Cryogenics 132 (2023) 103671

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Cryogenics
journal homepage: www.elsevier.com/locate/cryogenics

Preliminary development of emissivity measurement system at low

temperature based on radiometric method
Yuchen Zhao a, c, 1, Xu Li b, 1, Hengcheng Zhang a, *, Fuzhi Shen a, *, Chuanjun Huang a,
Huiming Liu a, Haoying Qi a, c, Zichun Huang a, c, Zhen Geng a, c, Jijun Xin d, Wei Wang d,
Laifeng Li a, c
a
State Key Laboratory of Technologies in Space Cryogenic Propellants, Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100190, China
b
Institute for Quantum Information & State Key Laboratory of High Performance Computing, College of Computer Science and Technology, National University of
Defense Technology, Changsha 410073, China
c
University of Chinese Academy of Sciences, Beijing 100049, China
d
Songshan Lake Materials Laboratory, Dongguan, Guangdong 523808, China

A R T I C L E I N F O A B S T R A C T

Keywords: Thermal radiation is a major part of heat transfer in cryogenic systems, especially in vacuum environment. The
Emissivity measurement emissivity of materials is an essential factor of thermal radiation, which is difficult to be precisely predicted by
Direct method theoretical calculation. Thus, the direct experimental measurement becomes an inevitable, reliable method. In
Low temperature
this paper, a preliminary emissivity measurement system using the direct radiometric method was designed and
Functional radiation materials
built with a G-M (Gifford-McMahon) cryocooler as the cold source. The sample plate in the apparatus can be
cooled to 9.2 K, while the sample thermal radiation shield and the optical path cover can respectively reach 46.7
K and 46.9 K. At present stage, MCT (HgCdTe) detector with an effective bandwidth 2–12 μm was used in this
system, which achieved the measurements of emissivities of coating Nextel 811–21, 304 stainless steel and G10
composite from 240 K to 300 K. The reliability of the system was verified by comparing the measurement results
with the data already published, and the dependence of the emissivities of these materials on temperature are
analyzed.

1. Introduction cryogenic radiative properties is needed for optimization of functional

As an important part of heat transfer at cryogenic temperatures,
thermal radiation has a significant influence on various cryogenic sys­
tems [1]. For different cryogenic applications, the demand on the
emissivity of the materials varied. High emissivity is required for
improving radiation heat transfer to take heat out of cryogenic system,
while low emissivity is required for decreasing the radiation to reduce
the heat leak into cryogenic system. For instance, in order to guarantee
the operation of the Planck satellite telescope at space, high emissivity
coating on supporting substrates is vital to maintain the temperature of
the telescope at 50 K by increasing the passive cooling procedure be­
tween the satellite and the deep space [2]. In another case, coating with
extremely low emissivity is needed to suppress the radiation flux be­
tween the cooling tube of the James Webb Space Telescope and the
warm surrounding environment [3]. Thus, the investigation of
material properties and for thermal design of cryogenic system.
The radiative properties of materials have been demonstrated to be
associated with several factors, i.e., the material’s composition, tem­
perature, as well as surface roughness [1], which makes it difficult to
accurately calculate the emissivity of materials from the theory. Thus, it
is crucial to experimentally determine the radiative properties of various
materials at cryogenic temperatures.
Emissivity measurement at cryogenic temperature is very chal­
lenging due to the fact that the thermal radiation power depends
strongly on the temperature of the radiator, and can turn very weak at
low temperature. The current methods for the emissivity measurement
at different temperatures can be divided into two categories, the calo­
rimetric method and the radiometric method [1]. As a simple and widely
used method, the calorimetric method usually has a radiator and a
receiver, and the sample can serve as the radiator or the absorber with

* Corresponding authors.
E-mail addresses: zhanghengcheng@mail.ipc.ac.cn (H. Zhang), shenfuzhi@mail.ipc.ac.cn (F. Shen).
1
These authors contributed to the work equally and should be regarded as co-first authors.

