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Semiconductor Measurement Technology 1> NBS SPECIAL PUBLICATION 400 U.S. DEPARTMENT OF COMMERCE / National Bureau of Standards I feurement Technology lugicdd iu:|juiy October 1, 1976 to March 31, 19771 NATIONAL BUREAU OF STANDARDS The National Bureau of Standards' was established by an act ot Congress on March 3, 1901. The Bureau's overall goal is to strengthen and advance the Nation's science and technology and facilitate their effective application for public benefit. To this end, the Bureau conducts research and provides: (1) a basis for the Nation's physical measurement system, (2) scientific and technological services for industry and government, (3) a technical basis for equity in trade, and (4) technical services to promote public safety. The Bureau's technical work is per- formed by the National Measurement Laboratory, the National Engineering Laboratory, and the Institute for Computer Sciences and Technology. THE NATIONAL MEASUREMENT LABORATORY provides the national system of physical and chemical and materials measurement; coordinates the system with measurement systems of other nations and furnishes essential services leading to accurate and uniform physical and chemical measurement throughout the Nation's scientific community, industry, and commerce; conducts materials research leading to improved methods of measurement, standards, and data on the properties of materials needed by industry, commerce, educational institutions, and Government; provides advisory and research services to other Government agencies; develops, produces, and distributes Standard Reference Materials; and provides calibration services. The Laboratory consists of the following centers: Absolute Physical Quantities' — Radiation Research — Thermodynamics and Molecular Science — Analytical Chemistry — Materials Science. THE NATIONAL ENGINEERING LABORATORY provides technology and technical ser- vices to the public and private sectors to address national needs aad to solve national problems; conducts research in engineering and applied science in support of these efforts; builds and maintains competence in the necessary disciplines required to carry out this research and technical service; develops engineering data and measurement capabilities; provides engineering measurement traceability services; develops test methods and proposes engineering standards and code changes; develops and proposes new engineering practices; and develops and improves mechanisms to transfer results of its research to the ultimate user. The Laboratory consists of the following centers: Applied Mathematics — Electronics and Electrical Engineering- — Mechanical Engineering and Process Technology' — Building Technology — Fire Research — Consumer Product Technology — Field Methods. THE INSTITUTE FOR COMPUTER SCIENCES AND TECHNOLOGY conducts research and provides scientific and technical services to aid Federal agencies in the selection, acquisition, application, and use of computer technology to improve effectiveness and economy in Government operations in accordance with Public Law 89-306 (40 U.S.C. 759), relevant Executive Orders, and other directives; carries out this mission by managing the Federal Information Processing Standards Program, developing Federal ADP standards guidelines, and managing Federal participation in ADP voluntary standardization activities; provides scientific and technological advisory services and assistance to Federal agencies; and provides the technical foundation for computer-related policies of the Federal Government. The Institute consists of the following centers: Programming Science and Technology — Computer Systems Engineering. 'Headquarters and Laboratories at Gaithersburg, MD, unless otherwise noted; mailing address Washington, DC 20234. -Some divisions within the center are located at Boulder, CO 80303. Semiconductor Measurement Technology October 1, 1976 to March 31, 1977 W. Murray Bullis, Editor Electron Devices Division Center for Electronics and Electrical Engineering National Engineering Laboratory National Bureau of Standards Washington, D.C. 20234 Jointly supported by: The National Bureau of Standards The Navy Strategic Systems Projects Office The Defense Nuclear Agency The Defense Advanced Research Projects Agency The Energy Research and Development Administration, and The Naval Ocean Systems Center U.S. DEPARTMENT OF COMMERCE Luther H. Hodges, Jr., Under Secretary Jordan J. Baruch, Assistant Secretary for Science and Technology NATIONAL BUREAU OF STANDARDS, Ernest Ambler, Director Issued November 1979 National Bureau of Standards Special Publication 400-38 Nat. Bur. Stand. (U.S.), Spec. Publ. 400-38, 95 pages (Nov. 1979) CODEN: XNBSAV U.S. GOVERNMENT PRINTING OFFICE WASHINGTON: 1979 For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, D.C. 20402 Stock No. 003-003-02139-3 Price $3.50 (Add 25 percent additional for other than U.S. mailing). li- U.S. GOVERNMENT PRINTING OFFICE: 1979 O— 311-065 (272) TABLE OF C 0 E NT S SEMICONDUCTOR MEASUREMENT TECHNOLOGY PAGE List of Figures iv List of Tables vii Preface viii Abstract and Key Words 1 1. Introduction 1 2. Highlights 2 3. Materials Characterization by Electrical Methods 6 3.1. Photovoltaic Method 6 3.2. Thermally Stimulated Current and Capacitance Measurements .... 