ETFE RFID Tag with heteroatom-doped conductive carbon by screen print

doi:10.21203/rs.3.rs-3461425/v1

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ETFE RFID Tag with heteroatom-doped conductive carbon by screen print

https://doi.org/10.21203/rs.3.rs-3461425/v1

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The Radio Frequency Identification (RFID) tag in Internet of Things (IoT) applications lacks high-performance substrates to meet the growing demand. Surprisingly, ethylene tetrafluoroethylene copolymer (ETFE) is the strongest and toughest fluoroplastic, which maintains good heat resistance and chemical resistance, possessing strong mechanical properties as well, suiting for RFID tag substrate materials. Herein, we have demonstrated a simple route for the made of RFID tag via self-made ETFE membrane and heteroatom-doped conductive carbon screen printing technology. The ETFE membrane that can be produced on a large scale by using extrusion calendaring method.The highly conductive heteroatom-doped conductive carbon is produced using solvothermal method. Using simple screen printing technology prepare the RFID tag. The ETFE membrane exhibits excellent mechanical properties, combined with the excellent conductivity of heteroatom-doped conductive carbon, providing a high-quality and high-performance substrate selection for RFID tag.

ETFE

heteroatom-doped conductive carbon

RFID tag

Nowadays, with the continuous progress of science and technology, all items can be connected to the Internet through information sensing devices such as Radio Frequency Identification (RFID), achieving an intelligent network.[1–3] RFID is an essential technology for the rapid development of the Internet of Things (IoT) industry and has attracted widespread interest in recent years.[4–6] The RFID tag is the core part of the RFID system, and the design of the tag determines whether the entire RFID system can work properly.[7, 8] [9]The working frequency of tag not only determines the working principle (inductive coupling or electromagnetic coupling) and recognition distance of the RFID system, but also determines the difficulty of implementing tags and readers, as well as the cost of equipment.[10–18] RFID tag mainly come in materials such as copper coated paper, PET, PVC, ABS, etc. and different materials correspond to different application scenarios.[19–24] Meanwhile, the current production processes for RFID tag mainly include etching, electroplating, and conductive ink printing. Due to the inherent defects of the etching and electroplating processes, a series of problems have arisen: severe environmental pollution, cumbersome manufacturing processes, and slow production speed. In contrast, the production process of conductive ink printing has many advantages: low printing production cost, simple operation of printing equipment, wide range of printing substrates and environmental friendly. In addition, the conductive inks used in printed RFID tag mainly include gold based conductive inks, silver based conductive inks, and new carbon based conductive inks doped with heteroatoms.[25–27]Xu et al. prepared graphene conductive ink, demonstrating good adhesion, acid resistance, and water resistance of the ink.[28] Wang et al. prepared graphene/carbon black conductive ink and directly printed it on a flexible paper substrate.[29] Carbon is a typical non-metallic material, and the doping of a series of heteroatoms (such as boron, nitrogen, phosphorus, or sulfur) can improve the conductivity of pure carbon materials, which is attributed to the electronic and surface physicochemical properties caused by structural distortion and charge density changes.[30, 31] Novel carbon based conductive ink doped with heteroatoms has low production cost, protecting circuits as well.Its chemical performance is stable so that it is resistant to corrosion and acid and alkali. There are some attempts on electronic tag using carbon based materials.[32–34]

ETFE is a chemical substance that is the strongest and toughest fluoroplastic.[35] It maintains the excellent heat resistance, chemical resistance, and electrical insulation properties of polytetrafluoroethylene (PTFE), while also greatly improving its radiation and mechanical properties. The tensile strength can reach 40 MPa, which is nearly twice that of PTFE.[36]ETFE membrane material is a transparent membrane material without fabric substrate, with an elongation rate of 420–440%. The transmittance spectrum of ETFE membrane material is similar to that of glass (commonly known as soft glass). It has excellent performance, chemical stability, corrosion resistance, lightweight, good toughness and high tensile strength. Strong weather resistance and chemical corrosion resistance, with a melting temperature of up to 200 ℃.

