Materials Chemistry and Physics 310 (2023) 128472
Contents lists available at ScienceDirect
Materials Chemistry and Physics
journal homepage: www.elsevier.com/locate/matchemphys
On the possibility of obtaining thermal control coatings for spacecraft
by printing
M.M. Mikhailov , A.N. Lapin , S.A. Yuryev *, V.A. Goronchko , S.A. Artishchev , N.S. Trufanova ,
O.A. Mikhailova , D.S. Fedosov
Tomsk State University of Control Systems and Radielectronics, 634050, 40 Lenina St., Tomsk, Russia
H I G H L I G H T S
• The printing method for obtaining reflective coatings was suggested.
• Two types of coatings based on conductor and dielectric pastes (inks) were obtained.
• The properties and diffuse reflectance spectra of the resulting coatings were studied.
• The solar absorptance values correspond to the “Optical Solar Reflector” class.
A R T I C L E I N F O
A B S T R A C T
Keywords:
Thermal control coatings
PCB printing
Reflectance
Aluminum oxide
Silver
There has been considered a method to produce “Optical Solar Reflector” (OSR) class thermal control coatings
(TCC) for spacecraft by applying a paste of required composition on a substrate by a printed circuit boards (PCB)
printer. 2 types of pastes were applied: dielectric ceramic paste (DCP), consisting of a filler – ground polycor
(Al2O3) – and a solvent with a thickener (terpineol with ethyl cellulose); conductor paste of PP-17 grade con­
sisting of silver particles and an organic terpineol-based binding medium. After heating the pastes at 150 ◦ C and
subsequent annealing at 850 ◦ C for 2 h, layers of aluminum oxide or silver are deposited on the surface of the
substrate, which have a high reflectance in the solar spectral range (0.2–2.5 μm). The solar absorptance (αs) is
0.143 for the coating based on the DCP paste and 0.23 for the coating based on the PP-17 paste, and these values
follow the requirements of the OSR class TCC. The coating based on the DCP paste features a high radiation
resistance (αs = 0.173 after irradiation by electrons with energy of 30 keV and fluence of 3⋅1016cm− 2).
1. Introduction
Since the beginning of space exploration and to date, the “Optical
Solar Reflector” (OSR) class thermal control coatings (TCC) for space­
craft (SC) of several types have been developed in different countries
[1–10]. They include paint and ceramic TCC consisting of pigments
(75–80%) and polymer binders (20–25%) (paint TCCs) or non-organic
binders – liquid glasses (ceramic TCCs); polymer films like kapton
with sprayed layers of aluminum and silver; silica glasses with sprayed
layers of aluminum and silver; plasma-sprayed coatings of metal oxides
and spinels. Each of these TCC types has its process-related specifics of
production and application, and possesses certain advantages and dis­
advantages during operation. The main performance characteristics of
such TCCs include emissivity (ε) and reflectance spectra in the solar
spectral range, based on which the solar absorptance (αs) is calculated.
The emissivity of such TCCs during SC orbital flights, as a rule, does not
change [3,11]. Therefore, the quality of OSR class TCCs during SC
orbital flights is determined by the stability of the solar absorptance αs,
which may change to increased values during long flights. Therefore, at
present, there exists a problem of creating TCCs capable to maintain the
SC temperature for flight time up to 15–20 years. For this purpose, new
types of coatings are required, which have a low solar absorptance αs in
their initial state and display high stability of this parameter during
orbital flights.
Moreover, the rapid development of small-sized SCs leads to a
problem of ensuring normal thermal conditions for instruments and
devices installed therein. Considering their small dimensions and low
weight, bulky cryogenic technology systems used in conventional
* Corresponding author.
E-mail address: yusalek@gmail.com (S.A. Yuryev).
https://doi.org/10.1016/j.matchemphys.2023.128472
Received 15 June 2023; Received in revised form 14 September 2023; Accepted 18 September 2023
Available online 19 September 2023
0254-0584/© 2023 Elsevier B.V. All rights reserved.
M.M. Mikhailov et al.
