NAT'L INST. OF STAND & TECH R.I.C.

AlllDM TDMlflB

pUBUCAT\ons

Nisr United States Department of Commerce

Technology Administration

National Institute of Standards and Technology

NIST Technical Note 1414

Liquid-Nitrogen-Cooled High To

Electrical Substitution Radiometer as a

Broadband IR Transfer Standard

J. p. Rice and Z. M. Zhang

c

00

5753

0.1414

996
The National Institute of Standards and Technology was established in 1988 by Congress to "assist industry

in the development of technology . . . needed to improve product quality, to modernize manufacturing processes,

to ensure product reliability . . . and to facilitate rapid commercialization ... of products based on new scientific discoveries." NIST, originally founded as the National Bureau of Standards in 1901, works to strengthen U.S. industry's

competitiveness; advance science and engineering; and improve public health, safety, and the environment. One of the agency's basic functions is to develop, maintain, and retain custody of the national standards of measurement, and

provide the means and methods for comparing standards used in science, engineering, manufacturing, commerce,

industry, and education with the standards adopted or recognized by the Federal Government.

As an agency of the U.S. Commerce Department's Technology Administration, NIST conducts basic and applied research in the physical sciences and engineering, and develops measurement techniques, test methods, standards, and

related services. The Institute does generic and precompetitive work on new and advanced technologies. NIST's

research facilities are located at Gaithersburg, MD 20899, and at Boulder, CO 80303. Major technical operating units and their principal activities are listed below. For more information contact the Public Inquiries Desk, 301-975-3058.

Office of the Director

• Advanced Technology Program

• Quality Programs

• International and Academic Affairs

Technology Services

• Manufacturing Extension Partnership

• Standards Services

• Technology Commercialization

• Measurement Services

• Technology Evaluation and Assessment

• Information Services

Materials Science and Engineering

Laboratory

• Intelligent Processing of Materials

• Ceramics

• Materials Reliability'

• Polymers

• Metallurgy

• Reactor Radiation

Chemical Science and Technology

Laboratory

• Biotechnology

• Chemical Kinetics and Thermodynamics

• Analytical Chemical Research

• Process Measurements^

• Surface and Microanalysis Science

• Thermophysics^

Physics Laboratory

• Electron and Optical Physics

• Atomic Physics

• Molecular Physics

• Radiometric Physics

• Quantum Metrology

• Ionizing Radiation

• Time and Frequency'

• Quantum Physics'

Manufacturing Engineering Laboratory

• Precision Engineering

• Automated Production Technology

• Intelligent Systems

• Manufacturing Systems Integration

• Fabrication Technology

Electronics and Electrical Engineering

Laboratory

• Microelectronics

• Law Enforcement Standards

• Electricity

• Semiconductor Electronics

• Electromagnetic Fields'

• Electromagnetic Technology'

• Optoelectronics'

Building and Fire Research Laboratory

• Structures

• Building Materials

• Building Environment

• Fire Safety

• Fire Science

Computer Systems Laboratory

• Office of Enterprise Integration

• Information Systems Engineering

• Systems and Software Technology

• Computer Security

• Systems and Network Architecture

• Advanced Systems

Computing and Applied Mathematics

Laboratory

• Applied and Computational Mathematics^

• Statistical Engineering^

• Scientific Computing Environments^

• Computer Services

• Computer Systems and Communications^

• Information Systems

'Ai Boulder. CO 80303. 'Some cicmenis at Boulder. CO 80303.
NIST Technical Note 1414

Liquid'Nitrogen-Cooled High To

Electrical Substitution Radiometer as a

Broadband IR Transfer Standard

J. p. Rice and Z. M. Zhang

Radiometric Physics Division

Physics Laboratory

National Institute of Standards and Technology

Gaithersburg, MD 20899-0001

January 1996

U.S. Department of Commerce

Ronald H. Brown, Secretary

Technology Administration

Mary L. Good, Under Secretary for Technology

National Institute of Standards and Technology

Arati Prabhakar, Director
National Institute of Standards U.S. Government Printing Office For sale by the Superintendent of and Technology Washington: 1996 Documents