https://doi.org/10.1016/j.cryogenics.2023.103671
Received 5 January 2023; Received in revised form 26 March 2023; Accepted 31 March 2023
Available online 2 April 2023
0011-2275/© 2023 Published by Elsevier Ltd.
Y. Zhao et al.
Fig. 1. Schematic of the measurement method of emissivity.
the radiative property of another part is known already. By detecting the
heat transferred from the radiator to the absorber, radiative properties
and total hemispherical emissivity of the sample can be calculated [1].
Tuttle J et. al measured the thermal absorptance of a gold-plated tubing
with different samples and surrounding temperatures to confirm the
cryocooler can meet the requirements of MIRI on James Webb Space
Telescope by using this method [3]. Besides, Ando M et. al measured
emissivities of several kinds of black coating and compared the emis­
sivity of flat surface with that of open honeycomb surface at tempera­
tures from 80 K to 20 K [4]. Musilova V et. al also measured emissivities
of several metallic materials between 30 K and 140 K, and presented the
influence of different sample treatments on the radiative properties [5].
However, it usually required a very long time for thermal equilibrium
between the radiator and the absorber. Moreover, the spectral emissivity
of materials cannot be measured by using this method.
In contrast to the calorimetric method, the radiometric method is
more complex but takes less time to obtain the radiative properties of
sample, and the spectral emissivity of materials can also be measured by
this method. A reference blackbody is usually needed in this method and
the emitted or reflected radiation from a sample and a blackbody at
same temperature will be measured by a sensitive detector respectively
[1,2,6–8]. The emissivity of the sample can be calculated in this way by
comparing the radiation power of the sample with the radiation power
of the blackbody. Measuring the reflected radiation can be an alternative
method, but it is unsuitable for measuring the emissivity of transparent
sample, since the relationship ε = 1 − ρ is invalid [2]. Thus, detecting the
emitted radiation from sample and reference blackbody directly can be
an appropriate method. To measure the emissivity of blackbody coatings
at cryogenic temperatures, Herve P et. al built an emissivity measure­
ment apparatus which used direct method, and emissivities of several
Fig. 2. Schematic of the emissivity measurement apparatus. (1) G-M cryocooler, (2) Cryocooler vacuum enclosure, (3) Cryocooler thermal radiation shield, (4) Disc
type bellows, (5) OFHC braids, (6) Sample vacuum enclosure, (7) Sample thermal radiation shield, (8) Stepping motor, (9) Magnetic fluid seal, (10) G10 rods;
Temperature measurement position: I-1st base plate, II-MCT detector, III-Optical path cover, IV-Sample plate.
2
Cryogenics 132 (2023) 103671
kinds of blackbody coatings were measured and analyzed [2]. Cold
shield cooled by liquid nitrogen was used in system to minimize the
influence of the signal of the background because that the radiation
signal of the sample is very weak compared to the background at
cryogenic temperature. Hao et. al used this method to reduce the in­
fluence of the background, and built an apparatus with a FTIR spec­
trometer to calibrate infrared remote sensors on metrological satellites
[7]. As an important part of these systems above, detector is all placed
outside the vacuum chamber, and the optical window and thermal ra­
diation of atmosphere will have influences on the measurement results.
Besides, the cold shield was all at liquid nitrogen temperature, which
can be lowered to further reduce the influence of the background.
In the present work, a preliminary emissivity measurement system
using direct radiometric method was designed and built. The measure­
ment method is described in section 2, while the experimental apparatus
is introduced in section 3. Uncertainty of this system is analyzed in
section 4. Finally, emissivities of coating Nextel 811–21, 304 stainless
steel and G10 composite were measured, and the results and tempera­
ture curves are discussed in section 5.
