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High-precision X-ray characterization for basic materials in modern high-end integrated circuit

Weiran Zhao1, 2, §, Qiuqi Mo1, 2, §, Li Zheng1, , Zhongliang Li3, Xiaowei Zhang4 and Yuehui Yu1

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 Corresponding author: Li Zheng, zhengli@mail.sim.ac.cn

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Abstract: Semiconductor materials exemplify humanity's unwavering pursuit of enhanced performance, efficiency, and functionality in electronic devices. From its early iterations to the advanced variants of today, this field has undergone an extraordinary evolution. As the reliability requirements of integrated circuits continue to increase, the industry is placing greater emphasis on the crystal qualities. Consequently, conducting a range of characterization tests on the crystals has become necessary. This paper will examine the correlation between crystal quality, device performance, and production yield, emphasizing the significance of crystal characterization tests and the important role of high-precision synchrotron radiation X-ray topography characterization in semiconductor analysis. Finally, we will cover the specific applications of synchrotron radiation characterization in the development of semiconductor materials.

Key words: X-ray topographysynchrotron radiationsemiconductor materialscrystal defects



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[10]
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[11]
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Moore M. White-beam X-ray topography. Crystallography Reviews, 2012, 18(3), 207 doi: 10.1080/0889311X.2012.697462
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Petroff J F, Sauvage M. Misfit dislocation characteristics in quarternary heterojunctions Ga1-xAlxAs1-yPy/GaAs analysed by synchrotron radiation white beam topography. Journal of Crystal Growth, 1978, 43(5), 628 doi: 10.1016/0022-0248(78)90052-0
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Oliver Ambacher. Growth and applications of group III-nitrides. Journal of Physics D: Applied physics, 1998, 31(20), 2653 doi: 10.1088/0022-3727/31/20/001
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Gibart P. Metal organic vapour phase epitaxy of GaN and lateral overgrowth. Reports on Progress in Physics, 2004, 67(5), 667 doi: 10.1088/0034-4885/67/5/R02
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Fujito K, Kubo S, Nagaoka H, et al. Bulk GaN crystals grown by HVPE. Journal of Crystal Growth, 2009, 311(10), 3011 doi: 10.1016/j.jcrysgro.2009.01.046
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Sintonen S, Suihkonen S, Jussila H, et al. Large-area analysis of dislocations in ammonothermal GaN by synchrotron radiation X-ray topography. Applied Physics Express, 2014, 7(9), 091003 doi: 10.7567/APEX.7.091003
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Neudeck P G, Huang W, Dudley M. Breakdown degradation associated with elementary screw dislocations in 4H-SiC p+n junction rectifiers. MRS Online Proceedings Library (OPL), 1997, 483, 285 doi: 10.1557/PROC-483-285
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Neudeck P G, Fazi C. Study of bulk and elementary screw dislocation assisted reverse breakdown in low-voltage (<250 V) 4H-SiC p+n junction diodes—Part II: Dynamic breakdown properties. IEEE Transactions on Electron Devices, 1999, 46(3), 485 doi: 10.1109/16.748866
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Fig. 1.  Schematic of the first transistor invented in 1947.

Fig. 2.  Common X-ray topography methods.

Fig. 3.  UPWT of a wedge-shaped float zone (FZ) silicon wafer taken at 5 different angular positions on the rocking curve[23].

Fig. 4.  Diffuse background contrast observed in ARPWT[23]: (a) $ \Delta \theta_{{\rm{in}}}=-2.7^{\prime \prime}, \Delta \theta_{{\rm{out}}}=-2.4^{\prime \prime} $, (b) $ \Delta \theta_{{\rm{in}}}=-2.7^{\prime \prime}, \Delta \theta_{{\rm{out}}}=+2.4^{\prime \prime} $, (c) $ \Delta \theta_{{\rm{in}}}= $$ +2.7^{\prime \prime}, \Delta \theta_{{\rm{out}}}=-2.4^{\prime \prime} $, (d) $ \Delta \theta_{{\rm{in}}}=+2.7^{\prime \prime}, \Delta \theta_{{\rm{out}}}=+2.4^{\prime \prime}. $

Fig. 5.  Comparison between the section topographs of two different wafer sample[24]. (a) Section transmission topograph of the reference wafer. (b) Section transmission topograph of a wafer underwent 166 seconds of RTO.

Fig. 6.  Dislocation half loops and tangled dislocations obtained from the neck region[20].

Fig. 7.  Optical images (a), (b) and topographs (c)−(e) of etched piece of sample for GaAs:Si ELO layers on GaAs substrate[30].

