CN106637388A - Heat field structure for growth of low-dislocation single crystals by czochralski method and growing process of single crystal - Google Patents
Heat field structure for growth of low-dislocation single crystals by czochralski method and growing process of single crystal Download PDFInfo
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- CN106637388A CN106637388A CN201510736494.4A CN201510736494A CN106637388A CN 106637388 A CN106637388 A CN 106637388A CN 201510736494 A CN201510736494 A CN 201510736494A CN 106637388 A CN106637388 A CN 106637388A
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- 239000013078 crystal Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000010899 nucleation Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 5
- 230000008018 melting Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 7
- 238000003466 welding Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000000155 melt Substances 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 229910052732 germanium Inorganic materials 0.000 description 6
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000004927 fusion Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
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Abstract
The invention discloses a heat field structure for growth of low-dislocation single crystals by a czochralski method and a growing process of the single crystals. The heat field structure comprises a main heater and a bottom heater, the main heater is arranged along the wall of a single crystal furnace, the bottom heater is arranged at the bottom of the single crystal furnace, the main heater is of a gradual cylinder structure, the upper portion of the gradual cylinder structure is thin, and the lower portion of the gradual cylinder structure is thick. The process for growth of the low-dislocation single crystals by the heat field structure at least includes the steps: (1) selecting dislocation-free single crystals as seed crystals, rising temperature, and melting materials to meet target temperature in the growth process of the crystals; (2) stabilizing melts for some time, enabling a heat field to stabilize, searching seeding temperature, performing seeding for 1 hour at a seeding temperature point, and directly crystallizing; (3) automatically controlling equal-diameter growth, closing, and cooling to the indoor temperature to finish growth of the low-dislocation crystals. By the aid of the heat field structure, temperature gradients in a heat field can be reduced, low-temperature gradient areas are enlarged, and the effective length of the low-dislocation crystals can be increased by the aid of the growing process of the crystals in low-temperature gradient heat field.
Description
Technical field
The present invention relates to the thermal field structure and its growth technique of a kind of Grown by CZ Method low dislocation monocrystalline, belong to low dislocation
Technical field of single crystal growth.
Background technology
Vertical pulling method is a kind of important method for monocrystal growth, and the method observable, crystal growth cycles are short, efficiency high,
Low cost, can obtain the high quality single crystal of major diameter.In vertical pulling method low dislocation crystal growth, thermograde is to affect
The key factor of dislocation density.Straight barrel type list heater structure as shown in figure 1, heater 1 be straight barrel type, up and down
Thickness is identical.Thermograde changes greatly in the thermal field, heater edge thermograde greatly, low-temperature gradient region compared with
It is little.Low dislocation monocrystalline is grown in such thermal field and there is reduction dislocation density hardly possible, length is short, the low problem of efficiency.
The content of the invention
It is an object of the invention to provide a kind of thermal field structure of Grown by CZ Method low dislocation monocrystalline, existing to solve
The thermograde that low dislocation growth thermal field system is present is big, the problems such as low-temperature gradient regional extent is little.
Another object of the present invention is to provide a kind of growth that low dislocation monocrystalline is grown using described thermal field structure
Technique, to effectively reduce the dislocation density of monocrystalline, lengthens the effective length of low dislocation crystal.
For achieving the above object, the present invention is employed the following technical solutions：
A kind of thermal field structure of Grown by CZ Method low dislocation monocrystalline, the thermal field structure includes what is arranged along single crystal growing furnace furnace wall
Primary heater and the bottom heater for being arranged on single crystal growing furnace furnace bottom.
Wherein, the primary heater is the gradation type tubular construction of upper-thin-lower-thick.The primary heater is from its height
It is downwards a constant thickness at 1/2, it is thinning successively upwards；Upper most thin at, its thickness is the 2/3-5/6 of constant thickness；
Bottom heater is the graphite resistance heater of flat round structure.
The power supply and control system of the primary heater and bottom heater is the autonomous system being connected with electrical source of power,
Therefore the power of the primary heater and bottom heater can be adjusted individually.
The growth technique of low dislocation monocrystalline is grown using described thermal field structure, is at least comprised the following steps：
(1) select dislocation-free single crystal as seed crystal, in crystal growing process, temperature increasing for melting materials reaches target temperature；
(2) after Melt Stability being ensured for a period of time, thermal field is stable, using seed crystal and melt welding, seed crystal is observed
With the method for solid liquid interface variable condition during melt contacts, suitable seeding temperature is found, seeding is adopted after 1 hour
Program is lowered the temperature shouldering automatically.
(3) Jing automatically controls isodiametric growth, finishes up, is cooled to room temperature, completes low dislocation crystal growth.
In the step (2), finding the method for suitable seeding temperature is：When observation seed crystal is with melt contacts
Solid liquid interface variable condition, when seed crystal, the crystal in 5 minutes is not substantially grown up or is reduced with melt weld, with this
Fusion temp is seeding temperature.
