CN1033179C - Controllable bi-spherical Ge mono crystal growth method and its moulding die - Google Patents

Controllable bi-spherical Ge mono crystal growth method and its moulding die Download PDF

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Publication number
CN1033179C
CN1033179C CN 92104643 CN92104643A CN1033179C CN 1033179 C CN1033179 C CN 1033179C CN 92104643 CN92104643 CN 92104643 CN 92104643 A CN92104643 A CN 92104643A CN 1033179 C CN1033179 C CN 1033179C
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China
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germanium
mould
growth
single crystal
spherical
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Expired - Fee Related
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CN 92104643
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CN1068156A (en
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吴雅颂
李昆
任敏
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KUNMING RESEARCH INST OF METALLURGY
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KUNMING RESEARCH INST OF METALLURGY
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Abstract

The present invention relates to a method and a mould for controlling the growth of dual-spherical germanium monocrystals, which belongs to the field of the growth of semiconductor metallurgical crystals. In the method, germanium metal and germanium monocrystal seed crystals are respectively loaded in a crystal seed chamber 4 on the lower part of a lower mould 3 between an upper graphite mould 2 and a lower graphite mould 3 of a mould in a common crystal growth device, and dual-spherical monocrystals with arbitrary curvature radii directly grow up through the thermal solidification of the mould. The present invention has the advantages of simple processes, low material consumption, high optical quality, no pollution, low cost, etc., and is suitable for the growth of lens blanks of dual-spherical or single-spherical germanium monocrystals.

Description

Controllable bi-spherical Ge mono crystal growth method and its moulding die
The present invention relates to a kind of controllable bi-spherical Ge mono crystal growth method and mould, belong to the metallurgical field of crystal growth of semi-conductor.
At present domestic and international thermal imaging system, night vision equipment and carbon dioxide laser device etc. use optics germainium lens blank forming method.Method one is after drawing body daraf(reciprocal of farad) production germanium single crystal rod on adopting, to make sphere germanium monocrystal lens blank through cut-out, cylindrical barreling, curvature grinding.This method high material consumption, processed complex, the cost height is with dust pollution.Method two is to adopt casting, by the lens blank geometrical shape processing mold of setting, and type in the casting in the mould of single crystal growth apparatus or vacuum oven.This method gained optics germainium lens blank is a polycrystal, and optical quality reduces.
The objective of the invention is to overcome the deficiency of prior art and a kind of controllable bi-spherical Ge mono crystal growth method and mould are provided.
The present invention is achieved in that and is respectively charged into germanium metal and germanium single crystal seed crystal between the patrix 2 of the mould in the single crystal growth apparatus and the counterdie 3 and in the crystal seed chamber 4 of counterdie 3 bottoms, patrix 2 is the sphere with any setting radius-of-curvature with counterdie 3, spherical radius(sph.r.) is determined by the shape of required germainium lens, is constituted through conventional machining.Germanium metal and germanium single crystal seed crystal are smelted in crystals growth equipment, the temperature of control germanium metal melt is 937 ℃-987 ℃, germanium metal melt and seed crystal interface temperature are 937 ℃, the temperature of germanium single crystal seed crystal is 787-937 ℃, in the control crystal growing process, counterdie 3 is per hour 0-5 centimetre with the position relative moving speed of well heater 1, and the mould speed of rotation is that per minute 10 changes, through crystal seed guiding in 1-4 hour, module thermosetting direct growth went out the two sphere single crystal of any radius-of-curvature.
Accompanying drawing 1 is technological process block-diagram of the present invention;
Accompanying drawing 2 is mould assembling synoptic diagram of the present invention.1 is that well heater, 5 is that thermal insulation layer, 6 is the germanium metal melt among the figure.
The present invention is described in further detail below in conjunction with accompanying drawing (embodiment): it is 80.6mm that patrix 2 and counterdie 3 combination sections are designed to diameter, and radius-of-curvature is respectively the sphere of 102.57mm and 207mm.With the dioxygen water law germanium is carried out clean, the germanium metal block of 165g is packed into go up between graphite mo(u)ld 2 and the following graphite mo(u)ld 3 subsequently, the single crystal seed of 4 * 4 * 40mm is put into the crystal seed chamber 4 of counterdie 3 bottoms.The mould that germanium metal block and single crystal seed will be housed is then put into the known single crystal growth apparatus (model is TDK-36AZ) that graphite heater 1 and thermal insulation layer 5 have been housed.Measure the temperature field with known common galvanic couple, adjust the temperature field and distribute, make it satisfy crystal growth condition d 2T/dr 2→ 0, dT/dQ → 0, dT/dz constant.When initial growth, the temperature and the seed crystal weld of control germanium metal melt are 937 ℃, another surface temperature is 987 ℃, the temperature of germanium single crystal seed crystal one end is 937 ℃, the other end temperature is 790 ℃, in the process of growth, graphite heater 1 relatively moves with graphite jig 3 and is per hour 4.0 centimetres, and the speed of rotation that is loaded on the mould in the rotating shaft of sweet pot is that per minute 2.5 changes.In the crystal growing process with known vacuum pump to vacuumizing in the crystal growth equipment, making the vacuum tightness in its crystal growth equipment is 8 * 10 -3The mmhg post.Furnace cooling after the guiding of 3 hours crystal seeds, module thermosetting obtains two sphere single crystal lens blanks of the required radius-of-curvature that direct growth goes out through the demoulding.The Kunming physics I of the institute class thermal imaging system of making of aforesaid method need with diameter be 80.6mm, radius-of-curvature is respectively 102.57mm and 207mm, the bi-spherical Ge single crystal lens blank of heavy 165g has higher optical quality.
The present invention compared with prior art has simplification molding procedure, material Material consumes low, the optical quality height, and the advantage such as cost is low, and is pollution-free, Be applicable to growth bi-spherical Ge monocrystal lens blank, also be suitable for simultaneously Single sphere germanium single crystal lens blank of growing.

