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A i L D ii d Ch i i fM Of Atomic Layer Deposition and Characterization of MgO from Atomic Layer Deposition and Characterization of MgO from Magnesium Bis(Di secbutylacetamidinate) and Water Magnesium Bis(Di-secbutylacetamidinate) and Water Magnesium Bis(Di secbutylacetamidinate) and Water P de Rouffignac a N Sullivan a D Beaulieu a P . de Rouffignac , N. Sullivan , D. Beaulieu J -S Park b A Hock c RG Gordon c J. S. Park , A. Hock , R. G. Gordon a A di I S db MA USA di a Arradiance Inc. – Sudbury, MA USA www.arradiance.com b Samsung Seoul Korea b Samsung – Seoul, Korea c Harvard University – Cambridge MA Harvard University Cambridge, MA INTRODUCTION Fil P ti INTRODUCTION Film Properties INTRODUCTION Film Properties M i id (M O) i d l hi hdi l i il8 10 ih id MO d it d b th Si d l b bt t Th iti f th Magnesium oxide (MgO) is a moderately high dielectric constant material: 8-10, with a wide MgO was deposited on both Si and glassy carbon substrates. The composition of the band gap: 7 8 eV Potential applications include: gate insulator buffer layer for superconductors films was measured using Rutherford Backscattering spectroscopy. A typical RBS plot is band gap: 7.8 eV . Potential applications include: gate insulator, buffer layer for superconductors df l ti dhi h d l t i i fil f l di l M Oh b films was measured using Rutherford Backscattering spectroscopy. A typical RBS plot is shown as well as a graph showing a decreasing O:Mg ratio with cycle number and ferroelectrics, and high secondary electron emission film for plasma displays. MgO has been shown as well as a graph showing a decreasing O:Mg ratio with cycle number . deposited via Atomic Layer Deposition using a variety of precursors 1 , however the full electrical Conformality was determined using fused silica capillary tubes and measuring the characterization of the material has yet to be published This work introduces the ALD of MgO penetration of the film using an optical microscope characterization of the material has yet to be published. This work introduces the ALD of MgO f M i Bi (Di b l idi ) d I ddi i h k penetration of the film using an optical microscope from Magnesium Bis(Di-secbutylacetamidinate) and water. In addition to the known 60 22 applications ALD of MgO is an important component of Arradiance high gain microchannel 60 2.2 Pure Mg(OH)2 applications, ALD of MgO is an important component of Arradiance high gain microchannel lt lifi d h lt t h l 50 2 2, Å 2 plate amplifiers and channeltron technology. 40 1.8 OH) 2 Ratio 40 16 Mg(O Mg R 30 14 1.6 s of M to M Precursor Synthesis and Properties 20 1.4 ness gen Precursor Synthesis and Properties 20 1.2 hickn Oxyg 10 1 Th O Pure MgO Th i i dil th i db th ti f i ll il bl dib t l 0 08 PureMgO The magnesium precursor is readily synthesized by the reaction of commercially available dibutyl 0 0.8 50 100 150 200 250 300 350 magnesium with the free amidine. The product is a colorless liquid which may be distilled at 80 Cycle Number magnesium with the free amidine. The product is a colorless liquid which may be distilled at 80 o C and 14mTorr The amidinate and precursor are a racemic and diastereomeric mixture with one Increasing c cle n mber sho s decreasing O:Mg Ass ming e cess O is o C and 14mTorr . The amidinate and precursor are a racemic and diastereomeric mixture with one Increasing cycle number shows decreasing O:Mg. Assuming excess O is in the form of Mg(OH) the thickness of the h dro ide la er seems to dominant diastereomer visible in the 1H NMR. in the form of Mg(OH) 2 , the thickness of the hydroxide layer seems to stabili e at 4nm of the total MgO film thickness stabilize at ~4nm of the total MgO film thickness. s-Bu s-Bu CH N N CH3 H CH3 RBS of a 300cycle (24nm) MgO film on carbon C M N H C N C C 0.5 Mg(n-Bu) 2 CH3 H2 C CH3 RBS of a 300cycle (24nm) MgO film on carbon. C and N <1%; composition is MgO 13 Al 01 Mg C N H3C C C C CH2 Glass capillary tube can be used to gauge the conformality of an ALD and N <1%; composition is MgO 1.3 Al 0.1 Film density is 3 06 g/cm 3 (similar to that reported CH3 N N B N N C C - 2 C 4 H 10 H3C CH2 Glass capillary tube can be used to gauge the conformality of an ALD process In this case the film penetrated 620μm into a 14μm diameter Film density is 3.06 g/cm (similar to that reported by Burton et al of 3 07) 1 s-Bu N N 3 H H H process. In this case, the film penetrated 620μm into a 14μm diameter tube yielding an AR of 45 by Burton et.al. of 3.07) s-Bu H H H tube, yielding an AR of 45. Electrical Measurements Racemic and diastereomeric mixture Electrical Measurements Racemic and diastereomeric