CN112941621A - CZ single crystal furnace static thermal field measuring device and measuring method of static thermal field - Google Patents
CZ single crystal furnace static thermal field measuring device and measuring method of static thermal field Download PDFInfo
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- CN112941621A CN112941621A CN202110420407.XA CN202110420407A CN112941621A CN 112941621 A CN112941621 A CN 112941621A CN 202110420407 A CN202110420407 A CN 202110420407A CN 112941621 A CN112941621 A CN 112941621A
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- 239000013078 crystal Substances 0.000 title claims abstract description 49
- 230000003068 static effect Effects 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 58
- 239000010439 graphite Substances 0.000 claims abstract description 58
- 239000000523 sample Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 210000001503 joint Anatomy 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000005611 electricity Effects 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 238000009434 installation Methods 0.000 description 7
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003631 expected effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- 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)
Abstract
The invention discloses a CZ single crystal furnace static thermal field measuring device and a measuring method of a static thermal field, the CZ single crystal furnace static thermal field measuring device comprises a furnace barrel, a furnace cover is arranged at the top of the furnace barrel, a crucible is arranged in the furnace barrel, a liftable seed crystal rod is arranged on the inner side of the furnace cover, and the CZ single crystal furnace static thermal field measuring device also comprises a graphite measuring bar and a temperature measuring instrument; the graphite measuring strip is in a strip shape, the graphite measuring strip is movably hung on the seed crystal rod, and the length direction of the graphite measuring strip is vertical to the axial direction of the furnace barrel; the upper surface of the graphite measuring strip is provided with gap marks which are arranged along the length direction at equal intervals; an observation hole is formed in the furnace cover, the temperature measuring instrument is installed in the observation hole through the joint bearing, and a temperature measuring probe of the temperature measuring instrument points to the interior of the furnace barrel. The device can obtain three-dimensional temperature distribution data in the furnace through the arrangement of the graphite measuring strip with the gap mark and the thermodetector, and further can adjust the thermal field in the furnace according to the measuring result; the operation is simple, and data can be obtained through experiments at any time; the raw materials are not wasted, only a small amount of electricity is consumed, and the cost is low.
Description
Technical Field
The invention relates to a CZ single crystal furnace static thermal field measuring device and a CZ single crystal furnace static thermal field measuring method, and belongs to the technical field of Z single crystal furnace static thermal field measurement.
Background
When growing single crystals by the CZ method (direct pulling), it is often necessary to adjust the thermal field in the furnace according to different requirements of customers (such as special diameter requirements, resistivity range requirements or low-volume raw point defects), and there are two common methods: firstly, a material feeding test furnace is used for producing a substitute test, but the material feeding test furnace has the possibility of failure and has a large risk of raw materials; secondly, the special thermal field simulation software is used for adjustment, the defect is that the price is high, certain products can reach 300 ten thousand yuan per year only by rent, and the cost is too high.
Disclosure of Invention
The invention provides a CZ single crystal furnace static thermal field measuring device and a CZ single crystal furnace static thermal field measuring method, aiming at solving the problems of raw material waste caused by production trial and generation of single crystal furnace thermal field adjustment and overhigh cost caused by simulating and adjusting a thermal field by using professional software.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a CZ single crystal furnace static thermal field measuring device comprises a furnace barrel, a furnace cover is arranged at the top of the furnace barrel, a crucible is arranged in the furnace barrel, a liftable seed crystal rod is arranged on the inner side of the furnace cover, and the CZ single crystal furnace static thermal field measuring device further comprises a graphite measuring bar and a temperature measuring instrument; the graphite measuring strip is in a strip shape, the graphite measuring strip is movably hung on the seed crystal rod, and the length direction of the graphite measuring strip is vertical to the axial direction of the furnace barrel; the upper surface of the graphite measuring strip is provided with gap marks which are arranged along the length direction at equal intervals; an observation hole is formed in the furnace cover, the temperature measuring instrument is installed in the observation hole through the joint bearing, and a temperature measuring probe of the temperature measuring instrument points to the interior of the furnace barrel.
