Measurement 39 (2006) 892900 www.elsevier.

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Inuence of heat treatment on hysteresis error of force transducers manufactured from 17-4PH stainless steel
Bulent Aydemir
a

a,*

, Erdinc Kaluc b, Sinan Fank

TUBITAK, Force Measurement Laboratory, National Metrology Institute (UME), P.K. 54, 41470 Gebze, Kocaeli, Turkey b Kocaeli University, Engineering Faculty, 41040 Kocaeli, Turkey Received 11 August 2005; received in revised form 20 March 2006; accepted 21 March 2006 Available online 24 May 2006

Abstract Dierent heat treatment processes can be applied on the spring element of a force transducer in order to obtain good and satisfactory performance. The study covers the attempts of dierent heat treatments on spring element using 17-4PH precipitation hardened stainless steel, which is regarded as one of the best and popular spring materials for force sensor applications. Heat treatments named as H900, H925, H1025, H1150 and S450 was applied, and dierent hardness values were reached. Especially, S450 heat treatment process was improved in this study. It was observed that heat treatments inuenced the transducer performance, particularly hysteresis behaviour point of view. The results have shown that; hysteresis characteristics were improved with increasing hardness and sub-zero treatment process. 2006 Elsevier Ltd. All rights reserved.
Keywords: Force transducer; 17-4 PH; Heat treatment; Hysteresis

1. Introduction Strain gage based force sensors or transducers are used extensively in dierent eld of industry. Several applications of force transducers in materials laboratories, manufacturing and control systems, where critical force measurements are strictly needed. In order to achieve low uncertainties in force measurements, the performance characteristics such as repeatability, linearity, hysteresis and creep errors inuence the measurement uncertainty
Corresponding author. Tel.: +90 262 679 50 00; fax: +90 262 679 50 01. E-mail address: bulent.aydemir@ume.tubitak.gov.tr (B. Aydemir).
*

of force transducer [1]. It is known that hysteresis error is one of the most important characteristics of force transducers [25]. It plays an important role on the measurement uncertainty of the force transducer. For this reason it must be as low as possible. It was determined that performance characteristics of force transducers were mostly aected by the heat treatment that was applied to spring element [2,6]. Spring materials may exhibit dierent hysteresis behaviour and the application of heat treatment on spring material causes important microstructural changes and respectively creates dierent hysteresis error performance in force transducers [1,7]. Various heat treatment procedures can be applied on the spring element of a force transducer in order to optimise performance characteristics. The study

0263-2241/$ - see front matter 2006 Elsevier Ltd. All rights reserved. doi:10.1016/j.measurement.2006.03.014

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covers the attempts of dierent ageing heat treatments on spring element using solution annealed 17-4PH precipitation hardened stainless steel which is regarded as one of the most popular spring materials for force transducer applications [5]. Precipitation hardened stainless steel usually exhibits a higher hysteresis error than alloyed tool steel or aluminum [3]. Application of specially selected heat treatment reduces the hysteresis error. In this study, various heat treatments were applied on the specimens to obtain minimum hysteresis error from the produced force transducers. It is essential to select good performance materials, to perform good design, and to apply carefully controlled manufacturing procedures for force transducers [8]. The use of high accuracy electronic instruments in transducer outputs and the use of dead weight force standard machines in determining the performance characteristics of transducers are also very important to get reliable results. After application of all heat treatment and ageing processes, nishing process was applied to get the resulting specimens. Then special strain gages were bonded on the specimen surface. Finally, the selection and application practice of strain gages have been done properly. After completing the strain gage circuits of transducers, all of specimens are calibrated with dead weight UME (National Metrology Institute) Force Standard Machine having 2 105 measurement uncertainties in a specied measurement procedure to obtain performance specications of each specimen. 2. Materials and heat treatments of spring element of transducer Test material for the spring element of force transducers is 17-4PH steel. 25.4 mm diameter with steel bar was procured in condition A (Table 1). The
Table 1 Heat-treating details of test specimens Specimen code (condition) Solution annealing processes Annealing temperature (K) 1313 1313 1313 1313 1313 1313 Annealing time (min) 30 30 30 30 30 30 Quenching medium Atmosphere Atmosphere Atmosphere Atmosphere Atmosphere Water

Fig. 1. Force transducer specimens technical dimensional.

tension type force transducer body specimens were rst machined roughly to their dimensions, as seen in Fig. 1. 17-4PH steel is one of most popular spring element material for the force transducer application due to corrosion resistivity [1,9]. In order to change the microstructure in 17-4PH stainless steel specimens, various annealing heat treatments were applied after solution annealing process. Although H900, H925, H1025 and H1150 heat treatments could be found in literature, S450 heat treatment was specially improved for this study. The details of heat treatment, which were applied to 17-4PH stainless steel, are given in Table 1. These heat treatment processes were applied on the ve groups of specimens. Each group has two identical specimens to determine eect of heat treatment on the hysteresis performance of force transducers. As a result of each heat treatment, hardness values were measured for each specimen using Zwick Z
Table 2 Average hardness values of specimens Specimen code H900 H925 H1025 H1150 S450 Hardness values (HRC) 44.90 41.35 37.34 32.57 45.29