Materials Chemistry and Physics 310 (2023) 128472
spacecraft are not suitable here. The necessary thermal conditions are
provided by passive systems with “optical solar reflector” class TCCs as
the main components. Thus, the development of new TCC types based on
the use of new materials and technologies for their production is an
urgent problem of spacecraft material science.
One rapidly developing technology of applying materials on various
types of surfaces and manufacturing of finished products is printing,
which is widely used in many areas of science and technology. Additive
manufacturing (3D printing) is utilized in medicine, automobile pro­
duction, aerospace and construction industries, etc. [12–17].
Printed circuit boards (PCB) is one of the printing technology ap­
plications, where sensors [18], transistors [19,20], solar cells [21],
radio-frequency identification tags [22,23], organic light-emitting di­
odes [24–27], RC-filter schemes [28] are produced on the basis of
conductor, semiconductor and dielectric pastes (inks). Among others,
compositions based on metal oxides [29] are used in PCB printing. In
conductor pastes, silver is mainly used [30,31].
ISO/ASTM 52900 Standard [32] provides the division of additive
manufacturing methods into seven categories of processes, which are
reviewed in detail in work [33]. PCB printing can be regarded as a
particular instance of the “material jetting” category of the Standard.
Powder materials in a binder are applied to a printed circuit board and
then annealed to remove the binder (in some cases — for powder
agglomeration). The process is reviewed in work [34]. In our case (to
receive a coating), the binder removal is a positive factor because
binders in TCCs have a negative effect both on their initial optical
properties and radiation resistance in the space environment.
Oxide pigments and silver are used in spacecraft TCCs as well as in
PCB printing. This is why manufacturing reflective or absorbing coatings
based on existing paste grades or pastes prepared on the basis of pig­
ments with required reflectance (e.g. ZnO, TiO2, Al2O3, ZrO2, BaSO4)
can become another topical application of the printing technology. This
technology, in contrast to traditional methods, allows to receive and
apply TCCs on small-sized manufactured articles, instruments and de­
vices with controlled parameters (thickness, sizes, shape, etc.)
In this study, a new method to produce TCCs of various classes,
including the OSR class TCCs, is proposed. It assumes preparation of a
mixture of necessary composition, including a filler and a solvent with a
thickener, which is applied on a substrate using a PCB printer. During
the subsequent heating of the mixture, the solvent and the thickener are
removed to produce a TCC of a metal or a metal oxide deposited on the
substrate.
hold at 22 ◦ C for 10 min to smooth the relief and then dried at 150 ◦ C for
15 min. The paste burn-in period was 60 min, the curing period at a
maximum temperature of 850 ◦ C was 10 min. After the burning-in at
850 ◦ C, ethyl cellulose and terpineol were completely removed from the
paste composition.
Laser diffraction particle size analyzer Shimadzu SALD-2300 equip­
ped with the sampler SALD-MS23 was used to study the DCP particlesize in the range of 0.1–40 μm. Optical profilometer Chotest Super­
View W1 was used to measure the surface roughness of the coatings. The
structure of the obtained samples was studied using the X-ray diffrac­
tometer Shimadzu XRD-6100, micrographs of their surfaces were ob­
tained by the scanning electron microscope Coxem EM-30 Plus, relevant
diffuse reflectance spectra were registered using the spectrophotometer
Shimadzu UV-3600 Plus. The solar absorptance was calculated accord­
ing to the diffuse reflectance spectra with the use of the international
standards [35,36].
3. Experimental results and discussion
The DCP particle size was studied in the range of 0.1–40 μm (Fig. 1)
to control the fineness of Al2O3 powder and choose the appropriate size
of the print-head nozzle. The particle size distribution was such that they
were distributed in the range of 0.1–25 μm with maxima at 0.39, 0.76,
1.9, and 11 μm. As the particle size increased, the intensity of the
maxima increased as well. The average particle size was 4.82 μm.
Minimum diameter of the print-head nozzle enables smoother coating
application, but it should be at least four times larger than the maximum
particle size of the paste. Nozzle diameter of 100 μm was chosen based
on the results of the particle size distribution measurement.