Fig. 8.  A back-reflection topograph showing TSDs and TMDs in GaN substrate[34].

Fig. 9.  $ (0 2 \overline{2} 1) $, $ (1 \overline{2} 1 0) $, $ (1 \overline{1} 0 0) $ reflection section transmission topographs of sample H-1. Sample H-1 is 50 mm long in diameter and grown by HVPE[36].

Fig. 10.  The left topograph is a $ (\overline{1} 1 0 5) $ reflection large-area SWXRT recorded from sample H-A, while the right one shows individual screw dislocations. Sample H-A is HVPE-GaN grown on an low defect density ammonothermal GaN-seed[36].

Fig. 11.  (Color online) Threading dislocations in 4H-SiC[40]. (a) Typical etch patterns obtained after etching in molten KOH at $ 520 $ °C for several minutes for substrate with $ [n] > 5 \times 10^{18} \ {\rm{cm}}^{-3} $ (figure on the left) and epitaxial layer with $ n \sim 10^{17} \ {\rm{cm}}^{-3} $(figure on the right). (b) Topographs for dislocation identification taken in back-reflection geometry with the given diffraction vectors $ {\bf{g}} $. (c) Comparison of etch pattern a with topograph b for an etched substrate. All TSDs identified by XRT are marked with blue squares in the topograph and the etch pattern.

Fig. 12.  Observed Berg–Barrett topography image of dissociated dislocation produced by light irradiation[41].

Fig. 13.  Defect structure in epilayer grown on on-axis SiC[42]. (a) Reflection X-ray topograph of the epitaxial on-axis 4H-SiC sample with diffraction vector g = $ (2 0 \overline{2} 10) $ (indicated in the bottom-left of the image). (b)Transmission X-ray topograph of the epitaxial on-axis 4H-SiC sample with diffraction vector g = $ (1 0 \overline{1}0) $ (indicated in the bottom-left of the image).

Fig. 14.  (Color online) Mapping of lattice strains in 4H-SiC wafers[22]. (a) SWBXT image recorded from the same sample showing the nucleation of large numbers of basal plane dislocations near the strain center. The density of dislocations is too high to resolve a single dislocation image. (b) Strain maps of four different strain components: (a) $ \frac{\partial u_1}{\partial x_1} $, (b) $ \frac{\partial u_2}{\partial x_2} $, (c) $ \frac{\partial u_1}{\partial x_3} $, and (d) $ \frac{\partial u_2}{\partial x_3} $, where $ \frac{\partial u_i}{\partial x_i} $ is lattice dilation/compression and $ \frac{\partial u_i}{\partial x_k} $ is lattice shear/rotation.

Fig. 15.  Defect structure in HPHT diamonds[45]. (a) Features of the actual structure of highly imperfect HPHT diamond crystals examined using double-crystal X-ray topography. The diamond plate with the (001) orientation is analyzed by recording its topographs on the opposite slopes of the rocking curve. (b) A double-crystal X-ray topograph of a synthetic HPHT diamond. Striations and different growth sectors can be observed (indicated by the black arrow).

Fig. 16.  (Color online) XRT images of sample diamond substrate before and after the homo-epitaxial film growth, taken by (044) diffraction vector[47].

Fig. 17.  (Color online) Transmission SWXRT topographs[50]. (a) a c-plane wafer (g = $( 11\overline{2}0 )$) from the tail end of an AlN boule showing a network of $ \langle 1\overline{1} 00\rangle $ LAGBs; (b) an axial m-plane wafer from the same boule showing TSDs enclosed by the network of $ \langle 1\overline{1} 00\rangle $ LAGBs.

Fig. 18.  The left topograph (a) is an enlarged SMBXT image of sample A displays segments of BPD that were imaged within a penetration depth of 30–48 $\mu{\rm{m}} $ by the X-rays[52], while the right one (b) is an enlarged SMBXT image of sample B exhibits TED arrays that have been polygonized along a $ \langle 1 \overline{1} 0 0\rangle $ direction[52].

Table 1.   Brief summary for all kinds of crystal defects and their impact on device performances.

