CN115148585B - High-temperature measurement method based on ion implantation doped SiC wafer - Google Patents
High-temperature measurement method based on ion implantation doped SiC wafer Download PDFInfo
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- CN115148585B CN115148585B CN202210815631.3A CN202210815631A CN115148585B CN 115148585 B CN115148585 B CN 115148585B CN 202210815631 A CN202210815631 A CN 202210815631A CN 115148585 B CN115148585 B CN 115148585B
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- 238000009529 body temperature measurement Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000005468 ion implantation Methods 0.000 title claims abstract description 20
- 238000009792 diffusion process Methods 0.000 claims abstract description 48
- 239000012535 impurity Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- 230000006399 behavior Effects 0.000 claims description 6
- 239000002344 surface layer Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 238000002513 implantation Methods 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000001004 secondary ion mass spectrometry Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract 3
- 235000012431 wafers Nutrition 0.000 description 56
- 230000008569 process Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- -1 infrared radiation Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000012942 design verification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000004861 thermometry Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/26—Bombardment with radiation
- H01L21/263—Bombardment with radiation with high-energy radiation
- H01L21/265—Bombardment with radiation with high-energy radiation producing ion implantation
- H01L21/26506—Bombardment with radiation with high-energy radiation producing ion implantation in group IV semiconductors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
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Abstract
The invention discloses a high-temperature measurement method based on an ion implantation doped SiC wafer, and belongs to the technical field of measurement and test. The method adopts an ion implantation doped SiC crystal as a temperature measuring element, and after the SiC crystal is subjected to high-temperature treatment in a temperature measuring environment, secondary ion mass spectrometry is carried out on the SiC crystal to obtain a concentration-depth curve of impurity distribution, the tail of the curve is fitted through a residual error function to obtain a diffusion concentration curve corresponding to the concentration-depth curve, the concentration value of the left end point of the diffusion concentration curve is used as a characteristic diffusion concentration N, standard reference data and curve of the characteristic diffusion concentration N changing along with temperature are established, when the temperature measuring element measures temperature, the standard reference curve can be contrasted, and the temperature value corresponding to the characteristic diffusion concentration N can be determined by utilizing an interpolation method to realize temperature measurement. The invention effectively solves the problem of difficult measurement at high temperature (more than 1700 ℃), and can be applied to the field of temperature measurement of aviation engines.
Description
Technical Field
The invention belongs to the technical field of measurement and test, and particularly relates to a high-temperature measurement method based on an ion implantation doped SiC wafer.
Background
With the further development of China in aviation and aerospace, higher requirements are also put forward on the performance of an aeroengine, and the temperature is an extremely important index for various parts of the engine, such as a combustion chamber, a turbine and a tail nozzle. In the development process of the aeroengine, the temperature is an important parameter for performance analysis, design verification improvement and flow heat exchange analysis of the aeroengine. The aeroengine has the characteristics of high temperature, high pressure, high rotating speed, complex internal flow, complex structure, narrow space and the like, and the temperature measurement under the working conditions is always a hot spot problem of an aero test technology, and is also one of difficulties of the aero engine test technology.
The existing temperature measurement method of high-temperature parts such as turbine blades of an aeroengine mainly comprises methods such as thermocouples, temperature indicating paint, infrared radiation, sapphire optical fibers, siC wafers and the like. The SiC wafer temperature measurement technology has the advantages of small temperature measurement wafer size, no need of leads, high temperature measurement precision, high-density array type point distribution, easy realization of test modification, capability of measuring special positions where other temperature measurement methods such as turbine blade edge plates and tenons are difficult to realize measurement, and the like. Therefore, many of the temperature measurement tasks in this respect are now performed by SiC wafers.
The main principle of the SiC thermometry technology currently in use is that SiC wafers generate defects under neutron irradiation, so that lattice swelling occurs. The wafers are annealed at different high temperature and then subjected to different degrees of lattice recovery, the parameters of the lattices can be determined by an X-ray diffraction method, and the annealing temperature of the SiC wafer can be obtained by comparing the parameters with calibration data, so that the purpose of measuring the temperature is achieved. The method has the advantages of maturity, high measurement precision and high temperature measurement precision. But has the defects of limited temperature measuring range and difficult temperature measurement above 1700 ℃.