This work utilizes extrusion calendaring method to prepare ETFE membrane and solvothermal method to prepare heteroatom-doped conductive carbon NOC. The resistivity of NOC powder is 0.9×10^− 4 Ω m, with a good conductivity of 1.1×10⁴ S m^− 1. This article introduces the high conductivity of a new type of carbon based conductive ink doped with heteroatoms, utilizing the excellent mechanical properties of ETFE membrane to prepare ETFE tag with good mechanical properties and sheet resistance. Therefore, this study provides certain application prospects for ETFE tag made using screen printing technology in the future. The entire process is shown in Fig. 1.

Chemicals required

ETFE resin with model C-88AXP (Japan AGC Company)(Figure S2(a), Supporting Information).

Pyridine, hexabromobenzene, and petroleum ether were all purchased from Aladdin Industrial Biochemistry Co., Ltd. and were not further purified during use. The binder slurry was purchased from Shenzhen Baojiayi Co., Ltd.

Preparation of ETFE membrane with a thickness of 50 µm

The melt index of ETFE resin is 11.2, and the extrusion frequency of the extruder is 4 Hz. The first zone is heated at 290 ℃, the second zone is heated at 300 ℃, the third zone is heated at 300 ℃, and the fourth zone is heated at 310 ℃. The operating speed of the electromagnetic forming roller is 5 m/min, and the traction speed is 6 m/min. Screw diameter 30mm; Tensile ratio: 5–30; Balance ratio: 1.05–1.10; The temperature of the electromagnetic forming rollers is all 80 ℃. The prepared membrane is named ETFE-F(Figure S1(a), Supporting Information). ETFE membrane equipment is called casting extruder.(Figure S2(b), Supporting Information).

Preparation of NOC

To synthesize NOC, 24.0 mL of pyridine and 2.0 g of hexachlorobenzene were added to a 50 mL Teflon high-pressure reactor and subjected to ultrasonic treatment for 10 minutes. Then place the sealed high-pressure reactor in an oven at 200 ° C for 6 hours. After naturally cooling the reactor to room temperature, the carbon precursor obtained was washed with petroleum ether and vacuum dried at 60 ° C for 8 hours. Subsequently, the carbon precursor was placed in a tubular oven and calcined for 2 hours under N₂ protection at a heating rate of 5 ° C min^− 1 at 1000 ° C, with a N₂ flow rate of 20 mL min^− 1. Finally, the product is named NOC.

Preparation of tag

Firstly, mix 5ml of adhesive slurry with 1g of NOC and sonicate for 5min. Secondly, corona the ETFE-F using an electric halo machine with a current of 5A, thereby reducing the activation energy of the membrane surface. Clean ETFE-F with ethanol and fix it. Use a scraper and a screen printing plate to coat the carbon material slurry on the surface of ETFE-F. Then place it in an oven and keep it at 80 ℃ for 10 minutes, then take it out and cut it to obtain the finished product. The prepared membrane is named C-ETFE-F(Figure S1(b), Supporting Information).

Study of structural, morphological properties of the synthesized materials

The surface morphology of the sample was observed using a scanning electron microscope (SEM, Nova Nanosem 200 system, operating at an accelerated voltage of 15 kV). X-ray diffraction (XRD) analysis using Bruker D8 propulsion diffractometer and Cu Ka radiation( λ = 0.15406 nm), data at 2 ° C between 20 and 80 ° C θ Collect within the range, with a step size of 0.02 °. Raman spectroscopy analysis was performed under a Raman microscope with a wavelength of 532 nm. The FTIR data results were measured by a Fourier transform infrared spectrometer (Thermo Fisher Scientific). Use a universal testing machine (Meister Industrial Systems (China) Co., Ltd.) to test the mechanical properties. Test the powder resistance by using an automatic powder resistivity tester (ROOKO company) with the Chinese standard GB/T24521-2018 measurement method. The coating sheet resistance tester (HPS2523) tests the sheet resistance.

Chemical structure of NOC

The scanning electron microscopy (SEM) images of NOC demonstrate the existence of good carbon spheres and layered porous carbon structures, with regular spherical parts being carbon spheres and sheet-like substances being carbon sheets. Both carbon sheets and spheres have rich porous structures. As shown in Figs. 2a and 2b, from a microscale perspective, even after 10 minutes of ultrasonic treatment, the carbon layer adheres tightly to the carbon sphere, indicating that the material has good structural stability and thus constructs an excellent conductive path.

