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Development of high-performance, chemical
pretreatment-free dye-based inks for digital printing
on polyester fabric
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Yufeng Chena, Lun Niea, Yingping Donga, Ruoxin Lia,b,* and Guangtao Changa,b,c,*
aCollege of Textile and Clothing Engineering, Soochow University, Suzhou 215000,
China.
bJiangsu Engineering Research Center of Textile Dyeing and Printing for Energy
Conservation, Discharge Reduction and Cleaner Production (ERC), Soochow
University, Suzhou 215123, China.
cNational Innovation Center of Advanced Dyeing and Finishing
Technology, China.
* Corresponding author.
E-mail address: changgt@suda.edu.cn (G. Chang); liruoxin@suda.edu.cn (R. Li)
Abstract:
A new thermal-sensitive ink that utilizes high-performance disperse dyes and a
biodegradable carrier molecule, a diblock dispersant made of PCLA-PEG-PCLA
hydrogel, has been successfully prepared and tested on polyester fabric. Unlike
traditional methods, this ink eliminates the need for chemical pretreatment on the fabric
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before printing or washing after printing, resulting in a significant reduction in chemical
usage and wastewater production during manufacturing. When the ink drops come into
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contacts with a heated surface, such as a fiber or textile, they quickly transition to a gellike state. This increased viscosity prevents the ink from spreading, resulting in a
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defined edge on the fabric. The performance of the polyester fabric printed with this
new ink has been thoroughly evaluated for the pH, particle size, surface tension,
viscosity, ink droplet formation, real-time photo-rheological, and LF-NMR analyses on
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the polyester fabric surface. The new inks are highly effective and suitable for digital
printing applications on various materials.
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Keywords: Pretreatment-free, high temperature disperse dyes, inkjet printing,
environmental protection
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1. Introduction
Inkjet printing is a popular method for coloring fabrics[1, 2], as it offers many
advantages over traditional printing methods. These include high precision, the ability
to handle small batches and a wide variety of substrates, low energy consumption, and
a more environmentally-friendly approach[3-5]. Polyester fabric is one of the most
commonly used substrates for inkjet printing, which is popular due to its high strength,
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elasticity, and resistance to heat, light, and mildew[6, 7]. Polyester became one of the
essential fabrics in today's people's lives and created research attention worldwide.
However, the chemical structure of polyester fabrics can make it challenging to
achieve clear, high-quality prints using inkjet printing[8, 9]. The lack of polar functional
groups[10, 11] on the fabric's surface can cause ink droplets to spread rapidly, resulting
in a blurry final image[12]. Researchers have focused on developing chemical or
physical pretreatment methods to overcome this challenge to improve printing
clarity[13, 14]. For example, Park et al. [15]used acrylic resins to modify the surface of
polyester fabrics, while others have used plasma or microwave methods to change the
fabric's morphology. Krump et al. [16] proposed using atmospheric plasma and
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microwave plasma methods to change the morphology of polyester fabric and improve
chemical reactivity for better printing quality. Their test results showed a strong
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relationship between printing quality and the fabric surface morphology. Chen et al.
[17]. treated polyester fiber surfaces with β-cyclodextrin and citric acid before printing
and successfully reduced the ink diffusion problem. Other pretreatment agents such as
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xanthan gum[18], curcumin[19], and sodium alginate[20, 21] have also been tested on
polyester fabric to improve image clarity and printing quality, but the process generates
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waste and is time-consuming. Therefore, much research is focused on developing ink
technology that can print directly on polyester fabric without chemical pretreatment.
Gao et al. [22] formulated PVA into a dispersed dye ink that can be printed directly on
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polyester fabric. Li et al. [23] prepared temperature-sensitive disperse-dye inks that
improve printing clarity under high temperatures. The most popular dispersed dyes for
printing on polyester fabrics are medium and low-temperature range dyes, but high-
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temperature dyes can also be used for direct print technology. The high-temperature
dye has a higher sublimation temperature and only be used for direct print technology.
Overall, current direct inkjet printing methods for high-temperature dyes require
chemical pretreatment and post-washing, which generates large waste[24].
New ink technology has been developed to fully leverage the benefits of high-
temperature dyes, such as improved heat stability, color fastness, and long storage life
under various conditions. This technology involves synthesizing a diblock dispersant
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made of polyether and incorporating it with high-temperature disperse dyes. The
resulting inks can be used to print directly on polyester fabrics without requiring
chemical pretreatment. The dispersant, PCLA-PEG-PCLA hydrogel, combined with
the high-temperature disperse dye ink, can print on any polyester fabric. This ink design
offers excellent printing precision and color fastness. Additionally, this ink eliminates
the need for chemical pretreatment or post-washing steps for the polyester material. A
visual representation of the printing process can be seen in Figure 1.