2. Measurement method
Fig. 1 shows the schematic diagram of this system. Two samples, gold
plane mirror and blackbody were placed in four directions and were
maintained at the same temperature. The lower off-axis parabolic gold
mirror can be rotated and can collect and reflect the emitted and re­
flected radiation power from the samples, gold plane mirror and
blackbody to the upper off-axis parabolic gold mirror in turn, and the
radiation power received by the detector can be listed as follows:
⎧ ( )2 ( )
⎪ 0 e1 e2
⎪ Ls (T) = 1 − εpm εs (T)Lλ (T) + (1 − εs (T) )Lλ (Te ) + Lλ (Te )
⎪
⎨
( )2 ( )
Lb (T) = 1 − εpm εb (T)L0λ (T) + (1 − εb (T) )Lλe1 (Te ) + Le2
λ (Te )
(1)
⎪
⎪
⎩ L (T) = ( 1 − ε )2 ( ε (T)L0 (T) + (1 − ε (T))Le1 (T ) ) + Le2 (T )
⎪
m pm m λ m λ e λ e
Where,
Ls (T), Lb (T), Lm (T) – The radiation power collected by the detector
from the sample, blackbody, and gold plane mirror at temperature T.
εpm – The emissivity of the off-axis parabolic gold mirror at tem­
perature Tpm .
L0λ (T) – The radiation power calculated as σT 4 at temperature T, σ is
Stefan–Boltzmann constant.
Y. Zhao et al.
Fig. 3. Photos of the optical measurement system: (a) Position calibration of the optical system; (b) The detector installation diagram.
Le1
λ (Te ) – The radiation power projected on the sample, gold plane
mirror and blackbody from surroundings at temperature Te .
εs (T) – The emissivity of sample at temperature T.
εb (T) – The emissivity of blackbody at temperature T (≈ 1).
εm (T) – The emissivity of gold plane mirror at temperature T (≈ 0).
Le2
λ (Te ) – The radiation power of detector surrounding at temperature
Te .
The radiation power emitted from the sample can be denoted as
εs (T)L0λ (T). Besides, while the sample is non-transparent, the reflectivity
of the sample has the relationship ρs (T) = 1 − εs (T), the radiation power
from the surrounding reflected by the sample can be expressed as
(1 − εs (T) )Le1
λ (Te ). The reflectivity of the off-axis parabolic gold mirror is
extremely high and also can be seen as ρpm = 1 − εpm . Furthermore, the
radiation power from surrounding of detector Le2 λ (Te ) are also collected
by the detector. Thus, the formula of Ls (T) of eq. (1) can be deduced, and
the radiation power collected by the detector from the blackbody and
gold plane mirror are similarly expressed.
In this system, a copper cavity coated with blackbody painting with
very high emissivity served as reference blackbody. Benefiting from the
cavity design, the multiple reflections will increase the light capture
ability of the blackbody, thus the emissivity of the blackbody εb (T) can
be considered as 1. The gold plane mirror has also been carefully
selected, whose emissivity εm (T) can be considered as zero. With these
values and using eq.1, the emissivity of test sample can be obtained as:
Ls (T) − Lm (T)
εs (T) =
Lb (T) − Lm (T)
3. Experimental apparatus
3.1. Emissivity measurement system
Fig. 2 shows the schematic of the emissivity measurement apparatus.
The cryogenic environment was provided through a two-stage G-M
cryocooler (Sumitomo model RDK-415D, with a cooling capacity of 1.5
W@4.2 K). As shown in Fig. 2(a), the cryocooler was connected to the
vacuum enclosure by a disc type bellows to decrease the influence of
vibration of the G-M cryocooler on the measurement. The cryocooler has
a radiation shield installed on its first stage, which was connected to the
1st base plate by four OFHC (oxygen-free high-conductivity copper)
braids to dampen the vibration from the G-M cryocooler. To lessen the
deformation of the 1st base plate, a thin 304 stainless steel plate was
used as the backing. The 1st base plate was fixed to the lower flange of
the vacuum enclosure by four G10 rods to reduce the thermal conduc­
tion loss. The sample thermal radiation shield was installed on the 1st
base plate, which is 450 mm in diameter and 330 mm in high. These two
Cryogenics 132 (2023) 103671
thermal radiation shields were all covered by 30 layers of commercial
multi-layer insulation (MLI) to reduce the heat leakage. With the usage
of sample thermal radiation shield, the cooling load of the 2nd stage of
the G-M cryocooler can be reduced.
