Ti Nano-Multilayers with Superior Performance in Plasma

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Functional Nanostructured Materials (including low-D carbon)

Reactive B/Ti nano-multilayers with superior performance in plasma generation Yuxin Zhang, Yao Wang, Mengting Ai, Hongchuan Jiang, Yichao Yan, Xiaohui Zhao, Liang Wang, Wanli Zhang, and Yanrong Li ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b08120 • Publication Date (Web): 06 Jun 2018 Downloaded from http://pubs.acs.org on June 6, 2018

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ACS Applied Materials & Interfaces

Reactive B/Ti Nano-multilayers with Superior Performance in Plasma Generation Yuxin Zhang,# Yao Wang,* , # ,† Mengting Ai,# Hongchuan Jiang,# Yichao Yan,# Xiaohui Zhao,# Liang Wang,#, † Wanli Zhang,# and Yanrong Li#

#

State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic

Science and Technology of China, Chengdu 611731, China †

Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang 621000,

China

ABSTRACT: In this study, reactive B/Ti nano-multilayers were fabricated by magnetron sputtering, and the structure and chemical composition were confirmed by TEM and XPS analyses. The periodic multilayer structure can be clearly visible, and the multilayer material is composed of B layers (amorphous), Ti layers (nano-polycrystalline) and intermixed reactants in a metastable system. The as-deposited B/Ti nano-multilayers exhibit a significantly high heat release of 3722 J/g, with an onset reaction temperature of 449 °C. Based on these properties, an integrated micro-igniter was designed and prepared by integration of the B/Ti nano-multilayers

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with a TaN film bridge for potential applications in plasma generation, and the electric ignition processes were investigated with discharge voltages ranging from 25 to 40 V. The integrated micro-igniter exhibits improved and stable ignition performances with a short burst time, high plasma temperature and violent explosion phenomenon in comparison with the TaN film igniter. Overall, the plasma generation of the micro-igniter can be enhanced substantially by integration with the B/Ti nano-multilayers. KEYWORDS: B/Ti, nanostructured energetic composites, reactive nano-multilayers, plasma generation, ignition, energetic multilayers

1. Introduction Recently, investigations into nanostructured energetic materials have continued to arouse great interest owing to their superior characteristics.1-8 Nanostructured energetic materials, which are characterized by maximum interfacial contact area and minimum molecular diffusion distance, exhibit excellent performances in terms of tunable ignition sensitivity, rapid energy release, high energy density and low ignition temperature compared to conventional energetic materials.9-15 Different types of nanostructured energetic materials based on intermetallic reactions or thermic reactions have been synthesized, such as the periodic deposition of multilayers,4 arrested milling of dense composite nano-powders,16 electrophoretic energetic nano-coating17 and physically mixed nano-powders.18 Among these means, the fabrication of multilayer films via periodically depositing two different materials provides an approach to building reactive systems consisting of high-purity reactants with carefully controlled structure scales. The multilayer films can also


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be easily integrated with microelectronic and mechanical systems (MEMS) to realize various functions such as non-contact ignition,19 power supply,20 joining of materials21 and exploding foil initiator.22 A film micro-igniter is often utilized to generate plasma to initiate a secondary reaction, and the generated plasma plays a key role during the ignition process. Many kinds of multilayer films such as Al/PTFE,23 Al/MoO3,7 Al/NiO,24 Al/CuO25 and Al/Ni26 have been integrated with film igniters to improve the performances of plasma generation. Among these materials, B/Ti multilayers exhibit superiority over most other aluminum-based reactive multilayers for the following reasons. First, it can provide a larger theoretical energy release of 5525 J/g (Table 1) between elemental B and Ti, and an extra heat release of 7875 J/g with the formation of TiO2 in the ambient environment.27, 28 Second, the processes of integrating energetic multilayers with a micro-chip by MEMS technology will inevitably meet with some acid-base environments. The physical and chemical properties of B/Ti multilayers are more stable than those of the Al/oxide reactive systems, which are beneficial for fabricating and storing integrated devices in various environments. Third, the O atoms will diffuse into the chamber during depositing the Al/oxide reactive materials, which will influence the deposition of the Al layers and the integration with the metal film bridge. However, the researches about the B/Ti multilayers and the integrated device based on B/Ti nano-multilayers are rare.