Therefore, in order to obtain a larger temperature measurement range and room for improvement in the temperature measurement technology, a new temperature measurement method needs to be developed to meet the requirements of the related applications.
Disclosure of Invention
The invention aims to provide a high-temperature measurement method based on an ion implantation doped SiC wafer. Compared with other leadless temperature measuring devices in use at present, the invention can be used for temperature test at 1700 ℃ or higher, and has important application value.
In order to achieve the above object, the present invention provides a method for measuring a high temperature based on ion implantation doped SiC wafers, comprising the steps of:
1) The front surface of the SiC wafer is implanted with ions, namely the SiC wafer with the front surface doped layer is prepared, the doped impurity ions are ions with diffusion behaviors, and the process ensures that the ion implantation doping of different positions of the whole SiC wafer surface is uniform. In addition, the implantation dosage is 10 14/cm2～1015/cm2, so that the maximum concentration of impurities in the SiC wafer is higher than 10 19/cm3;
2) Cutting the SiC wafer with doped surface into a plurality of smaller SiC wafer particles according to the temperature measurement task and the calibration requirement so as to be suitable for temperature measurement, namely a high-temperature measuring element, and screening the wafers for one time to remove the wafers with obvious damage, notch and the like;
3) And (5) preparing a standard reference curve. Processing doped SiC wafer particles at different temperatures respectively, obtaining an impurity concentration-depth curve by SIMS analysis, fitting the tail of the curve by a residual error function to obtain a diffusion concentration curve corresponding to the impurity concentration curve, taking the concentration value at the left end point of the diffusion concentration curve as a characteristic diffusion concentration N, establishing a standard reference data table of the characteristic diffusion concentration N changing along with the temperature, drawing a curve according to the data, and forming a standard reference curve;
4) The SiC wafer particles are distributed in a temperature measuring environment according to the requirement of a temperature measuring task, and are taken out from the high temperature environment after being subjected to high temperature;
5) SIMS analysis is carried out on the front surface layer of the SiC wafer particles for temperature measurement, so that an impurity concentration-depth curve of the SiC wafer particles is obtained;
6) And 5) extracting a characteristic diffusion concentration value N from the impurity concentration-depth curve obtained in the step 5), and comparing the characteristic diffusion concentration value N with a standard reference curve established in advance, and extracting the temperature corresponding to the characteristic diffusion concentration value N by utilizing an interpolation method, namely the temperature for measuring the temperature.
The ion implanted impurities selected in the invention can be selected from boron, lithium, hydrogen, nitrogen or aluminum, can have obvious concentration diffusion at high temperature, and are suitable for being used as impurities for temperature measurement characterization. In addition, the maximum concentration of ion-implanted impurities in the SiC wafer is not less than 10 19/cm3, the maximum concentration being high enough to support diffusion at high temperatures. Conversely, if the maximum concentration of the injected impurity is too low, or even below the characteristic diffusion concentration N at a certain temperature, the measurement of that temperature cannot be achieved.
The present invention utilizes the principle that the diffusion behavior of impurities in a SiC wafer at high temperature is related to the temperature experienced by the wafer, and when the SiC wafer is locally doped deeply, the distribution of impurities in the wafer in a smaller depth range of a front surface layer can be achieved by using an ion implantation technique, as shown in fig. 1. At high temperatures, diffusion of impurities occurs in SiC wafers, and at different temperatures, these diffusion behaviors are characterized differently. The treated SiC wafer is placed in a high-temperature environment, the SiC wafer also reaches the same temperature, and impurities in the wafer are diffused to a certain extent. Then, the SiC wafer is taken out, and the wafer is subjected to impurity concentration analysis, for example, a Secondary Ion Mass Spectrometry (SIMS) analysis technique is adopted to obtain a distribution curve of the concentration of the impurity after temperature measurement along with the change of depth, and it can be found that the concentration-depth distribution curve of the impurity changes regularly.
After high temperature, the impurity diffuses to the deep part of the wafer, a curve with larger depth appears at the tail part of the concentration curve, the newly added tail curve is formed by diffusion, the curve at the tail part is fitted by a residual error function, the part which can be fitted by the residual error function is the diffusion concentration curve of the impurity, the depth value of the diffusion concentration curve is the smallest, the concentration value of the left end point is the largest, and the concentration value of the left end point is called as characteristic diffusion concentration N.