Fig. 2(b) shows the schematic diagram of optical measurement sys­
tem. The samples, gold plane mirror and blackbody were all attached to
the sample plate in four directions with the usage of indium foil and
cryogenic grease (Apiezon N), which was connected to the 2nd stage of
the G-M cryocooler using four OFHC braids. Similar to the 1st base plate,
another 304 stainless steel backing was placed at the backside. The
whole plate was fixed to the 1st base plate with four G10 rods.
The sample was secured by bolts on an OFHC holder, which had a
diameter of 25.4 mm and a thickness of 6 mm. The gold plane mirror
(25.4 mm in diameter and 6 mm in thickness, Thorlabs model PF10-03-
M03) was selected carefully with the average reflectance of the gold
plane mirror being more than 0.98, and was secured by the cryogenic
glue on a holder. The blackbody is a cylindrical cavity whose diameter
was 30 mm with conical bottom [9]. As shown in Fig. 3(a), blackbody
coating (Nextel 811–21) was coated inside the inner of the blackbody.
By using ray tracing simulation, the emissivity of the blackbody cavity
can maintain 0.996 even if the emissivity of the blackbody coating re­
duces to 0.7.
Two off-axis parabolic gold mirrors (Thorlabs model MPD229-M03,
50.8 mm in diameter) were used in this system. A cold optical path cover
made from OFHC with inner surface coated with blackbody coating was
fixed on the 1st base plate, and was placed around these two off-axis
(2) parabolic gold mirrors to minimize the influence of the ambient radia­
tion. The upper mirror was fixed to the optical path cover while the
lower mirror was rotated by a stepping motor (Oriental motor model
AZM69M0K). Due to the sliding contact between the lower mirror with
its surroundings, its temperature may be higher than the 1st base plate.
However, according to the deduction process of Eq. (2), the influence is
minimum. Since the stepping motor was put outside the vacuum
chamber, a magnetic fluid seal was used in this system to maintain high
vacuum while the lower off-axis parabolic mirror was rotated by the
motor. Fig. 3(a) shows the position calibration of the optical measure­
ment system. A red light laser and a calibration plate were used to
determine the starting rotation angle of the system. Two ceramic bear­
ings were used to guarantee a stable rotation. Besides, Fig. 3(a) shows
that an extra inner shield with a 90◦ opening was put around the lower
off-axis parabolic gold mirror, which can suppress the influence of ra­
diation signal from the other three objects while measuring one of the
four objects.
An MCT (HgCdTe) detector with an effective bandwidth 2–12 μm
(VIGO system model PVM-10.6) was fixed to a side of the optical path
cover, as shown in Fig. 3(b). It was cooled by the 1st base plate through
two OFHC braids. To reduce the heat leakage from the detector to the
3
Y. Zhao et al.
Table 1
Uncertainty of the emissivity measurement.
T u1 u2 u3 u4 U resistance thermometer had a calibration interval of 0.05 Ω at resis­
240 K 0.001 0.00003 0.004 0.02 0.0204
optical path cover, a G10 block with a center hole was used in between,
and the polyetheretherketone (PEEK) bolts were also used to minimize
the heat leakage.
3.2. Control and instrumentation system
As shown in Fig. 2(a), eight 5 Ω resistors (CADDOCK ELECTRONICS
model MP930) and a thermometer (rhodium-iron resistance thermom­
eter, calibrated in range of 1.5 K to 300 K) were attached to the sample
plate while two 5 Ω resistors and a thermometer (PT100 resistance
thermometer, calibrated in range of 20 K to 300 K) were placed around
the detector to measure and control the temperatures of sample plate
and detector through a temperature controller (Lake Shore Cryotronics
model 336). Besides, there were two thermometers (PT100) placed in
the 1st base plate and the optical path cover, which were connected to a
digital multimeter (Keithley TEKTRONIX model 6510) to measure the
temperatures. The stepping motor was driven by a controller (Oriental
motor model AZD-KX) to rotate the lower off-axis parabolic gold mirror
90◦ at a time to switch the radiation power source. The radiation power
detected by the MCT detector was transformed into voltage signal and
sent to a nanovoltmeter (Keithley TEKTRONIX model 2182A). All of
above instruments were connected to a personal computer and were
controlled by LabVIEW.
