CN108061753B - Nondestructive characterization method for simultaneously detecting film adhesion property and Young modulus - Google Patents
Nondestructive characterization method for simultaneously detecting film adhesion property and Young modulus Download PDFInfo
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- CN108061753B CN108061753B CN201711191836.4A CN201711191836A CN108061753B CN 108061753 B CN108061753 B CN 108061753B CN 201711191836 A CN201711191836 A CN 201711191836A CN 108061753 B CN108061753 B CN 108061753B
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- 238000012512 characterization method Methods 0.000 title claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 32
- 238000012360 testing method Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 230000005284 excitation Effects 0.000 abstract description 8
- 239000010408 film Substances 0.000 description 19
- 239000000523 sample Substances 0.000 description 15
- 238000005259 measurement Methods 0.000 description 9
- 239000000758 substrate Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000000691 measurement method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000009659 non-destructive testing Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/04—Analysing solids
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Abstract
The invention relates to a nondestructive characterization method for simultaneously detecting the adhesion property and Young modulus of a film, which comprises the following steps: obtaining the sample to be tested by the ultrasonic surface wave test of laser excitation sample waferAnd measuring the experimental dispersion curve of the sample wafer to obtain the Young modulus value without considering the influence of the adhesion characteristic, and measuring the adhesion characteristic of the sample wafer as a known parameter. And determining the search range and the search step length of the Young modulus and the adhesion characteristic. Calculating a series of theoretical dispersion curves determined by Young's modulus and adhesion characteristic determined by the determined search step length in the search range, and calculating R of each theoretical dispersion curve and each experimental dispersion curve2Value for R2The values are sorted, R2The curve with the maximum value can be regarded as the curve with the highest matching degree, and the Young modulus value and the adhesion characteristic value corresponding to the curve are the Young modulus value and the adhesion characteristic value of the film to be measured.
Description
Technical Field
The invention belongs to the field of ultrasonic surface wave nondestructive testing, and relates to a method for simultaneously representing various characteristics of a film.
Background
As the low-k materials become more widely used in modern integrated circuit research and industry, techniques for non-destructive testing of thin film properties become more important. The laser excitation ultrasonic surface wave technology is a novel detection means which can be used for detecting the characteristics of the low-k material film, and has good engineering application prospect and profound research significance due to the advantages of being nondestructive, accurate in measurement result, rapid and simple in detection process, capable of realizing on-line detection and the like, and the laser excitation ultrasonic surface wave technology becomes an important means for nondestructive detection of the characteristics of the low-k material at present. For thin film materials, the young's modulus and adhesion characteristics are important characteristics of the thin film, which affect the service life and reliability of thin film devices. In the prior measurement technology, the traditional laser excitation ultrasonic surface wave method can only measure a certain characteristic of the film independently, and cannot simultaneously measure the Young modulus and the adhesiveness. In other film characterization techniques, such as nano-scratch and four-point probe, the measurement process cannot be realized simultaneously and all the measurement methods are lossy measurement methods. The invention researches the influence of the adhesion property on the measurement of the Young modulus, thereby inventing a method capable of simultaneously measuring the adhesion property and the Young modulus.
Disclosure of Invention
The patent provides a method for simultaneously measuring the adhesion property and Young modulus of a film aiming at a laser excitation ultrasonic surface wave method. The invention firstly determines the error range of the adhesion property to the Young modulus measurement, and matches the error range in a searching mode to finish the nondestructive quantitative measurement of the Young modulus and the film adhesion property at the same time. The technical scheme is as follows:
a nondestructive characterization method for simultaneously detecting the adhesion property and Young modulus of a film comprises the following steps:
(1) and (3) obtaining an experimental dispersion curve of the sample wafer to be tested by an ultrasonic surface wave test of exciting the sample wafer to be tested by laser, obtaining a Young modulus value E ' without considering the influence of the adhesion characteristic, and measuring the adhesion characteristic A ' of the sample wafer by taking the E ' as a known parameter.
(2) Determining the search range and the search step length of the Young modulus and the adhesion characteristic, wherein the method comprises the following steps: the Young's modulus search range was set to be 20% of the deviation from E ', and the Young's modulus search step was set to 0.1GPa, and the adhesion characteristic search step was set to 1 PPa/m.
