SIMS Quantification of Matrix and Impurity Species in Al x Ga 1-x N
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1 SIMS Quantification of Matri and Impurity Species in Al Ga 1- N Abstract C. J. Gu a, F. A. Stevie a*, C. J. Hitzman b, Y. N. Saripalli c, M. Johnson c, D. P. Griffis a a Analytical Instrumentation Facility, North Carolina State University, Bo 7531, Raleigh, NC b Full Wafer Analysis, 2326 Walsh Avenue, Bldg H Santa Clara, CA c Material Science and Engineering, North Carolina State University Bo 7907, Raleigh, NC * fred_stevie@ncsu.edu The quantification in Al Ga 1- N with different AlN mole fraction () is challenging because of matri effects and charging effects. For quantitative characterization of both matri and impurity elements in Al Ga 1- N, a novel charge neutralization method was employed and calibration curves were created using an O 2 + primary beam with positive secondary ion detection and a Cs + primary beam with negative and MCs + secondary ion detection. Over the range of 0<<0.58, the matri ion intensity ratios of Al + /Ga + and AlCs + /GaCs + appear linear with the mole fraction ratio /(1-), and the ratio of AlN - /GaN - is linear with AlN mole fraction (). The sputter rate decreases linearly with AlN mole fraction, while the relative sensitivity factors (RSF s) of impurities have an eponential relationship with AlN mole fraction. These calibration curves allow the quantification of both matri and impurity species in AlGaN with varying AlN mole fraction. The technique can be employed for impurity control, composition and growth rate determination, as well as structural analysis of the finished optoelectronic and electronic devices. Keywords: SIMS; Aluminum Gallium Nitride (AlGaN); Quantification; Calibration curve 1 Introduction New applications in optoelectronic devices and high power electronic devices continue to be developed using Al Ga 1- N. Due to the material's wide band gap range which etends from 3.4 ev to 6.2 ev depending on AlN mole fraction (), the Al Ga 1- N's are very attractive materials for applications in ultraviolet (UV) laser diodes (LD s), light emitting diodes (LED s) and photo detectors.[1] The large band gap, large electric field breakdown and good thermal/chemical stability makes Al Ga 1- N semiconductors the materials of choice for high power, high temperature electronic devices.[2] The properties of Al Ga 1- N materials are strongly influenced by alloy concentration and impurities such as Si, Mg, O, C, H, etc. Thus quantification of matri and impurity species in Al Ga 1- N is essential for compositional analysis, dopant control, and impurity control. Dynamic SIMS is commonly used for the quantification of Al Ga 1- N due to its capability of providing indepth profiles with high sensitivity and good depth resolution. However, quantification in Al Ga 1- N can be challenging because of matri and charging effects. The secondary ion yields of matri and impurity species vary in Al Ga 1- N with different AlN mole fraction. Sample charging which increases with AlN mole fraction must also be dealt with, particularly in the case of undoped Al Ga 1- N alloys having >0.4.[3] In this work, a SIMS quantification method is developed for the Al Ga 1- N system over the range of = 0 to 1. 2 Eperiment A set of Al Ga 1- N films with ranging from 0 to 0.58 were grown on graded Al Ga 1- N buffer layers on SiC or sapphire substrates using metal organic chemical vapor deposition (MOCVD). The AlN mole fraction of the Al Ga 1- N films was determined using Low Energy X- 1
2 Ray Emission Spectroscopy (LEXES).[4] These films were implanted with 24 Mg at 120 kev to a dose of 2E14 at/cm 2 and 29 Si at 150 kev to a dose of 5E14 at/cm 2. In order to etend the sample set to include an AlN mole fraction close to but not equal to 1, an AlN sample was implanted with 150 kev 1E17 at/cm 2 and 1E16 at/cm 2 of Ga resulting in AlN mole fraction of 0.79 and 0.98 respectively in the Ga peak position.