3.3. Uncertainty analysis
The expanded standard uncertainty of the system was derived from
several factors, including the thermometer, system temperature fluctu­
ation, the measurement instrument and the emissivity of the gold plane
mirror and blackbody, which can be described as [7]:
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
U = u21 + u22 + u23 + u24 (3)
Fig. 4. Temperature controlling during emissivity measurement.
4
Cryogenics 132 (2023) 103671
The thermometers used in the system were rhodium-iron resistance
thermometers and PT100 resistance thermometers. The rhodium-iron
tance below 10 Ω and 0.1 Ω when the resistance exceeds 10 Ω. The
PT100 resistance thermometer was calibrated at 0.5 K intervals at
temperatures below 77 K and 1 K intervals at temperatures between 77
and 300 K. Both thermometers have an uncertainty ΔT1 better than
0.010 K. The temperature fluctuation is mainly influenced by the
temperature-controlled accuracy, which ΔT2 can reach 0.060 K at 300 K
by using the Lakeshore 336 temperature controller provided by the
manufacturer. Thus, the influence of the temperature can be donated by
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
u1 , which can be seen as 4 • (ΔT21 + ΔT22 )/T [1,10].
The influence of the measurement instrument can be donated by u2 ,
and consists of the voltage measurement accuracy of the Keithley
2182A, which is 0.003 % provided by the manufacturer.
The influence of the blackbody cavity and the gold plane mirror can
be donated by u3 and u4 . By assuming the emissivity of blackbody as 1
and the emissivity of gold plane mirror as 0, the eq. (2) can be deduced.
As mentioned above, the emissivity of the blackbody cavity can main­
tain 0.996, and the reflectivity of the gold plane mirror can be above
0.98, and the uncertainty of the blackbody can be no more than 0.004
while the uncertainty of the gold plane mirror can be no more than
0.020 [2].
Thus, the uncertainty of the system can be calculated by using eq.
(3), and is less than 2.040 % when the temperature is higher than 240 K
as shown in Table 1.
4. Experimental results and discussion
4.1. Cooling and temperature controlling
Due to the good thermal contact between 1st base plate and the
sample thermal radiation shield, the temperature of these two parts can
be considered the same. The sample plate and the entire system reached
stable conditions in 18 h and 22 h respectively. The sample plate, the
sample thermal radiation shield, the optical path cover and the detector
reached 9.2 K, 46.7 K, 46.9 K and 50.6 K, respectively.
Once the system achieved thermal equilibrium, the temperatures of
the sample plate and the detector were controlled by the Model 336
Y. Zhao et al.
Fig. 5. Photos of the samples: (a) Coating Nextel 811–21; (b) Polished 304 stainless steel; (c) Polished G10.
Fig. 6. Dependence of emissivity on the temperature of the coating Nextel 811–21, polished 304 stainless steel and G10.
temperature controller. The temperature control curves of the sample
plate and the detector are shown in Fig. 4. The temperature of the
sample plate can be controlled between 160 K and 300 K at 10 K in­
tervals. When the sample plate was under 270 K, the detector was
controlled at 77 K, and when the sample plate was above 270 K the
temperature of detector was controlled to be 90 K. The temperatures of
the sample thermal radiation shield and the optical path cover were
under 64 K during the temperature control procedure, which indicated
that the influence of environmental radiation on the measurement was
effectively reduced. Fig. 4 also shows the detector and sample plate
temperature fluctuation with the temperature controller. It can be
concluded from the figure that the temperature fluctuations were within
5 mK, and therefore had a negligible effect on the measurements.