Sub-zero treatment

Ageing (precipitation) heat treatment Ageing temperature (K) 755 769 825 893 723 Ageing time (min) 60 240 240 240 120 Cooling medium Atmosphere Atmosphere Atmosphere Atmosphere Atmosphere

A (standard material) H900 H925 H1025 H1150 S450

1 h in liquid nitrogen

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2.5 model hardness machine in order to determine relation between performance and hardness. Average hardness values in Rockwell (HRC) scale are given in Table 2. 3. Transducer design and strain gage application All transducers were designed for 100 kN capacity and produced in tension type and circular bar shape for easy strain gage application. Tension type transducer enables easy and exact centering in force standard machine since it has spherical apparatus, which eliminates the bending eect during loading. The basic elementary elasticity calculations were employed in the design of cylindrical tension type transducer. In order to eliminate end eect, the diameter to length ratio was taken greater than ve. Diameter of tension bar is calculated as 20 mm for a strain level of 1500 lm/m for 100 kN capacity. After the application of heat treatments, specimen surfaces were nished to their exact dimensions by grinding to satisfy 0.002 mm tolerance in all dimensions for each specimen. In order to get output signal from transducer spring element, N2A type 350 X transducer class (Measurement Group Co., USA) strain gages were used and bonded in this study. Its STC (self temperature compensation) number is 06 associated with exactly 17-4PH stainless steel for approximating the thermal expansion coecients of the transducer material [10]. These strain gages are selected as 90 rosette to eliminate alignment errors. Correct application of strain gages is very important to obtain repeatable performance from the force transducers. Recommendations of strain gage producer were carefully applied to obtain better performance and quality bonding using M bond-610 adhesive for strain gage application. Since nal transducer performances are greatly depending on the application of a uniform and repeatable clamping pressure, strain gages are bonded according to manufacturer recommendations using special clamping apparatus [8,11]. Two rosettes pair is bonded on opposite side with a 180 angle between them to establish a full bridge wheatstone circuit. Another pair of rosettes is bonded on the spring element to obtain another full bridge circuit. As it mentioned before that each group has two identical specimens. Although each specimen has a full bridge circuits, one specimen from each group has two full bridges circuit due to determination of the installation errors of strain

Fig. 2. Completed force transducer specimen ready to performance test.

gage application. A completed specimen prepared as force transducer was shown in Fig. 2. 4. Calibration method for hysteresis error determination Hysteresis or reversibility error in force transducers is determined at each calibration procedure by taking the dierence of force measurements in increasing and decreasing order of force applications (Fig. 3). In other words, the dierence between the values obtained with increasing force and with decreasing force enables the relative hysteresis error (v), which can be calculated by using Eqs. (1) and (2) v12 vave X 012 X 12 100 X N 12 v1 v2 2 1 2

where v is the relative hysteresis error of force transducer, v1, v2 are the hysteresis errors in rst and sec-

Fig. 3. Schematic representation of hysteresis error on force transducer output graph.

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ond series of readings, vave is the average relative hysteresis error, X 012 are the readings on the indicator with decreasing test force in rst and second series, X12 are the readings on the indicator with increasing test force in rst and second series and XN(12) is the average reading on the indicator with maximum test force in rst and second series. A schematic representation of hysteresis error is given in Fig. 3. Increasing and decreasing forces in 10 steps with 10% increment of 100 kN load were applied on the force transducer in a dead weight force standard machine in two series. Before beginning of the force application, three preloading in 100 kN as dened EN ISO 376 were applied on it [12]. Transducer output were recorded at the end of 30 s after application of each force steps using high precision indicating instrument that is DMP 40 S2 located in Force Measurement Laboratory of UME. Fig. 4 shows the force transducers that are under test in 110 kN dead weight force standard machine. These test are performed at very ne controlled laboratory conditions with a temperature of 21 1 C and humidity 45 5%. The short-term temper-