Raman spectroscopy and XRD spectroscopy can be used to study NOC samples better. More intuitively, the XRD spectrum exhibits two typical diffraction peaks concentrated at 2 θ = 30 ° and 43 ° represent graphite carbon in terms of (002) and (100) in Fig. 3(a), respectively. In addition, Raman spectroscopy can monitor the degree of material graphitization, as shown in Fig. 3(b). The two peaks at wavelengths 1349 cm^− 1 and 1589 cm^− 1 of all NOC samples correspond to D and G bands, respectively. The intensity ratio (I_D/I_G) of the D and G bands is an indicator of the degree of graphitization. The D peak represents the crystal defect of the C atom, and the G peak represents the hybridization of SP². The smaller the I_D/I_G ratio, the higher the degree of graphitization. In this case, the I_D/I_G ratio of NOC is 0.92. With the increase of carbonization temperature, the conductivity of the material significantly increases, and 1000 ° C reaches the optimal equilibrium point between the degree of graphitization and nitrogen doping content.The conductivity of NOC powder measured by an automatic powder resistivity tester is 0.9 × 10^− 4 Ω m, and the conductivity is 1.1 ×10⁴ S m^− 1, which proves that the conductivity between powders is good and can be used to improve the conductivity of the matrix material. The excellent conductivity of NOC powder was demonstrated, which is consistent with the SEM, XRD, and Raman results of NOC mentioned earlier.

Chemical structure of ETFE-F and C-ETFE-F

Figures 4(a) and (b) show the DSC test results of ETFE-F with a melt index of 15.6 and ETFE-F with a melt index of 11.2, respectively, to better explore the Tm, Tc, and crystallinity of the ETFE membrane. These results are consistent with the theoretical values of the ETFE membrane. From Table 1, it can be seen that the crystallinity of ETFE-F with a melt index of 15.6 is 34.11%, which is lower than the crystallinity of ETFE-F with a melt index of 11.2 by 37.69%, indicating that the higher the resin melt index, the smaller the crystallinity of the membrane. The reason is that the higher the melt index of the polymer, the better the fluidity of the molecular chain, and the easier it is to move freely, which is not conducive to orderly arrangement, leading to a decrease in crystallinity and lower crystallinity. Overall, high crystallinity, high membrane strength, and decreased flexibility are important indicators for ETFE membranes as substrates. Based on the usage situation, we choose the ETFE membrane with 11.2 melt fingers as the substrate.

Table 1

DSC data.
Sample name	Tm (℃)	Tc (℃)	ΔHc (J g^− 1)	Xc (%)
15.6-ETFE-F	258.29	238.61	32.37	34.11
11.2-ETFE-F	255.78	239.57	34.01	37.69

Tm (℃) is melting temperature;Tc (℃) is crystallization temperature༛ΔHc (J g^-1) is enthalpy of crystallization༛Xc (%) is crystallinity.

From Fig. 5(a) and 5(b), it can be seen that the contact angle of ETFE-F is about 98.5 °, and the contact angle of C-ETFE-F is about 132.2 °, which can be attributed to the exposed hydroxyl groups on the surface. Prove that corona treatment of surface photophores alters the surface tension of ETFE-F, leading to enhanced wettability, and NOC can adhere to the surface of ETFE-F, demonstrating the feasibility of this scheme for preparing electronic labels.[37]

As shown in Fig. 6(a), the FTIR spectral strong absorption band of ETFE-F is analyzed as follows:2974cm^− 1 is the anti stretching vibration peak of - CH₂ -,2880cm^− 1 is the symmetric stretching vibration peak of -CH₃,1453cm^− 1 is the deformation vibration peak of CH₂, the absorption band 1248cm^− 1 is the deformation vibration peak of CH₃, and 1165cm^− 1.The stretching vibration peak representing - CF₂ -, the strong absorption at 1117cm^− 1 and 1043cm^− 1 can be attributed to the vibration on the - C- C carbon chain, and 744cm^− 1 is the in-plane rocking vibration peak of CH₂. The FTIR spectra of ETFE-F and C-ETFE-F are basically consistent, indicating that the influence of structural changes in ETFE materials on the membrane properties can be ignored during the experimental process.