Technical Note 1414 U.S. Government Printing Office

Natl. Inst. Stand. Technol. Washington, DC 20402

Tech. Note 1414

14 pages (January 1996)

CODEN: NTNOEF
Table of Contents

Abstract 1

1Introduction 2

2. Absolute Electrical-Substitution Radiometers 2

3. Transfer Standard ESR at 77 K 3

3.1 Design 3

3.2 Theoretical Performance Analysis 5

3.2.1 Temperature Stability 6

3.2.2 Operating Point 6

3.2.3 Ultimate Limits of Sensitivity 7

4. Conclusion 8

5. References 8

List of Figures

1. A map of infrared transfer standard radiometers that exist or are being developed at NIST, showing where the proposed

broadband radiometer would fit in 10

2. Proposed design for a liquid-nitrogen-cooled high-Tc ESR. ... 11

Liquid-Nitrogen-Cooled High 1^

Electricai Substitution Radiometer as a

Broadband IR Transfer Standard

J. p. Rice and Z. M. Zhang

Radiometric Physics Division, National Institute of Standards and

Technology, Gaithersburg, MD 20899, USA

Abstract

A requirement exists for broadband radiometers that can be used to

transfer NIST infrared radiometric scales to calibration laboratories

elsewhere. We discuss the design of a liquid-nitrogen-cooled transfer

standard radiometer that represents a practical tradeoff between roomtemperature and liquid-helium-cooled radiometers. The detector utilizes

high-Tc superconductors as temperature sensors for increased sensitivity.

Such sensors have already been shown to enable temperature regulation of

100 ^K peak-to-peak at 85 K, and have the potential for further

improvements by three orders of magnitude. Electrical substitution is

used to linearize the response over the dynamic range and to remove

susceptibility to sensor aging effects. A reflective light trap is used in

conjunction with a gold-black coating on the sensor to enable flat

spectral response over a broad infrared band. Ultimately, the radiometer

could have a noise-equivalent power of 10 pW/Hzi/2, which is sufficient

sensitivity to perform 1% uncertainty scale transfers over the milliwatt

to nanowatt power ranges.

Keywords

infrared, radiometer, electrical-substitution, high-Tc superconductors,

temperature control
1. INTRODUCTION

Currently there are several infrared transfer radiometers that have

been developed or are being developed at NISI for various purposes, as

shown in Figure 1. Although all these radiometers can be used to transfer

a radiometric scale (i.e., radiant power, irradiance, or radiance) they

differ in many other respects. Wavelength coverage, temperature of

operation, power range, and projected uncertainties in the transfer of

radiometric scale are some of the differences. In Figure 1 we have

grouped the IR transfer radiometers according to wavelength and

temperature of operation. This is a simplified way of demonstrating

where requirements are being fulfilled and where there is important need

for more development. Electrically calibrated pyroelectric detectors,

originally developed at NIST during the 1970's and now commercially

available, are the least sensitive but most convenient because they

operate at room temperature [1]. At the other extreme are blocked

impurity band (BIB) detectors and silicon bolometers. Custom-made BIB

detectors are currently being characterized as transfer standards for

low-background infrared detection [2]. A silicon bolometer device has

been characterized recently as a transfer standard for the IR detector

comparator facility at NIST [3]. BIB detectors and silicon bolometers are

the most sensitive but must be cooled to temperatures near that of liquid

helium. At liquid-nitrogen temperatures (77K), transfer radiometers

based on InSb are being developed at NIST [4], but they are limited to

wavelengths less than 5 jim. The radiometer proposed here would fulfill the need for a broadband radiometer at 77 K for wavelengths from 5 )im to

20 |im, with the required sensitivity level for most radiometric

applications.