Table 1. The maximum theoretical energy release of various reactive materials29

Reactant

B-Ti

Al-Ni

Al-MoO3

Al-NiO

Al/CuO

Al/PTFE

Energy release (J/g)

5525

1381

4705

3579

4077

5571


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A TaN film bridge can be used as a micro-igniter with excellent performances because of its properties including low temperature coefficient of resistance, adjustable resistivity, selfpassivation and resistance to corrosion.30 These characteristics lead to an improved stability and applicability over a wide temperature range in comparison with the traditional igniters. In this work, a TaN film bridge was prepared as a micro-igniter to generate plasma, and the B/Ti multilayer nanomaterials were deposited on it to enhance the plasma generation. The characteristics of the as-deposited B/Ti nano-multilayers were investigated, and the electric ignition performances including burst time, critical explosion energy and temperature variation of plasma were tested at different discharge voltages. Meanwhile, the reaction dynamic processes of plasma generation were also recorded synchronously by a high-speed camera.

2. Experimental Methods 2.1 Deposition of the B/Ti nano-multilayers The B/Ti nano-multilayers were fabricated by depositing alternately Ti layers and B layers on a polished substrate. The pressure of the chamber was evacuated less than 5×10-4 Pa before the films deposition. For optimized films quality and stable deposition rates, the Ti layers and B layers were sputtered from a titanium target (purity > 99.999%) and a boron target (purity > 99.999%) by direct-current (DC) magnetron and radio frequency (RF) magnetron sputtering, respectively. The sputtering power and pressure were set 100 W, 0.5 Pa for the Ti layers, and 300 W, 1.0 Pa for the B layers, respectively. Argon gas was used as the gas medium, and the sputtering pressure was tuned by changing the flow rate throughout the deposition.


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2.2 Fabrication of the integrated micro-igniter

Figure 1. Schematic drawing and fabrication process flow of the integrated micro-igniter

The fabrication of the integrated micro-igniter was based on MEMS techniques to ensure production accordance and a high level of integration, as shown in Figure 1. Hundreds of microigniter units can be prepared simultaneously on a 3 in. alumina substrate with a high consistency. Each unit consists of a TaN film bridge on the bottom, square B/Ti multilayer films deposited on the top of TaN film bridge, and two Cu contact pads located at the both ends of TaN film bridge. The TaN film bridge was initially prepared and patterned by magnetron sputtering and wetetching technology, and the processes were similar to our previous work.31 The dimension of the patterned TaN film bridge was 60 µm long and 30 µm wide. Subsequently, a square 4-µm-thick multilayer B/Ti films with a monolayer thickness of 50 nm was deposited on the top of the TaN film bridge through a designed mask with a size of 4 mm × 4 mm; the stacking sequence was B/Ti/B/Ti, and the Ti layer was left as the top layer. After the deposition of reactive layers, two rectangular Cu layers were deposited at both ends of the TaN film bridge for the power source connection. Finally, the finished sample was diced into individual units for testing.


