MIL-HDBK-17-1F Volume 1,Chapter 6 Lamina,Laminate,and Special Form Characterization CHAPTER 6 LAMINA,LAMINATE,AND SPECIAL FORM CHARACTERIZATION 6.1 INTRODUCTION The use of composite materials continues to increase as new performance,reliability,and durability requirements drive hardware designs to higher levels of structural efficiency.Additionally,government requirements are becoming more stringent to ensure proper levels of structural integrity are maintained. These design drivers,among others,have resulted in a growing recognition that certification or qualifica- tion of aerospace structure requires an extensive combination of analysis,testing,and documentation. Further,because of the large number of design variables inherent to composite structure,analytic models are even more necessary than for metallic structure to ensure completeness of the hardware qualification process.Inherent in all structural analysis models are material,physical,and mechanical property characterization data.Ideally,these analytic models would permit analysts to predict full-scale structural response (e.g.stability,deflections,strength,life)directly from a generic (lamina)material data- base.In truth,test data is required at design development(element,subcomponent,component)and full- scale article test levels as well as the generic(coupon)levels of evaluation. The purpose of Chapter 6 is to provide guidelines of testing procedures for characterization of physi- cal and mechanical lamina(ply)and laminate properties. A laminate is a product made by bonding together two or more layers of material or materials,and a lamina is a single ply or layer in a laminate.The material forming each layer typically consists of a car- bon,glass,or organic (polymeric)fiber reinforcement embedded in a thermoplastic or thermosetting resin matrix.While retaining their identities in the composite,the constituents combine to provide specific characteristics and properties. Many techniques are used to characterize the chemical,physical,and mechanical properties of com- posite materials.The purpose of this chapter is to provide information on techniques that may be used to analyze and evaluate these properties.The test methods discussed in each section may not be appro- priate for all types of composite materials.Currently,more studies are being conducted to investigate how variations in reinforcement and resin chemistry and morphology may affect the physical properties and long term performance of composites.Where possible,the limitations of existing test methods are discussed. 6.2 SPECIMEN PREPARATION 6.2.1 Introduction This section provides general recommendations for the fabrication and preparation of the test speci- mens detailed in this document.These recommendations cover specimen traceability,test article'fabri- cation,specimen location,configuration,and machining. The validity of material properties used in design of structure is dependent on the quality of the specimens being tested.If the objective of the testing is to provide comparative information of different materials,it is crucial that variability due to specimen preparation be kept to a minimum.If the data being generated are intended to be used to generate allowables,the goal is to reflect the interaction of the base material and processing which is expected to occur in production.In either case care must be taken in the specimen preparation process to minimize the variation which naturally occurs during the process. Specimen fabrication should be performed in compliance to ASTM D 5687(Standard Guide for Prepara- tion of Flat Composite Panels with Processing Guidelines for Specimen Preparation).Even test articles that are not flat can benefit from the ASTM guide. 1A test article is any construction from which individual specimens are extracted.Such a test article may be a flat panel fabricated specifically to develop material properties,or it may be a production part set aside for test purposes. 6-1
MIL-HDBK-17-1F Volume 1, Chapter 6 Lamina, Laminate, and Special Form Characterization 6-1 CHAPTER 6 LAMINA, LAMINATE, AND SPECIAL FORM CHARACTERIZATION 6.1 INTRODUCTION The use of composite materials continues to increase as new performance, reliability, and durability requirements drive hardware designs to higher levels of structural efficiency. Additionally, government requirements are becoming more stringent to ensure proper levels of structural integrity are maintained. These design drivers, among others, have resulted in a growing recognition that certification or qualification of aerospace structure requires an extensive combination of analysis, testing, and documentation. Further, because of the large number of design variables inherent to composite structure, analytic models are even more necessary than for metallic structure to ensure completeness of the hardware qualification process. Inherent in all structural analysis models are material, physical, and mechanical property characterization data. Ideally, these analytic models would permit analysts to predict full-scale structural response (e.g. stability, deflections, strength, life) directly from a generic (lamina) material database. In truth, test data is required at design development (element, subcomponent, component) and fullscale article test levels as well as the generic (coupon) levels of evaluation. The purpose