The applicant finds that the graphite measuring strip has the advantages of no metal ion pollution to a heat system, high heat conduction speed, good thermal stability and the like, and can accurately embody a thermal field in a furnace; the upper surface of the graphite measuring strip is provided with gap marks which are arranged along the length direction at equal intervals, and the three-dimensional temperature distribution data can be obtained by combining the lifting of the graphite measuring strip driven by the seed crystal rod; the temperature measuring instrument is used for testing the temperature of each notch mark of the graphite measuring strip; the temperature measuring instrument is arranged in the observation hole through the joint bearing, so that the temperature measuring instrument can adjust the testing angle, and the measurement of the temperature of different positions of the graphite measuring strip is convenient to realize.
The CZ single crystal furnace is the existing equipment, and the seed crystal rod can be lifted to the prior art.
According to the method for measuring the static thermal field by using the CZ single crystal furnace static thermal field measuring device, the space position in the furnace is simulated by using the graphite measuring strip, the temperature of each notch mark on the graphite measuring strip is measured by a thermodetector through the observation hole and is recorded, and the distribution condition of the whole thermal field is obtained.
In order to accurately represent the distribution condition of the whole thermal field, the method for measuring the static thermal field comprises the following steps which are connected in sequence:
1) loading a graphite measuring strip onto the seed rod, and loading a temperature measuring instrument onto the observation hole;
2) sealing the furnace, heating and keeping constant temperature;
3) lowering the graphite measuring strip to the bottom of the crucible and keeping the temperature for 8-12 minutes;
4) the sliding torsion thermodetector sequentially records the temperature value of each notch mark on the graphite measuring strip from left to right or from right to left;
5) raising the seed rod by 0.8-1.2 cm, keeping the temperature for 8-12 minutes, and then repeating the measuring action in the step 4);
6) and repeating the step 5) until the graphite measuring strip reaches the top of the CZ single crystal furnace heat preservation system, and obtaining three-dimensional temperature distribution data.
The method can obtain three-dimensional temperature distribution data, completely meets the requirement of static thermal field measurement, and can adjust the thermal field in the furnace according to the measurement result; the operation is simple, and data can be obtained through experiments at any time; the raw materials are not wasted, only a small amount of electricity is consumed, and the cost is low.
In order to improve the accuracy of measurement, the interval between two adjacent notch marks is 0.8-1.2 cm.
In order to improve the testing efficiency, the length of the graphite measuring strip is 450-550 mm, the width of the graphite measuring strip is 15-25 mm, and the thickness of the graphite measuring strip is 4-6 mm.
In order to facilitate the installation operation, the outer side of the observation hole is butted with an installation pipe, and the temperature measuring instrument is installed on the inner side of the installation pipe through a joint bearing.
The top of the temperature measuring instrument is an observation ocular lens, and the bottom of the temperature measuring instrument is provided with a temperature measuring probe. The thermometer is preferably a RAYTEK infrared thermometer.
In order to facilitate control, the joint bearing is provided with a tightening screw. As a common knowledge, the inner ring of the joint bearing can be adjusted in a rotating mode relative to the outer ring, when the tightening screw rotates to abut against the inner ring, the position of the temperature measuring instrument is fixed, and when the tightening screw rotates outwards to be separated from the inner ring, the temperature measuring instrument can flexibly adjust the angle.
In order to improve the stability of measurement, the central position of the graphite measuring strip in the length direction is movably hung on the seed rod.
The prior art is referred to in the art for techniques not mentioned in the present invention.
According to the CZ single crystal furnace static thermal field measuring device, the graphite measuring strip with the notch mark and the thermodetector are arranged, so that three-dimensional temperature distribution data in the furnace can be obtained, and further the thermal field in the furnace can be adjusted according to the measuring result; no metal ion is introduced; the operation is simple, and data can be obtained through experiments at any time; the raw materials are not wasted, only a small amount of electricity is consumed, and the cost is low.