The roughness of both types of pastes was studied at a base length of
1000 μm to evaluate the quality of printed coatings surface (Fig. 2). The
maximum deviation of the asperity distribution was approximately 6
μm. This value is satisfactory for the SC TCC.
The micrographs of the printed DCP sample (Fig. 3a) show that the
range of its particles varies from 1 to 13 μm. Most of the particles are less
than 5 μm, and a certain proportion are 2 μm particles. Most of the
particles are in the form of polyhedra, spherical particles make up a
small fraction of the total number of particles.
The PP-17 sample micrograph demonstrates a fundamental differ­
ence from the dielectric paste sample. In the conductor paste, the par­
ticles are in the sintered state and make up a unified particle
conglomerate with holes of various shapes filled with smaller particles of
less than 1 μm.
The XRD studies were carried out to control the presence in the
examined pastes of foreign substances that could affect the performance
characteristics of the received coatings. According to the results, the
DCP sample received by annealing at 850◦ С basically includes only
ceramic compound Al2O3 (Fig. 4a). The X-ray pattern also contains lowintensity peaks, which are determined by other compounds of low
concentration – SiO2 and FeF3. The X-ray pattern of the TCC sample
based on PP-17 conductor paste (Fig. 4b) shows intensive Ag peaks and
2. Experimental technique and results
Dielectric ceramic paste (DCP) was prepared with Al2O3 powder as
the main component. The powder was ground using the planetary micro
mill Fritsch PULVERISETTE 7 Premium Line in two stages: first, 6 min at
850 rpm, then another 4 min at 1000 rpm. S52-1 glass was added to the
paste composition to ensure proper adhesion between the film and the
substrate. Terpineol-based ethyl cellulose was used as an organic binder.
Terpineol-based ethyl cellulose was added to the paste to ensure its
required viscosity and flowability when applied by printing and to
improve the surface evenness of the received coating. The paste had the
following percent ratio: Al2O3 powder: S52-1 glass: terpineol-based
ethyl cellulose = 68:2:30. The components were mixed in the plane­
tary micro mill Fritsch PULVERISETTE 7 Premium Line. First, the Al2O3
and S52-1 powders were stirred for 5 min at 850 rpm. Then, the organic
binder was added, and the mixture was stirred for 60 min at the same
speed.
PP-17 conductor paste based on silver manufactured by Elma-Pasty
LLC, Zelenograd, Russia, was used as another sample for the study
conducted.
The samples were printed with the use of the PCB printer Voltera VOne, which implemented plunger-type dosing on 23 mm diameter
ceramic substrates made of polycor. After printing, the samples were
Fig. 1. Particle size of DCP filler (Al2O3 powder).
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M.M. Mikhailov et al.
Materials Chemistry and Physics 310 (2023) 128472
Fig. 2. Roughness of printed samples of DCP (а) and PP-17 (b) pastes.
Fig. 3. Micrographs of printed dielectric paste (a) and PP-17 conductor paste (b) samples.
Fig. 4. X-ray patterns of DCP (а) and PP-17 (b) pastes annealed at 850◦ С
low-intensity MgO peaks.
The comparison of the study results for the particle size, roughness
and micrographs allows to conclude that the TCC samples printed by the
PCB printer and annealed afterwards represent:
– a coating made of sintered Ag particles in the form of conglomerates
of various shapes with grains located in the pits of those conglom­
erates, produced using PP-17 paste.
– a ceramic coating sintered on the substrate and made of Al2O3
powder which includes grains of different sizes in the range of
0.1–25 μm, produced using DCP paste;
3.1. Studies of TCC samples diffuse reflectance spectra
The photos of the coating samples prepared for the diffuse reflec­
tance spectra record are presented in Fig. 5. The samples are made in the
form of disks of 23 mm diameter fixed on substrates. They are
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M.M. Mikhailov et al.