ature control is better than 1 C. Temperature variation is measured to be less than 0.2 C during full test of transducer. 5. Results and discussion The hysteresis error of several heat-treated spring materials are presented in Figs. 59. In these gures, measured data are shown with symbols (D, h, s) while corresponding tted curves are plotted with continuous lines. As it explained in transducer design section, that it was prepared two specimens for each group. One specimen has a full bridge circuits, other specimen has two full bridges circuit due to determination of the installation errors of strain gage application. In this case, three full bridge circuits which are named a, b, c on the graphs are used for H900, H925 and H1025. But, there are two full bridges on specimens H1150 and S450 due to some problem on the strain gages. Figs. 59 shows the hysteresis errors specimens represented with H900, H925, H1025, H1150, S450 coded, respectively. Average values of these data for each specimen groups are plotted to the graphs for comparison of the results to see eect of heat treatment on the hysteresis error of force transducers. The comparison of hysteresis error of several heat-treated spring materials are presented in Fig. 10. It is seen from Fig. 10 that the hysteresis error is strong function of the heat treatment and hardness. Even though, all the specimens have precipitation hardened martensitic structure, they exhibit dierent hysteresis errors. It is seen that the hysteresis error changes with changing hardness values. Similarly, hysteresis error is also a function of microstructure. These results can be attributed to crystal structure of the specimen forms after annealing and precipitation heat treatment. Heat treatment applied on the spring element inuence the hysteresis error of force transducer according to measurement results [2,5,7]. It is found that the hysteresis error decreases at high hardness and increases as materials soften. Even in elastic region of the material, dislocation motion plays an eective role in hysteresis loop establishment [2,3]. In this case, each aects which decrease to movement of dislocation in metal crystal cause to decrease hysteresis error of force transducer. It is known that increasing dislocation density causes the dislocation locking and resist to dislocation movement in the grains [2,4,5,7]. As a

Fig. 4. Force transducers under test in 110 kN dead weight force standard machine.

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B. Aydemir et al. / Measurement 39 (2006) 892900

Relative Hysteresis Error (%)

0.06 0.05 0.04 0.03 0.02 0.01 0.00 0 10 20 30 40 50 60 70 80

H900a H900b H900c

90

100

Force (kN)

Fig. 5. Hysteresis graph for H900 coded specimens.

0.07

H925a

Relative Hysteresis Error (%)

0.06

H925b H925c

0.05

0.04

0.03

0.02

0.01

0.00 0 10 20 30 40 50 60 70 80 90 100

Force (kN)

Fig. 6. Hysteresis graph for H925 coded specimens.

0.07

H1025a H1025b H1025c

Relative Hysteresis Error (%)

0.06

0.05

0.04

0.03

0.02

0.01

0.00 0 10 20 30 40 50 60 70 80 90 100

Force (kN)

Fig. 7. Hysteresis graph for H1025 coded specimens.

result of this resistance in high dislocation density material, the diculties of dislocation motion cause to decrease hysteresis error under load. The average

hysteresis error of the spring materials of the transducers which are H900, H925, H1025, H1150 and S450 coded specimens having precipitation

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0.25

897

H1150a

Relative Hysteresis Error (%)

H1150b
0.20

0.15

0.10

0.05

0.00 0 10 20 30 40 50 60 70 80 90 100

Force (kN)

Fig. 8. Hysteresis graph for H1150 coded specimens.

0.07

Relative Hysteresis Error (%)

0.06

S450a S450b

0.05

0.04

0.03

0.02

0.01

0.00 0 10 20 30 40 50 60 70 80 90 100

Force (kN)

Fig. 9. Hysteresis graph for S450 coded specimens.

H900
0.25

H925 H1025 H1150 S450

Relative Hysteresis Error (%)

0.20

0.15

0.10

0.05

0.00

10

20

30

40

50

60

70

80

90

100

Force (kN)

Fig. 10. Comparison graph for the hysteresis errors of all specimens.

hardened martensitic structure were compared in Fig. 10 that the hardest materials having 45.3HRC hardness have the highest dislocation density and

has the least hysteresis error. As a result of that the hardest specimens, S450 coded specimen show the best behaviour among all specimens or show the

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smallest hysteresis error. This behaviour may be attributed to dislocation density. Because changing hardness and changing yielding stress of the material due to dierent tempering temperature cause the change of dislocation density on the material [4,7]. Dislocation density increases up to 1012 cm2 during martensitic transformation of the steel [4]. After completing the martensitic transformation, application of dierent tempering temperature cause the diusion of carbon atoms from distorted lattice structure of martensite, then hardness and dislocation density of the material decrease with increasing temperature. Shortly, any treatment causing an increase in dislocation density results decrease in hysteresis error. Decreasing of hysteresis error with increasing hardness may also be explained by anelasticity. Detailed information about anelasticity can be found in Ref. [13]. Short information about anelasticity was given below. Anelastic deformation of a component of time dependent deformation which, in contrast to plastic deformation, is recoverable upon the removal of applied stress. For stresses below rE, Fig. 11, which can be called elastic limit, the material deforms in a fully elastic manner, without any measurable contribution of time dependent components. As one increases the stress above the elastic limit, one observes the formation of closed hysteresis ret loops. This fully elastic behaviour is seen in the REGION I Fig. 11, where r is the applied stress, rY is yielding stress, rA is anelastic stress, rE is fully elastic stress, et is the total strain, ey is yielding strain, eA is anelastic strain and eE is fully elastic strain. The fully elastic stress is proportional to the yield stress of the materials. Generally it is between 10% and 20% of the yield point. Some numerical values are given in Table 3 to show the level of rE for some materials [13]. These closed hysteresis loops reect the existence of recoverable time dependent strain, which is dened as anelastic strain shown in REGION II Fig. 11. These hysteresis stressstrain loops remain closed up to a stress level rA which shall call anelastic limit. When the stress exceeds the anelastic limit the hysteresis loops will cease to be closed when the specimen is unloaded to the zero stress. The existences of nonrecoverable time dependent strain are shown in REGION III Fig. 11. Since the stress level involved is still considerably below the yield stress of the material, the observed nonrecoverable strain is usually associated with microplasticity [13]. According to above explanation and Fig. 11,

