Kohli / Mittal Developments in Surface Contamination and Cleaning, Volume 7

Cleanliness Validation and Verification
1. Auflage 2014
ISBN: 978-0-323-31145-8
Verlag: Elsevier Science & Techn.
Format: EPUB
Kopierschutz: Adobe DRM (»Systemvoraussetzungen)

E-Book, Englisch, 206 Seiten

As device sizes in the semiconductor industries are shrinking, they become more vulnerable to smaller contaminant particles, and most conventional cleaning techniques employed in the industry are not as effective at smaller scales. The book series Developments in Surface Contamination and Cleaning as a whole provides an excellent source of information on these alternative cleaning techniques as well as methods for characterization and validation of surface contamination. Each volume has a particular topical focus, covering the key techniques and recent developments in the area. The chapters in this Volume address the sources of surface contaminants and various methods for their collection and characterization, as well as methods for cleanliness validation. Regulatory aspects of cleaning are also covered. The collection of topics in this book is unique and complements other volumes in this series. Edited by the leading experts in small-scale particle surface contamination, cleaning and cleaning control, these books will be an invaluable reference for researchers and engineers in R&D, manufacturing, quality control and procurement specification situated in a multitude of industries such as: aerospace, automotive, biomedical, defense, energy, manufacturing, microelectronics, optics and xerography.  - Provides a state-of-the-art survey and best-practice guidance for scientists and engineers engaged in surface cleaning or handling the consequences of surface contamination - Addresses the continuing trends of shrinking device size and contamination vulnerability in a range of industries, spearheaded by the semiconductor industry and others - Includes new regulatory aspects

Autoren/Hrsg.

Kohli, Rajiv

Mittal, Kashmiri L.

Inhaltsverzeichnis

1;Front Cover;1
2;Developments in Surface Contamination and Cleaning: Cleanliness Validation and Verification;4
3;Copyright;5
4;Contents;6
5;Contributors;10
6;Preface;12
7;About the Editors;16
8;Chapter 1: Sources and Generation of Surface Contaminants and Their Impact;18
8.1;1. Introduction;18
8.2;2. Surface Cleanliness Levels;19
8.3;3. Sources and Generation of Contaminants;28
8.3.1;3.1. Particles;32
8.3.2;3.2. Thin Film or Molecular Contamination;37
8.3.3;3.3. Ionic Contamination;39
8.3.4;3.4. Microbial Contamination;41
8.4;4. Impact of Contaminants;44
8.4.1;4.1. Particle Contamination;44
8.4.1.1;4.1.1. Health Effects;48
8.4.2;4.2. Molecular Contamination;50
8.4.3;4.3. Ionic Contamination;51
8.4.4;4.4. Microbial Contamination;53
8.5;5. Summary and Conclusions;55
8.6;Acknowledgments;55
8.7;Disclaimer;55
8.8;References;55
9;Chapter 2: Mid-IR Spectroscopy as a Tool for Cleanliness Validation;68
9.1;1. Background;68
9.2;2. Principles of Grazing-Angle FTIR;70
9.3;3. Description of the Method;71
9.4;4. Advantages and Disadvantages;74
9.4.1;4.1. Direct, Real-Time Method;74
9.4.2;4.2. Detect Anything With An IR Spectrum;75
9.4.3;4.3. Automation;75
9.4.4;4.4. Access to Small Spaces/Flat Surfaces;75
9.5;5. Results and Applications;75