Materials Chemistry and Physics 310 (2023) 128472
– the main absorption edge shifts further to the short-wave region, and
two of its values are recorded at 195 and 168 nm the same way as
during its heating at 150◦ С;
– with the wavelength being increased, the reflection coefficient in­
creases and reaches a maximum value in the range of 500–700 nm,
equal to 89%,
– in the region of λ > 700 nm, the reflection coefficient decreases
slightly, and at λ = 2500 nm it reaches 80%;
– dips in the reflectance spectrum completely disappear, but a new dip
appears at 412 nm, which can presumably be associated with the
absorption band of aluminum ions formed during the thermal ioni­
zation of interstitial atoms during the paste heating at 850 ◦ C. Similar
bands of interstitial zinc ions were previously recorded in the ab­
sorption spectra of zinc oxide after its heating at 800 ◦ C [39].
Fig. 5. TCC samples made of DCP dielectric paste and PP-17 conductor paste.
The shift of the main absorption edge to the short-wave region can be
determined by the formation of two modifications of aluminum oxide
during the oxidation of aluminum atoms during paste heating and
annealing: α-Al2O3 and γ-Al2O3. For the crude paste, the value obtained
is Еg = 4.43 eV, for the paste heated up at 150◦ С – 4.8 eV and 5.71 eV,
for the annealed paste – 6.37 eV and 7.38 eV. These values follow the
values which were obtained earlier. It is known that the band gap of
aluminum oxide in its various modifications varies from 8.75 [40,41] to
7 eV [42]. The calculations based on the first principles and density
functional theories give the following values of the band gap: from 6.24
[43–47] to 5.13 eV [48] for α-Al2O3 and γ- Al2O3 modifications,
respectively.
Thus, the applied technology of heating and subsequent annealing of
a crude paste consisting of Al2O3 powders, S52-1 glass and organic
binder (terpineol-based ethyl cellulose) in a ratio of 68:2:30 wt % made
it possible to receive a coating with a high reflectance in the solar
spectral range (0.2–2.5 μm). The solar absorptance of such coating
calculated as per the reflectance spectra (Fig. 6, spectrum 3) was αsо =
0.143. This value is close to the solar absorptance αs of the TCC based on
ZnO powders with lithium silicate (αsо = 0.136) [49].
Such coating represents a film with a high level of adhesion to the
substrate. It contains no binder, which is an important positive property,
since binders in TCCs have lower photo- and radiation resistances, as
compared to pigments. The study of its radiation resistance under
electron fluence F = 3⋅1016 cm− 2 with energy of 30 keV proved its high
radiation resistance: αsirr = 0.173, Δαs = αsirr - αsо = 0.03. This degra­
dation value is significantly lower than for titanium dioxide powder and
slightly lower than for wollastonite powder irradiated under the same
conditions [50]. The electrical resistance of such coating is 1.2⋅1011
Ohm.
characterized by good whiteness.
The diffuse reflectance spectra (ρλ) of the samples were recorded in
the range of 0.2–2.5 μm to study optical properties of the received
coatings and calculate their main performance characteristic — solar
absorptance. The study showed that they have the following specifics,
depending on the type and stage of the paste processing cycle:
3.1.1. TCC made of dielectric paste
The reflection coefficient (ρ) of crude paste, depending on the
wavelength, qualitatively changes in the same way as for powders of
dielectric compounds (Fig. 6). The main absorption edge (λg) is
distinctive and is 280 nm. With the wavelength being increased, the
reflection coefficient increases and reaches a maximum value in the
region of 800–1300 nm, equal to 70%. Then it slowly decreases, and at λ
= 2500 nm it is 27%. Minimum reflection coefficients (dips) are recor­
ded at 1,200, 1,420, 1,700, 2,100, and 2300 nm, which may be due to
the absorption bands of sorbed on the surface OH-groups (1,420, 1,700,
and 2100 nm), molecules of water and other compounds [37,38].
Heating at 150оС for 15 min leads to the following changes in the ρλ
spectrum:
– the main absorption edge shifts to the short-wave region, while two
of its values are recorded at 258 and 217 nm;
– a part of the dips disappears, the intensity of the remaining dips
decreases significantly, the reflection coefficient in the main part of
the spectrum increases, its highest value is recorded in the range of
800–2100 nm and reaches 86%.