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2.3 Characterization Methods The crystallinity and microstructure analyses at atomic level were performed by transmission electron microscopy (TEM). The chemical composition of the B/Ti nano-multilayers was determined by X-ray photoelectron spectroscopy (XPS). The heat release properties of the B/Ti nano-multilayers scraped from the substrate were measured by differential scanning calorimetry (DSC), and the tests were carried out from 50 to 900 °C at a heating rate of 10 °C/min under a nitrogen atmosphere. The effects of deposited B/Ti nano-multilayers on the heat transport property of the TaN film were investigated by an ultrafast measurement system for the thermal properties of film materials at room temperature. A 100-nm-thick platinum layer was coated on the surface of the samples, and the temperature variation of the samples was detected by the alteration of the reflectivity of the sample surface. The ignition performances of the samples were carried out at discharge voltages ranging from 25 to 40 V, and the test system (capacitor discharge, 47 µF) for electric ignition was shown in Figure 2. The temperature variations of the generated plasma during electric ignition processes were determined by comparing relative intensities of spectral lines from the Cu (Ι) 521.84 nm and Cu (Ⅱ) 455.59 nm.32-35 A ~10-nmthick copper layer was coated on the surface of sample for temperature measurement. Each type of sample was measured four times at the same discharge voltage, and then the results of peak temperature were averaged for calibration. The images of electric explosion phenomena for plasma generation were obtained synchronously by a high-speed camera connected to a computer.


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Figure 2. Schematic drawing of the test system used to apply electrical impulses across the micro-igniters and record data during the ignition processes

3. Results and discussion 3.1 Structure and composition characterization


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Figure 3. (a) Cross-sectional bright field TEM image of the B/Ti nano-multilayers, (b) electron diffraction pattern of the B layer, (c) electron diffraction pattern of the Ti layer, (d) highresolution image of the interface between B and Ti, (e) high-resolution image of the Ti layer, and (f) high-resolution image of the B layer

Figure 3(a) shows the cross-sectional bright field TEM image of the as-deposited B/Ti nanomultilayers. The B layers and Ti layers are arranged periodicity with controlled thickness, and different layers can be distinguished easily. The B layers appear as bright stripes, while the dark stripes correspond to the Ti layers. The selected area electron diffraction patterns of the B film and Ti film are shown in Figure 3(b) and (c), respectively. The B film exhibits broad and diffuse rings, indicating an amorphous structure. While the Ti film presents a well-defined nanopolycrystalline structure. The wavy interface between B layer and Ti layer is also visible in Figure (d), and the high-resolution images of the B layer and the Ti layer are shown in Figure 3 (e) and (f). We can see the lattice arrangement in Ti layer, while the random arrangement in B layer. Both B and Ti are present at a several nanometer thick volume interfacial region. It is not clear enough if there are intermixed reactants in this region. Compared to the thickness of the pure element regions, this region is slight so that the influence on the heat release might be minimal.


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Figure 4. (a) XPS survey spectrum of the B film with an ~1-nm-thick Ti overlayer, (b) highresolution spectrum of B 1s core level of the B film, (c) high-resolution spectrum of B 1s core level of the B film with an ~1-nm-thick Ti overlayer, and (d) high-resolution spectrum of Ti 2p core level of the B layer with an ~1-nm-thick Ti overlayer

To further confirm the interfacial chemical composition between the B layer and Ti layer, XPS was conducted on a B film with deposition of an ~1-nm-thick Ti layer, and the XPS survey spectrum is shown in Figure 4(a). The features corresponding to elements B, Ti, O and C are evident. The presence of oxygen is derived from surface oxidation during exposure to the ambient environment. Figure 4(b) shows the high-resolution spectrum of B 1s core level of the B film without a Ti layer deposited on the surface. Two peaks appear at binding energies (BEs) of


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188 and 191.5 eV. The BE of 188 eV can be assigned to boron, and that of 191.5 eV is typical of surface oxidation. Figure 4(c) shows the high-resolution spectrum of B 1s core level of the B film with depositing an ~1-nm-thick Ti overlayer. Three peaks appear at BEs of 187.3, 188.7 and 191.9 eV, respectively. The peak at 191.9 eV is due to the surface oxidation, and that of 188.7 eV is assigned to boron. This result is consistent with the observation from the B film without the Ti layer deposited on its surface. The peak at 187.3 eV can be attributed to B-Ti bonds in TiB2.36, 37

The peaks that match B-B and B-O bonds appear at slightly higher binding energy values,

which might be attributed to the deposition of Ti layer on surface. Meanwhile, as shown in Figure 4(d), the high-resolution XPS spectrum of the Ti 2p core level displays three major peaks, and the fitting peaks at Ti 2p1/2 460.3 eV and 2P3/2 454.3 eV match well those of Ti-B bonds in TiB2.36, 37 These results clearly suggest that the reaction occurs at the interface of Ti and B. Therefore, the B/Ti nano-multilayers are in a metastable system consisting of B layers, Ti layers and intermixed reactants layers. This feature is also evidenced by the aforementioned TEM results.

