CFC Fixture Advantages and Challenges in Vacuum Heat Treatment, Part 1

OCWhat happens when a lead engineer sticks his head in new advancements in materials from NASA? For the author of this article, it means the successful research and development of a new generation of workpiece carriers and fixtures made from “a high-tech ceramic matrix composite of very strong carbon fiber,” that is, CFC.

This Technical Tuesday article, written by Dr. Jorg Demmel, founder, 0wner, and President, High Temperature Concept, was first published in Heat Treat Today's November 2022 Vacuum print edition.


Introduction: From NASA to Industrial Heat Treatment

Dr. Jorg Demmel
Founder, Owner, President
High Temperature Concept

In the mid-1990s, a development in materials from NASA moved into my focus. I was an associate and lead engineer at the Fraunhofer Institute in Stuttgart, Germany, so I posed the question: Could CFC material (carbon fiber-reinforced carbon) substitute for non-abrasion-resistant and brittle graphite as the material used for workpiece carriers in the soldering process of drills? The answer: yes. The story did not end here. This project, which included the automated handling of the drills in some continuous furnaces, was just the first accomplishment. What ensued was a successful research and development of a new generation of workpiece carriers and fixtures made from CFC (“Carbon Fiber Carbon”).

Material Properties and Main Advantages of CFC

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CFC (aka, CFRC, or C/C), which stands for carbon fiber-reinforced carbon, is a high-tech ceramic matrix composite of very strong carbon fibers (or fiber rovings) in a compensative carbon (graphite) matrix. Material properties of some relevant heat treatment fixture materials were evaluated, and some are shown in Figure 1. These CFC properties have the following positive effects when used as CFC fixtures for heat treatment:

Figure 1. Left to right for 2D CFC SGL Sigrabond Performance, heat resistant austenitic cast alloy steel ASTM A297-HK (ISO G-X 40 CrNiSi 25-20; 1.4848), wrought and annealed Ni alloy Inconel 601 UNS N06601 (NiCr23Fe15Al; 2.4851) and mechanically alloyed Fe alloy, oxide dispersion strengthened Plansee PM ODS 2000 (Cr Al 21 6; 1.4768).

  • Because of their low density, CFC fixtures have a lower weight than their steel alloy counterparts (about five times), which reduces the efforts for manual handling.
  • Because of the increased strength of CFC at high temperature, the fixture weight can be reduced further. Additionally, fixture volume can be reduced — in some applications dramatically — so that, when combined with a specific CFC fixture design, furnace capacities can be increased up to 100%.
  • The following characteristics of CFC fixtures are responsible for the longer fixture life cycles (up to greater than five times), less workpiece distortion and rework, and make an automatic workpiece handling possible for the first time ever: the low CTE (coeffcient of thermal expansion) value for CFC in the direction of the fiber, the fact that CFC is chemically inert in vacuum or
    certain protective atmospheres, has an excellent thermal shock resistance, and it doesn’t grow, creep, or age like metals.
  • Although the specific heat of CFC is higher, the energy consumption can be reduced and shorter heating up and cooling down times can be reached, resulting in up to 30% shorter process cycle times for the same workpieces.

Figure 2. CFC fixture advantages in heat treatment

Figure 2 shows all potential advantages of CFC fixtures compared to state-of the- art steel alloy; a short payback time of the investment with high profitability are possible.

CFC Fixture Suitability in Vacuum Heat Treatment

Since CFC is made of carbon, it is not made for high temperatures above 752°F (400°C) in air or atmosphere with high percentages of oxygen, water vapor, hydrogen, or carbon dioxide for long periods of time. Therefore, vacuum or protective gas atmospheres are, in general, a suitable environment for CFC fixtures.

Table 1. Reaction rates and activation energies for graphite (800 °C; 0.1 bar). Equation (1) is the main combustion reaction, which has the strongest effect and is strongly exothermic (negative change of reaction enthalpies Δ"H). Reaction (2) is the so-called water gas reaction which shows the endothermic oxidation of carbon with vapor. Equation (3) is the Boudouard reaction which occurs endothermic above 700 °C. According to the Boudouard equilibrium the C0/CO2 ratio increases with increasing temperatures and decreasing pressures. Reaction (4) is the methane formation reaction: hydrogen reacts with carbon at temperatures above about 700 °C to CH4. Below 546 °C methane decomposes in carbon and hydrogen.

Table 1 shows the relative reaction rates for graphite according to H. Marsh in Introduction to Carbon Science, 1989 in the “reaction controlled” Zone I up to 1472°F (800°C) under oxygen, steam (H2O) Figure 3. Burning rates of graphite as a function of temperature

Industrial experience shows that CFC under vacuum of < 10-2 mbar at 1472°F or 1832°F (800°C or 1000°C) at a low dew point < -4°F (-20°C) (< 0.1 % vapor content) lasts at least 5,000 hours (real process time). At 3632°F (2000°C), the life is about 2,000 hours. Dew points of about 0°C (about 0.6 % vapor) cause higher reaction rates and reduce lifetime to about 800 to 1,000 hours.