Fig. 11. Schematic representation of stressstrain regions for anelastic stress and hysteresis loop establishment under yield stress.

Table 3 Elastic stress values of some materials depending on the yield stress [13] Material Yield stress Fully elastic (rE)/(rY) (rY) stress (rE) 101 MN/m2 101 MN/m3 5.86 19.50 27.00 0.50 2.30 4.31 0.08 0.11 0.15

Pure aluminium 304 stainless steel Pressure vessel

when the applied stress closes the elastic limit, hysteresis error decreases considerably. As a result, if any heat treatment increases the yield point of the material, it has benecial eect on the decreasing of hysteresis error. In this case, hysteresis error can be combined with the change of yield point, which depends on the hardness of material. As it known that yield point of material increases with increasing of material hardness. If the yield point of the material increases, anelasticity limit of the material are also increases. Since applied forces (applied stress level) on the specimens are identical for all type of specimens during performance test in this study, possible change on yield point of material due to heat treatment will cause the change of hysteresis error according to Fig. 11. If the yield point of material increases, hysteresis error of specimen decreases proportionally without changing the applied stress. Shortly, any treatment causing an increase in yield point or hardness of material results decrease in hysteresis error due to increasing anelastic stress (rA) of material. Anelastic deformation resulting from dislocation bowing

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and pile up against barriers to dislocation motion [13]. It is known that microstructural changes such as changing amount of residual austenite, Cu particles and precipitates due to dierent aging processes cause the hysteresis error change in martensitic stainless steel [2,3,5]. Since the main reason of hysteresis error change was caused by restriction of dislocation motion in structure, some mechanisms inuence the dislocation motion in the dierent microstructure of 17-4PH steel. Increase of strength in precipitated structure is due to ne Cu particle distribution. These ne distributed Cu particle cause to restrict dislocation motion; consequently, it causes to increase strength of material [2,5]. As a result of that existing precipitated Cu particles barrier to dislocation motion due to bowing and pile up dislocation and this cause to decrease hysteresis error in precipitated structure. The martensite type, residual austenite, shape, size and distribution of cementite and/or other carbides as well as dislocation density are the principal factors that are causing microstructural changes. Since the main reason of hysteresis error was mainly attributed to the restriction of dislocation motion in the structure, some factors and mechanisms should eectively inuence the mobility of dislocations in dierent microstructures of 17-4PH steel. The increase of strength in precipitated structure is due to ne Cu and Nb particle distribution in the structure. Because, distributed ne Cu and Nb particles in the martensite matrix cause very eective restriction to the movement of dislocations and consequently it results a considerable increase in the strength of material [2,3]. Martensitic structure obtained by martensitic transformation as in condition A in Table 1 has approximately 30HRC hardness. If this structure subjected to ageing heat treatment, its hardness reaches to 45HRC as in specimen S450 due to precipitated structure after ageing process. Dislocation density is one of the most important factors dictating the hysteresis error characteristics of materials [4,5]. The existing Cu and Nb particle barriers to movements of dislocations are playing a strong role in bowing and piling up dislocations eectively and this will cause decrease in hysteresis error for martensitic structures in steels [5]. 6. Conclusions The conclusions of the study can be outlined as follows:

(a) The hysteresis error of a force transducer using heat treated 17-4PH steel spring element, can be reduced by maintaining the hardness of spring element as high as possible. (b) Microstructural change plays an important role on the hysteresis error of 17-4PH steel spring element having the identical hardness values. In the other words, microstructural change results in hysteresis error change even the hardness are identical for the same material. (c) Increasing temperature and holding time during ageing heat treatment cause to increase hysteresis error due to coarsening of precipitates. Coarse precipitates have lower resistance to movements of dislocations. (d) Over ageing should be prohibited for the 17-4 PH steel due to harmful eect on the hysteresis error.

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[12] EN ISO 376, Calibration of force proving instruments used for the verication system of the uniaxial testing machine, BSI, London, 2002.