2. ABSOLUTE ELECTRICAL-SUBSTITUTION RADIOMETERS

Electrical-substitution radiometers (ESR) are commonly used to

establish absolute detector-based radiometric scales [5,6]. They operate

by heating a thermally isolated optical absorber with radiant power and

then with electrical power in alternate cycles. Using precision

thermometry to ensure that an equivalent temperature rise is attained by

the two heating methods, a measurement of the electrical power provides

an accurate measurement of the radiant power. While some ESR's have
been designed to work at ambient temperatures, the most sensitive

instruments are cryogenic radiometers cooled with liquid helium. At

liquid-helium temperatures (< 4.2 K) the heat capacity of materials such

as copper is very low. Thus the optical absorber can be made as a high

emissivity cavity while the time constant can be kept short enough to

complete a measurement cycle in a reasonable time. Such radiometers,

often called active-cavity radiometers, are absolute radiometers since

essentially all of the radiative power is converted to heat which is

measured by comparison to electrical power. Since they require liquid

helium for their operation, however, their use as portable transfer

standard radiometers for transferring radiometric scales is fraught with

difficulties of using bulky expensive equipment and bearing associated

costs.

3. TRANSFER STANDARD ESR AT 77 K

As transfer standards, the operation of an ESR near the temperature

of liquid nitrogen (77 K) would offer many advantages. Here the purpose

of electrical substitution is not to establish an absolute scale, but rather

to provide linearity of the radiometer over a wide dynamic range to enable

an accurate transfer of a radiometric scale from a primary facility to a

secondary facility. The advantage over a liquid-helium-cooled radiometer

is ease of use and operating cost. The heat of vaporization per volume of

liquid nitrogen is 59 times higher than that of liquid helium [7], and the

price per volume of liquid nitrogen is typically about 60 times lower.

Thus the total cryogen cost during operation is thousands of times cheaper

for liquid nitrogen operation than for liquid helium operation. The

advantage over an ambient temperature radiometer is that cooling from

300 K to 77 K reduces the background radiance by of factor of 230. Thus

as a transfer radiometer in the thermal infrared, where the precision of a

liquid-helium-cooled radiometer is often not necessary but roomtemperature background is not acceptable, a liquid-nitrogen-cooled

radiometer would be a welcome addition to satisfy the needs.

3.1 DESIGN

A simplified design for a liquid-nitrogen-cooled ESR to be developed

is illustrated in Figure 2. It consists of a temperature sensor and a heater
integrated onto a thin sapphire (or silicon micromachined) disk thermally

isolated from a heat sink. The disk is coated with a low-mass-density

infrared absorbing coating such as gold-black. The temperature sensor is

a thin film of YBa2Cu307-8 (YBCO) grown on the sapphire with a buffer

layer of Ce02. The heater is a thin film of a resistive alloy such as Ni-Cr.

Both the YBCO sensor and the heater are patterned as four-wire resistors.

The operation of the radiometer is as follows. YBCO is a high-Tc

superconductor having a sharp resistive superconducting transition near

90 K, as shown in the inset. Thus it provides a very sensitive temperature

sensor if its temperature is held near the midpoint of the resistive

transition, which we call the operating point. A feedback circuit is used

to supply the appropriate power to the heater to keep the sensor, and

hence the thermally isolated disk, at the operating point. The feedback

electronics consist of an ac bridge to monitor the four-wire resistance of

the YBCO sensor, a lock-in amplifier to demodulate the ac signal into a dc

signal, and a dc amplifier to drive the heater. The electrical power

supplied to the heater is measured as the product of the voltage across

the heater and the current through it. With the radiometer shutter closed,

a certain amount of electrical power is required to keep the sensor at the

operating point. When the shutter is opened, the radiant power

illuminating the disk will change, and hence the electrical power supplied

to the heater will change in order to keep the sensor at the operating

point. The difference in electrical power supplied to the heater is then a

measure of the difference in radiant power absorbed by the disk between

the shutter open and shutter closed conditions. This balancing between

radiant and electrical power provides an inherently linear measure of the

radiant power over the full dynamic range of the instrument.

Heat capacities of materials are relatively high at liquid nitrogen

temperatures, so it is necessary to minimize the sizes of components

which potentially heat and cool during measurements. Thus in the design

above we have incorporated a gold-coated reflective light trap in

conjunction with the gold-black coating on the disk. In this design, only

the disk heats. The radiation enters through a hole in the reflective light

trap and most rays are absorbed by the gold-black. The reflective light

trap redirects scattered rays toward the gold-black, thus increasing the

chances that they will ultimately be absorbed on the disk. It has been

shown that the spectral response of gold-black in such a reflective light

trap is much flatter than that for gold-black alone [8].
3.2 THEORETICAL PERFORMANCE ANALYSIS

As a first example, consider a design where the disk is at 90 K and

the heat sink is held at 77 K by good thermal contact with the nitrogen

bath. The maximum power Pmax that can be measured is determined by

P..X = GAT, (1)

where G is the thermal conductance between the disk and heat sink and AT

is the maximum allowable temperature difference between the disk and

heat sink. Assume that G = 10"* W/K (a practical value) and AT = 10 K.