Crystal defectsa Common causes Impact on device performances
Vacancy defects (0D) Lattice mismatch or thermal vibration Lower carrier transport rate
Interstitial defects (0D) Impurity induced in doping or crystal pulling Lower electron−hole recombination rate
Dislocationsb (1D) Inconsistent temperature gradient or growth rate Induced trap states, plastic deformation
Stacking faults (2D) Inconsistent temperature gradient or growth rate Photon scattering$ / $absorption enhancement
Grain boundariesc (2D) Different grain orientation Similar to stacking faults
Crystal twinning (2D) Fluctuations in growth rate or temperature Similar to stacking faults
Voids (clusters of vacancies) (3D) Inconsistent growth rate Trap states and photon scattering
Precipitates (clusters of impurities) (3D) Impurities accumulated growing crystals Potential trigger for additional defects
Growth stripes (2D/3D)d Fluctuation in temperature gradient or concentration /
a For following rows: 0D, 1D, 2D, and 3D stand for point defects, line defects, planar defects, and bulk defects respectively.
b There are mainly three kinds of dislocations: screw dislocations, edge dislocations, and mixed dislocations.
c Grain boundaries are naturally present in polycrystalline materials, resulting from the varied orientations of the grains. However, when single-crystal materials are inadequately processed, these grain boundaries are perceived as defects.
d This phenomenon cannot be strictly categorized as a "defect", but rather should be considered as nonuniform topography, specifically evident in the form of concentric circles on 300 mm silicon wafers.
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Table 2.   Observation scale and characteristics of relevant representation methods.