Drawings
FIG. 1 is a top view of a graphite measuring strip of the present invention;
FIG. 2 is a schematic structural view of the CZ single crystal furnace static thermal field measuring device of the present invention;
FIG. 3 is a schematic structural view of the temperature measuring instrument of the present invention;
in the figure, 1 is a graphite measuring strip, 11 is a notch mark, 2 is a furnace barrel, 3 is a furnace cover, 31 is an observation hole, 32 is an installation pipe, 33 is a joint bearing, 4 is a crucible, 5 is a seed rod, 6 is a temperature measuring instrument, 61 is an observation eye lens, 62 is a temperature measuring probe, and 63 is a tightening screw.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
The terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used herein in an orientation that is based on the orientation or positional relationship shown in the drawings or in use, and are used for convenience in describing the present application, but do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present application.
Example 1
As shown in FIG. 2, the CZ single crystal furnace static thermal field measuring device comprises a furnace barrel, a furnace cover is arranged at the top of the furnace barrel, a crucible is arranged in the furnace barrel, a seed crystal rod capable of lifting is arranged on the inner side of the furnace cover, and the CZ single crystal furnace static thermal field measuring device also comprises a graphite measuring strip and a temperature measuring instrument; as shown in fig. 1, the graphite measuring strip is in a strip shape, the central position of the graphite measuring strip in the length direction is movably hung on the seed crystal rod, and the length direction of the graphite measuring strip is vertical to the axial direction of the furnace barrel; the upper surface of the graphite measuring strip is provided with gap marks which are arranged along the length direction at equal intervals; an observation hole is formed in the furnace cover, as shown in fig. 2, the temperature measuring instrument is installed in the observation hole through the joint bearing, and the temperature measuring probe of the temperature measuring instrument points to the interior of the furnace barrel.
Practice shows that the graphite measuring strip has the advantages of no metal ion pollution to a heat system, quick heating, good thermal stability and the like, and can accurately reflect a thermal field in a furnace; the upper surface of the graphite measuring strip is provided with gap marks which are arranged along the length direction at equal intervals, and the three-dimensional temperature distribution data can be obtained by combining the lifting of the graphite measuring strip driven by the seed crystal rod; the temperature measuring instrument is used for testing the temperature of each notch mark of the graphite measuring strip; the temperature measuring instrument is arranged in the observation hole through the joint bearing, so that the temperature measuring instrument can adjust the testing angle, and the measurement of the temperature of different positions of the graphite measuring strip is convenient to realize.
The method for measuring the static thermal field by using the CZ single crystal furnace static thermal field measuring device comprises the following steps which are connected in sequence:
1) loading a graphite measuring strip onto the seed rod, and loading a temperature measuring instrument onto the observation hole;
2) sealing the furnace, heating and keeping constant temperature;
3) lowering the graphite measuring strip to the bottom of the crucible and keeping the temperature for 10 minutes;
4) the sliding torsion thermodetector sequentially records the temperature value of each notch mark on the graphite measuring strip from left to right or from right to left;
5) raising the seed rod by 1cm, keeping the temperature for 10 minutes, and repeating the measuring action of the step 4);
6) and repeating the step 5) until the graphite measuring strip reaches the top of the CZ single crystal furnace heat preservation system, and obtaining three-dimensional temperature distribution data.
The method can obtain three-dimensional temperature distribution data, completely meets the requirement of static thermal field measurement, and can adjust the thermal field in the furnace according to the measurement result; the operation is simple, and data can be obtained through experiments at any time; the raw materials are not wasted, only a small amount of electricity is consumed, and the cost is low.
Example 2
On the basis of the embodiment 1, the following improvements are further made: in order to improve the accuracy of the measurement, the interval between two adjacent notch marks is 1 cm. To improve the efficiency of the test, the graphite measuring strip had a length of 500mm, a width of 20mm and a thickness of 5 mm.
Example 3
On the basis of the embodiment 2, the following improvements are further made: as shown in figure 2, in order to facilitate the installation operation, the outer side of the observation hole is butted with an installation pipe, and the temperature measuring instrument is installed on the inner side of the installation pipe through a joint bearing.
