CN2666930Y - Apparatus for growing long-size semi-insulation gallium arsenide single crystal - Google Patents

Apparatus for growing long-size semi-insulation gallium arsenide single crystal Download PDF

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Publication number
CN2666930Y
CN2666930Y CN 200320129498 CN200320129498U CN2666930Y CN 2666930 Y CN2666930 Y CN 2666930Y CN 200320129498 CN200320129498 CN 200320129498 CN 200320129498 U CN200320129498 U CN 200320129498U CN 2666930 Y CN2666930 Y CN 2666930Y
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stay
warm case
millimeters
crucible
growing
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Expired - Fee Related
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CN 200320129498
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Chinese (zh)
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赖占平
高瑞良
齐德格
周春锋
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CETC 46 Research Institute
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CETC 46 Research Institute
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Abstract

The utility model provides a growth long-dimension semi-insulated device gallium arsenide single-crystal device with simple process device and little-polluted impurities produced in production process. The device is provided with a ring-shaped heat preservation cylinder; an edge of an internal ring of an upper cover of the heat preservation cylinder is provided with a frustum-shaped heat preservation cover; a lower round of the heat preservation cover is immerged into a hydraulic sealing layer of a crucible.

Description

A kind of device of the long size semi-insulating GaAs monocrystalline of growing
Technical field the utility model relates to a kind of device of growth compound semiconductor monocrystal, the device of the long size compound semiconductor single crystal of particularly a kind of employing LEC (liquid encapsulation Czochralski) technology (LEC) growth.
Device and circuit that background technology adopts semi-insulating GaAs single crystalline substrate material to make mainly comprise very high speed integrated circuit and microwave and millimeter wave monolithic integrated circuit.These circuit are Key Circuit of radar, electronic countermeasure, computer, satellite communication equipment raising speed, also are widely used in fields such as cell phone, digital personal communications, opticfiber communication and space system.Usually LEC (liquid encapsulation Czochralski) technology (LEC) is adopted in the semi-insulating GaAs single crystal growing, this technology also be used for growth as: gallium phosphide (GaP), indium phosphide (InP), indium arsenide (InAs), gallium antimonide compound semiconductor crystals such as (GaSb).Owing to continue the thermal field condition that changes in complex effects that thermograde in the LEC technology in the melt and melt turbulent flow are brought and the crystal growing process, make the still unusual difficulty of compound semiconductor single crystal of present LEC technology growth major diameter (〉=100 millimeters), long size (〉=130 millimeters), high integrality.Draw crystalline length and quality in order to improve, in early days comprise mainly that in the trial of control crystal growth technique the various processing parameters of control are as crucible or crystalline velocity of rotation, the crystalline pull rate, and the total heat of crucible input, also adopted magnetic field to suppress the turbulent flow that convection current forms in the melt, these attempt the raising for crystal length and quality, have played limited effect.The trial that also has is to use baffle plate or other device directly to suppress near the crucible relative position place the crystallization forward position or eliminate convection current under the crystallization forward position.United States Patent (USP) 4,645,560 have disclosed a kind of device that improves crystal length and crystal forming rate, shown in Fig. 1 b, mainly comprise cracking boron nitride (PBN) crucible 19, crucible tray 20, crystal pulling rod 24, crucible shaft 25, pressurized vessel 28, insulation construction 29, wherein seed crystal 27 is fixed on the crystal pulling rod 24, contact the GaAs melt 21 that is placed in the PBN crucible 19 by the seed crystal 27 that will be fixed on the crystal pulling rod 24, slowly reduce GaAs melt 21 temperature in the PBN crucible 19, promote the seed crystal 27 that is fixed on the crystal pulling rod 24 with certain speed, and growing gallium arsenide 26, boron oxide fluid-tight layer 23 is as fluid-tight.The employing of this device be a kind of Floating stay-warm case 22 of hollow, insert in the GaAs melt 21 lower edge of stay-warm case 22, because the material graphite that adopts is different with the thermal conductivity of melt, can in crystal growing process, cause the crystallization at pontoon edge, influence carrying out smoothly of crystal growth, in addition because the existence of stay-warm case can influence the observation to crystal growing process.Fig. 1 a is the pontoon part synoptic diagram of prior art.Researchist Hunter D.Marshall (J.Crystal