of Chapter 6 is to provide guidelines of testing procedures for characterization of physical and mechanical lamina (ply) and laminate properties. A laminate is a product made by bonding together two or more layers of material or materials, and a lamina is a single ply or layer in a laminate. The material forming each layer typically consists of a carbon, glass, or organic (polymeric) fiber reinforcement embedded in a thermoplastic or thermosetting resin matrix. While retaining their identities in the composite, the constituents combine to provide specific characteristics and properties. Many techniques are used to characterize the chemical, physical, and mechanical properties of composite materials. The purpose of this chapter is to provide information on techniques that may be used to analyze and evaluate these properties. The test methods discussed in each section may not be appropriate for all types of composite materials. Currently, more studies are being conducted to investigate how variations in reinforcement and resin chemistry and morphology may affect the physical properties and long term performance of composites. Where possible, the limitations of existing test methods are discussed. 6.2 SPECIMEN PREPARATION 6.2.1 Introduction This section provides general recommendations for the fabrication and preparation of the test specimens detailed in this document. These recommendations cover specimen traceability, test article1 fabrication, specimen location, configuration, and machining. The validity of material properties used in design of structure is dependent on the quality of the specimens being tested. If the objective of the testing is to provide comparative information of different materials, it is crucial that variability due to specimen preparation be kept to a minimum. If the data being generated are intended to be used to generate allowables, the goal is to reflect the interaction of the base material and processing which is expected to occur in production. In either case care must be taken in the specimen preparation process to minimize the variation which naturally occurs during the process. Specimen fabrication should be performed in compliance to ASTM D 5687 (Standard Guide for Preparation of Flat Composite Panels with Processing Guidelines for Specimen Preparation). Even test articles that are not flat can benefit from the ASTM guide. 1 A test article is any construction from which individual specimens are extracted. Such a test article may be a flat panel fabricated specifically to develop material properties, or it may be a production part set aside for test purposes
MIL-HDBK-17-1F Volume 1,Chapter 6 Lamina,Laminate,and Special Form Characterization 6.2.2 Traceability All specimens should be traceable to the material batch,lot,roll,process and test article.The re- questing organization may choose to require traceability of each specimen to its location within the test article. The specification,or purchasing paperwork,should require batch,lot,roll traceability and lot accep- tance test information.It is recommended that when uncured material is purchased it be required that all available traceability information,including vendor certifications and material receiving inspection data of acceptance test results,be delivered with the material.The organization conducting the investigation should review the information to ensure there is enough traceability information to proceed with test arti- cle and specimen fabrication. All prepreg material that is stored before fabrication should have a storage history record.Information such as accumulated time in and out of refrigeration should be recorded. For the test article,the prepreg batch number,lot number,roll number,and processing information should be recorded.Another piece of information which needs to be maintained throughout specimen fabrication is ply orientation.One method by which this may be accomplished is through the use of a wit- ness line.as discussed in the next section. 6.2.3 Test article fabrication The following is a list of important items that should be considered when fabricating test articles: a.Test articles should be built according to engineering drawing requirements or sketches.The drawing requirements or sketches should specify:ply materials,test article reference orientation, ply orientation,material and process specifications or equivalent process document,and inspec- tion requirements. b.Vital material and process identification,such as prepreg batch number,lot number,roll number, autoclave run,press,or other consolidation method and lay-up stacking sequence,should be re- corded.This information is stored to maintain traceability of the test articles.This same traceabil- ity should be maintained on any excess material left after the specimens have been removed. c.The test article identification code and witness line should be permanently identified on each test article.A witness line should be established on the fabrication tool to act as a reference to the fi- ber orientation on the test article.For hand lay-up methods a witness line which will be main- tained during the lay-up and curing process must be identified as the reference orientation.The angular tolerance between the plies put down and this line depends on the processing specifica- tion by which the material is being processed.In automated processes some other method of es- tablishing the reference orientation must be established.Once established,the witness line should be transferred to the test article,and maintained throughout specimen extraction. d.It is generally recommended that for cured test articles at least 1 in.