3.2 Thermal properties characterization


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Figure 5. Heat release characterization of the B/Ti nano-multilayers at a heating rate of 10 °C/min under a N2 atmosphere

The heat release characteristics of the B/Ti nano-multilayers were investigated by DSC in a nitrogen atmosphere, as shown in Figure 5. There is only one major exothermic peak during the period of temperature rise. The initial reaction temperature between B layers and Ti layers is 449 °C, and the major exothermic peak is located at 607 °C. The total heat release can be calculated by the integration of the positive exothermic area, which was determined to be 3722 J/g. This matches well with the literature value of 3694 J/g. The energy release is well below the maximum theoretical value; this might be caused by the formation of B-Ti compound layers during the film deposition and storage decrease the heat release, and/or the reactions between B layers and Ti layers are not completed during the rise in temperature. Although the exothermic performance might be diminished due to the intermixing of elemental B and Ti at the interfaces, the B/Ti nano-multilayers exhibit a significantly high energy output at a relatively lower onset reaction temperature.


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Figure 6. The heat transport performances of the TaN film covered with different thick B/Ti nano-multilayers on its surface

Figure 6 shows the heat transport performances of the TaN film covered with different layer of B/Ti films. After applying heat to the samples, the thermal reflectance signals begin to descend with time. A faster decreasing thermal reflectance signal indicates a better heat transport performance from the surface to the substrate. The heat transport performances of the samples decreases with growing number of layers. When the TaN film was covered with a 40-bilayer B/Ti films, the heat transport property decreases significantly. This phenomenon can be ascribed to the low thermal conductivity of boron, resulting in a declining heat transport performance with increasing thickness of B film.

3.3 Ignition performances tests

Figure 7. Typical experimental result of I-V variation curves for the ignition of the integrated micro-igniter at a discharge voltage of 10 V


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The electric ignition process of the integrated micro-igniter involves the ionization of the TaN film and the chemical combustion of the B/Ti nano-multilayers. After applying the electrical impulses, the high current density loaded at the TaN film causes a rapid rise in the temperature, leading to a rapid state change from solid to ionized plasma occurred on the TaN film bridge. The electrical ignition characteristics of the integrated micro-igniter at a 10 V discharge voltage is shown in Figure 7. The first peak is related to the melting and vaporization of the TaN film, and the second peak is due to the emergence of the plasma.38 Therefore, the time of the second peak is regarded as the burst time (Tb), and the energy deposited on the bridge during this time is regarded as the critical explosion energy (Ec). The critical explosion energy is calculated by integrating the power with respect to time, and the power is determined by voltage multiply current.


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Figure 8. The experimental results of the burst time (a) and critical explosion energy (b) for the TaN film igniter and the integrated micro-igniter with discharge voltages ranging from 25 to 40 V

The results of the burst time and the critical explosion energy obtained from the electric ignition tests at discharge voltages ranging from 25 to 40 V are shown in Figures 8(a) and (b), respectively. For the integrated micro-igniter, the Tb values decrease with increasing discharge voltage, and the Ec values increases with increasing discharge voltage. These are caused by the


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increased energy input. While for the TaN film igniter, the heat will diffuse from its surface during the rising of the temperature which is affected by the ambient environment easily, leading to an irregular variation of the Ec values. Meanwhile, the difference in Tb and Ec between the TaN film igniter and the integrated micro-igniter are diminished with increasing discharged voltage, which might be attributed to the reduction of heat loss, because the increased discharge voltage can accelerate the plasma generation. These results are consistent with the results of heat transport test. As a result, the integration with B/Ti nano-multilayers has a function of heat conservation and serves to decrease the burst time and improve the stability effectively. Moreover, the B/Ti nano-multilayers can also utilize this energy to react so that increase the energy output.

