CN114427826B - System and method for measuring thickness and quality of crystal during silicon carbide crystal growth - Google Patents

System and method for measuring thickness and quality of crystal during silicon carbide crystal growth Download PDF

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CN114427826B
CN114427826B CN202111676687.7A CN202111676687A CN114427826B CN 114427826 B CN114427826 B CN 114427826B CN 202111676687 A CN202111676687 A CN 202111676687A CN 114427826 B CN114427826 B CN 114427826B
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crystal
resistance
thickness
graphite
total
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CN114427826A (en
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李辉
王守琛
毛瑞川
苏闻峰
杨茜
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Nanjing Jingsheng Equipment Co ltd
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Nanjing Jingsheng Equipment Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/02Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
    • G01B7/06Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/002Controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/36Carbides
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/041Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body

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  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
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  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a system and a method for measuring the thickness and the quality of crystals during silicon carbide crystal growth, wherein the system comprises a graphite disc, a resistance detection module, a calculation module and a display module, seed crystals are arranged below the graphite disc, the silicon carbide crystals grow on the seed crystals, two conductive rods are arranged above the graphite disc and are electrically connected with the graphite disc, the resistance detection module is used for detecting the resistance between the two conductive rods in real time, the calculation module is used for calculating the thickness and the quality of the silicon carbide crystals according to the resistance detected by the resistance detection module, and the display module is used for displaying the thickness and the quality of the silicon carbide crystals obtained by the calculation module in real time. The electric connection between the conductive rods and the graphite disc is realized by measuring the resistance between the conductive rods in real time, converting the resistance into the thickness and the quality in the growth process of the silicon carbide crystal, displaying in real time, helping operators to observe whether the growth of the silicon carbide crystal meets the requirement in real time, and adjusting the process in time when the growth does not meet the requirement, without waiting for the crystal to be discharged.