[5] AlN sample was used for AlN mole fraction of 1. Secondary ion mass spectrometry measurements were performed using a CAMECA IMS- 6F. Depth profiles were acquired using 5.5 kev (impact energy) O 2 + ions at an angle of incidence of 41.3 monitoring positive secondary ions, using 14.5 kev (impact energy) Cs + ions at an angle of incidence of 24.8 monitoring negative secondary ions, and using 5.5 kev impact energy Cs + ions at an angle of incidence of 41.3 monitoring positive MCs + and MCs 2 + cluster ions. Low energy analyses using O 2 + (positive secondary ion detected) and Cs + beams (negative and MCs + secondary ions detected) were also performed, but only results from high energy analyses are presented in this paper. The primary beam was rastered over 180µm 180µm and secondary ions were collected from an optically gated area of 60µm in diameter. The depths of sputtered craters were measured using a KLA-Tencor P-20 profilometer. Electron beam charge neutralization was performed using the Normal Incidence Electron Gun (NEG) available on the CAMECA IMS-6F. For positive secondary ion detection, the NEG electron beam energy was chosen such that the electron beam could be positioned adjacent to but not overlapping the rastered area.[6] To achieve this condition, an NEG accelerating voltage of -2 kv was used with the +4.5 kv sample potential. For negative secondary ion detection, the NEG accelerating voltage was chosen to match the sample potential so that electrons were attracted to the sample only if the sample charged. The NEG was adjusted using the procedure described previously.[7] 3 Results and Discussion 3.1 Sputter Rate Sputter rates normalized to primary ion intensity obtained for the SIMS analytical conditions described above for the Al Ga 1- N samples are presented in Figure 1. The sputter rates decrease with increasing AlN mole fraction (), which is similar to the result previously reported for Al Ga 1- As.[8] sputter rate (um 3 /(s.na)) Cs 5.5 kev Cs 14.5 kev O2 5.5 kev in Al Ga 1-N Fig. 1. Sputter rate versus AlN mole fraction. Low mole fraction samples are grown on SiC substrates and the higher mole fraction samples are grown on sapphire substrates Two distinct linear slopes are seen in the curves. The change in slope occurs between the two sample sets used in this study. Samples with 0.21 were grown on SiC substrates and samples with 0.23 were grown on sapphire (Al 2 O 3 ) substrates. It is speculated that differing amounts of strain or differing densities of these samples contribute to the change in slope. Work is underway to determine the cause of this change in slope. From Figure 1, it can be seen that Cs + sputters faster 2
3 than O 2 + at 5.5 kev impact energy. Although the increase in the Cs + sputter rate for the 5.5keV (10 kv primary ion/4.5 kv sample bias) versus the 14.5keV (10 kv primary ion/-4.5 kv sample bias) impact energy may appear counter intuitive, the difference in sputter rates can be attributed to the 41.3 (with respect to sample normal) impact angle of the 5.5 kev Cs + versus the 24.8 impact angle of the 14.5keV Cs +.[9] 3.2 Matri Ion Intensity Ratio For Al Ga 1- N with 0<<0.58 analyzed using 5.5 kev O 2 +, the ratio of Al + /Ga + appears to be linearly proportional (slope of 2.34) to their mole fraction ratio (i.e. /(1-)) as shown in figure 2a. The linear correlation of matri intensity with mole fraction allows the use of a single standard for determination of the AlN mole fraction in an unknown sample simplifying matri element quantification. For >0.58, the Al + /Ga + intensity ratio increases faster than the ratio of the mole fraction. However, if plotted inversely, i.e. Ga + /Al + as a function of (1-)/, then the correlation appears linear for 0<(1-)<0.87, or 0.23<<1, as shown in figure 2b. 4.0 (a) Al + /Ga + intensity ratio vs. /(1-) 2.5 (b) Ga + /Al + intensity ratio vs. (1-)/ Al + /Ga y = =0.58 Ga + /Al y = = /(1-) (1-)/ Fig. 2. Matri ion intensity ratio versus mole fraction ratio in Al Ga 1- N using O 2 + analysis Similarly, when Cs + primary ions are used and positive MCs + clusters are detected, the matri ion intensity ratio of AlCs + /GaCs + appears linear with AlN and GaN mole fraction ratio (/(1-)) in the range of 0<<0.58, and the reverse plot (GaCs + /AlCs + vs. (1-)/) is linear for 1<(1-)<0.98 (figure 3). 1.2 (a) AlCs + /GaCs + vs. /(1-) 80 (b) GaCs + /AlCs + vs (1-)/ AlCs + /GaCs y = =0.58 GaCs+/AlCs y = = /(1-) (1-)/ Fig. 3. Matri ion intensity ratio versus mole fraction ratio in Al Ga 1- N using MCs + technique In contrast, the matri ion intensity ratio of AlN - /GaN - under Cs + bombardment is not linear with AlN and GaN mole fraction ratio (/(1-)) but does appear linear with AlN mole fraction (), 3