Then Pmax = 1 niW, which corresponds roughly to the typical laser power

routinely used for calibrations in the High Accuracy Cryogenic Radiometer

(HACR), a liquid-helium ESR which serves as the primary standard for

optical power in the Radiometric Physics Division at NIST.

The time constant for temperature changes is given by

x = C/G, (2)

where C is the heat capacity of the thermally-isolated components.

Assuming that the sapphire disk is 5 mm in diameter, 25 p.m thick, and

dominates the heat capacities of the thin films, C = 0.15 mJ/K at 90 K.

This gives x= 1.5 s, which is a practical value.

To estimate Pmin, the minimum power that can be calibrated at the

desired accuracy, we need to know the noise floor power Pnf. A typical

measurement cycle would take place over a time interval on the order of

100 time-constants. The ability to control temperature over this time

interval plays a role in determining Pnf according to

P^ = g7(5T,)' + (6TJ' , (3)

where 5Td and 5Th are the temperature stability of the disk and heat sink,

respectively. As discussed below, we estimate 5Td = 5Th = 100 |iK over

several minutes. Thus Equation (3) yields Pnf = 1.4 xlO'® W. To allow for

a relative expanded uncertainty of 1%, Pmin = lOOPnf = 1.4 |iW. Thus, this

transfer radiometer would enable a scale comparison from milliwatt

power levels to microwatt power levels at the 1% relative expanded
uncertainty level. This assumes, of course, that other considerations do

not degrade the accuracy. This level of sensitivity is roughly equivalent

to that quoted for commercially available room-temperature electrically

calibrated pyroelectric radiometers [9]. If temperature stability can be

made even better, as we discuss below, Pmin will likewise be lower and

the dynamic range will increase.

3.2.1 TEMPERATURE STABILITY

We now consider the temperature stability attainable using YBCO

sensors. Peak-to-peak temperature stability of 100 )iK over several

minutes has recently been achieved by the group of D. Robbes using a YBCO

strip and heater in a temperature control feedback loop [10]. The stage

being controlled was a cold finger made of an aluminum alloy having

C = 0.49 J/K in thermal contact with a liquid-nitrogen bath by a G of

50 mW/K. This stage is akin to what would be the heat sink in our

radiometer above. The stability under temperature control was several

times better than that achieved by having the cold finger in contact with

nitrogen and without controlling the temperature. This suggests that a

design involving independent temperature control for both the disk and the

heat sink, with a superconductive sensor on both disk and heat sink, would

be superior, since by controlling the temperature of the heat sink the

fluctuations of liquid nitrogen temperature from effects such as

atmospheric pressure fluctuations would be greatly reduced. The change

in the boiling point of liquid nitrogen with pressure is about 83 |iK/Pa

(11 mK/Torr) [7]. Since the disk is further isolated, we would expect to

attain as good or better stability for the disk temperature. Thus the

assumption of 100 ^K temperature stability for both disk and heat sink is

conservative.

3.2.2 OPERATING POINT

In the discussion above, we have assumed that the operating point

for each sensor is at the midpoint of the YBCO resistive transition. In order to maintain a temperature difference of AT = 10 K between heat sink

and disk, the two superconductive sensors must have Tc's that differ by

10 K. This presents a challenge, since pure YBCO films typically have a

1 K wide transition at 90 K. The heat sink sensor, which would require Tc
near 80 K, would need to be made from either YBCO doped with impurities

to reduce Tc or another high Tc material. An alternative solution is suggested by the experiments of Robbes, where the temperature

dependence of the critical current just below Tc is used as a

thermometer [10]. The critical current (Ic) is the current that drives the

sensor from the superconducting to the normal state. It is a strong

function of temperature just below Tc, dropping to zero at Tc. Using a bias

reversal technique and the appropriate compensation electronics, Robbes'

group demonstrated a method for using this sensitive variation of Ic with

temperature to measure temperature over a range of about 5 K below Tc in YBCO. The 100 |iK temperature stability quoted above was achieved using

this technique a few Kelvin below Tc. Thus, since the operating point

does not have to be at Tc, YBCO sensors having identical values of Tc may

be useable as both the disk and heat sink sensors.