(3) Calculating a series of theoretical dispersion curves determined by Young's modulus and adhesion characteristic determined by the determined search step length in the search range, and calculating R of each theoretical dispersion curve and each experimental dispersion curve2Value for R2The values are sorted, R2The curve with the maximum value can be regarded as the curve with the highest matching degree, the Young modulus value and the adhesion characteristic value corresponding to the curve are the Young modulus value and the adhesion characteristic value of the film to be measured, and if R is equal to R, the curve is regarded as the curve with the highest matching degree, and the Young modulus value and the adhesion characteristic value corresponding to the curve are the Young modulus value and the adhesion characteristic2And if the maximum value corresponds to the boundary value of the Young modulus or the adhesion property, expanding the search range of the corresponding variable and finishing the matching process.
Drawings
FIG. 1 Experimental Dispersion Curve for test coupons
FIG. 2 matching of test sample test dispersion curves
Detailed Description
Through calculation of a large number of calculation examples, the fact that in the laser excitation ultrasonic surface wave measurement method, due to the fact that the error of the adhesion property between the film substrates to Young modulus measurement is basically lower than 20%, simultaneous measurement of the Young modulus of the film substrate structure and the adhesion property between the film substrates can be achieved according to the rule. Firstly obtaining an experimental dispersion curve of a sample wafer to be tested, and secondly not obtainingAnd taking the influence of the adhesion characteristic into consideration, obtaining a value of the Young modulus without considering the influence of the adhesion characteristic through curve matching, marking the value as E ', taking the E ' as a known parameter, and measuring the adhesion characteristic of the sample wafer through a laser excitation ultrasonic surface wave method, and marking the value as A '. Taking 20% of E 'as a search boundary of Young modulus, 50% of A' as a search boundary of adhesion property, 0.1GPa as a search step length of Young modulus, 1PPa/m as a search step length of adhesion property, calculating a series of theoretical dispersion curves determined by Young modulus and adhesion property in a search range and determined by the determined search step length by a matrix method, and calculating R of each theoretical dispersion curve and each experimental dispersion curve2Value for R2The values are sorted, R2The curve with the maximum value can be regarded as the curve with the highest matching degree, and the Young modulus value and the adhesion characteristic value corresponding to the curve are the Young modulus value and the adhesion characteristic value of the film to be measured. If R is2And if the maximum value corresponds to the boundary value of the Young modulus or the adhesion property, expanding the search range of the corresponding variable and finishing the matching process.
The technical scheme of the invention is concretely illustrated by a sample wafer as follows:
1. and measuring by using a laser excitation ultrasonic surface wave system to obtain an experimental curve of the sample wafer to be measured. The sample wafer to be measured is made of compact Black Diamond, the thickness of the film is 1028nm, and the density of the film is 1.38g/cm3. The substrate material being silicon material and the measuring direction being silicon<110>And (4) direction. The experimental dispersion curve is shown in fig. 1, wherein the jagged is the experimental dispersion curve, and the smooth curve is the fitting curve of the experimental dispersion curve.
2. By matching the experimental dispersion curve with the dispersion curve without considering the adhesion characteristics, the approximate young's modulus of the sample piece was 9.3GPa without considering the influence of the adhesion characteristics. The adhesion characteristics were matched using 9.3GPa as a known parameter, and the approximate adhesion characteristic value of the sample was found to be 146 PPa/m.
3. The search matching work was performed with 120% of 9.3GPa as the search boundary, 0.1GPa as the search step, 50% of 146PPa/m as the search boundary of adhesion property, and 1PPa/m as the search boundary. The Young modulus is calculated to be 9.3 GPa-11.2 GPa, the adhesion property is between 73 PPa/m and 146PPa/m, and the total of 20 and 74 is 1480 theoretical dispersion curves.
4. Solving the R of 1480 theoretical dispersion curves and experimental dispersion curves2Value for R2The values are sorted, R2The curve with the largest value corresponds to values of Young's modulus and adhesion property of 9.7GPa and 120PPa/m, respectively, thus completing the simultaneous and accurate measurement of the model modulus and adhesion property of the sample. The experimental dispersion curve, the fitting curve of the experimental dispersion curve, and the estimated values of young's modulus and adhesion property after the initial matching, and the condition of the final exact matching result are also shown in fig. 2.
