Effects of gases on field emission performance were measured using silicon-gated field emitter arrays. Gas was injected into a vacuum chamber with a 1000 × 1000 tip array, which was driven by a DC gate and collector voltages. The collector voltage was fixed at 200 V while the gate voltage was swept to 40 V. For the gas exposure study, N2, He, and Ar were used. The sets of partial pressures, 5 × 10−6, 5 × 10−5, and 5 × 10−4 Torr, were used for the experiment. It was observed that N2 had the least effect and Ar had the worst effect on emission current performance. The degradation of collector current at 5 × 10−4 Torr pressure for Ar was ≈65% where for the N2, at the same level of pressure, the degradation was ≈41%. However, further experiments with high purity Ar gas showed that it was the water vapor present in the gas itself that was the primary cause of reduction in emission current and not the gas itself. The results expressed in reduction in emission current versus Langmuir exposure versus the current clearly showed the effect of water vapor. After the vacuum was recovered, the work function again restored partially to its original value. After ultraviolet light cleaning, the emission current was restored completely to the original state.

Field emitters are now widely discussed as an electron source for nanovacuum channel transistors.1–5 In field emitters, emission of electrons takes place by quantum mechanical tunneling from a micro- or nanometer scale tip by applying a positive potential on a gate electrode that surrounds the tip.6–9 During the operation of these devices, high vacuum is required to reduce the gas-electron collision probability between the electrodes. Field emitters can be used as a number of vacuum microelectronic devices, such as harsh environment electronics.10–12 One major hurdle to the successful application of silicon-gated field emitter arrays (GFEAs) is the rapid degradation of field emission current during operation.13–15 It is well known that field emission is quite sensitive to the surface condition16,17 and contamination of emitters, which can cause a problem when field emitters are vacuum packaged. Residual gases, particularly oxygen and water vapor not removed by the heat treatment, or gas desorbed by the electron bombardment of device components is known to interact with GFEAs and result in reduction in the field emission current. Research work on GFEAs has focused on assimilation of degradation mechanisms caused by oxidation of the tip material from residual gases, primarily oxygen and other gases containing oxygen.18,19 In contrast, previous works have demonstrated that the presence of hydrogen gas can improve the field-emission current of metal-based field emitter arrays.18,20 However, effects of gases on Si-GFEAs are reported to result in reduced field emission current.21 Only a few systematic study that examines the effects of different inert gases and different pressures, especially for an extended period of time, has been reported previously.19 Effects of inert (Ar and He) and less reactive (N2) gasses are important as they can be used as the backfilled gas during the packaging process. Also, most of the published work discussed about the effect of injected gas without considering the effect of water vapor associated with it. In this paper, we present experimental results conducted using silicon-gated field emitter arrays (Si-GFEA) fabricated using a novel method.22,23 The influence of gases as well as the effect of water vapor associated with the intended gas on the emission characteristics of field emitters was studied by introducing several inert gases and nitrogen gas within a vacuum chamber. The chamber setup and experimental process are explained including the results on emission performance.

The field emitter arrays, built on 150 mm diameter, n-type doped, single crystal, silicon wafers, have array sizes ranging from single emitters to 1000 × 1000 emitter arrays. Figure 1(a) shows the 3D schematic and Fig. 1(b) shows the SEM image of the emitter.22 The field emitter tips have 1 μm spacing (pitch). These arrays consist of self-aligned gated silicon emitters with integrated nanowires of 150 nm diameter and an 8 μm height. Detailed fabrication methods and descriptions can be found elsewhere.22,23 The 1000 × 1000 arrays were chosen for these experiments because they are able to produce current density greater than 100 A/cm2.23 Current–voltage (I–V) characterization measurements were carried out inside a stainless-steel vacuum chamber using a Keysight B2902A SMU. The chamber is equipped with electrical feedthroughs, thermocouple feedthroughs, a three-axis manipulator probe arm, and an Extorr Inc. XT100 residual gas analyzer (RGA). The system includes a UV lamp (RBD Instrument, Model- MiniZ, 350 μW/cm2, 2.75” CF flange mounted) that is used to desorb water vapor from the tips.24 A detailed description of the chamber and the experimental test setup can be found in our previous work.24,25

FIG. 1.

(a) 3D rendering of device structure. For clarity, layers have been omitted in different regions of rendering to show detail. In the front, the bare silicon nanowires [200 nm diameter and 10 μm height] with sharp tips are shown. (b) SEM image of the completed device at 45° tilt. (Ref. 22) [Reprinted from Guerrera and Akinwande, Nanotechnology 27, 295302 (2016). Copyright 2016 IOP Publishing].