Annealing at 850◦ С for 10 min leads to the following changes in the
ρλ spectrum:
Fig. 6. Diffuse reflectance spectra ρλ for dielectric paste (а) and PP-17 conductor paste (b) in crude condition (1), after drying at 150◦ С for 15 min (2) and after
annealing at 850◦ С.
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M.M. Mikhailov et al.
Materials Chemistry and Physics 310 (2023) 128472
3.1.2. TCC made of conductor paste
The reflection coefficient of the crude conductor paste is significantly
lower, as compared to the crude dielectric paste in the entire spectrum
range from 0.2 to 2.5 μm (Fig. 6b). The main absorption edge is welldefined and is 321 nm. With the wavelength being increased, the
reflection coefficient increases and reaches a maximum value in the
region of 2500 nm, equal to 17%. There are no dips in the values of the
reflection coefficient in this spectrum, as it was in the spectra of the
dielectric powder.
Heating at 150оС for 15 min leads to the following changes in the ρλ
spectrum:
CRediT authorship contribution statement
M.M. Mikhailov: Supervision, Writing – original draft, Writing –
review & editing. A.N. Lapin: Writing – original draft, Writing – review
& editing, Investigation, Visualization, Formal analysis. S.A. Yuryev:
Writing – original draft, Writing – review & editing, Investigation,
Visualization. V.A. Goronchko: Writing – review & editing, Investiga­
tion, Visualization, Validation. S.A. Artishchev: Funding acquisition,
Investigation. N.S. Trufanova: Investigation, Visualization. O.A.
Mikhailova: Investigation, Validation. D.S. Fedosov: Investigation,
Validation.
– the main absorption edge does not change;
– there are no dips in the spectrum;
– with the wavelength being increased, the reflection coefficient in­
creases and reaches a maximum value of 36% at λ = 1600 nm;
– with further wavelength increase, it decreases by 1–2%.
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.
Annealing at 850◦ С for 10 min leads to the following changes in the
Data availability
ρλ spectrum:
Data will be made available on request.
– the main absorption edge does not change; in the region λ > 400 nm
the reflection coefficient increases, and in the region of 1200–1600
nm it reaches a maximum value of 88%;
– in the longer wavelength region, the reflection coefficient decreases
by 2–4%, as the wavelength increases.
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Thus, the applied technique of heating and subsequent annealing of
PP-17 conductor paste made it possible to receive a coating with a high
reflectance in the solar spectral range (0.2–2.5 μm). The solar absorp­
tance of such coating calculated as per the reflectance spectrum (Fig. 6b)
was αsо = 0.23. This value is higher than the solar absorptance αs of the
TCC based on ZnO powders with liquid glass or polymer binders, but it is
lower than its values for the coatings based on pigment powders TiO2
(αs = 0.3 [51]).
Such coating represents a film with a high level of adhesion to the
substrate. It contains no binder, which is an important positive property,
since the binders in TCCs have lower radiation resistance, as compared
to pigments. The surface electrical resistance of such coating was 2.5
Ohm.
4. Conclusions
The performed studies showed the possibility of manufacturing
thermal control coatings for spacecraft based on pastes of various
compositions using PCB printing for their application on substrates and
further processing by heating and annealing. The studies were per­
formed for the pastes of two types allowing to receive dielectric and
conducting coatings the surface resistances of which differ by 14 orders
of magnitude. High reflectance is recorded after the heat treatment for
both types of coatings in almost the entire measurable solar spectral
range, which allows to receive low αs values — 0.143 for dielectric and
0.23 for conducting TCC. By their properties, the received coatings refer
to the “optical solar reflector” class, and after determination of their
radiation resistance can be used in actual SC structures. This method can
be utilized to receive not only thermal control coatings, but also coatings
of other types and for other SC classes, as well as coatings for other areas
of technology. Additive manufacturing of coatings seems to be partic­
ularly relevant due to the rapid development of small-sized SCs
(including nano-, pico- and femtosatellites).
Funding
The work was performed with the financial support of the Ministry of
Science and Higher Education of the Russian Federation. State assign­
ment (Goszadanie) – N◦ FEWM-2022-0005.
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