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RP016 - Dynamic Cure and Diffusion Monitoring in Thin Coatings
RP101 - Evaluation of Coil Coatings by Dielectric Analysis (DEA)
RP034 - Moisture Diffusion Monitoring in Polymers with Microdielectronic Sensors
RP109 -
A Study of the Drying and Curing Rates of Acrylic Automotive Topcoats Using Dielectric Analysis
RP123 -
A New Dielectric Measurement System for Monitoring the Drying and Curing of Coatings in Production Scale Conveyor Ovens
RP126 -
Cure Monitoring of Powder Coatings Using Dielectric Analysis
RP042 -
Moisture Monitoring at the PI-SiO2 Interface Using Microdielectric Sensors
RP050 -
Moisture Diffusion Monitoring of Polyetheretherketone (PEEK) with Microdielectric Sensors
RP113 -
Dielectric Analysis for Determining the Extent of Cure for UV / EB Systems

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RP016 - Dynamic Cure and Diffusion Monitoring in Thin Coatings; Micromet Instruments, Inc., Dr. David R. Day and David D. Shepard

ABSTRACT

The recent development of miniature microelectronic dielectric sensors enables relatively simple drying, curing, and diffusion studies in extremely thin films. The microdielectric sensor measures dielectric constant and loss factor of the first 12 microns of material in contact with the sensor. This paper discusses recent dielectric data reproduction techniques which simplify the frequency, temperature, and time dependent response into a single viscosity related curve. The data resulting from an epoxy coating cure is demonstrated and analyzed. The time required for moisture to influence the dielectric response is used to determine diffusion rates through thin coatings. Dielectric properties are used to analyze the post curing properties of a latex film.

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RP101 - Evaluation of Coil Coatings by Dielectric Analysis (DEA), GE Appliances, Jesse Howard

ABSTRACT

Dielectric analysis has existed for many years, however only lately has the technology advanced to the point that its true potential is being realized. It is felt that the information presented here offers finish formulators and processors in the coil coating industry the opportunity to more fully understand their products' cure kinetics much earlier in the development cycle and to optimize cure as it relates to performance.

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RP034 -Moisture Diffusion Monitoring in Polymers with Microdielectronic Sensors; Micromet Instruments, Inc., Dr. David R. Day and David D. Shepard

ABSTRACT

With the use of composites in space, there is always a concern for the moisture content and the rate of moisture uptake within the structure. For the past several years microdielectric sensors have been used to monitor curing reactions in composites, while recent work has shown that they can be used to monitor moisture diffusion in a composite part after cure has taken place. Due to the very localized measurement by the sensor, several sites within a part can be monitored individually. This paper describes preliminary diffusion work carried out in thin epoxy and polyimide films as a function of ultimate cure temperature and film thickness.

This work shows that microdielectric sensors are sensitive to moisture changes in both polyimide and epoxy thermoset systems. The sensors could not only monitor the curing of the structure during fabrication, but could also be used during the life of the part to monitor moisture uptake and moisture evolution in various regions within the structure.

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RP109 - A Study of the Drying and Curing Rates of Acrylic Automotive Topcoats Using Dielectric Analysis, Micromet Instruments, Inc. , David D. Shepard

ABSTRACT

The drying and curing rates of acrylic automotive topcoats are critical to the performance and appearance of the coating and the efficiency of the manufacturing process. Typical evaluations of coatings involve post-process tests which provide little information as to the actual drying and curing rates during processing.

Dielectric Analysis provides a means to study the drying and curing rates under actual or simulated processing conditions. The coating is applied to a planar dielectric sensor and dielectric measurements made during the drying and curing of the coating. This provides a continuous graph related to the rate of drying and curing or the coating. This paper looks at the drying and curing rates of both solvent based and water based automotive topcoats. The effect of applying a Clearcoat over a Basecoat is also examined.

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RP123 - A New Dielectric Measurement System for Monitoring the Drying and Curing of Coatings in Production Scale Conveyor Ovens, Micromet Instruments, Inc., David D. Shepard, Huan L. Lee

ABSTRACT

The drying and curing rates of coatings are critical to the performance and appearance of the coating and the efficiency of the manufacturing process. Processing of a coating often involves spraying the coating onto the metal substrate to be coated, allowing some of the solvents to evaporate, and then curing the coating onto the substrate at an elevated temperature. Previous work has shown that dielectric sensors mounted on the substrate can be used to monitor the drying and curing process for acrylic automotive coatings under simulated processing conditions.

In actual manufacturing, this process is automated into a continuous process on a conveyor system where the parts are sprayed, pass through a drying chamber, and then into the curing oven. This paper discusses a new dielectric maeasurement system that can travel through the process along with the sensor. This eliminates the need for long extension cables and enables the drying and curing behavior in production scale processes to be monitored. Data collected with the new dielectric measurement system is discussed.