(25 mm)of material be trimmed from the edges.One of the machined edges of the test article may be used to perma- nently maintain the reference orientation on the article. e.The requesting organization (or if required,the appropriate quality assurance organization) should inspect test articles.This inspection should be done before the specimens are fabricated to ensure they meet all requirements in the controlling process specification or appropriate equivalent document.If the test article does not meet all requirements,the requesting organiza- tion and,when applicable,the customer representative,should provide the final disposition of the test article. 6-2
MIL-HDBK-17-1F Volume 1, Chapter 6 Lamina, Laminate, and Special Form Characterization 6-2 6.2.2 Traceability All specimens should be traceable to the material batch, lot, roll, process and test article. The requesting organization may choose to require traceability of each specimen to its location within the test article. The specification, or purchasing paperwork, should require batch, lot, roll traceability and lot acceptance test information. It is recommended that when uncured material is purchased it be required that all available traceability information, including vendor certifications and material receiving inspection data of acceptance test results, be delivered with the material. The organization conducting the investigation should review the information to ensure there is enough traceability information to proceed with test article and specimen fabrication. All prepreg material that is stored before fabrication should have a storage history record. Information such as accumulated time in and out of refrigeration should be recorded. For the test article, the prepreg batch number, lot number, roll number, and processing information should be recorded. Another piece of information which needs to be maintained throughout specimen fabrication is ply orientation. One method by which this may be accomplished is through the use of a witness line, as discussed in the next section. 6.2.3 Test article fabrication The following is a list of important items that should be considered when fabricating test articles: a. Test articles should be built according to engineering drawing requirements or sketches. The drawing requirements or sketches should specify: ply materials, test article reference orientation, ply orientation, material and process specifications or equivalent process document, and inspection requirements. b. Vital material and process identification, such as prepreg batch number, lot number, roll number, autoclave run, press, or other consolidation method and lay-up stacking sequence, should be recorded. This information is stored to maintain traceability of the test articles. This same traceability should be maintained on any excess material left after the specimens have been removed. c. The test article identification code and witness line should be permanently identified on each test article. A witness line should be established on the fabrication tool to act as a reference to the fiber orientation on the test article. For hand lay-up methods a witness line which will be maintained during the lay-up and curing process must be identified as the reference orientation. The angular tolerance between the plies put down and this line depends on the processing specification by which the material is being processed. In automated processes some other method of establishing the reference orientation must be established. Once established, the witness line should be transferred to the test article, and maintained throughout specimen extraction. d. It is generally recommended that for cured test articles at least 1 in. (25 mm) of material be trimmed from the edges. One of the machined edges of the test article may be used to permanently maintain the reference orientation on the article. e. The requesting organization (or if required, the appropriate quality assurance organization) should inspect test articles. This inspection should be done before the specimens are fabricated to ensure they meet all requirements in the controlling process specification or appropriate equivalent document. If the test article does not meet all requirements, the requesting organization and, when applicable, the customer representative, should provide the final disposition of the test article