The analysis is carried out at different temperatures, and the characteristic diffusion concentration N at various different temperatures is extracted to form a standard reference curve of the characteristic diffusion concentration N changing along with the temperature. By using the standard reference curve, the corresponding temperature value can be obtained according to the characteristic diffusion concentration value extracted by the high-temperature SiC wafer by using an interpolation algorithm through comparison, so that the temperature measurement is realized.
Compared with the existing temperature measuring device, the invention has the following advantages:
1) The invention provides a temperature measurement method based on an ion implantation doped SiC wafer. The method does not need to erect any measuring equipment on site, does not need a signal transmission line, is suitable for a closed working system, moving parts and the like, and is simple and convenient to operate.
2) The invention has wide high-temperature measurement range, and is based on the diffusion behavior of impurities at different temperatures, so that the measurement of higher temperature is easier, and the diffusion behavior characteristics of the impurities in SiC can be used for measuring high temperature up to 2000 ℃.
3) The invention selects pure SiC as a temperature measuring wafer, and the required wafer and related processing and equipment can be obtained in the market, so that the universality is strong.
4) The application field is wide. For doping of SiC wafers, the temperature measurement effect can be changed by changing the types of doped impurities and the ion energy during ion implantation, and the temperature measurement device can be applicable to different temperature measurement requirements and is convenient to adjust. Has important application prospect.
Drawings
Fig. 1 is a schematic structural view of an ion implantation doped SiC wafer of the present invention. Wherein 1-impurity doping of the surface layer of the SiC wafer; 2-undoped region of the SiC wafer;
Fig. 2 is a schematic diagram of an impurity concentration-depth curve of a SiC wafer according to an embodiment of the present invention, which shows a comparison of concentration curves of two samples that have not undergone a high temperature process and a high temperature process, and shows that a residual error function fits a concentration curve in which diffusion occurs at a high temperature of an impurity, thereby determining an impurity diffusion concentration curve, and determining a characteristic diffusion concentration value from a left end point of the diffusion concentration curve.
Detailed Description
In order to make the technical scheme of the present invention more clear, the following detailed description is provided with reference to the accompanying drawings.
The invention provides a high-temperature measurement method of an ion implantation doped SiC wafer, which comprises the following steps:
a. preparing an intrinsic SiC wafer with the thickness of 300-500 micrometers and the thickness of 4 inches, and cleaning;
b. The front surface of the SiC wafer is doped with boron ions by an ion implantation method, and the process ensures that the surface of the SiC wafer is uniformly doped everywhere. The energy of the injected B ions is 50-100 keV, and the injection dosage is 10 14/cm2～1015/cm2;
c. The SiC wafer after ion implantation is cut into a plurality of small wafer particles of 3 to 7mm width. Screening the wafer particles, removing wafers with obvious defects, and forming qualified products into temperature measuring elements;
d. Arranging the obtained temperature measuring element in a high-temperature environment with known temperature, wherein the temperature is 1700-2000 ℃, selecting one temperature measuring element for performing a high-temperature experiment every 50 ℃ from 1700 ℃, after finishing a high-temperature process, recording the temperature, numbering the taken SiC wafer, and marking;
e. SIMS analysis of the front surface layer was performed on SiC wafers not subjected to high temperature and subjected to high temperature, respectively, to obtain a concentration-depth profile of boron ions in the wafers. Referring to fig. 2, by comparison, an impurity diffusion curve at the tail of a concentration curve is preliminarily determined, the tail of the curve is fitted through a residual error function, the fitted part is determined to be a diffusion concentration curve, the concentration value at the left end point of the diffusion concentration curve is taken as a characteristic diffusion concentration N, a standard reference data table of the characteristic diffusion concentration N changing along with the temperature is further established, a curve is drawn according to the data, and a standard reference curve of the characteristic diffusion concentration N changing along with the temperature is formed;
f. when the temperature measuring element is used for measuring temperature, small wafer particles of the temperature measuring element are arranged in a high-temperature environment of the temperature to be measured, then the characteristic diffusion concentration N is extracted according to the step e, and the characteristic diffusion concentration N is compared with a standard reference curve established in advance, and an interpolation method is utilized,
And extracting the temperature corresponding to the characteristic diffusion concentration value N, namely the temperature for measuring the temperature, and finishing the temperature measurement.