Example 4
On the basis of the embodiment 3, the following improvements are further made: as shown in fig. 3, the thermometer is a RAYTEK infrared thermometer, the top of the thermometer is an observation eyepiece, and the bottom of the thermometer is provided with a temperature measuring probe.
The practical case is as follows: customers need a zero-dislocation germanium single crystal which cannot be produced by using a thermal field in the existing single crystal furnace, and by using the device and the method, the radial average temperature gradient exceeds 3 ℃/cm through measuring the distribution of the thermal field in the furnace as shown in table 1, and the zero-dislocation single crystal cannot be grown.
TABLE 1 thermal field distribution in furnace before adjustment
According to the measured distribution of the thermal field in the furnace, new distribution of the thermal field is measured after being adjusted for several times and is shown in table 2, the average radial temperature gradient is about 2 ℃ per cm, the process requirements are basically met, the expected effect is achieved after feeding production, the growth cycle of the zero dislocation germanium single crystal is about one week generally, and a large amount of trial and error cost is saved by the method.
TABLE 2 adjusted in-furnace thermal field distribution
In tables 1-2, the units for the radial and longitudinal directions are in cm, and the temperature is in degrees Celsius.
Example 5
On the basis of the embodiment 4, the following improvements are further made: as shown in fig. 2-3, a tightening screw is provided on the spherical plain bearing for easy control. The inner ring of the joint bearing can rotate and be adjusted relative to the outer ring, when the tightening screw rotates to abut against the inner ring, the position of the temperature measuring instrument is fixed, and when the tightening screw rotates outwards to be separated from the inner ring, the temperature measuring instrument can flexibly adjust the angle.
According to the CZ single crystal furnace static thermal field measuring device, the graphite measuring strip with the notch mark and the thermodetector are arranged, so that three-dimensional temperature distribution data in the furnace can be obtained, and further the thermal field in the furnace can be adjusted according to the measuring result; the operation is simple, and data can be obtained through experiments at any time; the raw materials are not wasted, only a small amount of electricity is consumed, and the cost is low.
Claims (10)
1. The utility model provides a static thermal field measuring device of CZ single crystal growing furnace, includes the stove bucket, and stove bucket top is equipped with the bell, is equipped with the crucible in the stove bucket, and the bell inboard is equipped with the seed crystal pole of liftable, its characterized in that: the device also comprises a graphite measuring strip and a temperature measuring instrument; the graphite measuring strip is in a strip shape, the graphite measuring strip is movably hung on the seed crystal rod, and the length direction of the graphite measuring strip is vertical to the axial direction of the furnace barrel; the upper surface of the graphite measuring strip is provided with gap marks which are arranged along the length direction at equal intervals; an observation hole is formed in the furnace cover, the temperature measuring instrument is installed in the observation hole through the joint bearing, and a temperature measuring probe of the temperature measuring instrument points to the interior of the furnace barrel.
2. The CZ single crystal furnace static thermal field measuring apparatus of claim 1, wherein: the interval between two adjacent gap marks is 0.8-1.2 cm.
3. The CZ single crystal furnace static thermal field measuring apparatus of claim 1 or 2, wherein: the length of the graphite measuring strip is 450-550 mm, the width is 15-25 mm, and the thickness is 4-6 mm.
4. The CZ single crystal furnace static thermal field measuring apparatus of claim 1 or 2, wherein: the outer side of the observation hole is in butt joint with a mounting pipe, and the temperature measuring instrument is mounted on the inner side of the mounting pipe through a joint bearing.
5. The CZ single crystal furnace static thermal field measuring apparatus of claim 1 or 2, wherein: the top of the temperature measuring instrument is an observation ocular lens, and the bottom of the temperature measuring instrument is provided with a temperature measuring probe.
6. The CZ single crystal furnace static thermal field measuring apparatus of claim 1 or 2, wherein: the thermometer is a RAYTEK infrared thermometer.
7. The CZ single crystal furnace static thermal field measuring apparatus of claim 1 or 2, wherein: and a tightening screw is arranged on the joint bearing.