Growth109 (1991), p218-213) in order to improve crystalline length and quality, proposed in the crucible that fluid-tight agent and melt are housed, add the ring shielding cover of a PBN, shielding case is positioned over quartzy pontoon top, whole device is suspended in the fluid-tight layer, realizes the shape of control crystal growth forward position solid-liquid interface by this device, and then realizes improving the purpose of crystal length.Adopt this device to avoid crystalline dissociation on surface in the fluid-tight layer, but, can in process of growth, introduce impurity (Si), influence the semi-insulating performance of crystalline owing to used quartzy pontoon.In addition, in the document, also mentioned adopting and placed an annular molybdenum sheet below the quartzy pontoon, to reduce the calorific loss of fluid-tight layer, improve the shape in crystal structure forward position, by the same token, also can introduce impurity (Si), and then influence the semi-insulating performance of crystalline, simultaneously, need adopt special device, in order to avoid crystal diameter proposes the fluid-tight layer with stay-warm case when too big to crystal diameter control because the molybdenum sheet that adopts is opaque.Though above-mentioned trial is to improving crystal length and quality has certain effect, exist some common shortcomings: (1) crystal growing process is not directly observed, or needs special device, increases the complex process degree; (2) device directly contacts melt, can cause the contamination of melt to influence crystal mass.
It is comparatively simple that the summary of the invention the purpose of this utility model provides a kind of process unit, the device of the long size semi-insulating GaAs of the growth monocrystalline that the impurity contamination that produces in the production process is few.
The technical scheme that the utility model adopted is as follows:
The device of a kind of long size semi-insulating GaAs monocrystalline of growing that the utility model is designed comprises pressurized vessel, the interior crucible that is provided with of pressurized vessel and crucible tray, crystal pulling rod, centers on crucible and the well heater of crucible tray setting and the electrode that links to each other with well heater.The periphery of well heater is provided with annular heat-preservation cylinder, and annular heat-preservation cylinder top is provided with the heat-preservation cylinder loam cake, the bottom is provided with the heat-preservation cylinder lower cover, in the bottom of heat-preservation cylinder lower cover stent support is arranged, and the interior ring edge of heat-preservation cylinder loam cake is provided with the truncated cone shape stay-warm case.The circle outer of going up of stay-warm case is provided with ring-shaped platform, the ring-shaped platform outer highly is the annular brace of 40-80 millimeter to having, the annular brace of stay-warm case is positioned in the ring groove of heat-preservation cylinder loam cake, the following circle of stay-warm case is immersed in the fluid-tight layer in the crucible, difform stay-warm case all is fit to for growth technique, but also there is the limit in the upper and lower size of stay-warm case, mainly by following various decision (unit is a millimeter):
D 1>D 4+20
D 2<D 3+10
H 1<H 0-30
H 2=V×T+10
Wherein, D1 represents the lower edge diameter of stay-warm case, D2 represents the upper edge diameter of stay-warm case, D3 represents crucible diameter, D4 represents crystal diameter, H1 represents the whole height of stay-warm case, H0 represents the crystalline total length, and H2 represents the bearing height of stay-warm case, and promptly the ring-shaped platform outer is to the height of the annular brace that has, on behalf of crucible, V follow speed, promptly in crystal growing process, the speed that crucible moves up, T represents following the time of crucible, promptly in crystal growing process, the time that crucible moves up.
The top of above-mentioned pressurized vessel is provided with quartzy window, and its structure is to be arranged in the hole on pressurized vessel top a quartz pushrod is housed, and the two ends of rod are surface polishing, form optical window.
The fluid-tight layer that adopts in this device is a boron oxide.
The lower edge diameter D1 optimum range of stay-warm case is 110~220 millimeters in this device, the upper edge diameter D2 optimum range of stay-warm case is 110~300 millimeters, the whole height H1 optimum range of stay-warm case is 100~200 millimeters, and the bearing height H2 optimum range of stay-warm case is 40~80 millimeters.
The material that is suitable for making stay-warm case can adopt one of following material: high purity graphite is coated with graphite and PBN (cracking boron nitride) with BN (boron nitride).Because high purity graphite has high thermal, high purity graphite is a preferred material.
Obviously, the utlity model has following beneficial effect:
1,, is easy to make and install because this apparatus structure is very simple.
