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Manganin Pressure Gages

by Donald Newhall and Leonard Abbot
Of the various means of measuring high pressure, the most convenient is observation of the resultant change of resistance of a manganin wire. For high pressures, primary gages are cumbersome; Bourdon-type gages (including the long helical) and devices depending on elastic deformation are inferior in range* and are subject to some degree of hysteresis. Other metals or alloys have at times been used in the same manner as manganin but, all things considered, manganin is superior. This discussion covers the required characteristics of manganin, its incorporation into a high-pressure sensor, and the instrumentation employed for pressure readout.

Manganin as a pressure sensor was brought into prominence by Bridgman1, following the suggestion of Lisell2. Bridgman calibrated manganin gage coils directly3 and indirectly against a free piston primary-gage4, and employed the calibrated coils for nearly all of his subsequent high-pressure experimentation. His example has been widely followed5.

Manganin is an alloy composed approximately of 84 parts copper, 12 manganese and 4 nickel. It has long been used in the better grades of electrical instruments because of its favorable mechanical properties and low thermal-EMF against copper. Within the usual range of room temperature, there are few materials whose resistivities are less affected by temperature change.

Its value as a pressure sensor lies in the fact that, under pressure, its resistivity is appreciably increased, and the increase is nearly proportional to the applied pressure. The pressure coefficient of the manganin currently used in pressure cells by the Harwood Engineering Company is approximately 1.65 x 10-7 ohm per ohm per PSI (2.39 x 10-6 ohm/ohm/kP).

The behavior of manganin varies with its composition and its history. It is supplied by several manufacturers in U.S.A. and abroad, but it is impossible to procure a supply having a guaranteed pressure-resistance relation. Bridgman was fortunate in having at hand some German manganin which the Jefferson Physical Laboratory had acquired, probably before 1900, and which appears to have been particularly well-seasoned. In later years he bought spools of wire from two American manufacturers; one spool he found unsatisfactory, the other he used for his experiments to 30,000 Kg/cm2.

The pressure coefficient is affected by temperature. Compared with the value at 25°C, Birch and Roberson18 reported an increase of 0.2% at 50°, 0.8% at 75°, 1.7% at 100° and 2.8% at 125°; others5,19 are in rough agreement, but suggest wide variation of the effect according to the particular material used. The use of manganin as a pressure sensor has been a matter of interest at the National Bureau of Standards, and an attempt is being made to establish optimum specifications for material to be used for this purpose6.
 

Preparation

The preparation of a manganin gage is a matter of particular technique. Present experience indicates that the wire, a few mils in diameter, should be double silk covered. The important consideration in winding the coil is that it be subject to the minimum mechanical restriction.25 Bridgman's coils were noninductively-wound toroids, held in form by silk thread loosely tied in place. Harwood coils are multi-layer noninductively-wound helices; others have wound the wire loosely on suitable bobbins.

It is important that the structure be free of strain. Otherwise, variations of 2% or 3% in the pressure coefficient may result5,7. The winding process can be expected to impose some strain on the coil. The preferred way to overcome this is to subject the coil to extremes of temperature, alternatively -140° or as much as the insulation will stand, for several hours and then "dry-ice" temperature (or better, liquid air or nitrogen). Repetition may continue as much as a week. The coil is then pressure-seasoned by exposure well above the full use range (Harwood pressure-seasons at 30 kb). One application will probably be sufficient, but occasional coils may require more — if after a pressure run the coil does not return to its initial resistance, thus indicating an unstable zero.
 

Use in Cell

Manganin gage coils can be used separately in pressure cells which are suitably attached to a pressure system, or can be incorporated with other components within a pressure vessel. For example, Harwood supplies simple cells wherein the coil is placed at the inner face of a plug screwed into one port of a tee (or cross) high-pressure fitting that is subjected directly to the high-pressure fluid. In a more specialized cell, designed for systems where the high-pressure fluid is not compatible with manganin, the coil at the inner face of the closure is isolated from the system fluid by being sealed within a flexible bellows which transmits system pressure with negligible loss, the remaining space within the bellows being filled with pentane. The closure is held by a threaded retainer in one end of a heavy-walled cylinder forming the body of the cell.

Both types of cell are provided with a reference coil of manganin, having the same resistance as the active coil — 120 ohms ± 1/10 ohm — and set within a protective cap attached to the outer end of the closure. Its temperature matches that of the active coil as closely as possible. In contrast to this, since tubing for pressures above 200,000 PSI (1400 MP) is not available, it is necessary in the case of the 30-kilobar apparatus to place the gage coil in the same pressure vessel that contains the furnace, tensile jig or other experiment device.