In Fig. 6(b), the XRD spectrum of ETFE-F shows the presence of (120) crystal planes at 19.5 °, forming a tetragonal crystal system. The XRD spectrum of C-ETFE-F exhibits a (120) crystal plane at 19.5 °, forming a tetragonal crystal system. The sharp peak at 27° exhibits a (002) crystal plane, which is due to the introduction of carbon materials. Generally speaking, the higher the graphitization degree, the sharper the peak, and the narrower the half peak width. On the contrary, it is a low "Bulging peak".

Mechanical properties of the ETFE-F and C-ETFE-F

According to the testing requirements of ASTM D882, the specimen is stretched to failure to obtain mechanical properties. Plastic membrane sample is loaded into a fixture for testing, it is usually in a relaxed rather than tensioned state. The tensile strength test and elongation at break test molds are shown in Figure S3 (a), and the direction of force application is described in Fig. 7(d). The tear strength testing mold is shown in Figure S3 (b), and the direction of force application is described in Fig. 7(d). Samples 1 and 2 are ETFE-F, Samples 3 and 4 are C-ETFE-F in Figs. 7(a), 7(b) and 7(c).

Tear strength refers to the force required when a polymer membrane material is torn. It refers to the maximum tensile force per square millimeter applied to the transverse area of the membrane material when it is horizontally pulled apart.

Tear strength calculation formula:

TS = F/A

Among them, F is the force applied at the time of fracture, in kilograms; A is the cross-sectional area of the fracture, in square millimeters.

Measurement of tensile strength and elongation at break

The following equation is used to calculate elongation and tensile strength:

Elongation calculation formula E_B=(L₁-L₀/L₀) × 100

Formula for calculating tensile strength σ = F/(b × d)

In the formula, E_B: elongation, σ: Tensile strength (MPa)

F: Force value (N); b: Width (mm); d: Thickness (mm), L₁: Distance between scale lines, L₀: Distance between scales

Note that the thickness of the sample is 50 µm, and the width is 5 mm. The cross-sectional area of sample A is 1.25 mm². Test speed: 500 ± 30 mm/min

The tensile strength of various samples in Fig. 7 (a) at 20 ℃ is 33.4 MPa, 33.9 MPa, 32.9 MPa, and 33.1 MPa,The elongation at break of various samples in Fig. 7 (b) are 450.1%, 442.8%, 466.2%, and 486.2%, respectively. The tear strengths in Fig. 7 (c) are 69.5, 68.1, 66.8, and 66.1 Nmm^− 1, respectively. Therefore, the sample exhibits excellent mechanical properties, good tensile strength, elongation at break and tear strength, ensuring the stability of the substrate.

This article proposes an ETFE tag made by self-made heteroatom-doped conductive carbon screen printing technology. Heteroatom-doped conductive carbon was prepared by solvent method, and ETFE membrane was prepared by extrusion calendaring method. By using corona techniques, the difficulty of surface modification of traditional ETFE membrane has been successfully overcome, and the heteroatom-doped conductive carbon ETFE electronic tag antenna produced has good electrical and mechanical properties. The tensile strength reached 33.9 MPa, the elongation at break was 486.2%, the tear strength was 69.5 Nmm^− 1, and the sheet resistance reached 65 Ω. Therefore, the efficient preparation of ETFE tag has certain prospects in IoT applications.

Author contribution

Hao Fu wrote the main manuscript text and prepared all figures. All other authors reviewed the manuscript.

Availability of data and materials Not applicable.

Ethical approval Not applicable.

Competing interests The authors declare no competing interests.

Data availability. No additional data relating to this paper are publicly available.

Conflicts of interest. The authors declare no other conflicts of interest.

Declaration of funding. The work described herein was funded, in part, by he Basic Industrial Technology Projects of WenZhou City (G20210017).

Author affiliation

New Materials and Industrial Technology Research Institute of Wenzhou University, Wenzhou 325000, People’s Republic of China.

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No competing interests reported.

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ETFE RFID Tag with heteroatom-doped conductive carbon by screen print

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Abstract

Figures

Introduction

Experimental part

Chemicals required

Preparation of ETFE membrane with a thickness of 50 µm

Preparation of NOC

Preparation of tag

Study of structural, morphological properties of the synthesized materials

Results and Discussion

Chemical structure of NOC

Chemical structure of ETFE-F and C-ETFE-F

Mechanical properties of the ETFE-F and C-ETFE-F

Measurement of tensile strength and elongation at break

Conclusions

Declarations

References

Additional Declarations

Supplementary Files

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