9.5.1;5.1. Aerospace;75
9.5.2;5.2. Manufacturing;76
9.5.3;5.3. Pharmaceutical Applications;77
9.5.4;5.4. Explosives and Chemical Warfare Agents;78
9.5.5;5.5. Tank Trials;79
9.5.6;5.6. IRRAS by Direct Reflectance;80
9.6;6. Future Developments;81
9.7;7. Summary;82
9.8;References;82
10;Chapter 3: Optically Stimulated Electron Emission: A Powerful Tool for Surface Cleanliness Monitoring;86
10.1;1. Introduction;86
10.2;2. OSEE Principle;88
10.2.1;2.1. Resolution;91
10.2.2;2.2. Repeatability and Reproducibility;91
10.2.3;2.3. Calibration;92
10.2.4;2.4. Factors Affecting OSEE;93
10.2.4.1;2.4.1. Short-Term Factors;93
10.2.4.1.1;2.4.1.1. Length of Time the Sample Surface is Exposed to UV Light;93
10.2.4.1.2;2.4.1.2. Distance of the OSEE Sensor from the Surface;95
10.2.4.1.3;2.4.1.3. Line Voltage;95
10.2.4.1.4;2.4.1.4. Ambient Temperature;96
10.2.4.1.5;2.4.1.5. Atmospheric Pressure;96
10.2.4.1.6;2.4.1.6. Sample Not Properly Grounded;97
10.2.4.1.7;2.4.1.7. Surface Finish;97
10.2.4.1.8;2.4.1.8. Air Flow/Turbulence Past the OSEE Sensor;97
10.2.4.1.9;2.4.1.9. Humidity;97
10.2.4.1.10;2.4.1.10. Static Charge;98
10.2.4.2;2.4.2. Long-Term Factors;99
10.2.4.2.1;2.4.2.1. UV Light Intensity;99
10.2.4.2.2;2.4.2.2. Collector Bias Voltage;99
10.3;3. Photoemitting Materials;99
10.3.1;3.1. Substrate Emitting and Contaminant Nonemitting;99
10.3.2;3.2. Substrate Nonemitting and Contaminant Emitting;102
10.3.3;3.3. Both Substrate and Contaminant Emitting;102
10.3.4;3.4. Both Substrate and Contaminant Nonemitting;104
10.4;4. Applications of OSEE;104
10.4.1;4.1. Surface Cleanliness Monitoring;104
10.4.1.1;4.1.1. Establishing Surface Cleanliness Level;105
10.4.1.1.1;4.1.1.1. Selecting an Appropriate Cleanliness Monitoring Technique;105
10.4.1.1.2;4.1.1.2. Establishing Acceptable Level of Cleanliness;106
10.4.1.1.2.1;4.1.1.2.1. Empirical Approach;106
10.4.1.1.2.2;4.1.1.2.2. Quantitative Approach;106
10.4.1.2;4.1.2. Example Applications of Surface Cleanliness Monitoring;107
10.4.1.2.1;4.1.2.1. Prebond Surface Quality;107
10.4.1.2.1.1;4.1.2.1.1. Application 1;107
10.4.1.2.1.2;4.1.2.1.2. Application 2;108
10.4.1.2.1.3;4.1.2.1.3. Application 3;108
10.4.1.2.2;4.1.2.2. Surface Finish;109
10.4.1.2.3;4.1.2.3. Selecting the "Right" Cleaning Process;110
10.4.1.2.4;4.1.2.4. Optimizing a Cleaning Process;110
10.4.1.2.5;4.1.2.5. Contamination Detection on Weld Surfaces;111
10.4.1.2.6;4.1.2.6. Copper Foil Characterization and Cleanliness Testing;111
10.4.1.2.7;4.1.2.7. Inspection for Flux Residue on Electronics Assemblies;112
10.4.1.2.8;4.1.2.8. Detecting of Fingerprints on Beryllium Mirrors;112
10.4.1.2.9;4.1.2.9. Graphite/Epoxy, Composite Skins on Honeycomb Panels;113
10.4.1.2.10;4.1.2.10. Battery Vent Discs;113
10.4.1.2.11;4.1.2.11. Solvent Rinse Cleanliness Verification;113
10.4.1.2.12;4.1.2.12. Steel Surface Oxidation After Pickling;115
10.4.1.2.13;4.1.2.13. Performance Monitoring of an Aqueous Cleaner for Metal Surface Finishing Processes;115
10.4.1.2.14;4.1.2.14. Other Applications;116
10.4.2;4.2. Detecting Absence/Presence of Films/Coatings;117
10.4.2.1;4.2.1. Establishing Acceptance Criteria;117
10.4.2.2;4.2.2. Example Applications;118
10.4.2.2.1;4.2.2.1. Computer Hard Disk Manufacturing;118
10.4.2.2.2;4.2.2.2. Aircraft Industry;118