Unwanted Contact Reactions

Contact reactions between the CFC fixtures and the workpieces, primarily made of steel, can lead to changes in the workpieces: for example, carburization of the workpiece in contact with the CFC. It is important to avoid these contact reactions since the properties of the workpieces must under no circumstances be changed in an uncontrolled manner. Neither the chemical composition nor mechanical properties nor the surface may change beyond the permissible tolerance limits. The CFC fixture should also not be subject to any changes that could adversely affect its properties and, above all, its service life.

The following materials, consisting of mainly workpiece materials made of steel, were used in direct contact with CFC, especially in heat treatment and brazing. CFC 1501G (SGL), CF222 (Schunk), or CX-27C1 (GTD, Toyo Tanso) were used as CFC workpiece carrier materials. Table 2 gives an overview of the results. The symptoms columns with “none” indicate no problems. The colored cells showed problems. The last column references the application or the results.

Table 2. Contact/carburization test results from field trial, updated 2022

Figure 4a. CFC level grid (case hardening, oil quench)

Figure 4b: CFC-Rack CVD-Coating

The contact partners and processes in which unwanted contact reactions occurred in the field test (colored in Table 2) and which are not confidential (bold font) are examined more closely in Part 2. See Figure 5 which shows some contact reactions on tempered steel drills after vacuum hardening at 2066°F (1130°C) under vacuum of 0.3 mbar (0.3 hPa or 225 mm Hg or “micron”).

Figure 5. Contact reactions on drill blanks (1.6582) with SiC-coated CFC (Schunk CF222P75 and SGL 1601YI); Scale left about 2:1 and right microsection about 400:1

Figure 6 shows some heavy melting reactions of high-speed steel after vacuum hardening at 2264°F (1240°C) under vacuum of 0.1 mbar (0.1 hPa or 75 mm Hg or “micron”).

Figure 6. 1.3343 after contact with CFC CF222 at 2282°F (1250 °C) (left approx. 25:1; right detail 100:1)

The carbon transmission mechanism with unwanted carburization, along with eutectic reaction of some workpieces made of steel with CFC, and some technical solutions will be explained in Part 2 of this article.

References

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Demmel, J.: Advanced CFC-Fixture Applications, their scientific challenges and economic benefits, In: 30th Heat Treating Society Conference & Exposition, Detroit, MI, USA, 15th Oct. 2019.

Demmel, J.: Werkstoffwissenschaftliche Aspekte der Entwicklung neuartiger Werkstückträger für Hochtemperaturprozesse aus Faserverbundkeramik C/C und weiteren Hochtemperaturwerkstoffen, Dissertation, TU Freiberg, Germany, 2003.

Demmel, J.: Why CFC-Fixtures are a Must for Modern Heat Treaters, FNA 2020 Technical Session Processes & Quality, USA, 30th Sept. 2020.

Demmel, J., et al: Applications of CMC-racks for high temperature processes. In: 4th Int. Conf. on High-Temperature Ceramic Matrix Composites, 3.10.2001, p. A-17.

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Demmel, J. und U. Nägele: CFC revolutioniert die Wärmebehandlung. In: 53. Härterei-Kolloquium, Wiesbaden, 10.10.97. Vortrag und Tagungsbericht.

Demmel, J., Lallinger, H.: CFC-Werkstückträger revolutionieren die Wärmebehandlung. In: Härtereitechnische Mitteilungen 54, No. 5, p. 289-294, 1999.

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Kriegesmann, J.: Technische Keramische Werkstoffe. Loseblattwerk mit 6 Ergänzungslieferungen pro Jahr.

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Lay, L.: Corrosion Resistance of Technical Ceramics. 1. Aufl ., Teddington, Middlesex, Crown-Verlag, 1983 – ISBN 0-11-480051-0.

Marsh, H.; u.a.: Introduction to Carbon Science. 1. Aufl ., London, Butterworths-Verlag, 1989 – ISBN 0-40803837-3.

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Schulten, R.: Untersuchungen zum Kohlenstofftransportmit Carbidbildung in Nickelbasis-legierungen. RWTH Aachen, Fakultät für Maschinenbau, Diss., 1988 Deutsche Keramische Gesellschaft, 1990 following. ISBN 3-87156-091-X.

 

About the Author: Dr. Jorg Demmel is the founder, owner, and president of High Temperature Concept. He received his Engineering Doctorate in the field of CFC workpiece carriers for heat treatment and served in different leading positions for Volkswagen before moving to the U.S. In this article, Demmel draws on his dissertation, “Material scientific aspects of the development of new Fixtures for high temperature processes made of fiber-composite ceramics C/C and other high temperature materials” (Technical University Mining Academy Freiberg, Germany, 2002/3), and his personal experiences. For more information Contact Jorg at jorg.demmel@high-temperature-concept.com


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