Beneficial effects of the present invention are：
The thermal field structure of the present invention increased bottom heater on existing single heater (primary heater) architecture basics,
The gradation type tubular resistance heater for being shaped as upper-thin-lower-thick of primary heater, reduce thermograde in thermal field,
Increase low-temperature gradient region；With reference to crystal growth technique in low-temperature gradient thermal field, low dislocation can be lengthened brilliant
The effective length of body.
Description of the drawings
Fig. 1 is the structural representation of single heater.
Fig. 2 is the double-heater structural representation.
Fig. 3 is different thermal field system Axial Temperature Distribution schematic diagrames.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is specifically described with specific embodiment.
As shown in Fig. 2 the thermal field structure of the Grown by CZ Method low dislocation monocrystalline of the present invention includes being set along single crystal growing furnace furnace wall
The primary heater 2 put and the bottom heater 3 for being arranged on single crystal growing furnace furnace bottom.Wherein, the top of primary heater 2 is most thin,
It is gradually thickening, the resistance heater of the gradation type straight tube structure of upper-thin-lower-thick.Primary heater 2 and bottom heater 3
Power can individually adjust.
The thermal field structure of the present invention is the resistance heater of the gradation type straight tube structure for including upper-thin-lower-thick and bottom heating
The double-heater structure of device.As shown in figure 3, wherein solid line is existing single heater structure thermal field axial temperature point
Cloth, dotted line is the double-heater structure thermal field Axial Temperature Distribution of the present invention.It is main to add in the thermal field structure of the present invention
The change of hot device shape, reduces the thermograde on thermal field top；The addition of bottom heater improves thermal field bottom
Temperature, reduces the thermograde of thermal field bottom, so as to reduce thermal field integral gradient, and increases low temperature ladder
Degree region, realizes the low-temperature gradient on a large scale needed for long low dislocation crystal growth.
During crystal growth, crucible is placed in into correct position, after heat temperature raising melting sources, adjusts primary heater and bottom
Heater power stably a period of time (by the determination such as weight of loading and material thermal conductivity), obtains stable low temperature
Gradient thermal field；Suitable controllable seeding temperature is then looked for, method is：Observation seed crystal and solid-liquid circle during melt contacts
Face variable condition, when seed crystal, the crystal in 5 minutes is not substantially grown up or is reduced with melt weld, with this welding temperature
Spend for seeding temperature.The crystalline substances such as shouldering, isodiametric growth, ending, cooling are carried out after completing seeding under the fusion temp
Bulk-growth process.
Seed crystal used is dislocation-free single crystal in crystal growth, and in crystal growing process, temperature increasing for melting materials reaches target temperature
After degree, to avoid the thermal shock of seeding process, melt from stablizing a period of time (by weight of loading and material thermal conductivity
Deng determining) ensure that thermal field is stable after, just start seeding, then direct shouldering, Jing automatically controls isodiametric growth, receives
Tail, it is cooled to room temperature etc. and completes low dislocation crystal growth overall process；In the crystal growing process, using seed crystal with it is molten
Body welding, the method for observing seed crystal and solid liquid interface variable condition during melt contacts, it is low dislocation to find seeding temperature
The key of crystal growth.During due to crystal growth, seeding is carried out after low-temperature gradient thermal field is stable, without the need for length
Time seeding process, it is time-consuming, growth efficiency is improved, so as to cost-effective.
Comparative example
In charge 40kg, 4 inches of low dislocation germanium single crystal thermal field systems, 4 inches of low dislocation germanium single crystals are grown,
Using diameter 450mm, the straight barrel type structure graphite resistance list heater of long 650mm, power about 45kw；
Near 937 DEG C of germanium fusing point, it is low-temperature gradient scope that central region is about 180mm, and the thermograde of acquisition is about
For 2k/cm, stable 2-5 hours of heater power or so, adopt high bushing position (high-temperature before seeding during seeding
Gradient region) crystal pulling, low bushing position (low-temperature gradient region) position seeding, usual seeding speed is about
6mm/ hours, seeding length about 200mm eliminates the dislocation that thermal shock is introduced, and takes 30-40 hours, then
Using the programmable program controller control primary heater power of industry, turn that 4-10 turns, crucible turns 2-8 and turns with crystalline substance per minute,
The speed of growth about 2-6mm/ hours carry out crystal growth, can grow 4 inches of diameter, long 150mm, dislocation
Density is about 3000cm-2Germanium single crystal.