Claims (2)

1. controllable bi-spherical Ge mono crystal growth method, process of growth is carried out in single crystal growth apparatus, and known single crystal growing condition: d is satisfied in the controlled temperature field 2T/dr 2→ 0, dT/dQ → 0, dT/dz ≈ constant, it is characterized in that this method is that the curvature by two spheres of the germanium monocrystal of required shaping is determined that upper and lower mould curvature and the germanium metal melt that adds in the closed mould cavity that forms through conventional machine worker draw under the germanium single crystal seed crystal, oriented growth becomes to set the bi-spherical Ge single crystal of curvature; The temperature of germanium metal melt is 937 ℃-987 ℃, and when initial growth, the patrix 2 of mould is 937 ℃-987 ℃ with the temperature of germanium metal melt in the equipment, and melt and germanium single crystal seed crystal interface temperature are 937 ℃, and the temperature of germanium single crystal seed crystal is 787 ℃-937 ℃; The counterdie 3 that constitutes the mould of die cavity moves down with respect to well heater 1, translational speed is per hour changing in the 0-5 cm range, the mould speed of rotation is that per minute 10 changes, and through crystal seed guiding in 1-4 hour, module thermosetting direct growth went out two sphere single crystal of any setting radius-of-curvature.
2. a mould of implementing claim 1 is characterized in that this mould constitutes the die cavity with any setting radius-of-curvature, is made up of counterdie that is provided with crystal seed chamber 43 in the crucible rotating shaft that is arranged in crystal growth equipment and patrix 2; Patrix 2 covers on solid-state germanium metal, behind the germanium melting of metal, relies on the weight effect of patrix 2 and with the sliding friction of counterdie 3 and cooperates the composition closed mould cavity; Patrix 2 is to have the sphere of setting radius-of-curvature with the surface shape that counterdie 3 contacts with metal melt; Moulding stock is a high purity graphite, and the surfaceness that directly contacts the germanium metal melt is better than 1.6, and counterdie 3 internal diameters are not more than 70% of monocrystalline burner hearth internal diameter.
CN 92104643 1992-06-11 1992-06-11 Controllable bi-spherical Ge mono crystal growth method and its moulding die Expired - Fee Related CN1033179C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 92104643 CN1033179C (en) 1992-06-11 1992-06-11 Controllable bi-spherical Ge mono crystal growth method and its moulding die

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 92104643 CN1033179C (en) 1992-06-11 1992-06-11 Controllable bi-spherical Ge mono crystal growth method and its moulding die

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CN1068156A CN1068156A (en) 1993-01-20
CN1033179C true CN1033179C (en) 1996-10-30

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105803518B (en) * 2016-05-31 2018-02-06 中国工程物理研究院化工材料研究所 Class Czochralski crystal growth device and method
CN108048904B (en) * 2017-11-30 2021-02-26 安徽省恒伟铋业有限公司 Bismuth crystal manufacturing equipment
CN108277531A (en) * 2017-12-26 2018-07-13 广东先导先进材料股份有限公司 The growing method of germanium single crystal
CN108560049B (en) * 2018-04-16 2019-09-06 湖南柿竹园有色金属有限责任公司 The preparation method of the colorful bismuth crystal of the large scale of color controllable

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