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RP126 - Cure Monitoring of Powder Coatings Using Dielectric Analysis, McWhorter Technologies, Milind Sohoni, Micromet Instruments, David D. Shepard

ABSTRACT

As dielectric analysis has become a more accepted method of monitoring the cure characteristics of thermoset resin systems, the applications for this analytical technique have become more commonplace. Traditionally, dielectric analysis has been used in the aerospace industry to help understand cure related phenomena and determine process parameters for advanced composite manufacturing. In recent years dielectric analysis has seen growth in its use for research and development, quality assurance and production control in industries such as industrial molding, electronics, medical and paints and coatings. The rapid growth of powder coatings in an increasing number of applications has led to a greater number of formulation requirements as well as the need for a better understanding of the effect of processing conditions on cure characteristics. This paper reviews the theory of dielectric measurements and analyzes and discusses dielectric data collected from various powder coating formulations processed under different temperature conditions.

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RP042 - Moisture Monitoring at the PI-SiO2 Interface Using Microdielectric Sensors; Micromet Instruments, Inc., Dr. David R. Day

ABSTRACT

Reaction and diffusion in polyimide was studied using microdielectric sensors. Onset of imidization was observed at 135C while reaction and/or loss of volatiles was observed up to the final temperature of 240C. Microdielectric sensors were found to monitor moisture concentration changes at the PI-SiO2 interface of a polyimide film on the sensor. Data were fit with a Fickian model and exhibited excellent agreement. Calculated diffusion coefficients ranged from 2.2 to 4.8 x 10-9(cm2/sec). The polyimide diffusion coefficient was found to be nearly constant with reaction temperatures ranging from 160C to 240C.

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RP050 -Moisture Diffusion Monitoring of Polyetheretherketone (PEEK) with Microdielectric Sensors; Micromet Instruments, Inc., Dr. David R. Day, David D. Shepard, and Kelly J. Craven

ABSTRACT

Classical diffusion analysis involves weight uptake measurements as a function of time on thin polymeric samples. The use of Microdielectrometry to monitor the diffusion of moisture through polymers is a relatively new technique. Sensors have been developed which are sensitive to the small changes in permittivity (dielectric constant) of polymeric materials as water concentration (and thereby, mobile dipole concentration) increases. In addition, sensors exist which can withstand the high temperatures (greater than 350C) required for the consolidation of high temperature thermoplastics. The diffusion coefficient can be estimated through a simple Fickian diffusion model of the dynamic dielectric response. The Microdielectric sensors measure a very localized area of approximately 0.01cm into the material. This allows monitoring diffusion properties of thin films, or of many simultaneous and independent locations in a bulk material.

Previous work has studied the diffusion characteristics of epoxies and polyimides by this technique. This study examines the diffuson of water through a thin film of polyetheretherketone (PEEK) and compares it with published data obtained by weight uptake studies. The diffusion rate of moisture through amorphous PEEK is shown to be slightly faster than diffusion through more crystalline PEEK.

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RP113 -Dielectric Analysis for Determining the Extent of Cure for UV/EB Systems, Thomas F. O'Malley, Sun Chemical Corporation and Nathaniel T. Smith, Micromet Instruments, Inc.

ABSTRACT

In the past dielectric analysis (DEA) has been used as an important measurement component in the overall analysis of polymer resin systems. Much of this work has been done at the research level in determining viscosity behavior, rate of cure, and cure endpoint. In the areas where DEA has been used in the production environment, it has been in the low volume applications of aerospace composites. Within the last several years there has been an expansion of the applications were dielectric cure analysis has been used. One of those areas is the analysis of both UV and EB curing systems. For UV systems the reaction can be monitored during the exposure and during post cure. For EB systems the change in cure state is measured before and after EB exposure. Both processes can be measured in real-time, in-situ. By monitoring the change in electrical properties of the resin system the rate and extent of cure can be determined. With sampling rates down to 55 milliseconds, measurements can be taken during the exposure process. Diffusion properties can also be monitored. Films down to 1 micron in thickness can be measured.

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NETZSCH offers precision thermal analysis instruments including advanced dilatometers (with a new basic R&D/QC dilatometer), classical DSC & TGA (with a new economical DSC), high temperature DSC to 1650°C for specific heat, very high temperature STA (TGA-DSC/DTA) to 2400°C (featuring the new STA 409-PC Luxx®), thermal / evolved gas analysis with fully-integrated FTIR & MS, plus high resolution TMA and DMA. We also feature leading technology for thermal conductivity and diffusivity measurement as well as refractories testing including HMOR, CIC, and RUL.

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