MIL-HDBK-17-1F Volume 1,Chapter 6 Lamina,Laminate,and Special Form Characterization 6.2.4 Specimen fabrication The following is a list of important items that should be considered when fabricating specimens. a. Specimens should be extracted from test articles in the region that meets all process,engineering drawing,and specimen drawing requirements. b. Specimens should be located on the test article according to the cutting diagram provided by the re- questing organization.If a test article does not pass the inspection criteria,the requesting organiza- tion may choose to cut specimens relative to identified test article defects to make the effect of the de- fects on the specimen response representative of the full-scale item. NOTE:When defining specimen locations,allow for material removed in the cutting operation. c.A specimen identification code should be defined in the test plan,referenced in the test instructions, and recorded in the data sheets.The specimen identification code should be permanently marked on each specimen.Care should be taken to keep the code outside the failure area of the specimen. d.For specimens too small to mark the complete code,mark only the unique serial number on the specimen.It is recommended that care be taken to place small specimens in bags properly labeled with that specimen's full identification. e.If it is required that the location of the specimen on the test article be known,specimens should be labeled before being extracted.This labeling should allow all specimen and excess material locations to be known after cutting. f.The reference edge of the specimen should be aligned within the specified orientation using the wit- ness line.In instances where a smaller subtest article is machined and used to make several speci- mens at once,a reference line or edge should be transferred to this subtest article from the witness line.This transferred line should be orientated within t0.25 with respect to the witness line. g.Before cutting,the specimen location and orientation should be verified by the requesting organiza- tion or an independent reviewer. h.Specimens should be extracted from the fabricated test articles according to the appropriate machin- ing procedure as specified.Specimens may be machined with a variety of machining tools.In gen- eral the final cutting tool should have a fine grit,be hardened,and run at a high tool speed without wobble.The cut itself should be executed to minimize excess heating of the laminate. i.The added cost and manufacturing associated with tabbed specimens should be considered when selecting specimen type.The limitations and problems associated with the tabbing of specimens is stated in each individual test method.If bonded tabs are required.the cure of the adhesive should be evaluated to determine if it is compatible with the composite system and tab material(if different).If the tab configuration produced in the bonding process is not within the geometry requirements of the specimen configuration,further machining of the tabs may be required. j.Holes in specimens should be drilled in accordance to the applicable process specification. k.Any fasteners that are required should be installed in accordance to the applicable process specifica- tion. 1.Completed specimens should be inspected prior to testing to ensure conformance with the standards being used.Variations in individual specimen thickness should be within the applicable test method tolerances.Larger variations may cause improper loading when used with close tolerance test fix- tures.These variations may indicate that the specimen was fabricated improperly (e.g.,ply drop-off or resin bleed). 6-3
MIL-HDBK-17-1F Volume 1, Chapter 6 Lamina, Laminate, and Special Form Characterization 6-3 6.2.4 Specimen fabrication The following is a list of important items that should be considered when fabricating specimens. a. Specimens should be extracted from test articles in the region that meets all process, engineering drawing, and specimen drawing requirements. b. Specimens should be located on the test article according to the cutting diagram provided by the requesting organization. If a test article does not pass the inspection criteria, the requesting organization may choose to cut specimens relative to identified test article defects to make the effect of the defects on the specimen response representative of the full-scale item. NOTE: When defining specimen locations, allow for material removed in the cutting operation. c. A specimen identification code should be defined in the test plan, referenced in the test instructions, and recorded in the data sheets. The specimen identification code should be permanently marked on each specimen. Care should be taken to keep the code outside the failure area of the specimen. d. For specimens too small to mark the complete code, mark only the unique serial number on the specimen. It is recommended that care be taken to place small specimens in bags properly labeled with that specimen’s full identification. e. If it is required that the location of the specimen on the test article be known, specimens should be labeled before being extracted. This labeling should allow all specimen and excess material locations to be known after cutting. f. The reference edge of the specimen should be aligned within the specified orientation using the witness line. In instances where a smaller subtest article is machined and used to make several specimens at once, a reference line or edge should be transferred to this subtest article from the witness line. This transferred line should be orientated within ±0.25° with respect to the witness line. g. Before cutting, the specimen location and orientation should be verified by the requesting organization or an independent reviewer. h. Specimens should be extracted from the fabricated test articles according to the appropriate machining procedure as specified. Specimens may be machined with a variety of machining tools. In general the final cutting tool should have a fine grit, be hardened, and run at a high tool