8. The CZ single crystal furnace static thermal field measuring apparatus of claim 1 or 2, wherein: the central position of the graphite measuring strip in the length direction is movably hung on the seed rod.
9. A method for measuring a static thermal field using the CZ single crystal furnace static thermal field measuring apparatus of any one of claims 1 to 8, characterized in that: and simulating the space position in the furnace by using the graphite measuring strip, measuring the temperature of each notch mark on the graphite measuring strip by using a temperature measuring instrument through the observation hole, and recording to obtain the distribution condition of the whole thermal field.
10. The method of any of claims 9, wherein: comprises the following steps that:
1) loading a graphite measuring strip onto the seed rod, and loading a temperature measuring instrument onto the observation hole;
2) sealing the furnace, heating and keeping constant temperature;
3) lowering the graphite measuring strip to the bottom of the crucible and keeping the temperature for 8-12 minutes;
4) the sliding torsion thermodetector sequentially records the temperature value of each notch mark on the graphite measuring strip from left to right or from right to left;
5) raising the seed rod by 0.8-1.2 cm, keeping the temperature for 8-12 minutes, and then repeating the measuring action in the step 4);
6) and repeating the step 5) until the graphite measuring strip reaches the top of the CZ single crystal furnace heat preservation system, and obtaining three-dimensional temperature distribution data.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110420407.XA CN112941621A (en) | 2021-04-19 | 2021-04-19 | CZ single crystal furnace static thermal field measuring device and measuring method of static thermal field |
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| CN202110420407.XA CN112941621A (en) | 2021-04-19 | 2021-04-19 | CZ single crystal furnace static thermal field measuring device and measuring method of static thermal field |
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| CN112941621A true CN112941621A (en) | 2021-06-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115652290A (en) * | 2022-09-28 | 2023-01-31 | 新美光(苏州)半导体科技有限公司 | Chemical vapor deposition equipment |
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| CN104864974A (en) * | 2015-05-29 | 2015-08-26 | 中国科学院上海硅酸盐研究所 | Furnace temperature field measurement device |
| CN105716722A (en) * | 2016-04-06 | 2016-06-29 | 江苏中电振华晶体技术有限公司 | Method for temperature calibration of infrared thermometer for sapphire crystal growth |
| CN206204483U (en) * | 2016-12-02 | 2017-05-31 | 珠海鼎泰芯源晶体有限公司 | A kind of indium phosphide single crystal stove of application non-contact temperature measuring |
| CN207570431U (en) * | 2017-11-07 | 2018-07-03 | 山西潞安太阳能科技有限责任公司 | One kind installs fast aligning tool for thermal field of single crystal furnace |
| CN214572356U (en) * | 2021-04-19 | 2021-11-02 | 中锗科技有限公司 | CZ single crystal growing furnace static thermal field measuring device |
-
2021
- 2021-04-19 CN CN202110420407.XA patent/CN112941621A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104864974A (en) * | 2015-05-29 | 2015-08-26 | 中国科学院上海硅酸盐研究所 | Furnace temperature field measurement device |
| CN105716722A (en) * | 2016-04-06 | 2016-06-29 | 江苏中电振华晶体技术有限公司 | Method for temperature calibration of infrared thermometer for sapphire crystal growth |
| CN206204483U (en) * | 2016-12-02 | 2017-05-31 | 珠海鼎泰芯源晶体有限公司 | A kind of indium phosphide single crystal stove of application non-contact temperature measuring |
| CN207570431U (en) * | 2017-11-07 | 2018-07-03 | 山西潞安太阳能科技有限责任公司 | One kind installs fast aligning tool for thermal field of single crystal furnace |
| CN214572356U (en) * | 2021-04-19 | 2021-11-02 | 中锗科技有限公司 | CZ single crystal growing furnace static thermal field measuring device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115652290A (en) * | 2022-09-28 | 2023-01-31 | 新美光(苏州)半导体科技有限公司 | Chemical vapor deposition equipment |
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