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K.-K. Yu et al.: Effect of Surface Shallow Traps on Flashover Characteristics across Machinable Ceramic in Vacuum

Effect of Surface Shallow Traps on Flashover Characteristics across Machinable Ceramic in Vacuum
Kai-Kun Yu, Guan-Jun Zhang*, Guo-Qing Liu
State Key Laboratory of Electrical Insulation and Power Equipment, School of Electrical Engineering, Xian Jiaotong University Xian, Shaanxi 710049, China *Beijing Key Laboratory of High Voltage and EMC, North China Electric Power University Dewai Zhuxin Zhuang, Beijing 102206, China

Xin-Pei Ma and Guang-Xin Li State Key Laboratory for Mechanical Behavior of Materials, School of Material Science and Engineering, Xian Jiaotong University Xian, Shaanxi 710049, China ABSTRACT
The electrical strength of the surface of low-temperature melting machinable glass ceramic, prepared by using several different methods, is investigated before and after treatment with diluted hydrofluoric acid (HF). Using the surface potential decay method, the surface trap density and the energy of each sample are measured. The influence of acid treatment on the trap distribution is analyzed. Concurrent optical and electrical measurements allow surface flashover phenomena in vacuum under impulse voltage to be investigated, along with the influence of surface trapping parameters on flashover performance. It is shown that the glass phase on the surface of machinable ceramic greatly influences the shallow traps, which in turn degrade the flashover characteristics. Removing the glass phase with HF treatment reduces the concentration of shallow traps and stabilizes the flashover voltage. Index Terms Flashover, machinable ceramic, trapping parameter, vacuum insulation.

1 INTRODUCTION
INSULATORS are important components that are used for mechanical bracing and electrical insulation in vacuum. Insulators are widely used in high-voltage and power devices. However, the flashover across the insulator in vacuum is the primary limitation to many electrical and electronic systems, as it typically takes place on the surface region at much lower electric stress than the bulk breakdown strength of the material [1]. This phenomenon in vacuum has been studied for many years, but some processes are still not understood clearly [2]. Because of its excellent electrical and mechanical properties, alumina ceramic is widely used as the insulation system of highvoltage electro-vacuum devices. But this traditional sintering ceramic cannot be manufactured in some complex shape owing to the restriction of die arrangements. For its excellent machinable performance, low-melting temperature machinable glass ceramic (machinable ceramic) provides the possibility to
Manuscript received on 23 May 2008, in final form 6 July 2008.

produce the vacuum insulator with much better profile [3, 4]. Machinable ceramic can also be called microcrystallite glass or glass ceramic, melted with proper glass materials by adjusting the crystallization with controlling the heat. The machinable ceramic is made to be microcrystal and glass phase void-free complex material suitable for vacuum insulation [5]. The microstructure, performance, and manufacturing method of this material are very different from that of the traditional glass and ceramic; it shows the advantages of both glass and ceramic. Owing to the particular natural mica-like structure, it has excellent machinable performance similar to metals. The machinable ceramic material can be machined by normal turning machine even with continuous straps of the cutting swarf. The comparison of surface flashover performances between the glass ceramic and other materials have been performed very recently [6], and historically similar work was also reported [7]. In this paper, the samples are obtained by adding different additives to the crude materials of machinable ceramic. Because the flashover phenomena across the materials are greatly affected by the surface condition [2], hydrofluoric acid (HF) is used to

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modify the surface of the samples. Combining with the surface potential decay method and isothermal decay current (IDC) theory, the surface trap distribution of each sample before and after HF treatment has been calculated. Based on the concurrent optical and electrical measurements, the surface electric strength has been investigated in vacuum under impulse voltage application. Because the traps can capture and release electric charges, they may bring some effect on the flashover phenomena [8-13]; the influence of the surface trapping parameter on the surface flashover voltage has been explored.