FIG. 1.

(a) 3D rendering of device structure. For clarity, layers have been omitted in different regions of rendering to show detail. In the front, the bare silicon nanowires [200 nm diameter and 10 μm height] with sharp tips are shown. (b) SEM image of the completed device at 45° tilt. (Ref. 22) [Reprinted from Guerrera and Akinwande, Nanotechnology 27, 295302 (2016). Copyright 2016 IOP Publishing].

Close modal

I–V sweeps were carried out for different gases and gas pressures. Time taken for each test was ≈10 min. At first, the tip surfaces were cleaned using the UV light,24 and then the backfill gas was injected slowly using a leak valve until the pressure inside the chamber reached the desired value. After achieving the desired pressure, gate voltage sweeps were carried out keeping the collector voltage fixed (200 V). Collector distance was ≈1 mm. Each voltage sweep took ≈2 min. Similar experimental steps were repeated for each gas pressures (5 × 10−6, 5 × 10−5, and 5 × 10−4 Torr) and backfill gas (N2, Ar, and He). From the experiments (Fig. 2), it was observed that for a gate voltage of 40 V, the collector current decrease was the least for N2 [Figs. 2(a) and 2(b)] for each partial pressure, where a drop of 41% was observed for the pressure of 5 × 10−4 Torr; He [Figs. 2(c) and 2(d)] has a decrease of ≈52%, and Ar [Figs. 2(e) and 2(f)] had the greatest decrease (65% drop for pressure of 5 × 10−4 Torr). Figures 2(a) (inset), 2(c) (inset), and 2(e) (inset) show the Fowler–Nordheim (F–N) plots for N2, He, and Ar, respectively, to demonstrate the field emission nature of the device. After the exposure, vacuum was restored by pumping down and the I–V sweep was repeated. It was observed that after pump back down, the collector current was restored to preexposure conditions (≈98%), which suggests that most of tips were not physically damaged. Corresponding F–N plots for N2 [Fig. 2(a) inset], He [Fig. 2(c) inset], and Ar [Fig. 2(d) inset] also became more linear after the pump down and UV exposure, which suggest that degradation was not permanent.

FIG. 2.

(a) Collector current for pregas exposure, N2 gas exposure pressures, and postgas exposure (inset: F–N plot) and (b) gate current for N2 gas exposure, (c) collector current for pregas exposure, He gas exposure pressures, and postgas exposure (inset: F–N plot) and (d) gate current for He gas exposure, (e) collector current for pregas exposure, Ar gas exposure pressures, and postgas exposure (inset: F–N plot), and (f) gate current for Ar gas exposure.

FIG. 2.

(a) Collector current for pregas exposure, N2 gas exposure pressures, and postgas exposure (inset: F–N plot) and (b) gate current for N2 gas exposure, (c) collector current for pregas exposure, He gas exposure pressures, and postgas exposure (inset: F–N plot) and (d) gate current for He gas exposure, (e) collector current for pregas exposure, Ar gas exposure pressures, and postgas exposure (inset: F–N plot), and (f) gate current for Ar gas exposure.

Close modal

A degradation in emission current and increase in gate current can be observed after the N2 exposure experiment and at the beginning of the He exposure experiment (at high vacuum condition, before the gas injection). This degradation is permanent and assumed to be the result of tip damage due to arcing. However, this phenomenon is not in the scope of this study. To keep the consistency, we used the same device throughout this study.