10.4.2.2.3;4.2.2.3. Automotive Industry;119
10.4.3;4.3. Measuring Thickness of Thin Films/Coatings;119
10.4.3.1;4.3.1. Establishing OSEE versus Thickness Relationship;120
10.4.3.2;4.3.2. Example Applications;121
10.4.3.2.1;4.3.2.1. Computer Hard Disk;121
10.4.3.2.2;4.3.2.2. Welding Wire;122
10.5;5. Summary;122
10.6;References;123
11;Chapter 4: Methods for Verifying Medical Device Cleanliness;126
11.1;1. Background;126
11.2;2. Cleaning Issues and Concerns with Medical Devices;128
11.3;3. Extraction Techniques;130
11.4;4. Cleaning of Metal and Ceramic Components;132
11.5;5. Device Compatibility-Types of Tests and Description;134
11.6;6. Test Methods to Identify Contaminants in Extracts;136
11.6.1;6.1. Chromatographic Analysis;136
11.6.2;6.2. Spectrophotometric Analysis;136
11.6.2.1;6.2.1. Infrared;136
11.6.2.2;6.2.2. Ultraviolet/Visible Spectroscopy;137
11.6.3;6.3. Total Organic Carbon;137
11.6.4;6.4. Gravimetric Analysis;137
11.7;7. Setting Limits and Biological Safety Assessment;137
11.8;8. Validation;139
11.9;9. Sources of Contamination;140
11.10;10. Cleanliness Standards, Nonviable Contamination;141
11.10.1;10.1. Setting Allowable Limits;141
11.10.2;10.2. Extraction and Gravimetric Analysis;142
11.10.3;10.3. Quality Management Systems;142
11.11;11. Future Developments;142
11.12;12. Conclusion;143
11.13;References;144
12;Chapter 5: Cleaning Validation and Its Regulatory Aspects in the Pharmaceutical Industry;146
12.1;1. Introduction;148
12.1.1;1.1. Purpose;149
12.1.2;1.2. Reasons;149
12.1.3;1.3. Contaminant;150
12.1.3.1;1.3.1. Types of Contamination;151
12.2;2. Good Manufacturing Practice in API Manufacturing;151
12.2.1;2.1. Designing the Cleaning Process in Manufacturing Plants;151
12.2.2;2.2. Equipment in the Manufacturing Plant;151
12.2.2.1;2.2.1. Equipment Design Considerations;151
12.2.2.2;2.2.2. Equipment Characteristics;152
12.2.2.3;2.2.3. Construction Materials;152
12.2.2.4;2.2.4. Dedicated and Nondedicated Manufacturing Equipment;152
12.2.3;2.3. Personnel;153
12.2.4;2.4. Heating, Ventilation, and Air Conditioning System;153
12.2.5;2.5. Clothing and Footwear;153
12.3;3. Establishing the Acceptance Limits;153
12.3.1;3.1. Doses;154
12.3.2;3.2. Approaches in Establishing the Acceptable Carryover Quantity;154
12.3.2.1;3.2.1. Approach 1 (Dose Criterion);154
12.3.2.2;3.2.2. Approach 2 (10ppm Criterion);155
12.3.2.3;3.2.3. Approach 3 (Visually Clean Criterion);155
12.3.3;3.3. Limits Based on Medical or Pharmacological Potency of the Product;155
12.3.3.1;3.3.1. The Basis for Quantitative Limits;155
12.3.4;3.4. Limits Based on Toxicity of the Residue;156
12.3.5;3.5. Risk Levels in Cleaning Validation;157
12.3.6;3.6. Use of ACQ for a Level 0 or Level 1 Changeover;158
12.4;4. Cleaning of Equipment;158
12.4.1;4.1. Cleaning Methods;158
12.4.1.1;4.1.1. Types of Residue;158
12.4.2;4.2. Cleaning Mechanisms;158
12.4.2.1;4.2.1. Types of Cleaning Mechanisms;160
12.4.2.1.1;4.2.1.1. Mechanical Action;160
12.4.2.1.2;4.2.1.2. Dissolution;160
12.4.2.1.3;4.2.1.3. Saponification;160
12.4.2.1.4;4.2.1.4. Detergency;161
12.4.2.1.4.1;4.2.1.4.1. Wetting;161
12.4.2.1.4.2;4.2.1.4.2. Emulsification;161
12.4.2.1.5;4.2.1.5. Chemical Reaction;161
12.4.3;4.3. Grouping of Products;162
12.4.4;4.4. Cleaning Process;162
12.4.4.1;4.4.1. Types of Cleaning Processes;162