Description

System and method for measuring thickness and quality of crystal during silicon carbide crystal growth
Technical Field
The invention relates to a semiconductor crystal growth auxiliary system, in particular to a system and a method for measuring the thickness and the quality of crystals during crystal growth of silicon carbide.
Background
Most of the semiconductor single crystal furnaces are high temperature furnaces, taking silicon carbide as an example, the core temperature of a thermal field is about 2300 ℃, the growth period of crystals is long, the current silicon carbide single crystal growth furnace (PVT) cannot observe the growth condition of silicon carbide crystals in real time, and the height and quality of the crystals cannot be observed in real time in the growth process, so that the quality of the obtained silicon carbide crystals is not expected after the process period is finished, the process is frequently regulated for many times, the process is tested for many times, the process cannot be regulated in real time according to the quality of the crystals, the period of the crystal growth process is usually as long as several days, and the production efficiency is seriously affected by the test production for many times.
Disclosure of Invention
The invention aims to: aiming at the defects, the invention provides a measuring system for the thickness and the quality of the silicon carbide crystal in the crystal growth process, which displays data in real time.
The invention also provides a method for measuring the thickness and the quality of the crystal during the crystal growth of the silicon carbide.
The technical scheme is as follows: in order to solve the problems, the invention adopts a system for measuring the thickness and the quality of crystals during the growth of silicon carbide, which comprises a graphite disc, wherein seed crystals are arranged below the graphite disc, the silicon carbide crystals grow on the seed crystals, the system further comprises a resistance detection module, a calculation module and a display module, two conductive rods are arranged above the graphite disc, the two conductive rods are electrically connected with the graphite disc, the graphite disc is electrically connected with the silicon carbide crystals, the resistance detection module is used for detecting the resistance between the two conductive rods in real time, the calculation module is used for calculating the thickness and the quality of the silicon carbide crystals according to the resistance detected by the resistance detection module, and the display module is used for displaying the thickness and the quality of the silicon carbide crystals obtained by the calculation module in real time.
The invention also adopts a method for measuring the thickness and the quality of the crystal during the crystal growth of the silicon carbide, which comprises the following steps:
(1) Detecting to obtain the resistance of the conductive rod and the resistance of the graphite disc when the crystal is not grown initially;
(2) Performing silicon carbide crystal growth, and measuring a real-time resistance value between two conductive rods;
(3) Calculating according to the real-time resistance, the resistance of the conductive rod and the resistance of the graphite disc to obtain the resistance of the crystal at the moment;
(4) Calculating according to the resistivity of the crystal and the calculated crystal resistance to obtain the thickness of the crystal;
(5) Calculating according to the density and thickness of the crystal to obtain the crystal quality;
(6) And displaying the calculated crystal thickness and crystal quality in real time.
Further, the specific steps in the step (1) are as follows:
(1.1) measuring the resistance R Total (S) 0 between two conductive rods when the graphite disk is not provided with seed crystals;
(1.2) measuring a resistance R Total (S) 1 between two conductive rods when the graphite disk is provided with seed crystals with the thickness delta; (1.3) measuring a resistance R Total (S) 2 between two conductive rods when the graphite disk is provided with seed crystals with the thickness of 2 delta; and (1.4) calculating according to R Total (S) 0、R Total (S) 1、R Total (S) 2 to obtain the resistance value of the conductive rod and the resistance value of the graphite disk. Further, the calculation formula of the resistance value R Total (S) 0 is:
R Total (S) 0=R Guide rail +R Graphite disc
Wherein R Guide rail is the total resistance of the conductive rod, and R Graphite disc is the resistance of the graphite disk;
the calculation formula of the resistance R Total (S) 1 is as follows:
Wherein R Seed crystal 1 is the resistance of seed crystal with the thickness delta;
The calculation formula of the resistance R Total (S) 2 is as follows:
Wherein R Seed crystal 2 is the resistance value of the seed crystal with the thickness of 2 delta, and R Seed crystal 2=(1/2)R Seed crystal 1.
Further, the calculation formula of the crystal resistance R Crystal body in the step (3) is as follows:
wherein R Total (S) is the real-time resistance between the two conductive bars measured.
Further, the calculation formula of the crystal thickness δ in the step (4) is as follows:
Wherein R Crystal body is the resistance value of the crystal, R is the radius of the cross section of the crystal, and ρ is the resistivity of the crystal.
Further, the calculation formula of the crystal mass m in the step (5) is as follows:
m=ε·δ·πr2
where ε is the density of crystals.
The beneficial effects are that: compared with the prior art, the invention has the remarkable advantages that the electric connection between the conductive rods and the graphite disc is realized, the resistance between the conductive rods is measured in real time, the resistance is converted into the thickness and the quality in the growth process of the silicon carbide crystal, and the thickness and the quality are displayed in real time, so that an operator can observe whether the growth of the silicon carbide crystal meets the requirement in real time, and the process is regulated in time when the growth of the silicon carbide crystal does not meet the requirement, and the next furnace is regulated according to the quality of the crystal after the crystal is discharged from the furnace.