A subsequent UV exposure restored the pre-exposure collector current completely. It was hypothesized that the exposed gases or water vapor were adsorbed by emitter tips during gas exposure, which increased the work function. Restoring the high vacuum and subsequent UV exposure desorbed the gases and water vapor and recovered the Si work function. This recovery strongly suggests that no physical damage occurred to the tips such as ion bombardment26 or tip runaway.27 However, the RGA data also showed that a large percentage of the gas introduced into chamber was H2O, which is known to increase the tip work function.28 This phenomenon can be seen in Fig. 3. In Fig. 3(a), the partial pressure of N2 and water vapor is plotted for different vacuum levels, where Fig. 3(b) shows the collector and gate current with respect to different vacuum levels. Similarly, Fig. 3(c) shows the partial pressure of He and water vapor. Figure 3(d) shows the collector and gate current with respect to different vacuum levels for injected He. Figure 3(e) shows the partial pressure of industrial grade Ar (Ar purity is ≈99.98%) and water vapor, and Fig. 3(f) shows the collector and gate current with respect to different vacuum levels for Ar injection. Figure 3(g) shows the partial pressure of high purity Ar (Ar purity is >99.999) and water vapor. Figure 3(h) shows the collector and gate current with respect to different vacuum levels for injected Ar (high purity). From Fig. 3, it can clearly be seen that the partial pressure of the water vapor, for all the case, except the high purity Ar, was ≈10% of the injected gas, which has a large known effect on the work function. Change in work function for all the cases was extracted using the Fowler–Nordheim (F–N)6,9 equation. The F–N equation is given below:
(1)
Here, VG is the applied gate voltage in V, aFN and bFN are F–N coefficients and are defined as follows:
(2)
(3)
where φ is the emitter work function (eV) and β is the field enhancement factor. Here, the work function of the UV cleaned tip is assumed to be 4.05 eV for Si. The values of ln(aFN) and bFN were extracted from the slope and intercept of F–N plots for all the gate sweeps, and the work functions for each case were calculated using Eq. (3). Here, the field enhancement factor (β) is assumed to be constant, as β is the geometry-dependent parameter, and no damage to tip geometry was observed. Such damage would have degraded the emission current permanently even after the pump down and subsequent UV cleaning. Figure 4 shows the extracted work function for each case. From Fig. 4, it can clearly be seen that the Ar has the worst effect on the work function while N2 has the least effect. However, as it was observed in the RGA data that all the gases (except high purity Ar) have a large portion of water vapor (Fig. 3), it was necessary to determine whether the water vapor in the gas caused the effect on the work function of the tips. Figure 5 compares the water vapor partial pressure for different injected gases, which further established that all of the gases have large portion of water vapor.
FIG. 3.

(a) Partial pressure of N2 and water vapor. (b) Collector and gate current for different total pressure for N2 injection. (c) Partial pressure of He and water vapor. (d) Collector and gate current for different total pressure for He injection. (e) Partial pressure of Ar and water vapor. (f) Collector and gate current for different total pressure for Ar injection. (g) Partial pressure of Ar (high purity) and water vapor. (h) Collector and gate current for different total pressure for Ar (high purity) injection.

FIG. 3.

(a) Partial pressure of N2 and water vapor. (b) Collector and gate current for different total pressure for N2 injection. (c) Partial pressure of He and water vapor. (d) Collector and gate current for different total pressure for He injection. (e) Partial pressure of Ar and water vapor. (f) Collector and gate current for different total pressure for Ar injection. (g) Partial pressure of Ar (high purity) and water vapor. (h) Collector and gate current for different total pressure for Ar (high purity) injection.

Close modal
FIG. 4.

Normalized work function as a function of total gas pressure. Work function is normalized to clean state work function of silicon tips.

FIG. 4.

Normalized work function as a function of total gas pressure. Work function is normalized to clean state work function of silicon tips.

Close modal
FIG. 5.

Water vapor partial pressure associated with different injected gasses.

FIG. 5.

Water vapor partial pressure associated with different injected gasses.

Close modal

Further study was carried out using both industrial grade (I.G.) and high purity (H.P.) Ar (≈99.999%) to find out the effect of the Ar gas versus the water vapor on the collector current and can be seen in Figs. 3(g) and 3(h). At first, the surface was cleaned using UV light, and then the industrial grade Ar was injected into the chamber until the chamber total pressure reached ≈5 × 10−6 Torr. This pressure was kept for 30 min by adjusting the leak valve. The I–V sweeps were then carried out every 5 min. The gate voltage was swept to 40 V, and the collector voltage was fixed at 200 V. After 30 min, the collector current degraded ≈60%. For the case of high purity Ar also, similar steps were repeated. However, for this case, it took ≈120 min of gas exposure for the current to degrade ≈60%, and the gate sweep was carried out every 10 min. The experimental data are plotted in Fig. 6 in terms of the normalized collector current versus the gas exposure in Langmuir. One Langmuir corresponds to an exposure of 10−6 Torr during 1 s. The collector currents were normalized to the pregas injection current. Figure 6(a) shows the total volume of I.G. Ar and H.P. Ar injected during the experiment, where Fig. 6(b) shows the total volume of water vapor that was included in the injected Ar gases. The total volume of Ar is much higher than the total volume of water vapor present in the gas exposure effects. From Fig. 6, it can clearly be observed that the water vapor present in the gas is the primary cause of degradation as there is clear correlation between H2O exposure and current decrease.