4 as shown in figure 4. The reverse plot of GaN - /AlN - versus (1-) is also linear in the range of 0<(1- )<0.61 (not shown). Note that the ion intensity ratio of AlN + /GaN + under O 2 + ion beam is also linear with instead of /(1-) within 0<<0.58. Work is under way to understand the cause of this difference in behavior for AlN ± /GaN ±. 8.0 AlN - /GaN y = = Impurity RSF s The relative sensitivity factors for Mg and Si were calculated by normalizing to selected Ga matri ions. The secondary ions monitored for different analysis conditions are listed in table 1. Table 1. List of impurity secondary ions and the matri ion to normalize Primary Beam Secondary Polarity Impurity Ions Matri Ion O Fig. 4. Matri ion intensity ratio versus AlN mole fraction () in Al Ga 1- N using Cs + analysis with negative secondary ion detection positive Mg + and Si + Ga + Cs + negative MgN - and Si - GaN - Cs + positive MgCs + GaCs + The dependence of the respective RSF s on AlN mole fraction obtained using the SIMS analytical conditions described above is presented in Figure 5. All RSF's appear to have an eponential correlation with AlN mole fraction. The RSF data for Mg + and Si - are in agreement with results previously reported for AlN mole fraction of 0<<0.21.[10, 11] Mg RSF (at./cm 3 ) E+24 E+23 E+22 MgN- RSF MgCs+ RSF Mg+ RSF Si RSF (at./cm 3 ) E+25 E+24 E+23 E+22 E+21 Si+ RSF Si- RSF E E Fig. 5. RSF s of Mg (left) and Si (right) under O 2 + and Cs + beam versus AlN mole fraction in Al Ga 1- N 4
5 The eponential correlation of RSF s with the AlN mole fraction is consistent with the eponential correlation of ionization probability with the local surface work function.[12] When AlN mole fraction increases, the sputter rate is reduced. The resulting increase in the surface concentration of primary species alters the local surface work function and the ion yields.[13] 4 Summary Using the sputtering conditions presented in this study, the sputter rate decreases with AlN mole fraction () in Al Ga 1- N which is similar to the trend previously observed in Al Ga 1- As. Although there is a linear correlation of sputter rate with, the slope of the correlation differs for the two sample sets analyzed. It is speculated that the change in sputter rates for the two sample sets is due to differences in strain in the films grown on different substrates. In the range of 0<<0.58, the matri ion intensity ratios of Al + /Ga + obtained using 5.5keV O + 2 and AlCs + /GaCs + obtained using 5.5keV Cs + appear to increase linearly with matri mole fraction ratio (/(1-)). However, the ratios of AlN - /GaN - and AlN + /GaN + increase linearly with AlN mole fraction instead of mole fraction ratio. If plotted inversely, i.e. Ga + /Al + or GaCs + /AlCs + versus (1-)/, or GaN - /AlN - versus (1-), the linear correlation appears to increase to 0<(1-)<0.61, or 0.39<<1. The overlap of these apparent linear ranges allows quantification of matri over the entire range of Al Ga 1- N's i.e. from 0<<1 under these analytical conditions. The RSF's for Si and Mg normalized to the appropriate Ga matri signal (see Table 1) decrease eponentially with in the range of 0<<0.58. This is consistent with the eponential correlation of ion yield with the surface work function. With the linear and eponential relationships shown in this work, the matri elements in Al Ga 1- N can be quantified in the range of 0<<1, and the impurity species can be quantified over 0<<0.58. The material composition, growth rate, and structure of finished devices can be adequately determined. References [1] J.C. Carrano, T. Li, D.L. Brown, P.A. Grudowski, C.J. Eiting, R.D. Dupuis, J.C. Campbell, Electronics Letters 34 (1998) [2] K. Zhu, M.L. Nakarmi, K.H. Kim, Appl. Phys. Lett. 8 (2004) [3] S.N. Mohammad, A.A. Salvador, H. Morkoc, Proceedings of the IEEE 83 (1995) [4] C. Hombourger, R. Staub, M. Schuhmacher, F. Desse, E. de Chambost, C. Hitzman, Applied Surface Science 203 (2003) [5] C.J. Gu, F. Stevie, Y.N. Saripalli, M. Johnson, D.P. Griffis, (to be published 2005 MRS Proceedings). [6] A.L. Pivovarov, F.A. Stevie, D.P. Griffis, Applied Surface Science (2004) [7] A. Pivovarov, C. Gu, F. Stevie, D. Griffis, Applied Surface Science (2004) [8] M. Meuris, W. Vandervorst, G. Borghs, H.E. Maes, Secondary Ion Mass Spectrometry SIMS VI, edited by A. Benninghoven, A.M. Huber, and H.W. Werner, John Wiley & Sons (1988) [9] K. Wittmaack, in: D. Briggs, M.P. Seah (Eds.), Practical Surface Analysis, 1992, p [10] D.P. Griffis, R. Loesing, D.A. Ricks, M.D. Bremser, R.F. Davis, Secondary ion Mass Spectrometry SIMS XI, edited by G. Gillen, R. Lareau, J. Bennett and F. Stevie, John Wiley & Sons (1997) [11] D.L. Lefforge, Y.L. Chang, M. Ludowise, E.L. Allen, Mat. Res. Soc. Symp. Proc. 510 (1998) [12] M.L. Yu, J. Vac. Sci. Technol. A 1 (1983) [13] V.R. Deline, C.A. Evans, P. Williams, Applied Physics Letters 33 (1978)
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