10 3.3. Indium-Doped Silicon 15 4. Materials Characterization by Physical Analysis Methods 17 4.1. Electron Spectroscopy Techniques 17 4.2. Techniques for Chemical Diagnostics in Semiconductor Processing 20 4.3. Optical Test for Surface Quality of Sapphire Substrates 22 5. Materials and Procedures for Wafer Processing 25 5.1. Sodium Contamination in Oxidation Furnaces 25 6. Photolithography 26 6.1. Calibration Standards for Optical Photomask Line-Width Measurements 26 6.2. Optical Line-Width Measurements on Silicon and Iron-Oxide Photomasks 28 6.3. Optical Line-Width Measurements in Reflected Light 32 6.4. Submicrometer Line-Width Measurements 35 6.5. Primary Line-Width Calibration 39 7. Test Patterns 43 7.1. Test Patterns for Resistivity-Dopant Density Evaluation 43 7.2. Sheet Resistor Test Structures 43 7.3. Overetch Structure for Visual Measurement 48 7.4. Test Pattern Design Concepts 49 7.5. Probe Pad Evaluation 52 7.6. Computer Aided Design and Layout of Test Pattern Photomasks 53 7.7. Advanced Planar Silicon Test Structures 54 7.8. Test Pattern Design and Analysis for SOS/LSI 56 8. Assembly and Packaging 61 8.1. Radioisotope Leak Test 61 9. Device Inspection and Test 65 9.1. Scanning Acoustic Microscopy 65 9.2. Integrated Circuit Die Attachment Evaluation 70 9.3. Transistor Collector-Emitter Saturation Voltage 72 10. References 75 Appendix A Semiconductor Technology Program Staff 78 Appendix B Semiconductor Technology Program Progress Reports 79 Appendix C Computation of Dark-Field Line Images 81 iii LIST OF FIGURES PAGE 1. Photograph of probe holder with point contacts for photovoltaic scanning apparatus 6 2. Examples of radial resistivity profiles measured on 2-in. diameter, n-type, float-zoned silicon slices with photovoltaic and four-probe methods 7 | 3. Results of repeatability study of photovoltaic method for measuring radial resistivity profiles 8 | 4. Schematic diagram of specimen geometry used for analysis of photovoltaic method for measuring radial resistivity variation 9 5. Typical thermally stimulated capacitance and current responses of a gold-doped i n+p diode 11 ' 6. Wafer maps of gold donor and boron acceptor densities in a 2-in. diameter sili- ' con wafer 12 7. Mesa diode fabrication process 13 8. Photomicrograph of typical ultrasonically formed mesa diode 13 9. Photomicrograph of typical plasma-etched mesa diode 13 j' 10. Postulated mesa-diode fabrication process using five-level photomask set .... 14 ' 11. Resistance of an indium-doped silicon specimen at 77 K as a function of added donor concentration 16 12. Computed signal obtained from a step interface with an Auger electron spectrome- ter with a cylindrical mirror analyzer 18 • 13. Oxygen concentration profile in MNOS structure 18 14. Oxygen KLL and silicon LVV signals as a function of distance near the interface between silicon dioxide and silicon 19 15. Model for silicon-silicon dioxide interface 19 16. Diagram of variable speed spinner for controlled wet chemical etching 21 17. The oxygen-to-silicon ratio in a silicon-dioxide film as a function of distance from the oxide-silicon interface 22 18. Example of data enhancement techniques 22 19. Correlation of SOS MOSFET channel current with infrared reflectance data of | corresponding sapphire substrates 23 20. Correlation of gated Hall mobility of SOS structures with infrared reflectance data of corresponding sapphire substrates 23 21. Correlation of SOS MOSFET channel current with ultraviolet reflectance data of corresponding epitaxial silicon films 24 22. Correlation of gated Hall mobility of SOS structures with ultraviolet reflec- tance data of corresponding epitaxial silicon films 24 I Iv LIST OF FIGURES PAGE 23. A view of a pattern group on the chromium-on-glass line-width measurement artifact 26 , 24. Computed image profiles of a 2-pm clear line for an objective lens with numerical aperture of 0.90 and various condenser and 30 i lenses phase shifts .... 25. Schematic illustration showing method of computing threshold at edge with phase shift present 31 j 26. Schematics of optical microscope systems 33 27. Theoretical dark-field image of clear lines for 0.60 objective N.A. and 0.80 to 0.95 condenser N.A 34 28. Theoretical calibration curve for dark-field illumination, line width
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