2. Materials and Methods
2.1. Materials
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All materials for the experiments come from local suppliers. Shanghai Textile
Industry Technical Supervision Institute supplied polyester fabrics (130 g/m2).
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Polyethylene glycol monomethyl ether (MPEG) with 3000 molecular weight came
from Jiangsu Province Haian Petrochemical. ε-Caprolactone (CL) is from Hunan Juren
Chemical New Material Technology Company. Evonik Specialty Chemicals (Shanghai)
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supplied the defoamer 825 and nonionic surfactant 465 agents.High temperature
disperse dye B291purchased from Mangosteen Group Co. LTD. Other common agents
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were purchased from local suppliers, such as stannous octanoate, polyethylene glycol
1500, L-lactide, and triethanolamine.
2.2. Synthesis of diblock dispersants
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Raw materials, Poly(ethylene glycol) monomethyl ether, ε-caprolactone, and
stannous octanoate, were mixed together according to a certain weight ratio under argon
conditions (Table 1). After stirring for 8 hours at 160 ℃, the reaction was cooled to
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room temperature, and the polyether/polyester diblock copolymer was collected as a
dispersant (Figure 2a). The final products with different ratios of starting materials were
labeled as D1, D2, D3, and D4, respectively. The initial mixing experiments indicated
that the D3 material is the most compatible with high-temperature Disperse Blue 291
and was used for the rest of the analysis.
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2.3. Synthesis of PCLA-PEG-PCLA hydrogels
To synthesize a diblock dispersant for use in high-temperature inkjet printing,
dihydroxy polyethylene glycol (80 g) with a molecular weight of 1500 was dried in a
vacuum oven at 120 °C for 4 hours. All the starting materials, including dihydroxy
polyethylene glycol, glycol (80 g), ε-caprolactone (80 g), L-lactide (80 g), and
stannous octanoate (400 mg), were then added to a 500 mL flask and mixed at room
temperature. The reaction was conducted at 130 °C for 12 hours under an argon
atmosphere. The final products were collected at the end of the reaction (Figure 2b).
2.4. Preparation of thermosensitive ink
The thermosensitive direct-jet ink was prepared according to the formulation in
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Table 3. The pH of the ink was adjusted to neutral with triethanolamine. All inks were
filtered with 0.8 μm and 0.6 μm filter membranes to remove large particles before use.
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2.5. Characterization methods
To ensure the accuracy and reproducibility of the results, particle size was measured
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using a Nano Particle Size Analyzer on three separate occasions. The viscosity of the
ink was also measured at 30 different points, with a temperature range of 20-70 °C and
a heating rate of 1 °C/min. The surface tension of the ink was tested using a BP-100
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bubble pressure spectrometer at 25 °C. IF-NMR measured by a Niumag Pulsed NMR
analyzer (PO001, Niumag ElectricCorporation, Shanghai, China). The condition
includes magnetic field strength of 0.50 . The injection performance of droplet is
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monitored and recorded by a Jetxpert analytical instrument at 20 ℃(X-BT, 220.0 V
50.0 Hz, Suzhou Sigmatek Trading Co., Ltd, China).To evaluate the printing
performance, the line width of the inkjet printing was set at 360 μm in both the warp
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and weft direction on polyester fabric. The actual line width was then measured using
Pinnacle Studio version 8.0 software with 10 points taken in both the warp and weft
direction to calculate the average line width. The equation used to calculate the rate of
change of line width is provided
W=
𝐸1 ― 𝐸0
𝐸0
*100%
W is the line width change rate used to describe the print pattern outline clarity.
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The larger the W value, the worse the pattern clarity. E1 is the actual line width, and
E0 is the 360μm set line. The color strength (K/S) was measured using an Ultra Scan
Hunter Lab K/S (USA) reflectance spectrophotometer (illuminant D65, 10 standard
observer, d/8 °sphere geometry). The bending length of the pristine and printed fabrics
were tested by the YG(B)022D automatic fabric stiffness tester according to GB/T
18318.1-2009. The rubbing fastness and soaping fastness were determined based on
standard methods. Fabrics' dry and wet rubbing fastness were evaluated with a rubbing
color fastness tester according to ISO 105-X12: 2016. Washing fastness was measured
with a washing tester according to ISO 105-C10:2010. The Surface properties of the
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fabric are measured and recorded by the FB4 Automatic Surface Tester.
3. Results and Discussion
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3.1. Synthesis and dispersion effect of diblock dispersants
The prepared dispersant has the best dispersion capability when the ratio of
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reactants is 10:3 and the ratio of dispersant to dispersion blue is 60 % (Table 1).