3.2.3 ULTIMATE LIMITS OF SENSITIVITY

From a consideration of the minimum detectable temperature

fluctuation, or noise equivalent temperature (NET), we can determine the

ultimate limits on temperature stability and sensitivity. The lowest

values of NET measured until now on YBCO sensors are below

1 X 10'^ K/Vhz [11,12]. This is close to the so-called phonon noise

contribution to the NET, which is a result of thermodynamic temperature

fluctuations:

4koT^

NKT,. = ^^ (4)

With G =10'"^ W/K and T = 90 K this is 7 x

10"® K/VHi". Thus, for a

bandwidth of 1 Hz the ultimate temperature stability is about 70 nK, so it

is feasible that we could improve on the 100 |iK stability used in our

estimate above by more than three orders of magnitude [13]. A

temperature stability of 70 nK would lead to a Pnt of 10 pW, surpassing

the sensitivity of the electrically calibrated pyroelectric detectors by a

factor of 1000. At this level of performance, scale comparisons at the 1%

relative expanded uncertainty level could be made between milliwatt

power levels and nanowatt power levels.
4. CONCLUSION

We have outlined the design and estimated the performance level for a

liquid-nitrogen-cooled high-Tc superconductive infrared radiometer that

offers a practical tradeoff between cost, convenience, and sensitivity. It will be a broadband detector, will have an ultimate sensitivity of as low

as 10 pW, and will be capable of measuring radiant power levels up to

1 mW.

5. REFERENCES

[1] R. J. Phelan, J. H. Lehman, and D. R. Larson, "Electrically calibrated

pyroelectric detector - refinements for improved optical power

measurements," SPIE 2Q2Z, 160 (1993).

[2] S. L. Lorentz, Radiometric Physics Division, MIST, Gaithersburg,

(private communication).

[3] G. Eppeldauer, A. L. Migdall, and 0. L. Cromer, "Characterization of a

high sensitivity composite silicon bolometer," Metrologia 211, 317-

320 (1993).

[4] G. Eppeldauer, Radiometric Physics Division, MIST, Gaithersburg,

(private communication).

[5] R. U. Datia, K. Stock, A. C. Parr, C. C. Hoyt, P. J. Miller, and P. V. Foukal,

"Characterization of an absolute cryogenic radiometer (ACR) as a

standard detector for radiant power measurements," Appl. Opt. ^, pp.

7219-7225 (1992).

[6] J. E. Martin, N. P. Fox, and P. J. Key, "A cryogenic radiometer for

absolute radiometric measurements," Metrologia £1, 147-155 (1985).

[7] Experimental techniques in low-temperature physics by G. K. White

(Oxford, New York, 1968).

8
[8] G. W. Day, C. A. Hamilton, and K. W. Pyatt, "Spectral reference detector

for the visible to 12 ^im region; convenient, spectrally flat," Appl. Opt.

15., 1865 (1976).

[9] Rs-5900 ECPR Product Literature, Laser Probe Inc., Utica, New York.

[10] E. Lesquey, C. Gunther, S. Flament, R. Desfeux, J. F. Hamet, and D.

Robbes, "Progress towards a low noise temperature regulation using a

superconductive high Tc microbridge," preprint submitted to the 1994

Applied Superconductivity Conference.

[11] J. C. Brasunas and B. Lakew, "Transition-edge noise in YBa2Cu307-x

thin films before and after exposure to ionizing radiation,"

J. Appl. Phys. Z^, 7565 (1994).

[12]S. Verghese, P. L. Richards, K. Char, D. K. Fork, and T. H. Geballe,

"Feasibility of infrared imaging arrays using high-Tc superconducting

bolometers," J. Appl. Phys. 21, 2491 (1992).