The connection of the manganin wire to the coil leads is a matter of considerable delicacy. Harwood practice, following Bridgman, is to ground one end of the coil at the inner end of the closure and connect the other end to a lead passing through the closure. In view of possible future disconnections and re-connections it is convenient to attach short lengths of copper wire, about ½ inch long, permanently to the coil ends. Shifting of the coil, as from one closure to another, then can be made without changing the resistance of the coil.

There is some doubt as to the best type of connection of the copper to the manganin. Spot-welding may be the best, but to produce a secure joint with confidence requires artistry. Hard solder should give a good result, but special equipment and considerable care are necessary as there is danger of over-heating the wire. Probably the safest method is to use rather soft solder, but one must make the joint as small as possible — be meticulous in trimming the ends and apply only as much heat and solder as required.

Gages at the National Bureau of Standards are provided with four leads in order that lead resistance may be eliminated. This imposes the use of two more leads through the closure, with consequent greater chance for leak, as well as more complex instrumentation for measuring resistance change. The standard Harwood coils are 120 ohms and, since the lead resistance is 1/100 ohm or less, the added refinement appears unjustified for most work.
 

Instrumentation

As noted previously, the change of resistance due to pressure of a manganin coil is a convenient measure of that pressure. This change is small but measurable — about 1/30 for 200,000 PSI or 14 kb (1400 MP).

The Carey-Foster bridge is not popularly well-known, but has long been used for measuring small differences of resistance between two resistors.8 Almost from the beginning of his experiments with high pressure, Bridgman used such a bridge in connection with his manganin gages. Such a bridge, as used by Bridgman, is shown in Figure 1. The gage coil is represented by X and its resistance by x. C is a manganin coil of nearly the same resistance, c, as X, mounted outside of the pressure cell, at atmospheric pressure. It might be called the reference coil. R1 and R2 are ratio coils, each approximately 120 ohms. W is a slidewire, 100 cm long, of bare manganin of about 20 mil diameter, stretched over a good meter stick. S is a shunt selected to give the desired effective resistivity to the slidewire. B is a voltage source consisting of 2 dry cells. RB is a current-control rheostat and KB a contactor. G is a sensitive galvanometer. RG is a protective rheostat, and KG a contactor. A slider-contactor can be moved along the slidewire to balance the bridge.

The essential characteristic of a Carey-Foster bridge is that if the bridge is balanced with the contactor at some point r (identified as centimeters on the meter scale), and if coils C and X are then interchanged by a suitable switch, with a new balance point (r'), the difference between c and x is simply

c-x = r(r-r')
where r is the effective resistivity of the slidewire, expressed in ohms per centimeter. Using the bridge for a pressure gage, Bridgman determined the balance points r0 and r0' at atmospheric pressure, and at experimental pressure the points r1 and r1'. The change in resistance of the gage coil X due to pressure (x1 - x0) may then be written
(c-x0) - (c-x1) = x1-x0 = r[(r0-r0') - (r1 - r1')]

In practice, Bridgman balanced the bridge at atmospheric pressure and at the fixed point (the freezing pressure, 7640 kg/cm2**, of mercury at 0°C) and computed the slider displacement for a pressure difference of 1000 kg/cm2, or about 4½ cm. A scale then was constructed with divisions corresponding to 1000 kg/cm2, and 500 kg/cm2 subintervals. This was laid beside the meter scale and was a convenient index by which approximate pressure could be read at a glance for any bridge balance. A pressure setting was measured as:
       K[(r1-r0) + (r0'-r1')]
p = ----------------------
                   2
where p was the pressure in kg/cm2 and K was the calibrated constant (kg/cm2 per centimeter displacement of the slider) determined by the mercury fixed point experiment.
 

Other Bridges

Other experimenters have used bridges of other types.5,20,25 Elaborate models of Mueller bridge can be purchased, but instrumentation good enough for most purposes is available at less expense. Mueller bridges are well-known and need not be described here. Designed especially for this work are two bridges supplied by Harwood.