The following summarizes the determination method of the present invention:
(1) and obtaining an experimental dispersion curve of the sample to be measured, obtaining the Young modulus value E ' without considering the influence of the adhesion characteristic, and measuring the adhesion characteristic A ' of the sample by taking the E ' as a known parameter.
(2) All theoretical dispersion curves in the range were calculated with E 'to 120% E' as the search boundary of the Young's modulus, 0.1GPa as the search step of the Young's modulus, 50% A 'to A' as the search boundary of the adhesion property, and 1PPa/m as the search step of the adhesion property.
(3) Calculating R of each theoretical frequency dispersion curve and each experimental frequency dispersion curve2Value for R2The values are sorted, R2The curve with the maximum value can be regarded as the curve with the highest matching degree, and the Young modulus value and the adhesion characteristic value corresponding to the curve are the Young modulus value and the adhesion characteristic value of the film to be measured.
(4) If R is2And if the maximum value corresponds to the boundary value of the Young modulus or the adhesion property, expanding the search range of the corresponding variable, and repeating the process to finish the matching process.
The method is a nondestructive quantitative characterization method which is suitable for all types of film substrate structures, can realize the simultaneous and accurate characterization of the film adhesion property and the Young modulus, and is an effective method in the field of film property characterization.
Claims (1)
1. Simultaneous detection of low-kThe nondestructive characterization method of the adhesion property and Young modulus of the film material comprises the following steps:
(1) through an ultrasonic surface wave test of a sample wafer to be tested excited by laser, obtaining an experimental dispersion curve of the sample wafer to be tested, obtaining a Young modulus value E ' without considering the influence of adhesion characteristics, and measuring the adhesion characteristics A ' of the sample wafer by taking the E ' as a known parameter;
(2) determining the search range and the search step length of the Young modulus and the adhesion characteristic, wherein the method comprises the following steps: taking the deviation of 20% of E 'as a search boundary of the Young modulus, taking 50% of A' as a search boundary of the adhesion property, setting the search step of the Young modulus as 0.1GPa and the search step of the adhesion property as 1 PPa/m;
(3) calculating a series of theoretical dispersion curves determined by Young's modulus and adhesion characteristic determined by the determined search step length in the search range, and calculating R of each theoretical dispersion curve and each experimental dispersion curve2Value for R2The values are sorted, R2The curve with the maximum value is regarded as the curve with the highest matching degree, the Young modulus value and the adhesion characteristic value corresponding to the curve are the Young modulus value and the adhesion characteristic value of the film to be measured, and if R is equal to R, the curve is regarded as the curve with the highest matching degree, the Young modulus value and the adhesion characteristic value corresponding to the curve are the Young modulus value and the adhesion characteristic value2And if the maximum corresponding condition is the boundary value of the Young modulus or the adhesion property, expanding the search range of the corresponding variable and finishing the matching process.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996023205A1 (en) * | 1995-01-24 | 1996-08-01 | Massachusetts Institute Of Technology | Optical measurements of stress in thin film materials |
| CN101876647A (en) * | 2010-07-05 | 2010-11-03 | 天津大学 | Bidirectional detection method of Young modulus and Poisson constant by ultrasonic surface wave |
| CN102183441A (en) * | 2011-02-18 | 2011-09-14 | 华东理工大学 | Method for measuring surface adhesive capacity and elastic modulus of soft material |
| CN105651689A (en) * | 2015-12-28 | 2016-06-08 | 天津大学 | Nondestructive testing method for adhesion of thin film based on cohesion model |
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2017
- 2017-11-24 CN CN201711191836.4A patent/CN108061753B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996023205A1 (en) * | 1995-01-24 | 1996-08-01 | Massachusetts Institute Of Technology | Optical measurements of stress in thin film materials |
| CN101876647A (en) * | 2010-07-05 | 2010-11-03 | 天津大学 | Bidirectional detection method of Young modulus and Poisson constant by ultrasonic surface wave |
| CN102183441A (en) * | 2011-02-18 | 2011-09-14 | 华东理工大学 | Method for measuring surface adhesive capacity and elastic modulus of soft material |
| CN105651689A (en) * | 2015-12-28 | 2016-06-08 | 天津大学 | Nondestructive testing method for adhesion of thin film based on cohesion model |
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