (zh) 基于多加热器的铸锭炉热场结构
CN103132130B (zh) 一种使用悬浮衬套管氨热法生长氮化镓体单晶的装置和方法
CN113638048B (zh) 一种vgf法生长磷化铟单晶的方法
CN111020689A (zh) 晶体生长装置及方法
CN113213971A (zh) 一种pbn坩埚氧化预处理装置、方法及其应用
CN210711818U (zh) 一种基于VGF法的减少GaAs晶体孪晶的装置
CN104498901B (zh) 一种碳化硅单晶片的镀膜方法和装置
CN210620996U (zh) 一种炉体温度可调的冷壁单晶炉
CN207294942U (zh) 一种带石墨和水冷复合热屏的高效单晶生长炉
CN201024211Y (zh) 真空蒸发物理气相沉积薄膜生长装置
CN209260248U (zh) 一种vb/vgf法晶体生长用石英管及装置
CN106521615A (zh) 一种基于VGF法的InP晶体生长炉
CN203923441U (zh) 内置排气装置的单晶炉
CN110565168A (zh) 一种炉体温度可调的冷壁单晶炉及砷化镓晶体生长方法
US20130029278A1 (en) Method for synthesizing group ii-vi compound semiconductor polycrystals
CN214529324U (zh) 一种生长半绝缘砷化镓单晶的掺碳装置
CN206396351U (zh) 一种基于VGF法的InP晶体生长炉
CN206204470U (zh) 一种可实现单晶在线退火的生长设备

Legal Events

Date Code Title Description
ENP Entry into the national phase

Ref document number: 2020522301

Country of ref document: JP

Kind code of ref document: A

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 19895223

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 19895223

Country of ref document: EP

Kind code of ref document: A1