Figure 9. The temperature variation curves for the TaN film igniter and the integrated microigniter during the electric ignition processes at a 25 V discharge voltage

The temperature variations of the generated plasma during the electric ignition process are investigated by comparing relative intensities of spectral lines, and the results after data


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processing are shown in Figure 9. After the electrical pulse is applied to the TaN film igniter, the plasma temperature increases abruptly and reaches a peak value of 3762 K. While for the integrated micro-igniter, the maximum temperature is over 6000 K, which is significantly higher than the peak value of the TaN film igniter. With increasing discharge voltage, the maximum temperatures of the integrated micro-igniter are all obviously higher than those of the TaN film igniter, as shown in Figure 10. The increments of peak temperature confirm that the chemical reaction between B and Ti is involved in the formation of plasma, accompanied with a large number of heat release. The high temperature will contribute to the vaporization and ionization of the TaN film, and the consequent expansion of the generated plasma.

Figure 10. The peak temperatures of the generated plasma during the electric ignition processes at discharge voltages ranging from 25 to 40 V

Based on the electric ignition tests, the dynamic reaction processes of plasma generation are recorded synchronously, and a series of high-speed video frames are shown in Figure 11. A violent explosion reaction associated with a plasma generation takes place on the TaN film


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igniter, while the explosion phenomenon for the integrated micro-igniter is more intensity, which is accompanied by a substantially brighter flash and larger plasma volume. In addition, the reaction courses of integrated micro-igniter are in accordance with those of the TaN film igniter, we can hardly see the chemical combustion phenomenon lag after the ionization of the TaN film. These clearly indicate that the energy release by the B/Ti nano-multilayers is effectively combined with the Joule heat of the TaN film, leading to a concentrated energy burst and strong output. The maximum plasma height is over 7 mm with the substrate as reference, which exhibits a high energy output with a smaller device size.7 As shown in Figure 12, compared to the microinitiator integrated with Al/NiO multilayers reported in our previous work,24 the micro-igniter integrated with B/Ti nano-multilayers also exhibits superior performance in plasma generation with an intense electric ignition phenomenon accompanied with obviously larger plasma volume and significantly brighter flash at the same discharge voltage of 40 V. Moreover, with increasing discharge voltage, the materials are vaporized and ionized more completely to form plasma, resulting in the performances of plasma generation are tunable via changing the discharge voltages.


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Figure 11. High-speed camera observation of the dynamic reaction processes of the plasma generation for the TaN film igniter (a) and the integrated micro-igniter (b), and the interval between adjoining photographs is 0.05 ms

Figure 12. High-speed camera observation of the ignition process for the micro-igniter integrated with Al/NiO multilayers at a 40 V discharge voltage, and the interval between adjoining photographs is 0.05 ms

4. Conclusions


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In summary, an integrated micro-igniter was realized through depositing the B/Ti nanomultilayers on a TaN film, and the performances of the plasma generation were investigated through electric ignition tests. The results indicate that the B/Ti nano-multilayers have the function of heat conservation and serves to decrease the burst time and improve the ignition stability effectively. The higher explosion temperature and more violent ignition phenomenon also confirm that the chemical reaction of the B/Ti nano-multilayers is involved in the plasma generation accompanied with a large number of heat release. Overall, the integrated B/Ti nanomultilayers can improve the plasma generation of micro-igniter substantially without increasing the device size and input energy, and the tunable performances of plasma generation also extend the applicability of the integrated micro-igniter in both civil and military fields.

AUTHOR INFORMATION Corresponding Author *E-mail: [email protected] Notes The authors declare no competing financial interest.

ACKNOWLEDGMENT This work was supported by the military support project fund (No. JPPT-125-5-161)

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Graphical Abstract


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Ti Nano-Multilayers with Superior Performance in Plasma

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