Drawings
FIG. 1 is a schematic diagram of the structure of a seed crystal connected with a graphite disk at the beginning of the measuring method of the invention;
FIG. 2 is a schematic diagram of the structure of the connection between the crystal and the graphite disk during the crystal growth in the measuring method of the invention;
FIG. 3 is a schematic diagram of the cross-section of a crystal in the calculation of the resistance of the crystal according to the present invention.
Detailed Description
Example 1
As shown in fig. 1 and fig. 2, a system for measuring crystal thickness and quality during silicon carbide crystal growth in this embodiment includes a conductive rod 1, a graphite plate 2, a seed crystal 3, a resistance detection module, a calculation module and a display module, wherein the seed crystal 3 is disposed below the graphite plate 2, a silicon carbide crystal 4 grows on the seed crystal 3, two conductive rods 1 are disposed above the graphite plate 2, in this embodiment, the conductive rod 1 is made of graphite material, the two conductive rods 1 are electrically connected with the graphite plate 2, the graphite plate 2 is electrically connected with the silicon carbide crystal 4, the two conductive rods 1 are respectively used as an input end and an output end of a circuit, the resistance between the two conductive rods 1 is detected in real time through the resistance detection module, and the calculation module calculates the thickness and quality of the silicon carbide crystal 4 according to the resistance detected by the resistance detection module. Before crystal growth, the calculation module calculates the resistances of the conductive rod 1 and the graphite disc 2 through the resistance detected by the resistance detection module; and when the crystal is grown, the calculation module obtains the resistance of the crystal according to the real-time total resistance of the system detected by the resistance detection module and the pre-calculated resistance of the conductive rod and the graphite disc. The display module is used for displaying the thickness and the quality of the silicon carbide crystal obtained by the calculation module in real time, and operators can adjust the process in real time according to the data displayed by the display module.
Example 2
The method for measuring the thickness and the quality of the crystal during the growth of the silicon carbide in the embodiment adopts the measuring system in the embodiment to measure, and the measuring system is not described herein, and the measuring method comprises the following steps:
(1) Detecting to obtain the resistance of the conductive rod and the resistance of the graphite disc when the crystal is not grown initially;
(1.1) when the resistance detection module measures that the graphite disc is not provided with seed crystals, the resistance R Total (S) 0 between the two conductive rods;
(1.2) when the resistance detection module measures seed crystals with the thickness delta of the graphite disc, the resistance R Total (S) 1 between the two conductive rods;
(1.3) when the resistance detection module measures the seed crystal with the thickness of 2 delta of the graphite disc, the resistance R Total (S) 2 between the two conductive rods;
(1.4) the calculation module calculates to obtain the resistance value of the conductive rod and the resistance value of the graphite disc according to R Total (S) 0、R Total (S) 1、R Total (S) 2;
the calculation formula of the resistance R Total (S) 0 is:
R Total (S) 0=R Guide rail +R Graphite disc
Wherein R Guide rail is the total resistance of the conductive rod, and R Graphite disc is the resistance of the graphite disk;
The calculation formula of the resistance R Total (S) 1 is:
Wherein R Seed crystal 1 is the resistance of seed crystal with the thickness delta;
the calculation formula of the resistance R Total (S) 2 is:
Wherein R Seed crystal 2 is the resistance of the seed crystal with the thickness of 2 delta, wherein the cross section area of the seed crystal with the thickness of 2 delta is the same as that of the seed crystal with the thickness of delta, and other conditions such as materials and the like except for the thickness are the same;
According to the calculation formula of the semiconductor resistance: r=ρ 0(l0/s0), where ρ 0 is the semiconductor resistivity, l 0 is the semiconductor length, s 0 is the cross-sectional area through which the semiconductor current flows, R Seed crystal 2=(1/2)R Seed crystal 1 can be obtained;
The resistance R Guide rail of the conductive rod and the resistance R Graphite disc of the graphite disk can be calculated through the R Total (S) 0、R Total (S) 1、R Total (S) 2 obtained through detection.
(2) Performing silicon carbide crystal growth, and measuring a real-time resistance value R Total (S) between two conductive rods;
(3) Calculating according to the real-time resistance R Total (S) , the resistance R Guide rail of the conductive rod and the resistance R Graphite disc of the graphite disk to obtain the resistance R Crystal body of the crystal at the moment; the calculation formula of the crystal resistance R Crystal body is as follows:
(4) Calculating according to the resistivity of the crystal and the calculated crystal resistance to obtain the thickness of the crystal; the calculation formula of the crystal thickness delta is as follows:
Wherein R Crystal body is the resistance value of the crystal, R is the radius of the cross section of the crystal, and ρ is the resistivity of the crystal.
(5) Calculating according to the density and thickness of the crystal to obtain the crystal quality; the calculation formula of the crystal mass m is as follows:
m=ε·δ·πr2
where ε is the density of crystals.
(6) And displaying the calculated crystal thickness and crystal quality in real time.