The high-temperature dye blue 291 was mixed with the dispersant D1 for 6 hours,
resulting in a final particle size of approximately 210 nm, as shown in Figure 3. The
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particle size remained stable without significant changes after 6 hours. Using a
biodegradable dispersant in the ink preparation is important for improving clean
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polyester dyeing technology. The dispersant D1 was specifically chosen for its ability
to disperse the high-temperature dye and create a high-temperature direct print ink. The
reactant ratios used in synthesizing the copolymer dispersant are outlined in Table 1.
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3.2. Preparation of thermosensitive ink
Table 2 presents the formulation for high-temperature dispersion dye ink.
Different amounts of the building block, PCLA-PEG-PCLA polymer, were used in the
ink formulations, marked as B0, B2, B4, B6, and B8, respectively. All ink parameters
were measured and tested as indicated in Table 3. By incorporating the PCLA-PEGPCLA into the ink, the surface tension and viscosity of the ink only increased slightly,
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from 2.19 to 4.27 mPa·s for viscosity and 35 mN/m to 39 mN/m for surface tension.
The particle size and copolymer content did not show a significant linear relationship,
according to Table 3. The final particle size in the formulation is about 200 nm, which
meets the requirements for digital printing[25].
3.3. Properties of thermosensitive inks
Although the surface tension of the ink is affected by the amount of copolymer
present, as shown in Figure 4a, the ink still meets the printing requirements based on
the dynamic surface tension data. The gel transition properties of the ink were also
studied by closely monitoring its viscosity change using a rotational viscometer at
temperatures ranging from 20 °C to 70 °C, as shown in Figure 4b. The ink viscosity
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started to decrease as the temperature increased from 20 °C to 37 °C due to the thermal
movement of molecules intensifying at high temperatures. However, when the
temperature reached 37 ℃, the triblock began to transition to a gel state, resulting in an
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increase in viscosity. Since our inks contain a triblock and are sensitive to temperature
changes on polyester fabric, the viscosity of the ink increases suddently when it comes
into contact with heated fabrics. This gel state with high viscosity prevents the ink from
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spreading, reducing ink bleeding[26, 27].
Low-field Nuclear Magnetic Resonance (LF-NMR) is an efficient method to study
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ink's internal structure by measuring the free water content changes. The movement
characteristics of molecules can be determined by their transverse relaxation time, as
different molecules have different relaxation times[28-30]. Different phase states and
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environments for the same molecule lead to different transverse relaxation times. When
the degree of hydrogen bonding is higher, the relaxation time is shorter[31]. The
interaction of ink components with water molecules and the mobility of water were
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studied by LF-NMR. Figure 5 presents the prepared thermosensitive ink's T2 relaxation
time inversion spectrum. It was found that the ink has two prominent peaks - one
representing low fluidity bound water (T22) and the other representing high fluidity
free water (T23). As the amount of PCLA-PEG-PCLA in the ink increases, the peak
area of the bound water (T22) increases, and the transverse relaxation time increases,
indicating that the content of bound water in the system increases and the fluidity
decreases from B0 to B8. The peak area of free water (T23) in ink decreases, and the
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transverse relaxation time decreases, indicating that the free water content in ink drops
and the fluidity weakens. This is consistent with the observed increase in ink viscosity.
The ink components' different structures and molecular weights lead to different
transverse relaxation times and weak interactions with water, limiting water mobility.
3.4. The ejection properties of ink
Inkjet printing relies on the ejection of ink droplets from a nozzle at a pressure high
enough to overcome the ink's viscosity, inertia, and surface tension[32]. When the
pressure in the chamber drops below a critical value, ink droplets undergo a stretching
and thinning process due to the inertia of the jet[1, 33]. Low pressure enough causes
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the liquid breaks and forms a droplet with a tether. If the secondary droplet is unable to
catch up with the primary droplet, satellite droplets are generated. Figure 6 shows
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images of the patterns of the ink droplets at different times when they are ejected from
the nozzle. The formation of satellite droplets can reduce the definition of the printed
pattern and contaminate the printer. Since the invention of inkjet printing, efforts have
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been made to avoid the formation of satellites and mitigate their negative effects[34].
In B6 and B8, the secondary droplet catches up with the primary droplet within about
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55 microseconds to form a complete droplet, avoiding the formation of satellite droplets.
This is due to the addition of PCLA-PEG-PCLA, which changes the rheological
properties of the ink and increases its viscosity and surface tension, inhibiting the
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formation of satellite droplets. This improves the anti-seepage effect of the
thermosensitive ink even without heating, making it better than regular ink.