The type "S" Direct Reading Bridge (Figure 2) is intended for routine measurement of pressure. The active and reference coils are Harwood cells (described above) connected as shown. The four arms of the bridge are then nearly equal. The slidewire is a 1000-ohm, 1000-division potentiometer of high resolution, and the matching coil is trimmed to match it precisely. By the use of a 1-ohm calibrating coil and range-adjusting shunts, full scale of the slidewire can be made to coincide with full scale of the pressure range, normally either 100,000 or 200,000 PSI (700 or 1400 MP). In operation, with the cell at atmospheric pressure and the slidewire contactor set at zero, the bridge is balanced by means of the ZERO ADJUST. When pressure is applied, the bridge is again balanced by means of the slidewire, which gives a direct reading of the pressure in thousandths of the selected pressure range. The bridge operates with 3 No. 6 dry cells. Appropriate current controls are provided. For establishing bridge balance, a sensitive galvanometer (about ½ microvolt per millimeter deflection at 1 meter) can be used; preferably, a guarded DC null detector having a maximum sensitivity of 1/10 microvolt per scale division is recommended.

The Harwood type "G" bridge has practically the same components as the type "S" but, in addition, provision is made for short-circuiting the slidewire matching coil and for interchanging the reference and active for true Carey-Foster operation. Additional calibrating coils are provided, enabling the operator to check the resistivity of the slidewire or the resistance of a new gage coil without resort to external means. Pressure can be measured in the manner of the type "S" bridge or by the Carey-Foster method. The latter should be twice as accurate because it has the advantage of two slidewire displacements rather than one. Used in this way, the bridge should be good to better than 0.1%.
 

Indication

For many operations it is necessary to indicate the pressure directly and automatically. This may be done by using a Foxboro Dynalog indicator/recorder with one of the Harwood pressure cells. The active and reference coils of the cells form two arms of a bridge, the other two being components of the Dynalog. The instrument supplies about 5 volts at 1000 Hz to energize the bridge, and the unbalance caused by pressure is amplified to drive a pen on a round chart. (The instrument may also be specially modified for strip charts.) The instrument is provided with a zero-set and adjustment for cell factor — i.e., pressure coefficient of resistance of the manganin gage, and usually permits a selection among three pressure ranges: 0-50,000, 0-100,000, and 0-200,000 PSI (350, 700, and 1400 MP). It is considered to be accurate and readable to about ½% of scale.

For use as a pressure gage, the pressure coefficient of resistance, or pressure factor, of the particular coil must be precisely known. As previously stated, one has no assurance that the coefficient will be the same for any two spools. One can expect uniformity within a particular melt, but there may be slight difference in tension as the wire is wound onto different spools, and it has recently been pointed out9 that strain may vary between the inner and outer layers of a spool. Differences due to strain may presumably be ironed out in the seasoning process, but this would not be true regarding variation among various melts. It is evident that, for precise work, coils should be individually calibrated after seasoning.
 

Linearity

At the 1962 annual winter meeting of the A.S.M.E. in New York, Babb10 reported a study of linearity of Bridgman's manganin pressure scale. Bridgman's early experiments indicated that the pressure-resistivity relation is linear within about 1/10% to the limit of his normal range, 0-12,000 kg/cm2. About 25 years later, with indirect measurement of manganin against a free piston gage, he reported a somewhat greater deviation from linearity in the range of 0-30,000kg/cm2. Babb, noting the discrepancy between Bridgman's figure for freezing pressure of mercury and the corresponding values obtained by three other observers, concluded that Bridgman's manganin must have differed from linearity by something of the order of ½%.

Experiments at Harwood using a number of coils from a single spool indicate that, while there is some slight variation of pressure resistivity relation among the coils,  the deviation from linearity is nearly uniform among them. A typical characteristic is shown in Figure 3. The upper curve, for the cell factor, was obtained by subjecting the coil to a series of pressures established by a controlled clearance free piston gage, and plotting the resistance response.

The lower curve shows the corrections to be applied if the cell factor found at 100,000 PSI is used over the whole range (0-200,000). The cell factor determined at any particular pressure may vary as much as perhaps 1% among coils from the same spool but, with this single determination, the curve of corrections should permit the accurate specification of pressure by resistance readings taken throughout the range. This is particularly fortunate because, lacking a free piston gage, many laboratories depend on a single fixed point, probably the freezing point of mercury at 0°C, for the calibration of their coils. Data is lacking for manganin from other sources, though one experimenter reports the use of gage coils having 3 times the slope shown in Figure 3.14

With present equipment at Harwood Engineering Co., correction curves (Figure 3) cannot be made for pressures greater than 200,000 PSI. Two fixed points are now well established — the mercury point mentioned and the transition pressure of BiI-II, which is has been investigated by several4, 11, 12, 13, most recently (and probably most authoritatively) by Heydemann.15 These two points should define the curvature of the resistivity curve. If further refinement is necessary, one might also use the freezing pressure of mercury at elevated temperatures,16, 17 and other satisfactory references will doubtless be established. If available, a free piston gage will remain the most trustworthy means for calibration.