2 SAMPLE PREPARATIONS AND EXPERIMENTAL SYSTEM


2.1 SAMPLE PREPARATION The machinable ceramic is composed of SiO2B2O3 Al2O3ZnOMgOF system and alkali metal oxides. SiO2 is the main component. The samples used are obtained by adding different additives to the crude materials. Adopting hightemperature feed method, with heating the quartz crucible in a furnace up to 11001200 C, the crude materials are put into the quartz crucible with low secondary electron emission (SEE) yield metal oxides such as Cu2O and Cr2O3 (0%, 1%, or 3%), then heating to the smelting temperature, and after thermal retardation for 12 h, the materials are agitated and kept at this temperature for additional 0.51 h. Then, they are poured to the cast-iron die arrangement to form the crystal, in order to ensure that all samples have good machinable performance. The employed samples are machined as circular wafers with a diameter of ~ 80 mm and thickness of ~ 3 mm. All samples are polished by UNIPOL802 precision buffing machine with the abrasive disk of 240# for ~ 2 h, to make the surface smooth and with consistent surface roughness. For this material, some electrical parameters of the machinable ceramic have been measured to compare with alumina ceramic (99% purity). The measurement frequency is 50 Hz as shown in Table 1. In comparison with alumina, the machinable ceramic samples show relatively lower resistivity and lower permittivity, and have similar dielectric loss. The low resistivity is possibly attributed to the additives and complex components. However, it still can be considered as an insulating material.
Table 1 Comparison of electrical parameters between alumina ceramic and machinable ceramic samples Samples Al2O3 Not doped 1% Cu2O 1% Cr2O3 3% Cr2O3 Volume resistivity (v) (cm) 3.441015 8.041013 1.191014 8.341013 7.5810
13

2.2 EXPERIMENTAL ARRANGEMENT Recently, the authors have reported that surface traps play an important role in the flashover phenomena across a material [6]. Here, the trap distribution is obtained by measuring the surface potential decay, and calculated by the isothermal decay current theory. The experiments are carried out in an adiabatic airtight chamber, with the temperature and humidity inside approximately constant at, respectively ~25 C and ~30%. For each sample, before and after HF erosion, it is stuck on a grounded stainless steel dish with electric silicone resin, respectively, with the polished surface facing toward the multineedle electrodes, as shown in Figure 1. 3 kV dc voltage is used to generate corona discharge to charge the sample surface, respectively, with the charged area of ~2 cm2 cm, the distance between needle tips and the sample surface is ~2 mm. In each experiment, immediately after charging the sample for ~3 min, the needle electrodes are removed and a vibration electrostatic probe is moved just above the charged area. Via a surface potentiometer, the surface potential decay is continuously recorded with a sampling rate of 1 s.

Figure 1. Experimental setup for trapping parameter measurement.

After removing the applied voltage, the charge carriers inside the shallow trap of the dielectric are first released, then the deeper trap charge carriers are released. Under a constant temperature condition, the released current changes with time. This current is related to the trap energy level distribution pattern. The relationship between the surface potential decay Vs and the current density J is (1) Supposing the released charge carriers do not get trapped again, then the relationship between the trap energy Et, the trap density Nt, and the isothermal decay current density J is shown as follows [14,15]:

J (t ) =

0 r d Vs (t )
d dt

Permittivity (r) 9.13 6.84 6.46 6.85 7.71

Dielectric loss (tan ) (%) 0.030 0.023 0.022 0.039 0.065

Et = kT ln(t ) J (t ) = qdkT f ( E ) N ( E ) 0 t t t 2t

(2)

Moreover, diluted HF is used to erode and modify the sample surface. The concentration is H2O: HF = 40:1 (ratio by volume) with the application time of ~ 2 min. Before trap and flashover measurements, all samples are sequentially cleaned with 95% acetone, alcohol, and de-ionized water in an ultrasonic cleaner, dried in a baking oven at a temperature of 150 C for 2 h.

where Et is the trap energy, k the Boltzmann constant, T the absolute temperature, the electron vibration frequency, d the sample thickness, f0(Et) the initial occupation probability of traps, and Nt(Et) is the trap energy distribution function. According to equations (1) and (2), the electron and hole trap energy distribution of these machinable samples can be calculated. Here, according to the assumption of [16], the electron vibration frequency is set as 1012 s1, and the initial trap occupation probability f0(Et) is 1/2.