Embodiment
Thermal field structure in comparative example 1 is changed into the thermal field structure of the present invention, during material, primary heater power is about
42kw；Bottom heater power about 10kw；At this moment in primary heater, (diameter and length add with the list in comparative example 1
Hot device is identical) on below about 1/4 length about 450mm scopes, it is obtainable near 937 DEG C of germanium fusing point
Thermograde is reduced to below 0.3k/cm, the stable 6-10 hours of heater power before seeding, directly in low crucible
Position (low-temperature gradient region) is become using seed crystal and melt welding, observation seed crystal with solid liquid interface during melt contacts
The method of change state, finds seeding temperature, then seeding directly shouldering after about 1 hour at the seeding temperature, adopts
The programmable program controller of industry independently controls primary heater, bottom heater power, with crystalline substance per minute turn 4-10 turn,
Crucible turn 2-8 turn, the speed of growth about 2-6mm/ hours carry out crystal growth, can obtain 4 inches of diameter, long 200mm,
Dislocation density is less than 500cm-2Dislocation-free germanium single crystal.
Claims (7)
1. a kind of thermal field structure of Grown by CZ Method low dislocation monocrystalline, it is characterised in that the thermal field structure includes edge
The primary heater that single crystal growing furnace furnace wall is arranged and the bottom heater for being arranged on single crystal growing furnace furnace bottom.
2. the thermal field structure of Grown by CZ Method low dislocation monocrystalline as claimed in claim 1, it is characterised in that institute
State the gradation type straight tube structure that primary heater is upper-thin-lower-thick.
3. the thermal field structure of Grown by CZ Method low dislocation monocrystalline as claimed in claim 2, it is characterised in that institute
It is downwards a constant thickness that primary heater is stated from the 1/2 of its height, thinning successively upwards；It is upper most thin at, its
Thickness is the 2/3-5/6 of constant thickness.
4. the thermal field structure of the Grown by CZ Method low dislocation monocrystalline as any one of claim 1-3, it is special
Levy and be, the bottom heater is the graphite resistance heater of flat round structure.
5. the thermal field structure of the Grown by CZ Method low dislocation monocrystalline as any one of claim 1-3, it is special
Levy and be, the power supply and control system of the primary heater and bottom heater are the independent system being connected with electrical source of power
System, its power can be adjusted individually.
6. the thermal field structure any one of a kind of employing claim 1-5 grows the growth work of low dislocation monocrystalline
Skill, it is characterised in that at least comprise the following steps：
(1) select dislocation-free single crystal as seed crystal, in crystal growing process, temperature increasing for melting materials reaches target temperature；
(2) after Melt Stability being ensured for a period of time, thermal field is stable, using seed crystal and melt welding, seed crystal is observed
With the method for solid liquid interface variable condition during melt contacts, suitable seeding temperature is found, seeding is adopted after 1 hour
Program is lowered the temperature shouldering automatically；
(3) Jing automatically controls isodiametric growth, finishes up, is cooled to room temperature, completes low dislocation crystal growth.
7. thermal field structure according to claim 6 grows the growth technique of low dislocation monocrystalline, it is characterised in that
In the step (2), finding the method for suitable seeding temperature is：Observation seed crystal and solid-liquid during melt contacts
Interface variable condition, when seed crystal, the crystal in 5 minutes is not substantially grown up or is reduced with melt weld, with this welding
Temperature is seeding temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111379018A (en) * | 2020-04-02 | 2020-07-07 | 徐州鑫晶半导体科技有限公司 | Method for growing semiconductor silicon crystal bar |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101043A (en) * | 1984-08-06 | 1987-01-10 | 索尼公司 | Single-crystal growing apparatus (equipment) |
| US4863554A (en) * | 1983-08-23 | 1989-09-05 | Sumitomo Electric Industries, Ltd. | Process for pulling a single crystal |
| CN101063227A (en) * | 2007-05-24 | 2007-10-31 | 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 |
| CN104818524A (en) * | 2015-04-28 | 2015-08-05 | 汤灏 | Method and heater for improving quality of monocrystal silicon grown by Czochralski method |
-
2015
- 2015-11-03 CN CN201510736494.4A patent/CN106637388A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4863554A (en) * | 1983-08-23 | 1989-09-05 | Sumitomo Electric Industries, Ltd. | Process for pulling a single crystal |
| CN85101043A (en) * | 1984-08-06 | 1987-01-10 | 索尼公司 | Single-crystal growing apparatus (equipment) |
| CN101063227A (en) * | 2007-05-24 | 2007-10-31 | 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 |
| CN104818524A (en) * | 2015-04-28 | 2015-08-05 | 汤灏 | Method and heater for improving quality of monocrystal silicon grown by Czochralski method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111379018A (en) * | 2020-04-02 | 2020-07-07 | 徐州鑫晶半导体科技有限公司 | Method for growing semiconductor silicon crystal bar |
| CN111379018B (en) * | 2020-04-02 | 2021-08-27 | 徐州鑫晶半导体科技有限公司 | Method for growing semiconductor silicon crystal bar |
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Application publication date: 20170510 |