3.5. Ink printing
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The performance of the thermosensitive ink was evaluated by printing it on
polyester fabric and measuring the line width under various conditions. As the amount
of triblock polymer (PCLA-PEG-PCLA) in the ink formulation increased, the K/S
value of the printed fabric also increased (as seen in Figure 7). The added triblock
polymer increased the ink's viscosity at high temperatures, causing the colorants to
concentrate at one point on the fabric, resulting in a higher K/S value. Figure 8
illustrated the difference in performance when the ink was printed on heated or
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unheated fabrics and the effect of triblock polymer on the ink formulation. When no
triblock polymer was added, the ink bleeding problem was slightly improved at 60 ℃
(Figure 8a, b). However, when the ink formulation contained triblock polymer and was
printed on heated fabrics, the ink bleeding problem was significantly reduced (Figure
8c, d). This is because the triblock polymer caused the ink to enter a gel stage at 60 ℃ ,
preventing the ink droplets from spreading and producing a clear and precise image.
3.6. Line Width Test
The effectiveness of thermosensitive ink was evaluated by assessing line width
changes on the polyester fabric under different conditions. The line width change rate
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(W value) was measured and calculated under different temperature conditions (Figure
9a, b). It was observed that the rate of change in the weft direction was more significant
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than that in the warp direction. Furthermore, the W value for line width decreased with
increasing concentration of triblock polymer in the ink formulation, both in the warp
and weft direction, even when the fabric was not heated. This trend can be explained
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by increased viscosity when more tri-block polymers are added to an ink formulation.
When comparing the two inks, B8 and B0, under heating conditions, it was found that
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the line width change for ink B8 decreased significantly from 70% to 29% in the weft
direction and from 54% to 3% in the warp direction. This was attributed to the increased
viscosity of the thermal-sensitive ink, which limited the spread of the ink drops on the
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fabric.
3.7. Fabric handling feel test
The surface properties of the fabric were also measured using an automatic surface-
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measuring instrument. The MIU and MIU(H) in Figure 10, respectively, represent the
average coefficient of dynamic friction on the fabric surface under the condition that
the printing substrate is not heated and the substrate is heated. The MIU number of all
samples is less than 0.2, indicating that the fabric's surface is relatively smooth. MMD
and MMD(H) represent the deviation of the mean coefficient of kinetic friction under
heating or not, which is less than 0.1, and the relative surface error is small. SMD is the
surface roughness of the fabric, and the larger the value, the rougher the surface of the
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fabric. MIU(H) in B2-B6 is greater than MIU. MIU(H) in B2-B6 is greater than MIU.
This is because the gel transformation property of the thermosensitive ink makes more
dye particles stay on the fabric's surface under heating conditions, increasing the fabric's
surface roughness. The results indicated that the thermosensitive ink had a minimal
effect on the smoothness and feel of the fabric but did cause an increase in the surface
roughness due to more dye particles staying on the surface under heating conditions.
Additionally, Table 4 shows the bending length and bending stiffness of polyester
printed fabric in warp direction. As the amount of polymer added to ink increases, the
bending length of the fabric increases due to the print coating on the fabric, which
fabric.
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3.8. Fastness test
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prevents the slip between the fibers and yarns, adversely affecting the softness of the
Triblock copolymer PCLA-PEG-PCLA can trigger a gel transition change and
increase ink viscosity on a heated substrate. High viscosity inhibited ink drop
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spreading, giving more dense colorants on substrate surfaces with higher K/S values.
Dry and wet rubbing fastness tests for printed fabric indicate that triblock polymers
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have little effect on color fatness and soaping fastness (Table 5). Therefore, thermalsensitive ink technology is feasible for pretreatment-free digital print applications on
polymers fabric.
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4. Conclusion
An eco-friendly polyether/polyester-based diblock copolymer dispersant was
explicitly developed for use with high-temperature disperse dye 291, which currently
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requires chemical pretreatment and post-washing. By adding the PCLA-PEG-PCLA
copolymer, humectant, surfactant, and water to the color paste, a pretreatment-free
high-temperature disperse ink was prepared. This ink uses the gel transformation
property of PCLA-PEG-PCLA on the heated printing substrate to prevent ink
bleeding and has good rub resistance, meeting the goal of a treatment-free inkjet
printing process. The ink was fully evaluated on polyester fabric and can significantly
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reduce the amount of chemicals used for pretreatment and waste generated during the
process.
CRediT authorship contribution statement
Yufeng Chen: Conceptualization, Methodology, Validation, Formal analysis,
Investigation, Resources, Writing original draft, Visualization. Lun Nie: Validation,
Resources. Yingping Dong: Validation, Resources. Guangtao Chang: Formal
analysis, Writing – review & editing, Visualization, Supervision. Ruoxin Li: Formal
analysis, Writing – review & editing, Visualization, Supervision, Project
administration, Funding acquisition.
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Declaration of Competing Interest
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The authors declare no conflict of interest.
Acknowledgements
This research was funded by the Research Funding of Soochow University
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(Q411500218) and Soochow University-Suzhou Central Asia Ink Co., Ltd. Co-
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innovation Center Co-Construction Agreement (P111500219).
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of Satellite Droplets for Inkjet Printing: A Review, Processes, 10 (2022) 17.
This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4379402