FIG. 6.

(a) Normalized collector current vs. exposure for Ar. (b) Normalized collector current vs. exposure for water vapor. I.G. denotes industrial grade and H.P. denotes high purity.

FIG. 6.

(a) Normalized collector current vs. exposure for Ar. (b) Normalized collector current vs. exposure for water vapor. I.G. denotes industrial grade and H.P. denotes high purity.

Close modal

I–V characterization of Si-GFEA with 1000 × 1000 tip arrays was carried out after UV light exposure and then after exposure to gases (N2, Ar, and He) at different vacuum levels. It was found that the water vapor present in these gases was the major cause of the work function increase. At first, it was observed that the collector current was least effected by N2 and mostly affected by the Ar gas exposure. The degradation of collector current at 5 × 10−4 Torr pressure for Ar was ≈65% where for the N2, at the same level of pressure, the degradation was ≈41%. It was assumed that the gases adsorbed into the tips changed the work function, which, in turn, affected the collector current. Upon pump down, the adsorbed gases were removed from the tips, which restored the pre-exposed collector current. Further experiments carried out with high purity Ar (≈99.999%) revealed that the water vapor present in the gas is the primary reason behind collector current degradation. Further experiments with the water vapor trap is required to find out the effect of gases itself.

Material support for this work was provided by the Air Force Office of Scientific Research under Grant No. FA9550-18-1-0436. The authors would also like to thank support from undergraduate students Brady Sainz, Gerardo Herrera, and John McClarin.

The authors have no conflicts to disclose.

Ranajoy Bhattacharya: Data curation (lead); Formal analysis (lead); Investigation (lead); Methodology (lead); Writing – original draft (lead). Mason Cannon: Investigation (supporting). Girish Rughoobur: Resources (equal). Nedeljko Karaulac: Resources (equal). Winston Chern: Resources (supporting). Reza Farsad Asadi: Data curation (equal); Validation (equal). Zheng Tao: Formal analysis (equal); Validation (equal). Bruce E. Gnade: Funding acquisition (equal); Supervision (equal); Validation (equal); Writing – review & editing (equal). Akintunde Ibitayo Akinwande: Funding acquisition (lead); Project administration (equal); Resources (equal); Supervision (equal). Jim Browning: Conceptualization (equal); Funding acquisition (equal); Supervision (equal); Validation (equal); Writing – review & editing (equal).

The data that support the findings of this study are available from the corresponding author upon reasonable request.