[13]D. G. McDonald, Boulder Metric, Boulder, Colorado (private

communication).
300

Electr cally-calibrated Pyroelectric

. InGaAs

100 - —InSb

\c Need for a broadband radiometeT]^

Temperature

(K)

BIB detectors

1 10

1 1

4 • f Silicon Bolometer

1

i i

1

1 1 1 1 10 15 20 25

Wavelength (^im)

Figure 1. A map of infrared transfer standard radiometers that exist or are being developed at NIST, showing where the proposed broadband

radiometer would fit in.

10
REFLECTIVE LIGHT TRAP

INCOMING

RADIANT

POWER

LOCK-IN

AMPLIFIER

THERMALLY-ISOLATED

GOLD-BLACK-COATED DISK

AMP

Operating

' point

YBCO

SHUTTER

CLOSED

SHUTTER

OPEN

Figure 2. Proposed design for a liquid-nitrogen-cooled high Tc ESR.

11

NISTTechnical Publications

Periodical

Journal of Research of the National Institute of Standards and Technology—Reports NIST research and development in those disciplines of the physical and engineering sciences in which the Institute is active. These include physics, chemistry, engineering, mathematics, and computer sciences. Papers cover a broad range of subjects, with major emphasis on measurement methodology and the basic technology

underlying standardization. Also included from time to time are survey articles on topics closely related to the Institute's technical and scientific programs. Issued six times a year.

Nonperiodicals

Monographs—Major contributions to the technical literature on various subjects related to the

Institute's scientific and technical activities. Handbooks—Recommended codes of engineering and industrial practice (including safety codes) devel- oped in cooperation with interested industries, professional organizations, and regulatory bodies. Special Publications—Include proceedings of conferences sponsored by NIST, NIST annual reports, and

other special publications appropriate to this grouping such as wall charts, pocket cards, and bibliographies.

National Standard Reference Data Series—Provides quantitative data on the physical and chemical

properties of materials, compiled from the world's literature and critically evaluated. Developed under a worldwide program coordinated by NIST under the authority of the National Standard Data Act (Public

Law 90-396). NOTE: The Journal of Physical and Chemical Reference Data (JPCRD) is published

bimonthly for NIST by the American Chemical Society (ACS) and the American Institute of Physics (AIP).

Subscriptions, reprints, and supplements are available from ACS, 1155 Sixteenth St., NW, Washington, DC

20056.

Building Science Series—Disseminates technical information developed at the Institute on building

materials, components, systems, and whole structures. The series presents research results, test methods, and

performance criteria related to the structural and environmental functions and the durability and safety

characteristics of building elements and systems.

Technical Notes—Studies or reports which are complete in themselves but restrictive in their treatment of

a subject. Analogous to monographs but not so comprehensive in scope or definitive in treatment of the subject area. Often serve as a vehicle for final reports of work performed at NIST under the sponsorship of

other government agencies.

Voluntary Product Standards—Developed under procedures published by the Department of Commerce

in Part 10, Title 15, of the Code of Federal Regulations. The standards establish nationally recognized

requirements for products, and provide all concerned interests with a basis for common understanding of

the characteristics of the products. NIST administers this program in support of the efforts of private-sector

standardizing organizations.

Order the following NIST publications—FIPS and NISTlRs—from the National Technical Information

Service, Springfield, VA 22161.

Federal Information Processing Standards Publications (FIPS PUB)—Publications in this series

collectively constitute the Federal Information Processing Standards Register. The Register serves as the

official source of information in the Federal Government regarding standards issued by NIST pursuant to the Federal Property and Administrative Services Act of 1949 as amended, Public Law 89-306 (79 Stat.

1 127), and as implemented by Executive Order 11717 (38 FR 12315, dated May 11, 1973) and Part 6 of

Title 15 CFR (Code of Federal Regulations).

NIST Interagency Reports (NISTIR)—A special series of interim or final reports on work performed by

NIST for outside sponsors (both government and nongovernment). In general, initial distribution is handled

by the sponsor; public distribution is by the National Technical Information Service, Springfield. VA 22161,

in paper copy or microfiche form.
9t

E

EoU

8

o on is

o> _ O I 3Z

Q (/) ;^ >,S u

rt W) . c > 3 £

OQ

.o

c5> '^ >» io O £