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K.-K. Yu et al.: Effect of Surface Shallow Traps on Flashover Characteristics across Machinable Ceramic in Vacuum

In Figure 1, the injected homocharges just exist in a surface layer as thin as 12 m, which dominates the surface potential [17]. Thus the measured trap parameters mainly reveal the trap distribution in the surface layer of a sample. After the traps measurements, each sample is cleaned and employed again to measure the flashover. The electrodes shape used in the experiment is plane structure as shown in Figure 2. The best advantage of this electrode structure is suitable for optical observation and it is applicable to the flat plate samples. Each sample is placed on an organic glass substrate. Two stainless steel electrodes are pressed on the sample with springs between the PTFE brace and the substrate, for achieving a close contact between the electrode and the sample. The electrode gap spacing is 10 mm and the diameter of the stainless steel electrodes is 20 mm.

value of these applied voltages is called the conditioned voltage Uco. Above Uco, the applied impulse voltage can lead to flashover every time. After reaching the conditioned flashover voltage, the applied voltage is reduced by a step of 1 kV until no flashover occurs. This voltage is defined as the hold-off voltage Uho.

3 EXPERIMENTAL RESULTS AND DISCUSSION


3.1 MEASUREMENT OF TRAP PARAMETERS For each machinable ceramic sample, the surface trap measurement is performed at room temperature before and after HF erosion. After charging the sample with positive or negative corona discharges, the surface potential decay curve is recorded immediately, as shown in Figure 4. It usually takes less than 30 min for the potential to decrease to zero, much shorter than that of polymeric materials [19].

Figure 2. Electrode-sample configuration.

The high voltage impulse is supplied by one stage Marx generator with the main capacitor being 0.0111 F. The output voltage can be up to 80 kV with the waveform of 0.42/2.5 s double exponential pulse without a load. Figure 3 shows a typical voltage waveform used in this experiment. The electrode system is fastened on the ground of a vacuum chamber at a pressure of ~ 4104 Pa. The applied voltage is measured via a high voltage divider, the flashover current by a 25.6 m noninductive resistor. Both voltage and current waveforms are recorded by a fourchannel digital oscilloscope [6].

Figure 4 Surface potential decaying characteristic curves (a) before treatment with HF, (b) after treatment with HF.

Figure 3. Typical impulse voltage waveform.

In the experiment, the applied voltage is increased from 10 kV charging voltage with a step of 1 kV, and the impulse voltage is applied 10 times at each step. Several voltage levels are used to characterize the flashover phenomena [18]. With the increase in applied voltage, the flashover phenomena will appear at a critical voltage; this voltage is recorded as Ufb (first breakdown voltage). The applied voltage is gradually increased until each of the 10 impulses can induce the flashover across the sample; the average

From Figure 4, it can be seen that after treatment with HF, the surface potential decay of the samples is much quicker than that of untreated with HF. Based on numerical differential calculation, the current density can be obtained. From equations (1) and (2), the electron and hole trap parameters of these samples before and after eroding can be calculated as shown in Figure 5. In Figure 5, the trap energy interval of machinable ceramic is about 0.710.87 eV, which belongs to the relatively shallow traps [16]. It is believed that the shallower or deeper traps can also be reflected under lower or higher temperature, respectively.