4.2. Experimental results
Three materials widely used in cryogenic systems were selected and
measured, i.e., a kind of blackbody coating (Nextel 811–21, surface
roughness Ra = 5.549μm), metallic material (304 stainless steel, Ra =
0.849μm) and non-metallic material (G10, Ra = 1.528μm). The coating
was sprayed onto the aluminum surface by compressed air. The surface
of the 304 stainless steel and G10 were polished. The photos of the
samples are shown in Fig. 5.
After the objects of sample plate and detector temperatures were
5
Cryogenics 132 (2023) 103671
stabilized, the lower off-axis parabolic gold mirror was rotated accord­
ing to the experimental procedure. The detector collected the radiation
power from different objects on the sample plate and converted it to
voltage values. The emissivities of the samples were calculated by using
the eq. (2), and the results are shown in Fig. 6.
As can be seen in Fig. 6, the emissivity of the coating Nextel 811–21
changed within the range from 0.951 to 0.941, at the temperature be­
tween 240 K and 300 K. The emissivity of the coating was 0.949 when
the temperature was 300 K, which is close to the experimental value
(0.941, 298.15 K) in [11]. The measurement at room temperature with
FTIR (Fourier Transform Infrared Spectroscopy, Bruker INVENIO S) was
carried out, and the value (0.955) was also close to the result from this
apparatus. It can be concluded that the emissivity of this coating during
2–12 μm is not extremely sensitive to the temperature from 240 K to 300
K. Difference in surface roughness may cause the different emissivity,
but the trend is similar to [12].
The emissivity measurement results of 304 stainless steel are also
shown in Fig. 6. The emissivity of 304 stainless steel decreased from
0.186 to 0.155 when the temperature decreased from 300 K to 240 K.
The result at 300 K was close to the measurement with FTIR at room
temperature (0.190). [13] points out that, as a kind of thermally-
emitting sample, there is no relationship between emissivity and
wavelength, and the temperature dependence of emissivity is propor­
tional to the resistivity of the sample. The resistivity of the 304 stainless
Y. Zhao et al.
steel decreased with the temperature decreasing, thus the emissivity also
decreased, which is similar to the polished SS304L measured in [11].
Unlike the metallic material, the emissivity of the polished G10
fiberglass-epoxy laminate had a different trend with temperature. The
emissivity increased from 0.889 to 0.910 with the temperature
decreased from 300 K to 240 K, which is similar to the glass that has an
infrared cutoff [13].
5. Conclusion
A preliminary emissivity measurement system with all optical mea­
surement system being placed in the vacuum chamber was designed and
built in this paper. By using cryogenic thermal radiation shield and
optical path cover, the influence of the ambient radiation was reduced
effectively. The measured objects, including the samples, gold plane
mirror and blackbody were all attached to the sample plate in four di­
rections. A G-M (Gifford-McMahon) cryocooler was used to cool down
the radiation shield and the sample plate through OFHC (oxygen-free
high-conductivity copper) braids. By driving a stepping motor, the ra­
diation power signal received by the detector can be switched one by
one. Limited by the effective bandwidth of MCT (HgCdTe) detector,
which was 2–12 μm, emissivity measurements were performed at tem­
peratures ranging from 240 K to 300 K. Using gold plane mirror and
blackbody measurements as the reference, emissivities of the coating
Nextel 811–21, 304 stainless steel and G10 were measured. It was
observed that the emissivity of the coating Nextel 811–21 had no
extreme sensitive to temperature between 240 K and 300 K. The emis­
sivity of 304 stainless steel decreased when the temperature decreased
from 300 K to 240 K. Emissivity of G10 has a different trend with its
temperature. Bolometer with wider effective band will be used in the
future to achieve the detection at cryogenic temperature, and the design
of the system will also be improved.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
No data was used for the research described in the article.
Cryogenics 132 (2023) 103671
Acknowledgement
This work was supported by the National Key R&D Program of China
(Grant No.: 2022YFB3804003), the National Natural Science Founda­
tion of China (Grant Nos.: 52007186), the Key Research Program of the
Chinese Academy of Sciences (Grant No.: ZDRW-CN-2021-4-1), and the
Scientific Instrument Developing Project of Chinese Academy of Sci­
ences (Grant No.: YJKYYQ20200070).
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