12.4.5;4.5. Cleaning Porous Equipment;163
12.4.6;4.6. Cleaning Frequency;163
12.4.7;4.7. Product Attributes;164
12.4.7.1;4.7.1. Between Batches of Different Products;164
12.4.7.2;4.7.2. Between Batches of the Same Product;164
12.4.8;4.8. Postcleaning Equipment Storage;164
12.4.9;4.9. Microbiological Considerations;164
12.4.10;4.10. Documentation;165
12.4.11;4.11. Inspection and Sampling Plan;165
12.5;5. Sampling Methods for Cleaning Validation;165
12.5.1;5.1. Swabbing Technique;165
12.5.2;5.2. Rinse Sampling;166
12.5.3;5.3. Placebo Sampling;168
12.5.4;5.4. Microbiological Sampling;168
12.6;6. Cleaning Method Specificity;168
12.6.1;6.1. Recovery in Swab Sampling;168
12.6.1.1;6.1.1. Chemical Recovery from Spiked Swabs;169
12.6.1.2;6.1.2. Recovery from Spiked Plates/Coupons;169
12.6.1.3;6.1.3. Microbial Recovery from Spiked Swabs and Plates/Coupons;169
12.6.2;6.2. Stability Issues in Cleaning Method;169
12.6.2.1;6.2.1. Surface Aging;170
12.6.2.2;6.2.2. Swab Aging;170
12.6.2.3;6.2.3. Timing of Sampling;170
12.6.2.4;6.2.4. Time Between End of Manufacturing to Beginning of Cleaning;170
12.6.2.5;6.2.5. Number of Sample Sites;170
12.6.2.6;6.2.6. Diagram of Sampling Sites;170
12.6.2.7;6.2.7. Microbiological Sampling Sites;170
12.6.2.8;6.2.8. Sample Storage and Identification;171
12.6.2.9;6.2.9. Sampling Documentation: Data Sheet;171
12.7;7. Solvents Used for Cleaning;171
12.7.1;7.1. Builders;172
12.7.2;7.2. Cleaning Cycle;172
12.7.2.1;7.2.1. Prewash;172
12.7.2.2;7.2.2. Alkali Wash;173
12.7.2.3;7.2.3. Postalkali Wash;173
12.7.2.4;7.2.4. Acid Wash;173
12.7.2.5;7.2.5. Final Rinse;173
12.7.2.6;7.2.6. Air Flushing for Storage;173
12.8;8. Cleaning Agents;174
12.8.1;8.1. Grouping of Cleaning Agents;174
12.8.2;8.2. Selection of a Cleaning Agent;175
12.8.3;8.3. Water;175
12.8.4;8.4. Alkaline Agents;175
12.8.4.1;8.4.1. Sodium Hydroxide;176
12.8.4.2;8.4.2. Sodium Hydroxide/Hypochlorite Solutions;176
12.8.5;8.5. Acidic Agents;176
12.8.5.1;8.5.1. Phosphoric Acid;176
12.9;9. Analytical Methods;176
12.9.1;9.1. Specific Methods;178
12.9.2;9.2. Nonspecific Methods;178
12.9.3;9.3. Various Analytical Techniques in Cleaning Validation;179
12.9.3.1;9.3.1. pH;179
12.9.3.2;9.3.2. Conductivity;179
12.9.3.3;9.3.3. Total Organic Carbon;179
12.9.3.4;9.3.4. Enzymatic (Bioluminescence);180
12.9.3.5;9.3.5. Light Microscopy;180
12.9.3.6;9.3.6. Gravimetric Method;180
12.9.3.7;9.3.7. Thin-Layer Chromatography;181
12.9.3.8;9.3.8. Capillary Zone Electrophoresis;181
12.9.3.9;9.3.9. Fourier Transform Infrared Spectroscopy;181
12.9.3.10;9.3.10. Enzyme-Linked Immunosorbent Assay;182
12.9.3.11;9.3.11. Atomic Absorption Spectroscopy;182
12.9.3.12;9.3.12. Ultraviolet Spectrophotometry;183
12.9.3.13;9.3.13. Microbial and Endotoxin Detection and Testing;183
12.10;10. Cleaning Development Phase;183
12.10.1;10.1. Standard Operating Procedures;183
12.10.2;10.2. Operator;184
12.10.3;10.3. Operator Training;184
12.11;11. Cleaning Validation Protocol;185
12.11.1;11.1. A Model Cleaning Validation Protocol;185
12.12;12. Validation Report;194
12.13;13. The FDA Cleaning Validation Guideline;194
12.13.1;13.1. FDA Requirements;195
12.13.2;13.2. Acceptance Criteria;195
12.14;14. Effective Cleaning Validation Maintenance Program;196
12.14.1;14.1. Equipment Cleaning Validation and Maintenance;196