speed without wobble. The cut itself should be executed to minimize excess heating of the laminate. i. The added cost and manufacturing associated with tabbed specimens should be considered when selecting specimen type. The limitations and problems associated with the tabbing of specimens is stated in each individual test method. If bonded tabs are required, the cure of the adhesive should be evaluated to determine if it is compatible with the composite system and tab material (if different). If the tab configuration produced in the bonding process is not within the geometry requirements of the specimen configuration, further machining of the tabs may be required. j. Holes in specimens should be drilled in accordance to the applicable process specification. k. Any fasteners that are required should be installed in accordance to the applicable process specification. l. Completed specimens should be inspected prior to testing to ensure conformance with the standards being used. Variations in individual specimen thickness should be within the applicable test method tolerances. Larger variations may cause improper loading when used with close tolerance test fixtures. These variations may indicate that the specimen was fabricated improperly (e.g., ply drop-off or resin bleed)
MIL-HDBK-17-1F Volume 1,Chapter 6 Lamina,Laminate,and Special Form Characterization 6.3 CONDITIONING AND ENVIRONMENTAL EXPOSURE 6.3.1 Introduction Conditioning is the process of exposure of material to a potentially property-altering environment prior to subsequent test.'This section focuses on conditioning of materials subjected to moisture exposure (immersion in all types of fluids,but especially humid air).There are,of course,many other types of con- ditioning environments.An incomplete list includes:subambient(moderately low temperatures),cryo- genic(very low temperatures),elevated temperature(dry),oxidizing,low-Earth orbit simulation(including exposure to monatomic oxygen),and exposure to various types of radiation.Conditioning issues in these other environments will not be explicitly discussed in this section.A related,but much more difficult,ex- tension of material conditioning is associated with the issue of long-term aging(for example,10,000 to 80,000 or more hours of exposure).which for practical engineering purposes requires development of procedures for accelerated conditioning.While some very limited and restricted guidelines for accelera- tion of basic moisture conditioning are discussed in the following subsections,acceleration of long-term aging processes is a state-of-the-art topic that is beyond the scope of this section. Most polymeric materials,whether unreinforced resin,polymeric composite matrix,or a polymer- based fiber,are capable of absorbing relatively small but potentially significant amounts of moisture from the surrounding environment.The physical mechanism for moisture mass change,assuming there are no cracks or other wicking paths,is generally assumed to be mass diffusion following Fick's Law(the moisture analog to thermal diffusion is discussed in Section 6.4.8).Fickian moisture diffusion into or out of the interior occurs relatively slowly;many orders of magnitude slower than heat flow in thermal diffu- sion.Nevertheless,given enough exposure-time in a moist environment,a significant amount of moisture may be absorbed into the material.This absorbed moisture may cause material swelling,and,particularly at higher temperatures,may soften and weaken the matrix and matrix/fiber interface,which is deleterious to many mechanical properties that are often design drivers for structural applications.Absorbed mois- ture effectively lowers the maximum use temperature of the material(see Sections 2.2.7 and 2.2.8).The effect is demonstrated by a lowering of the glass transition temperature(thus the particular interest in Ts test results) The two main types of basic moisture conditioning of materials are:fixed-time conditioning,where a material specimen is exposed to a conditioning environment for a specified period of time;and equilibrium conditioning,where a specimen is exposed until the material reaches equilibrium with the conditioning environment.While fixed-time conditioning is still in common use when screening materials,it usually results in a material condition that is substantially non-uniform through the thickness;subsequent test re- sults are,therefore,considered only a qualitative assessment rather than a quantitative result.Except for certain screening-level purposes,or as part of application-specific structural-level tests.fixed-time condi- tioning as summarized in Section 6.3.2 is not considered sufficient or representative;only equilibrium conditioning as discussed in Section 6.3.3 provides a true assessment of comparable material response. When absorbed moisture is a potential design concern,a material testing program should evaluate both the moisture absorption material properties(diffusion rate and equilibrium content)and the effect of absorbed moisture on key design properties after equilibrium moisture exposure.An ASTM moisture ab- sorption conditioning/material property test method,ASTM D 5229/D 5229M(Reference 6.3.1),has been created to define the conditioning parameters and procedures needed to assure that uniform through- 'Nonambient testing is another subject,and,for mechanical testing,is covered in Section 6.5.3. While certain polymers,like polybutadiene,resist water vapor absorption to the point that humidity conditioning may not be re- quired,these materials are still considered rare exceptions.On the other hand,most reinforcements,including those of the carbon glass,metallic,and ceramic fiber families,are not hygroscopic.As a result,except for polymeric fibers like aramid,it is usually as- sumed that any water vapor absorption is limited to the polymer matrix. 6-4