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metal oxide, the trap densities of the samples are reduced significantly. The sample doped with 3% Cr2O3 shows the lowest trap density. After HF treatment, the trap density and energy distribution of the samples change. For the original samples without HF treatment, both the electron and hole trap distributions have density peaks at the energy interval of about 0.770.81 eV. After a minimal value at the energy interval of about 0.820.85 eV, the trap density increases appreciably, as shown in Figures 5a and 5c. After erosion by HF, as shown in Figures 5b and 5d, the peak value of the trap density corresponding to the shallow traps decreases significantly. Table 2 summarizes the changes of trap density peak value of the machinable ceramic samples near the energy level of 0.770.81 eV before and after HF treatment. For the machinable ceramic samples with 3% Cr2O3, no trap density peak is observed after HF treatment.
Table 2 Comparison of trap density peak for different samples Trap density (eV)1/m3 Electron trap Net Hole trap Nht Samples Before After Before After erosion erosion erosion erosion No doped 1.421018 1.811017 1.901018 8.701016 1% Cu2O 1.031018 6.511016 1.341018 6.271016 4.621017 1.221017 9.491017 1.751017 1% Cr2O3 2.261017 2.931016 4.211017 3% Cr2O3

3.2 SURFACE MICROSTRUCTURE OBSERVATION The changes of surface trap density before and after diluted HF treatment imply the surface condition of the sample changed. Machinable ceramic has a glass phase structure, and it is supposed that diluted HF might erode the surface of the glass component. The undoped machinable ceramic and 3% Cr2O3 doped sample before and after HF treatment were selected to observe their surface microstructure, as shown in Figure 6.

Figure 5. Surface trap density distributions before and after HF treatment (a) electron trap before treatment; (b) electron trap after treatment; (c) hole trap before treatment; (d) hole trap after treatment.

According to Figure 5, different samples show quite different trap density distributions. When compared with the undoped machinable ceramic sample. After adding some low SEE yield

Figure 6. Typical SEM microstructure of test samples. (a) original no-doped sample; (b) no-doped sample after HF treatment; (c) original doped 3% Cr2O3 sample; (d) doped 3% Cr2O3 sample after HF treatment.

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K.-K. Yu et al.: Effect of Surface Shallow Traps on Flashover Characteristics across Machinable Ceramic in Vacuum

The photographs clearly indicate that after HF erosion, the glass phase components on the surface of the samples have been eroded, and the crystal phase components, displayed as the sectional shape of sticks in Figures 6b and 6d, emerge on the surface. It is believed that further erosion will bring the appearance of more crystal phase (Figure 6d). Combining Figures 5 and 6, it is considered that the surface glass phase structure has a definite relationship with the trap parameters in the surface layer of a sample. Reduction of glass phase components induces the decrease of trap density, especially for the shallower traps, as in Figure 5. 3.3 FLASHOVER CHARACTERISTICS IN VACUUM In the flashover experiment, the pulsed voltage was applied from the charging voltage of 10 kV and raised with a step of 1 kV. At each step the impulse was applied 10 times. At each voltage step, the average value of maximal voltage and current of 10 times were calculated, respectively, as shown in Figure 7. This indicates the peak value relationship between the voltage and current during the increase of the voltage. The case when the voltage decreases, after flashover, all 10 applications are not shown in Figure 7 in order not to clutter the figure.

Several voltage levels are used to characterize the flashover phenomena for each sample, i.e., the first breakdown voltage Ufb, the conditioned voltage Uco, and the hold-off voltage Uho, as shown in Tables 3 and 4. The flashover performance of alumina ceramic (99% purity) is tested with the same electrode configuration. There is no significant difference observed before and after HF treatment, possibly because of the chemical stability of alumina ceramic. Its voltage values exhibit a poorer flashover performance than that of eroded machinable ceramic samples.
Table 3 Flashover performance of samples before HF treatment Samples Ufb (kV) Uco (kV) Uho (kV) Al2O3 27.3 41.1 32.2 No doped 27.5 45.6 39.7 22.2 43.5 41.0 1% Cu2O 18.1 43.2 37.0 1% Cr2O3 20.9 41.2 40.2 3% Cr2O3

Table 4 Flashover performance of samples after HF treatment Samples Ufb (kV) Uco (kV) Uho (kV) Al2O3 28.4 40.5 31.3 No doped 29.0 42.3 40.2 33.2 45.0 44.5 1% Cu2O 36.9 45.8 42.9 1% Cr2O3 41.6 41.6 41.3 3% Cr2O3

Figure 7. Peak value relationship of voltage and current for different samples before and after HF treatment. (a) before HF treatment; (b) after HF treatment.