Characterization methods Detection scale Characteristics
Optical microscope (OM) Larger than 200 nm Easy to operate.
Scanning electron microscope (SEM) Nanometer level Provide information about the sample's surface topography and composition.
Transmission electron microscope (TEM) Angstrom level Very high resolution but the sample needs to be very thin.
Atomic force microscope (AFM) Angstrom level Surface topography and measurements of the material properties through probe detecting. Longer operation time.
Scanning tunneling microscope (STM) Sub-atom level Mapping the surface of the sample, with a lateral resolution about 1 Å and a vertical resolution up to 0.01 Å. The sample should be conductive.
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[1]
Bardeen J, Brattain W H. The transistor, a semi-conductor triode. Physical Review, 1948, 74(2), 230 doi: 10.1103/PhysRev.74.230
[2]
Moskalyk R R. Review of germanium processing worldwide. Minerals engineering, 2004, 17(3), 393 doi: 10.1016/j.mineng.2003.11.014
[3]
Kilby J S. Invention of the integrated circuit. IEEE Transactions on Electron Devices, 1976, 23(7), 648 doi: 10.1109/T-ED.1976.18467
[4]
Newman R C. Defects in silicon. Reports on Progress in Physics, 1982, 45(10), 1163 doi: 10.1088/0034-4885/45/10/003
[5]
Dash W C. Growth of silicon crystals free from dislocations. Journal of Applied Physics, 1959, 30(4), 459 doi: 10.1063/1.1702390
[6]
Chin A K. The effect of crystal defects on device performance and reliability. Journal of Crystal Growth, 1984, 70(1), 582 doi: 10.1016/0022-0248(84)90320-8
[7]
Barrett C S. A new microscopy and its potentialities. Trans Aime, 1945, 161, 15
[8]
Ramachandran G N. X-ray topographs of diamond. In Proceedings of the Indian Academy of Sciences-Section A, Springer India, 1944, 19(5), 280 doi: 10.1007/BF03173455
[9]
Shul’Pina I L, Argunova T S. Detection of dislocations in strongly absorbing crystals by projection X-ray topography in back reflection. Journal of Physics D: Applied Physics, 1995, 28(4A), A47 doi: 10.1088/0022-3727/28/4A/009
[10]
Lang A R. Direct observation of individual dislocations by X-ray diffraction. Journal of Applied Physics, 1958, 29(3), 597 doi: 10.1063/1.1723234
[11]
Lang A R. The projection topograph: a new method in X-ray diffraction microradiography. Acta Crystallographica, 1959, 12(3), 249 doi: 10.1107/S0365110X59000706
[12]
Lefeld-Sosnowska M, Gronkowski J, Kowalski G. A study of defects generated in Czochralski-grown Si during two-step annealing. Journal of Physics D: Applied Physics, 1995, 28(4A), A42 doi: 10.1088/0022-3727/28/4A/008
[13]
Goorsky M S, Feichtinger P, Fukuto H, et al. X-ray topography and diffraction studies of misfit dislocation nucleation in Si-based structures. Philosophical Transactions of the Royal Society of London. Series A: Mathematical, Physical and Engineering Sciences, 1999, 357(1761), 2777 doi: 10.1098/rsta.1999.0465
[14]
Authier A. Contrast of a stacking fault on X-ray topographs. physica status solidi (b), 1968, 27(1), 77 doi: 10.1002/pssb.19680270107
[15]
Moore M. White-beam X-ray topography. Crystallography Reviews, 2012, 18(3), 207 doi: 10.1080/0889311X.2012.697462
[16]
Lang A R. Studies of individual dislocations in crystals by X-ray diffraction microradiography. Journal of Applied Physics, 1959, 30(11), 1748 doi: 10.1063/1.1735048
[17]
Haruta K. New method of obtaining stereoscopic pairs of X-ray diffraction topographs. Journal of Applied Physics, 1965, 36(5), 1789 doi: 10.1063/1.1703131
[18]
Tuomi T, Kelhä V, Naukkarinen K, et al. Multistereo synchrotron X-ray topography. Zeitschrift für Naturforschung A, 1982, 37(6), 607
[19]
Ludwig W, Cloetens P, Härtwig J, et al. Three-dimensional imaging of crystal defects by topo-tomography. Journal of Applied Crystallography, 2001, 34(5), 602-607 doi: 10.1107/S002188980101086X
[20]
Kawado S, Taishi T, Iida S, et al. Three-dimensional structure of dislocations in silicon determined by synchrotron white X-ray topography combined with a topo-tomographic technique. Journal of Physics D: Applied Physics, 2005, 38(10A), A17 doi: 10.1088/0022-3727/38/10A/004
[21]
Moore M. Synchrotron X-ray topography. Radiation Physics and Chemistry, 1995, 45(3), 427 doi: 10.1016/0969-806X(94)E0061-M
[22]
Guo J Q, Yang Y, Raghothamachar B, et al. Mapping of lattice strain in 4H-SiC crystals by synchrotron double-crystal X-ray topography. Journal of Electronic Materials, 2018, 47, 903 doi: 10.1007/s11664-017-5789-x
[23]
Ishikawa T. Synchrotron X-ray topographic studies on minute strain fields in as-grown silicon single crystals. Journal of Crystal Growth, 1990, 103(1), 131 doi: 10.1016/0022-0248(90)90181-J
[24]
Lowney D, Perova T S, Nolan M, et al. Investigation of strain induced effects in silicon wafers due to proximity rapid thermal processing using micro-raman spectroscopy and synchrotron X-ray topography. Semiconductor Science and Technology, 2002, 17(10), 1081 doi: 10.1088/0268-1242/17/10/309
[25]
Hobgood H M, Thomas R N, Barrett D L, et al. Semi-insulating III-V materials. In Proc. 3rd Conf. Shiva Nantwich, 1984, 149
[26]
Matsumura T, Obokata T, Fukuda T. Two-dimensional microscopic uniformity of resistivity in semi-insulating GaAs. Journal of Applied Physics, 1985, 57(4), 1182 doi: 10.1063/1.334513
[27]
Wurzinger P, Oppolzer H, Pongratz P, et al. TEM characterization of defects in LEC-grown GaAs substrates. Journal of Crystal Growth, 1991, 110(4), 769 doi: 10.1016/0022-0248(91)90635-I
[28]
Petroff J F, Sauvage M. Misfit dislocation characteristics in quarternary heterojunctions Ga1-xAlxAs1-yPy/GaAs analysed by synchrotron radiation white beam topography. Journal of Crystal Growth, 1978, 43(5), 628 doi: 10.1016/0022-0248(78)90052-0
[29]
Prieur E, Tuomi T, Partanen J, et al. Synchrotron topographic study of defects in liquid-encapsulated Czochralski-grown semi-insulating gallium arsenide wafers. Journal of Crystal Growth, 1993, 132(3), 599
[30]
Rantamäki R, Tuomi T, Zytkiewicz Z R, et al. Synchrotron X-ray topography analysis of GaAs layers grown on GaAs substrates by liquid phase epitaxial lateral overgrowth. Journal of Physics D: Applied Physics, 1999, 32(10A), A114 doi: 10.1088/0022-3727/32/10A/324
[31]
Oliver Ambacher. Growth and applications of group III-nitrides. Journal of Physics D: Applied physics, 1998, 31(20), 2653 doi: 10.1088/0022-3727/31/20/001
[32]
Gibart P. Metal organic vapour phase epitaxy of GaN and lateral overgrowth. Reports on Progress in Physics, 2004, 67(5), 667 doi: 10.1088/0034-4885/67/5/R02
[33]
Fujito K, Kubo S, Nagaoka H, et al. Bulk GaN crystals grown by HVPE. Journal of Crystal Growth, 2009, 311(10), 3011 doi: 10.1016/j.jcrysgro.2009.01.046
[34]
Sintonen S, Suihkonen S, Jussila H, et al. Large-area analysis of dislocations in ammonothermal GaN by synchrotron radiation X-ray topography. Applied Physics Express, 2014, 7(9), 091003 doi: 10.7567/APEX.7.091003
[35]
Yao Y, Ishikawa Y, Sugawara Y, et al. Observation of threading dislocations in ammonothermal gallium nitride single crystal using synchrotron X-ray topography. Journal of Electronic Materials, 2018, 47, 5007 doi: 10.1007/s11664-018-6252-3
[36]
Kirste L, Danilewsky A N, Sochacki T, et al. Synchrotron white-beam X-ray topography analysis of the defect structure of HVPE-GaN substrates. ECS Journal of Solid State Science and Technology, 2015, 4(8), 324, doi: 10.1149/2.0181508jss
[37]
Dudley M, Wang S P, Huang W, et al. White-beam synchrotron topographic studies of defects in 6H-SiC single crystals. Journal of Physics D: Applied Physics, 1995, 28(4A), A63 doi: 10.1088/0022-3727/28/4A/012
[38]
Neudeck P G, Huang W, Dudley M. Breakdown degradation associated with elementary screw dislocations in 4H-SiC p+n junction rectifiers. MRS Online Proceedings Library (OPL), 1997, 483, 285 doi: 10.1557/PROC-483-285
[39]
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    Received: 15 March 2024 Revised: 26 April 2024 Online: Accepted Manuscript: 29 May 2024Uncorrected proof: 30 May 2024Published: 15 July 2024