While the invention has been described with reference to specific embodiments, those skilled in the art will recognize that insubstantial changes in form and content can be made in terms of the steps described above without departing from the spirit or scope of the invention. Therefore, the present invention is not limited to the above embodiments, and the scope of the present invention shall be defined by the claims.
Claims (4)
1. The high-temperature measurement method based on the ion implantation doped SiC wafer is characterized by comprising the following steps of:
1) Ion implantation is carried out on the front surface of the SiC wafer, and ions doped in the SiC wafer are ions with diffusion behaviors;
2) Cutting the doped SiC wafer into a plurality of SiC wafer particles;
3) The SiC wafer particles are respectively subjected to SIMS analysis at different temperatures to obtain impurity concentration-depth curves, the tail parts of the curves are fitted through residual error functions to obtain diffusion concentration curves corresponding to the impurity concentration-depth curves, the concentration value at the left end point of the diffusion concentration curves is used as characteristic diffusion concentration N, a standard reference data table of the characteristic diffusion concentration N changing along with the temperature is established, and curves are drawn according to the standard reference data table to form standard reference curves;
4) Arranging SiC wafer particles serving as a temperature measuring element in a temperature measuring environment, and taking the SiC wafer particles out of the high-temperature environment after the SiC wafer particles are subjected to high temperature;
5) SIMS analysis is carried out on the front surface layer of the temperature measuring element to obtain an impurity concentration-depth curve;
6) Extracting a characteristic diffusion concentration value N of the impurity concentration-depth curve in the step 5), comparing a standard reference data table, and extracting a temperature corresponding to the characteristic diffusion concentration value N by using an interpolation method to obtain a measured temperature.
2. The method for measuring the high temperature of the doped SiC wafer based on the ion implantation according to claim 1, wherein the ion implantation of the front surface of the SiC wafer in step 1) is uniform.
3. The method for measuring the high temperature of an ion implantation-doped SiC wafer according to claim 1, wherein the ions implanted in step 1) are boron, lithium, hydrogen, nitrogen or aluminum.
4. The method for measuring the high temperature of an ion implantation-based doped SiC wafer according to claim 1, wherein the implantation concentration in step 1) is higher than 10 19/cm3.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101598606A (en) * | 2009-07-22 | 2009-12-09 | 中国航空工业集团公司沈阳发动机设计研究所 | A kind of carborundum crystals with neutron irradiation is the temp measuring method of sensor |
| WO2011136294A1 (en) * | 2010-04-28 | 2011-11-03 | 株式会社デンソー | Temperature sensor element, method for manufacturing same, and temperature sensor |
| CN106098522A (en) * | 2016-06-30 | 2016-11-09 | 中国电子科技集团公司第四十八研究所 | A kind of SIC high temperature high energy implanters high energy measurement apparatus |
| CN107957299A (en) * | 2017-11-27 | 2018-04-24 | 电子科技大学 | A kind of carborundum linear temperature sensor and its temp measuring method and manufacture method |
| CN109030544A (en) * | 2018-06-06 | 2018-12-18 | 中国航空工业集团公司北京长城航空测控技术研究所 | A kind of maximum temperature measurement method based on the variation of minicrystal lattice parameter |
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- 2022-07-11 CN CN202210815631.3A patent/CN115148585B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101598606A (en) * | 2009-07-22 | 2009-12-09 | 中国航空工业集团公司沈阳发动机设计研究所 | A kind of carborundum crystals with neutron irradiation is the temp measuring method of sensor |
| WO2011136294A1 (en) * | 2010-04-28 | 2011-11-03 | 株式会社デンソー | Temperature sensor element, method for manufacturing same, and temperature sensor |
| CN106098522A (en) * | 2016-06-30 | 2016-11-09 | 中国电子科技集团公司第四十八研究所 | A kind of SIC high temperature high energy implanters high energy measurement apparatus |
| CN107957299A (en) * | 2017-11-27 | 2018-04-24 | 电子科技大学 | A kind of carborundum linear temperature sensor and its temp measuring method and manufacture method |
| CN109030544A (en) * | 2018-06-06 | 2018-12-18 | 中国航空工业集团公司北京长城航空测控技术研究所 | A kind of maximum temperature measurement method based on the variation of minicrystal lattice parameter |
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