MIL-HDBK-17-1F Volume 1, Chapter 6 Lamina, Laminate, and Special Form Characterization 6-4 6.3 CONDITIONING AND ENVIRONMENTAL EXPOSURE 6.3.1 Introduction Conditioning is the process of exposure of material to a potentially property-altering environment prior to subsequent test.1 This section focuses on conditioning of materials subjected to moisture exposure (immersion in all types of fluids, but especially humid air). There are, of course, many other types of conditioning environments. An incomplete list includes: subambient (moderately low temperatures), cryogenic (very low temperatures), elevated temperature (dry), oxidizing, low-Earth orbit simulation (including exposure to monatomic oxygen), and exposure to various types of radiation. Conditioning issues in these other environments will not be explicitly discussed in this section. A related, but much more difficult, extension of material conditioning is associated with the issue of long-term aging (for example, 10,000 to 80,000 or more hours of exposure), which for practical engineering purposes requires development of procedures for accelerated conditioning. While some very limited and restricted guidelines for acceleration of basic moisture conditioning are discussed in the following subsections, acceleration of long-term aging processes is a state-of-the-art topic that is beyond the scope of this section. Most polymeric materials, whether unreinforced resin, polymeric composite matrix, or a polymerbased fiber, are capable of absorbing relatively small but potentially significant amounts of moisture from the surrounding environment.2 The physical mechanism for moisture mass change, assuming there are no cracks or other wicking paths, is generally assumed to be mass diffusion following Fick’s Law (the moisture analog to thermal diffusion is discussed in Section 6.4.8). Fickian moisture diffusion into or out of the interior occurs relatively slowly; many orders of magnitude slower than heat flow in thermal diffusion. Nevertheless, given enough exposure-time in a moist environment, a significant amount of moisture may be absorbed into the material. This absorbed moisture may cause material swelling, and, particularly at higher temperatures, may soften and weaken the matrix and matrix/fiber interface, which is deleterious to many mechanical properties that are often design drivers for structural applications. Absorbed moisture effectively lowers the maximum use temperature of the material (see Sections 2.2.7 and 2.2.8). The effect is demonstrated by a lowering of the glass transition temperature (thus the particular interest in Tg test results). The two main types of basic moisture conditioning of materials are: fixed-time conditioning, where a material specimen is exposed to a conditioning environment for a specified period of time; and equilibrium conditioning, where a specimen is exposed until the material reaches equilibrium with the conditioning environment. While fixed-time conditioning is still in common use when screening materials, it usually results in a material condition that is substantially non-uniform through the thickness; subsequent test results are, therefore, considered only a qualitative assessment rather than a quantitative result. Except for certain screening-level purposes, or as part of application-specific structural-level tests, fixed-time conditioning as summarized in Section 6.3.2 is not considered sufficient or representative; only equilibrium conditioning as discussed in Section 6.3.3 provides a true assessment of comparable material response. When absorbed moisture is a potential design concern, a material testing program should evaluate both the moisture absorption material properties (diffusion rate and equilibrium content) and the effect of absorbed moisture on key design properties after equilibrium moisture exposure. An ASTM moisture absorption conditioning/material property test method, ASTM D 5229/D 5229M (Reference 6.3.1), has been created to define the conditioning parameters and procedures needed to assure that uniform through- 1 Nonambient testing is another subject, and, for mechanical testing, is covered in Section 6.5.3. 2 While certain polymers, like polybutadiene, resist water vapor absorption to the point that humidity conditioning may not be required, these materials are still considered rare exceptions. On the other hand, most reinforcements, including those of the carbon, glass, metallic, and ceramic fiber families, are not hygroscopic. As a result, except for polymeric fibers like aramid, it is usually assumed that any water vapor absorption is limited to the polymer matrix