12.14.2;14.2. Overview of Cleaning Validation Program;197
12.14.3;14.3. Cleaning Validation Lifecycle Management;197
12.14.4;14.4. Cleaning Validation Chart;198
12.15;15. Summary;198
12.16;References;199
13;Index;204

Leseproben

Chapter 1 Sources and Generation of Surface Contaminants and Their Impact
Rajiv Kohli    The Aerospace Corporation, NASA Johnson Space Center, Houston, Texas, USA Abstract
Surface contaminants are ubiquitous. The most common types of contamination are particles, molecular contamination, ionic contamination, and microbial contamination. This chapter provides an overview of the sources and generation of these contaminants and discusses some of the impacts of the contaminants. Keywords Contaminants Sources Generation Impact Particles Molecular contamination Microbial contamination Ionic contamination Chapter Outline 1 Introduction   1 2 Surface Cleanliness Levels   2 3 Sources and Generation of Contaminants   11 3.1 Particles   15 3.2 Thin Film or Molecular Contamination   20 3.3 Ionic Contamination   22 3.4 Microbial Contamination   24 4 Impact of Contaminants   27 4.1 Particle Contamination   27 4.1.1 Health Effects   31 4.2 Molecular Contamination   33 4.3 Ionic Contamination   34 4.4 Microbial Contamination   36 5 Summary and Conclusions   38 Acknowledgments   38 Disclaimer   38 References   38 Acknowledgments
The author would like to thank the staff of the STI Library at the Johnson Space Center for help with locating obscure reference articles. 1 Introduction
Contaminants are ubiquitous in nature as by-products of natural processes as well as by-products of human and industrial activities. A contaminant is any material, substance, or energy that is unwanted or adversely affects the product [1]. Surface contamination, the subject of this chapter, can be in many forms and may be present in a variety of states on the surface. For example, typical surface defects on hard disk drive (HDD) components include roughness and wear, flaking, porosity, loose debris, nonvolatile residue (NVR), flash, bloom and inclusions on plastics, burrs and rust on metals, lubricant leakage in ball bearings, packaging debris, and uncured adhesives [2,3]. A particle with dimensions similar to the flying height between the recording head and the disk that is trapped between the head and the disk in a disk drive can cause catastrophic failure of the drive [3–6]. Ionic contaminants also can lead to corrosion of the recording head and failure of the drive [7]. In semiconductor wafer processing, airborne molecular contaminants (AMCs) can cause various defects, such as haze on the wafer surface or introduction of foreign dopants, which can lead to loss of the entire product yield [8–10]. The most common categories of surface contaminants are given below. • Particles such as dust, metals, ceramics, glass, and plastics in the submicrometer to macro size range • Thin film or molecular contamination that can be organic (hydrocarbons) or inorganic (acids gases, bases) • Cationic (such as Na+ and K+) and anionic (such as Cl-, F-, Br-, 3-, 33-, and 43-) contamination • Microbial contamination (bacteria, fungi, and algae). Other contaminant categories include toxic and hazardous chemicals, radioactive materials, and by-products of manufacturing