1.
J.-W.
Han
,
D.-I.
Moon
, and
M.
Meyyappan
,
Nano Lett.
17
,
2146
(
2017
).
2.
J.-W.
Han
,
J.
Sub Oh
, and
M.
Meyyappan
,
Appl. Phys. Lett.
100
,
213505
(
2012
).
3.
J.-W.
Han
,
M.-L.
Seol
,
D.-I.
Moon
,
G.
Hunter
, and
M.
Meyyappan
,
Nat. Electron.
2
,
405
(
2019
).
4.
S. A.
Guerrera
,
L. F.
Velasquez-Garcia
, and
A. I.
Akinwande
,
IEEE Trans. Electron Devices
59
,
2524
(
2012
).
5.
L. F.
Velasquez-Garcia
,
S. A.
Guerrera
,
Y.
Niu
, and
A. I.
Akinwande
,
IEEE Trans. Electron Devices
58
,
1783
(
2011
).
6.
R. H.
Fowler
and
L.
Nordheim
,
Proc. R. Soc. A
119
,
173
(
1928
).
7.
K. L.
Jensen
,
E. G.
Zaidman
,
M. A.
Kodis
,
B.
Goplen
, and
D. N.
Smithe
,
J. Vac. Sci. Technol. B
14
,
1942
(
1996
).
8.
E. L.
Murphy
and
R.
Good
, Jr.
,
Phys. Rev.
102
,
1464
(
1956
).
9.
R. G.
Forbes
,
Mod. Dev. Vac. Electron Sources
135
,
387
(
2020
).
10.
W.
Kang
,
J.
Davidson
,
K.
Subramanian
,
B.
Choi
, and
K.
Galloway
,
IEEE Trans. Nucl. Sci.
54
,
1061
(
2007
).
11.
W.
Kang
,
J.
Davidson
,
Y.
Wong
, and
K.
Holmes
,
Diamond Relat. Mater.
13
,
975
(
2004
).
12.
H. D.
Nguyen
, J. S. Kang, M. Li, and Y. Hu,
Nanoscale
11
,
3129
(
2019
).
13.
J.
Browning
,
N. E.
McGruer
,
W.
Bintz
, and
M.
Gilmore
,
IEEE Electron Device Lett.
13
,
167
(
1992
).
14.
J.
Browning
,
N.
McGruer
,
S.
Meassick
,
C.
Chan
,
W. J.
Bintz
, and
M.
Gilmore
,
IEEE Trans. Plasma Sci.
20
,
499
(
1992
).
15.
M.
Gilmore
,
N.
McGruer
,
J.
Browning
, and
W.
Bintz
,
Rev. Sci. Instrum.
64
,
581
(
1993
).
16.
F.
Allen
,
J.
Eisinger
,
H.
Hagstrum
, and
J.
Law
,
J. Appl. Phys.
30
,
1563
(
1959
).
17.
D.
Temple
,
W.
Palmer
,
L.
Yadon
,
J.
Mancusi
,
D.
Vellenga
, and
G.
McGuire
,
J. Vac. Sci. Technol. A
16
,
1980
(
1998
).
18.
B. R.
Chalamala
,
R. M.
Wallace
, and
B. E.
Gnade
,
J. Vac. Sci. Technol. B
16
,
2859
(
1998
).
19.
S.
Itoh
,
T.
Niiyama
, and
M.
Yokoyama
,
J. Vac. Sci. Technol. B
11
,
647
(
1993
).
20.
S. H.
Jo
,
B. G.
Park
, and
J. D.
Lee
,
Appl. Phys. Lett.
68
,
2234
(
1996
).
21.
S.
Edler
et al,
J. Appl. Phys.
122
,
124503
(
2017
).
22.
S.
Guerrera
and
A. I.
Akinwande
,
Nanotechnology
27
,
295302
(
2016
).
23.
S. A.
Guerrera
and
A. I.
Akinwande
,
IEEE Electron Device Lett.
37
,
96
(
2016
).
24.
R.
Bhattacharya
,
N.
Karaulac
,
G.
Rughoobur
,
W.
Chern
,
A. I.
Akinwande
, and
J.
Browning
,
J. Vac. Sci. Technol. B
39
,
033201
(
2021
).
25.
R.
Bhattacharya
,
N.
Karaulac
,
W.
Chern
,
A. I.
Akinwande
, and
J.
Browning
,
J. Vac. Sci. Technol. B
39
, 023201 (
2021
).
26.
I. W.
Rangelow
and
St.
Biehl
,
J. Vac. Sci. Technol. B
19
,
916
(
2001
).
27.
H. F.
Gray
and
G.
Campisi
,
MRS Online Proc. Libr.
76
, 25 (
1986
).
28.
Y.
Kayaba
,
K.
Kohmura
, and
T.
Kikkawa
,
Jpn. J. Appl. Phys.
47
,
8364
(
2008
).

Ranajoy Hattacharya received his Ph.D. degree from the Department of Electrical and Computer Engineering, Seoul National University, Seoul, South Korea in 2018. At present, he is working as a research scientist at Boise State University.

Girish Rughoobur received the M.Eng. degree in Electrical and Electronic Engineering from the University College London (UCL), UK, in 2012, and the Ph.D. degree in engineering from the University of Cambridge, UK, in 2017.

Nedeljko Karaulac received the B.S. degree in Electrical Engineering with the Georgia Institute of Technology (Georgia Tech), Atlanta, GA, USA, in 2015 and the M.S. degree in electrical engineering and computer science (EECS) from the Massachusetts Institute of Technology, Cambridge, MA, USA, in 2019. He is currently pursuing the Ph.D. degree in electrical engineering and computer science (EECS) from the Massachusetts Institute of Technology, Cambridge, MA, USA.

Winston Chern received the B.S. degree in Materials Science and Engineering from the University of Illinois at Urbana-Champaign, Champaign, IL, USA, in 2010, and the M.S. degree in Electrical Engineering and Computer Science (EECS) from the Massachusetts Institute of Technology, Cambridge, MA, USA. He received his Ph.D. degree in Electrical Engineering and Computer Science (EECS) from the Massachusetts Institute of Technology, Cambridge, MA, USA, in 2017.

Reza Farsad Asadi is currently pursuing his Ph.D. degree in Electrical and Computer Engineering from the Southern Methodist University, TX, USA.