Claims (8)

1. The utility model provides a crystal thickness and measurement system of quality when carborundum grows crystal, includes the graphite dish, the graphite dish below sets up the seed crystal, carborundum crystal growth on the seed crystal, its characterized in that still includes resistance detection module, calculation module and display module, the graphite dish top sets up two conductive bars, and two conductive bars are connected with the graphite dish electricity, and the graphite dish is connected with carborundum crystal electricity, resistance detection module is used for the resistance between two conductive bars of real-time detection, calculation module is used for calculating carborundum crystal's thickness and quality according to the resistance that resistance detection module detected, display module is used for the thickness and the quality of carborundum crystal that real-time display calculation module obtained.
2. The measurement system of claim 1, wherein the conductive rod is a graphite material.
3. A measurement method of a measurement system according to claim 1 or 2, comprising the steps of:
(1) Detecting to obtain the resistance of the conductive rod and the resistance of the graphite disc when the crystal is not grown initially;
(2) Performing silicon carbide crystal growth, and measuring a real-time resistance value between two conductive rods;
(3) Calculating according to the real-time resistance, the resistance of the conductive rod and the resistance of the graphite disc to obtain the resistance of the crystal at the moment;
(4) Calculating according to the resistivity of the crystal and the calculated crystal resistance to obtain the thickness of the crystal;
(5) Calculating according to the density and thickness of the crystal to obtain the crystal quality;
(6) And displaying the calculated crystal thickness and crystal quality in real time.
4. A measurement method according to claim 3, wherein the specific steps in step (1) are:
(1.1) measuring the resistance R Total (S) 0 between two conductive rods when the graphite disk is not provided with seed crystals;
(1.2) measuring a resistance R Total (S) 1 between two conductive rods when the graphite disk is provided with seed crystals with the thickness delta;
(1.3) measuring a resistance R Total (S) 2 between two conductive rods when the graphite disk is provided with seed crystals with the thickness of 2 delta;
and (1.4) calculating according to R Total (S) 0、R Total (S) 1、R Total (S) 2 to obtain the resistance value of the conductive rod and the resistance value of the graphite disk.
5. The method for measuring according to claim 4, wherein,
The calculation formula of the resistance R Total (S) 0 is as follows:
R Total (S) 0=R Guide rail +R Graphite disc
Wherein R Guide rail is the total resistance of the conductive rod, and R Graphite disc is the resistance of the graphite disk;
the calculation formula of the resistance R Total (S) 1 is as follows:
Wherein R Seed crystal 1 is the resistance of seed crystal with the thickness delta;
The calculation formula of the resistance R Total (S) 2 is as follows:
Wherein R Seed crystal 2 is the resistance value of the seed crystal with the thickness of 2 delta, and R Seed crystal 2=(1/2)R Seed crystal 1.
6. The method according to claim 3, wherein the formula for calculating the crystal resistance R Crystal body in the step (3) is:
wherein R Total (S) is the real-time resistance between the two conductive bars measured.
7. The method according to claim 3, wherein the calculation formula of the crystal thickness δ in the step (4) is:
Wherein R Crystal body is the resistance value of the crystal, R is the radius of the cross section of the crystal, and ρ is the resistivity of the crystal.
8. The method according to claim 7, wherein the calculation formula of the crystal mass m in the step (5) is:
m=ε·δ·πr2
where ε is the density of crystals.
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CN206033927U (en) * 2016-08-17 2017-03-22 重庆工业职业技术学院 Novel daraf crystal growth is carried in liquid seal device
CN110349875A (en) * 2018-04-03 2019-10-18 江苏微导纳米装备科技有限公司 A method of measurement crystal column surface charge density variation
CN111364099A (en) * 2020-04-21 2020-07-03 宁夏银和新能源科技有限公司 Method for calculating resistivity of materials in residual pot for continuously drawing single crystal rod
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CN112748155A (en) * 2019-10-29 2021-05-04 Skc株式会社 Method and apparatus for measuring graphite-containing article, and ingot growing system
CN111364099A (en) * 2020-04-21 2020-07-03 宁夏银和新能源科技有限公司 Method for calculating resistivity of materials in residual pot for continuously drawing single crystal rod
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