2, the stay-warm case lower edge owing to this device is positioned near the crystal growth crystallization forward position, highly beneficial for the interface shape of improving the crystal growth forward position, because what adopt is high-purity high-density degree graphite, make because the impurity contamination that graphite material causes minimizes, improve crystalline length, guaranteed the semi-insulating performance of crystalline.
Attemperator when 3, the stay-warm case of this device also can be used as the crystal cooling can reduce the thermal stresses in the crystal, improves the mechanical property that crystal adds man-hour.
4, owing to be provided with quartzy window on the top of pressurized vessel, stay-warm case is a truncated cone shape, can the direct viewing crystal growing process, improved the ability of control crystal growing process.
It below the description of drawings description of drawings
Fig. 1 a is the pontoon part synoptic diagram of prior art
Fig. 1 b is the one-piece construction synoptic diagram of prior art,
Fig. 2 is an one-piece construction synoptic diagram of the present utility model.
Fig. 3 is testing data figure of the present utility model
Among the figure: PBN crucible 1 crucible tray 2 GaAs melts 3 stay-warm cases 4 crystal pulling rods 6 crucible axis 7 gallium arsenides 8 seed crystals 9 pressure vessels 10 insulation construction loam cake 11a annular heat-preservation cylinder 11b insulation construction lower cover 11c heater 12 heater electrodes 13 insulation construction supports 14 quartzy window 15 crystallization front interface shape 16 prior art Interfacial Edges of the present utility model are along crystallization front interface shape 18 PBN crucibles 19 crucible trays 20 GaAs melts 21 stay-warm cases 22 boron oxide fluid-tight layers 23 crystal pulling rod 24 crucible axis 25 gallium arsenides 26 seed crystals 27 pressure vessels 28 insulation constructions 29 heaters 30 of crooked 17 prior aries
Embodiment is described further the utility model below in conjunction with accompanying drawing and specific embodiment.
As shown in Figure 2, a kind of device of the long size semi-insulating GaAs monocrystalline of growing comprises pressurized vessel 10, the pressurized vessel 10 interior crucibles 1 that are provided with and crucible tray 2, crystal pulling rod 6, centers on crucible 1 and the well heater 12 of crucible tray 2 settings and the electrode 13 that links to each other with well heater 12.The periphery of well heater 12 is provided with annular heat-preservation cylinder 11b, and annular heat-preservation cylinder 11b top is provided with heat-preservation cylinder loam cake 11a, the bottom is provided with heat-preservation cylinder lower cover 11c, has support 14 to support in the bottom of heat-preservation cylinder lower cover 11c.The top of pressurized vessel 10 is provided with quartzy window 15, and its structure is to be arranged in the hole on pressurized vessel top a quartz pushrod is housed, and the two ends of rod are surface polishing, form optical window.The interior ring edge of heat-preservation cylinder loam cake 11a is provided with truncated cone shape stay-warm case 4, the circle outer of going up of stay-warm case 4 is provided with ring-shaped platform, the ring-shaped platform outer highly is 60 millimeters a annular brace to having, the annular brace of stay-warm case is positioned in the ring groove of heat-preservation cylinder loam cake, the following circle of stay-warm case 4 is immersed in the fluid-tight layer 5 in the crucible 1, difform stay-warm case all is fit to for growth technique, but also there is the limit in the upper and lower size of stay-warm case, mainly by following various decision (unit is a millimeter):
D 1>D 4+20
D 2<D 3+10
H 1<H 0-30
H 2=V×T+10
Wherein, D 1Represent the lower edge diameter of stay-warm case 4, D 2Represent the upper edge diameter of stay-warm case 4, D 3Represent crucible 1 diameter, D 4Represent crystal diameter, H 1Represent the whole height of stay-warm case 4, H 0Represent the total length of crystal 8, H 2Represent the bearing height of stay-warm case 4, on behalf of crucible 1, V follow speed, and T represents following the time of crucible 1.
In the device, fluid-tight layer 5 is boron oxides.
The lower edge diameter D1 of stay-warm case 4 is 120 millimeters in the device, and the upper edge diameter D2 of stay-warm case 4 is 230 millimeters, and the whole height H1 of stay-warm case 4 is 180 millimeters, and the bearing height H2 of stay-warm case 4 is 60 millimeters.
Be suitable for making the material employing high purity graphite of stay-warm case 4, because high purity graphite has high thermal, high purity graphite is a preferred material.
Fig. 3 is testing data figure of the present utility model, adopt device of the present utility model, guaranteed the shape 16 at solid-liquid interface place in gallium arsenide 8 process of growth, avoided because crystalizing interface edge curvature 17 causes that the gallium arsenide 8 of growth is become the generation of polycrystalline situation by monocrystalline, when the gallium arsenide charge amount is 8 kilograms, the length of monocrystalline 8 has reached 150 millimeters, and crystal 8 quality are significantly improved.