MIL-HDBK-17-1F Volume 1,Chapter 6 Lamina,Laminate,and Special Form Characterization thickness equilibrium'is obtained during conditioning.ASTM D 5229/D 5229M also defines how to de- termine the moisture absorption properties,and its use for this purpose is discussed in more detail in Sec- tion6.6.8. 6.3.2 Fixed-time conditioning As stated above,fixed-time conditioning is only of limited usefulness2,it cannot generally provide the desired uniform moisture condition through the thickness of the material.The shortcomings of the fixed- time approach are illustrated in Figure 6.3.2 for a simulated 30-day exposure of IM6/3501-6 carbon/epoxy at 140F(60C)and 95%RH.Using known values for moisture diffusivity and moisture equilibrium con- tent,the calculated average moisture content of various laminate thicknesses is plotted and shown as a smooth curve.From this curve,it can be seen that the maximum laminate thickness that can reach equi- librium at this temperature during this fixed,though fairly lengthy,conditioning exposure,is 0.035 in.(0.89 mm).For greater thicknesses,the moisture distribution through the thickness will not be uniform,as the interior moisture levels will be below equilibrium moisture content.This is further illustrated by an exam- ple in Section 6.3.3. SPECIMEN THICKNESS (mm) 0.0 1.0 2.03.0 4.0 5.0 6.0 7.0 2.00 1.80 1.60 1.40 1.20 1.00 0.80 0.60 0.40 0.20 0.00 0.00 0.05 0.100.15 0.20 0.25 0.30 SPECIMEN THICKNESS (in) FIGURE 6.3.2 Two-sided moisture absorption of carbon/epoxy laminate after 30 days exposure at 140F(60C)/95%RH. As will be discussed in Section 6.3.3.1,with lower target relative humidity levels,it is common to try to accelerate conditioning by subjecting the material to a higher relative humidity level for a shorter period of time.The objective is to introduce the same average moisture content in the material as would be seen in equilibrium conditioning at the lower relative humidity level,although the distribution of moisture content distribution will be less uniform through the thickness.Using a single-humidity level,fixed-time condition- ing example,again illustrated by Figure 6.3.2,equilibrium at 78%RH(1.2%equilibrium moisture content for this material)can be approximated only at a thickness of 0.070 in.(1.8 mm).For a thickness greater than 0.070 in.(1.8 mm),the average moisture content will be insufficient,and for a thickness less than The discussion focuses on through the thickness moisture absorption;however,in-plane moisture absorption will locally dominate near edges,and may even dominate the overall absorption process in those cases where edge area is a substantial portion of the total exposed area. 2Examples of fixed-time conditioning methods that should specifically be avoided include:ASTM D 618(Reference 6.3.2(a)),ASTM D 570(Reference 6.3.2(b)),and SACMA RM 11-88 Method I(Reference 6.3.2(c)). 6-5
MIL-HDBK-17-1F Volume 1, Chapter 6 Lamina, Laminate, and Special Form Characterization 6-5 thickness equilibrium1 is obtained during conditioning. ASTM D 5229/D 5229M also defines how to determine the moisture absorption properties, and its use for this purpose is discussed in more detail in Section 6.6.8. 6.3.2 Fixed-time conditioning As stated above, fixed-time conditioning is only of limited usefulness2 , it cannot generally provide the desired uniform moisture condition through the thickness of the material. The shortcomings of the fixedtime approach are illustrated in Figure 6.3.2 for a simulated 30-day exposure of IM6/3501-6 carbon/epoxy at 140°F (60°C) and 95% RH. Using known values for moisture diffusivity and moisture equilibrium content, the calculated average moisture content of various laminate thicknesses is plotted and shown as a smooth curve. From this curve, it can be seen that the maximum laminate thickness that can reach equilibrium at this temperature during this fixed, though fairly lengthy, conditioning exposure, is 0.035 in. (0.89 mm). For greater thicknesses, the moisture distribution through the thickness will not be uniform, as the interior moisture levels will be below equilibrium moisture content. This is further illustrated by an example in Section 6.3.3. FIGURE 6.3.2 Two-sided moisture absorption of carbon/epoxy laminate after 30 days exposure at 140°F (60°C)/95% RH. As will be discussed in Section 6.3.3.1, with lower target relative humidity levels, it is common to try to accelerate conditioning by subjecting the material to a higher relative humidity level for a shorter period of time. The objective is to introduce the same average moisture content in the material as would be seen in equilibrium conditioning at the lower relative humidity level, although the distribution of moisture content distribution will be less uniform through the thickness. Using a single-humidity level, fixed-time conditioning example, again illustrated by Figure 6.3.2, equilibrium at 78% RH (1.2% equilibrium moisture content for this material) can be approximated only at a thickness of 0.070 in. (1.8 mm). For a thickness greater than 0.070 in. (1.8 mm), the average moisture content will be insufficient, and for a thickness less than 1 The discussion focuses on through the thickness moisture absorption; however, in-plane moisture absorption will locally dominate near edges, and may even dominate the overall absorption process in those cases where edge area is a substantial portion of the total exposed area. 2 Examples of fixed-time conditioning methods that should specifically be avoided include: ASTM D 618 (Reference 6.3.2(a)), ASTM D 570 (Reference 6.3.2(b)), and SACMA RM 11-88 Method I (Reference 6.3.2(c))