With respect to this deviation from linearity, it is to be noted that by special circuitry, and by special arrangement of the pen linkage, the response of the Foxboro Dynalog to pressure can be made more nearly linear. Unfortunately, this treatment cannot anticipate the employment of manganin from a different melt.



* Manganin has been used to 30 kilobars (108 N/m2 or 105 kP) or more.
** This value has been found by later experiments to be about 1% lower.

References

1. Bridgman, P.W., The Physics of High Pressure, p. 72, G. Bell and Son, Ltd., London; Macmillan, New York, 1952.
2. Lisell, E., Upsala Univ. Arsskrift, Matematik och Naturvetenskap, No. 1, (1903).
3. Bridgman, P.W., Proc. Am. Acad. Arts Sci. 47, p. 321, (1911).
4. Bridgman, P.W., Proc. Am. Acad. Arts Sci. 74, p. 1, (1940).
5. Babb, Jr. S.E., The Technique of Inorganic Chemistry, Vol. VI, H.B. Jonassen and A. Weissberger, Eds., p. 188, Interscience Publishers, (John Wiley & Sons), New York, London, Sydney, 1966. (A comprehensive discussion of secondary pressure gages).
6. Cross, J.W., Personal communications.
7. Adams, L.H., Goranson, R.W. and Gibson, R.E., Rev. Sci. Instru. 8, 230, (1937).
8. Laws, F.A., Electrical Measurements, p. 175, McGraw-Hill, New York, 1938.
9. Darling, H.E., Personal communications.
10. Babb, Jr. S.E., High Pressure Measurements, A.A. Giardini and E.C. Lloyd, Eds., p. 115, Butterworths, Washington, 1963.
11. Zeto, R.J., Vanfleet, H.B., Hryckowian, E. and Bosco, C.D., Characterization of the Bismuth I-II and Barium I-II Points under Hydrostatic Pressure, Symp. on the Accurate Characterization of the High Pressure Environment, U.S. Dept. of Commerce, N.B.S. Gaithersburg, Maryland, Oct 14-18, 1968.
12. Kennedy, G.C. and LaMori, P.N., J. Geophys. Res., 67, 851, (1962).
13. Giardini, A.A., Personal communications.
14. Gielessen, J. Personal communications.
15. Heydemann, P.L.M., J. Appl. Phy. 38, No. 5, (1967).
16. Atonov, Y.A. and Ivanova, E.M. "Manganin Resistance Gauges as Accurate Instruments for High Pressure Measurements," Symp. on the Accurate Characterization of the High Pressure Environment, U.S. Dept. of Commerce, N.B.S., Gaithersburg, Maryland, Oct. 14-18, 1968.
17. Bogdanov, V.S., Levin, Y.L., Skoyan, S.S. and Shimin, Y.I., "On Application of the Mercury Melting Curve for Accurate High Pressure Measurements," Symp. on the Accurate Characterization of the High Pressure Environment, U.S. Dept. of Commerce, N.B.S., Gaithersburg, Maryland, Oct. 14-18, 1968.
18. Birch, F. and Robertson, E.C., Final Report, Contract N5ori-07644, Office of Naval Research, 1957.
19. Chi-yuen Wang, Rev. Sci. Inst., 38, No. 1, 24-26, (1967).
20. Cross, J.L. and Johnson, D.P., Nat. Bur. Stds. Report No. 2900, Oct. 20, 1953.
21. Yamamoto, S., Properties of Manganin Resistance Manometer, 9th Symp. on High Pres., Chem. Soc. of Japan, Nagoya, Japan, Oct. 5, 1967.
22. Mii, H., Fujishiro, I., Senowo, M. and Nomura, T., "Press. Induced Transformations of Bi, Sn, and Fe in NaCl. Internal Std. (II)," 10th Symp. on High Pres., Chem. Soc. of Japan, Kyoto, Japan. Sept 18-20.
23. Osugi, J., Shimizu, K., Yasunami, K., Moritoki, M. and Onodera, A., "Some Remarks on Fixed Pts. of Press.," 10th Symp., Kyoto.
24. Yamamoto, S., "Seasoning of Manganin Resistance Manometer," 10th Symp., Kyoto.
25. Bett, K.E., Cappi, J.B., and Harlow, A., "A Precision Manganin Resistance Pressure Gauge," manuscript personally communicated.
Reprinted from Measurements & Data, November-December 1969

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