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      Weiran Zhao, Qiuqi Mo, Li Zheng, Zhongliang Li, Xiaowei Zhang, Yuehui Yu. High-precision X-ray characterization for basic materials in modern high-end integrated circuit[J]. Journal of Semiconductors, 2024, 45(7): 071101. doi: 10.1088/1674-4926/24030016 W R Zhao, Q Q Mo, L Zheng, Z L Li, X W Zhang, and Y H Yu, High-precision X-ray characterization for basic materials in modern high-end integrated circuit[J]. J. Semicond., 2024, 45(7), 071101 doi: 10.1088/1674-4926/24030016Export: BibTex EndNote
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      Weiran Zhao, Qiuqi Mo, Li Zheng, Zhongliang Li, Xiaowei Zhang, Yuehui Yu. High-precision X-ray characterization for basic materials in modern high-end integrated circuit[J]. Journal of Semiconductors, 2024, 45(7): 071101. doi: 10.1088/1674-4926/24030016

      W R Zhao, Q Q Mo, L Zheng, Z L Li, X W Zhang, and Y H Yu, High-precision X-ray characterization for basic materials in modern high-end integrated circuit[J]. J. Semicond., 2024, 45(7), 071101 doi: 10.1088/1674-4926/24030016
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      High-precision X-ray characterization for basic materials in modern high-end integrated circuit

      doi: 10.1088/1674-4926/24030016
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      • Weiran Zhao received the bachelor’s degree in Electronic Engineering from ShanghaiTech University, Shanghai, China, in 2022. He is currently working toward the master’s degree in Materials Science and Engineering with the School of Physical Science and Technology under the supervision of Prof. Yuehui Yu, at ShanghaiTech University, Shanghai, China. His research focuses on semiconductor crystal defect evolution mechanism study with multiple methods, especially synchrotron radiation X-ray topography
      • Qiuqi Mo received the bachelor's degree in Nanomaterials and Technology from Soochow University, Suzhou, China. He is currently working toward the Ph.D. degree in Materials Science and Engineering with the School of Physical Science and Technology under the supervision of Prof. Yuehui Yu, at ShanghaiTech University, Shanghai, China. His research focuses on characterization technique of semiconductor materials, especially synchrotron radiation X-ray topography
      • Li Zheng is a Professor and Doctoral supervisor of Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences. He earned his Ph. D degree in microelectronics and solid-state electronics from University of Chinese Academy of Sciences. He has extensive experience in semiconductor and integrated circuit chips with over 90 SCI papers and over 40 patent applications. He has received numerous national and provincial honors, including the National Youth Post Expert, the CAS Science and Technology Promotion Award, the National Youth Skills Competition Gold Award, Shanghai 35U35, Shanghai May Fourth Medal and other national and provincial-level accolades
      • Corresponding author: zhengli@mail.sim.ac.cn
      • Received Date: 2024-03-15
      • Revised Date: 2024-04-26
      • Available Online: 2024-05-29

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