It is clearly seen that the flashover data for the original samples with no HF treatment have much scatter. However, the scatter decreases after HF treatment, and there are fewer flashover events before the stable flashover voltage is reached.

3.4 RELATION BETWEEN FLASHOVER PERFORMANCE AND TRAP DENSITY As shown in Table 2, the surface trap densities of samples doped with metal oxide are significantly reduced, especially for the sample doped with 3% Cr2O3. After the HF treatment, the trap density peak values corresponding to the shallower traps decrease greatly. For instance, for the undoped machinable ceramic sample, the peak value of the shallower electron trap density drops from 1.421018 to 1.811017 (eV)1m3. For the doped sample with 3% Cr2O3 drops from 2.261017 to 2.931016 (eV)1m3, and all decrease by about one order of magnitude. With the addition of lower SEE yield metal oxide, the trap density decreases significantly and the surface trap density of the sample doped with Cr2O3 is much lower than that of the sample with Cu2O. However, for the deeper traps with the energy level above 0.85 eV, the density decline after HF treatment is not more than twofold. It should be noted that for the undoped machinable ceramic sample, after HF erosion, the surface electron trap density even increases from 2.991017 to 4.751017 (eV)1m3, and there is also slight abnormity for the hole traps of 3% Cr2O3 doped ceramic sample. One reasonable supposition is that some chemical elements emerge on the surface after HF erosion, resulting from the complicated contents in machinable ceramic. They act as new trap centers. It is considered that the existing traps result from the glass phases and the interfaces between the glass and the crystal phases. Most of the shallower traps can be effectively eliminated by eroding off the glass phase structure. Based on the secondary electron emission avalanche (SEEA) model [2, 20], which is widely accepted to describe the flashover phenomena, the flashover developing process is strongly dominated by the surface SEE and charging phenomena. Under an applied voltage even lower than the flashover voltage, there is SEE phenomenon and the generation

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of holes with positive charges on the sample surface. The generated electrons can be captured for a short time or permanently captured by electron traps. When the holes have not been captured by hole traps, they may easily recombine with electrons. While some holes are captured by hole traps, it will be difficult for their recombination, leading to more positive charges on the surface. And based on our proposed charge injection model, charge carriers injected from the electrodes can be trapped in trap centers [9, 10]. The trapped charges will nonuniformly accumulate on the surface between the electrodes, leading to an apparent distortion of the local electric field on the surface, and make the flashover easier in the next application of higher impulse voltage. Thus, it is easy to understand that a higher surface trap density corresponds to a lower flashover voltage. In this paper, it is preliminarily concluded that the flashover across machinable ceramic samples is mainly dominated by the shallower traps with energy below 0.85 eV. As in Tables 3 and 4, after treating the machinable ceramic samples with HF, the characterization voltages of all samples increase. The conditioned voltage Uco does not change, but the first breakdown voltage Ufb is effectively increased. It can be seen from the tables that for the original samples, their average Ufb values are lower by about 48.9% than the Uco values, but after HF treatment, these values reduce to 19.5%, and for the sample doped with 3% Cr2O3, its Ufb is even consistent with the Uco value. After HF treatment, the hold-off voltage Uho improved too, their values increasingly approach the conditioned voltage Uco, and the differences between these two voltages are reduced. All machinable ceramic samples with HF treatment exhibit a much better flashover performance than the traditional alumina ceramic. Promotion of the stability of flashover across machinable ceramic sample is very useful for high-voltage electro-vacuum devices. For a device operating under high electric field, the Uco value of its insulating material employed is important, but the flashover stability of the material is much more important, because the first breakdown voltage Ufb usually dominates the design of its insulation level. The machinable ceramic is promising for future high-power equipment as it is more compact and reliable.