processes, which are identified on surfaces employed in specific industries, such as metals processing, chemical production, nuclear industry, pharmaceutical manufacture, and food processing, handling, and delivery. Energy sources or changes of state, such as light, electric and magnetic fields, heat, and radiation, can also be contaminating. For example, light is usually desirable, but in the photographic film development process, it becomes a contaminant. Magnetic fields can contaminate iron and nickel magnets. Many plastics, when exposed to ultraviolet light, slowly release inert particles due to their degradation. Common contamination sources include machining oils and greases, hydraulic and cleaning fluids, adhesives, waxes, human contamination, and particulates. In addition, a whole host of other chemical contaminants from a variety of sources may also soil a surface. The emphasis in this chapter will be on particles as contaminants deposited on the surface of products manufactured in controlled environments such as clean rooms. Aerosol particles and their behavior will not be considered here. There are numerous references, including books and journals, which address all aspects of aerosols, including single aerosol particles [11–24]. The discussion in this chapter is necessarily an overview of the subject matter and no attempt is made at comprehensiveness. Each of the thousands of references to contamination, cleanliness, and cleaning published each year mentions some aspect of the sources and generation of contaminants, making it nearly impossible to comprehensively treat the subject matter in this chapter. The references cited do provide sources of additional information. 2 Surface Cleanliness Levels
Surface cleaning specifications are typically based on the amount of specific or characteristic contaminant remaining on the surface after it has been cleaned. Space agencies worldwide specify surface precision cleanliness levels for space hardware by particle size (in the micrometer (µm) size range) and number of particles, as well by film contamination represented by NVR [25,26]. The cleanliness levels are based on contamination levels established in industry standard IEST-STD-CC1246D (which replaced the original cleanliness standard MIL-STD-1246 [27]) for particles from Level 1 to Level 1000 and for NVR from Level AA5 (10 ng/0.1 m2) to Level J (25 mg/0.1 m2) as shown in Table 1.1 [28]. The cleanliness levels have been revised or redesignated in revision E of this standard [29]. The maximum allowable number of particles for each particle size range has been rounded in revision E, while the NVR designation levels have been replaced with a single letter R followed by the maximum allowable mass of NVR. For example, former NVR level J has the new designation R25; level A/2 is now R5E-1; and level AA5 is now R1E-5. However, this revision has not yet been officially adopted by the space agencies. Table 1.2 lists the surface cleanliness levels for particle contamination in revision E of IEST-STD-CC1246. Table 1.3 compares NVR contamination designation levels between revisions D and E of the standard. Table 1.1 Product Surface Cleanliness Levels for Commercial and Noncommercial Applications Defined in IEST-STD-CC1246 Revision D...