Claims (10)

1, a kind of device of the long size semi-insulating GaAs monocrystalline of growing, comprise crucible and crucible tray, the crystal pulling rod that is provided with in pressurized vessel, the pressurized vessel, well heater and insulation construction and the stay-warm case that centers on crucible and crucible tray setting, it is characterized in that, insulation construction is made up of annular heat-preservation cylinder (11b), heat-preservation cylinder loam cake (11a) and heat-preservation cylinder lower cover (11c), wherein annular heat-preservation cylinder (11b) is provided with around well heater (12), the top of annular heat-preservation cylinder (11b) is provided with heat-preservation cylinder loam cake (11a), and the bottom is provided with heat-preservation cylinder lower cover (11c); There is support (14) to support in the bottom of heat-preservation cylinder lower cover (11c); The stay-warm case of truncated cone shape (4) is provided with along the interior ring edge of heat-preservation cylinder loam cake (11a);
The circle outer of going up of stay-warm case (4) is provided with ring-shaped platform, the ring-shaped platform outer highly is the annular brace of 40-80 millimeter to having, the annular brace of stay-warm case is positioned in the ring groove of heat-preservation cylinder loam cake (11a), and the following circle of stay-warm case (4) is immersed in the fluid-tight layer (5) in the crucible (1);
2, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 1, the top that it is characterized in that pressurized vessel (10) is provided with quartzy window (15), its structure is for being equipped with a quartz pushrod in the hole on top that is arranged on pressurized vessel (10), the two ends of rod are surface polishing, form optical window.
3, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 1 or 2 is characterized in that the upper edge diameter of stay-warm case (4) and lower edge diameter are by following various decision:
D 1>D 4+20
D 2<D 3+10
H 1<H 0-30
H 2=V×T+10
Wherein, D 1Represent the lower edge diameter of stay-warm case (4), D 2Represent the upper edge diameter of stay-warm case (4), D 3Represent crucible (1) diameter, D 4Representative is placed on the diameter of the gallium arsenide (8) in the crucible (1), H 1Represent the whole height of stay-warm case (4), H 0Represent the total length of gallium arsenide (8), H 2Represent the bearing height of stay-warm case (4), V represents the speed of following of crucible (1), and T represents following the time of crucible (1).
4, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 1 or 2 is characterized in that fluid-tight layer (5) adopts boron oxide.
5, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 3 is characterized in that fluid-tight layer (5) adopts boron oxide.
6, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 1 or 2, the scope that it is characterized in that stay-warm case (4) lower edge diameter D1 is 110~220 millimeters, the scope of stay-warm case (4) upper edge diameter D2 is 110~300 millimeters, the scope of stay-warm case (4) whole height H1 is 100~200 millimeters, and the scope of stay-warm case (4) bearing height H2 is 40~80 millimeters.
7, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 3, the scope that it is characterized in that stay-warm case (4) lower edge diameter D1 is 110~220 millimeters, the scope of stay-warm case (4) upper edge diameter D2 is 110~300 millimeters, the scope of stay-warm case (4) whole height H1 is 100~200 millimeters, and the scope of stay-warm case (4) bearing height H2 is 40~80 millimeters.
8, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 5, the scope that it is characterized in that stay-warm case (4) lower edge diameter D1 is 110~220 millimeters, the scope of stay-warm case (4) upper edge diameter D2 is 110~300 millimeters, the scope of stay-warm case (4) whole height H1 is 100~200 millimeters, and the scope of stay-warm case (4) bearing height H2 is 40~80 millimeters.
9, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 7, the lower edge diameter D1 that it is characterized in that stay-warm case (4) is 120 millimeters, the upper edge diameter D2 of stay-warm case (4) is 230 millimeters, the whole height H1 of stay-warm case (4) is 180 millimeters, and the bearing height H2 of stay-warm case (4) is 60 millimeters.
10, the device of a kind of long size semi-insulating GaAs monocrystalline of growing as claimed in claim 8, the lower edge diameter D1 that it is characterized in that stay-warm case (4) is 120 millimeters, the upper edge diameter D2 of stay-warm case (4) is 230 millimeters, the whole height H1 of stay-warm case (4) is 180 millimeters, and the bearing height H2 of stay-warm case (4) is 60 millimeters.
CN 200320129498 2003-12-22 2003-12-22 Apparatus for growing long-size semi-insulation gallium arsenide single crystal Expired - Fee Related CN2666930Y (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100513652C (en) * 2007-05-24 2009-07-15 北京有色金属研究总院 Process and device for growing low dislocation germanium single crystal by crucible lowering Czochralski method
CN113913920A (en) * 2021-10-18 2022-01-11 北京工业大学 Preparation method and preparation device of AlGaAs single crystal

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100513652C (en) * 2007-05-24 2009-07-15 北京有色金属研究总院 Process and device for growing low dislocation germanium single crystal by crucible lowering Czochralski method
CN113913920A (en) * 2021-10-18 2022-01-11 北京工业大学 Preparation method and preparation device of AlGaAs single crystal
CN113913920B (en) * 2021-10-18 2024-05-03 北京工业大学 AlGaAs single crystal preparation method and preparation device

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