ACKNOWLEDGMENTS
This work was in part supported by the National Natural Science Foundation of China (50777051) and by the Program for New Century Excellent Talents in University of MOE (NCET-04-0943), China.

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[11]

[12]

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4 CONCLUSIONS
Based on the experimental results and analysis, it is considered that the glass phase on the surface of machinable ceramic materials is important for shallow traps that exist on the surface. The surface glass phase components can be effectively eroded by HF treatment. The experimental results indicate that after treatment with this acid, the shallow trap energy densities decline, the first breakdown voltage of the samples increase greatly, and the overall flashover performance appears to be more stable. The shallow trap energy can be considered as the reason for the low first flashover voltage. Eliminating the shallow trap distribution with HF erosion treatment can improve the stabilization of the flashover characteristics of the material. The machinable ceramic is a promising alternative for future high power equipment to make it more compact and reliable. It is needed to clarify the influence of the surface traps with different energy levels, and also the effects of traps under different applied waveforms.

[15] [16] [17] [18] [19] [20]

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K.-K. Yu et al.: Effect of Surface Shallow Traps on Flashover Characteristics across Machinable Ceramic in Vacuum
Kai-Kun Yu was born in Shaanxi Province, China, in 1981. He received the B.S. and M.S. degrees in electrical engineering from Xian Jiaotong University (XJTU), China, in 2003 and 2006, respectively. He is presently a Ph.D. candidate at the same university. His current research interests are pulsed surface flashover phenomena across the ceramic and composite organic materials. Guo-Qing Liu was born in Henan Province, China, in 1983. He completed his Bachelor program in material science engineering at Xi'an Jiaotong University (XJTU), China, in 2006. He is presently a master student in the School of Electrical Engineering at the same university. Since 2007, He has committed himself to the research of pulsed surface flashover phenomena in vacuum.

Guan-Jun Zhang (M02) was born in Shandong Province, China, in 1970. He received the M.S. and Ph.D. degrees in electrical engineering from Xian Jiaotong University (XJTU), China, in 1994 and 2001, respectively. Since 1994, he has been employed as a teaching assistant at the same university. From 1998 to 1999, he joined Tokyo Institute of Technology as a visiting researcher, engaged in surface electroluminescence and discharge phenomena of solid insulating materials. From 2006 to 2007, he joined Princeton University as a senior visiting fellow, engaged in secondary electron emission characteristic and plasma simulation. Since 2004, he is presently a professor at State Key Laboratory of Electrical Insulation and Power Equipment and School of Electrical Engineering in XJTU. He is also an adjunct professor at Beijing Key Laboratory of High Voltage and EMC, North China Electric Power University. He has obtained many awards and prizes from Chinese government. His current research interests are electrical discharge and plasma, pulsed power technology and condition maintenance of power equipment. He has published more than 80 journal articles and conference papers.

Xin-Pei Ma was born in Jiangsu Province, China, in 1952. She received the M.S. and Ph.D. degrees in material science and engineering from Xian Jiaotong University (XJTU), China, in 1989 and 2003, respectively. Since 1977, she has been employed as a teaching assistant at the same university. Since 2002, she has been a professor at State Key Laboratory for Mechanical Behavior of Materials and School of Material Science and Engineering in XJTU. Her current research interests are mechanical and electrical performance of materials, based on the 4 elements of processing, composition, microstructure and properties of advanced structure materials. She has published more than 30 journal articles and conference papers. Guang-Xin Li was born in Jilin Province, China, in 1950. Since 1993, he has been an associate professor at State Key Laboratory for Mechanical Behavior of Materials and School of Material Science and Engineering in XJTU. His current research interests are mechanical and electrical performance of materials, based on the 4 elements of processing, composition, microstructure and properties of advanced structure materials. He has published more than 40 journal articles and conference papers