mixture s-Bu = CH(CH 3 )(CH 2 CH 3 ) El i l d i NiC (4 5 10 3 2 ) IV i K i hl 2400 d Mi i l P b 3 2 3 Racemic and diastereomeric mixture Electrical measurements made using NiCr contacts (4.5 x 10 -3 cm 2 ). IV measurements using a Keithley 2400 and Micromanipulator Probe t ti CV t i HP 4275 LCR t Racemic and diastereomeric mixture station, CV measurements using HP 4275a LCR meter Electric Field (MV/cm) 1.0E+00 Electric Field (MV/cm) 1 0E 01 1.50 2.50 3.50 4.50 5.50 s-Bu = CH(CH3)(CH2CH3) 100nm NiCr 1.0E-01 100nm NiCr 1.0E-02 24nm MgO 1.0E-03 15 SiO 24nm MgO 1 0E 04 m2) Si 1.5nm SiO 2 1.0E-04 s/cm s-Bu = CH(CH3)(CH2CH3) n-type Si 1.0E-05 mps B 1.0E-06 J (am s-Bu = CH(CH3)(CH2CH3) s-Bu = CH(CH3)(CH2CH3) Contact evaporated from NiCr wire (80:20) yields an 1 0E-07 J Minor ohmic contact with good adhesion. Si back contact. 5% Residue 10 08 1.0E 07 Minor isomer 1.0E-08 1.0E-09 MgO shows low leakage and a rel. high breakdown field of ~5MV/cm. Th i ti l i f th d M( sec B tAMD) Th 1 H NMR t i di t th di till d t ilif f Thermogravimetric analysis of the crude Mg( sec ButAMD). T f 10 K i 1 i N fl 1 The 1 H NMR spectrum indicates the distilled material is free of i i ii d l h h h i Electrical measurements of MgO thin films 0.35 Temperature ramp rate of 10 K min í1 in an N 2 flow at 1 atm. S l i i 0 GA h l id f h any organic impurities and also shows that the precursor is a i fi d di h diff Electrical measurements of MgO thin films show a dielectric constant similar to that of 0.30 m2 Sample size is 50mg. TGA shows very low residue for the mixture of isomers and diastereomers. The different show a dielectric constant similar to that of Al O ll l l k t 0 25 /cm crude product and <1% residue for the precursor after conformations should show similar surface reactivity. Al 2 O 3 , as well as, low leakage current d ii h l l k d ii 0 20 0.25 μF/ distillation. densities. The low leakage current densities 0.20 ce, are consistent with a material with a large ALD Growth Characteristics 0.15 tan band gap (7.8 eV). CV measurements show ALD Growth Characteristics 0.10 paci As-deposited 250C band gap (7.8 eV). CV measurements show well defined behavior and both V and 0 05 0.10 Cap As deposited 250C 400C 3hr Anneal well defined behavior and both V FB and h t i l t th t d id l th 0.05 C 400C 3hr Anneal hysteresis are closer to the accepted ideal than di l fil i 0.00 • All film depositions performed in an Arradiance GEM-D2 ALD system corresponding Al 2 O 3 films on Si. Future -3.00 -2.00 -1.00 0.00 1.00 2.00 3.00 • Films grown in a temperature range of 225 275 °C work will examine the electrical behavior of Gate Voltage (V) NiCr/24nmMgO/SiO2/Si • Films grown in a temperature range of 225 – 275 C M i Bi (Di b l idi ) di ultra thin (<10nm) MgO films within MIM Dielectric constant pre-anneal is 9 8 including 16Å SiO 2 (EOT = • Magnesium Bis(Di-secbutylacetamidinate) was used in a temperature ultra thin ( 10nm) MgO films within MIM and MIS devices Dielectric constant pre anneal is 9.8 including 16Å SiO 2 (EOT 11nm) and decreases to 5 5 after anneal V FB shifts from -0 7V range of 105-118 °C and was directly dosed from a 150cc precursor and MIS devices. 11nm) and decreases to 5.5 after anneal. V FB shifts from 0.7V to +0 15V Hysteresis improves from 200mV to 20mV range of 105 118 C and was directly dosed from a 150cc precursor d li b ttl to +0.15V. Hysteresis improves from 200mV to 20mV. delivery bottle Application of MgO Microchannel Plate Amplifiers • H 2 O was used as the oxidant at room temperature and was directly dosed Application of MgO – Microchannel Plate Amplifiers 2 to process chamber 8 000 100000 to process chamber 6 920 8,000 100000 M 6,920 7,000 Mgx Alx 6,000 s 10000 Alx Uncoated Bias Nominal Dose Exposure 5,000 Volts B n Precursor Nominal Precursor Temp Dose Time Exposure Time Purge Time 4,000 00 Vo 1000 Gain Precursor Temp Time Time 3 000 at 70 G H O 28 C 20ms 0 5s 70s 3,000 Gain a 100 H 2 O 28 C 20ms 0.5s 70s 1 130 2,000 G 100 1,130 1,000 Mg( sec ButAMD) 109 C 1s (x2) 1.5s 30s 134 1,000 10 0 Uncoated Alx Mgx 500 600 700 800 900 1000 Bi V Uncoated Alx Mgx Bias, V Microchannel plate amplifiers are electron multipliers that can directly detect charged particles X Rays and UV Microchannel plate amplifiers are electron multipliers that can directly detect charged particles, X-Rays, and UV. Wh ld ith ht th d it b dt dt t i ibl li ht di tl iti l t f When coupled with a photocathode it can be used to detect visible light and is currently a critical component of ih ii d i Th l d i l i i i d i 450 night vision devices. They are also used extensively in mass spectrometers, imaging and spectroscopy in space, 1.00 y = 0.789x - 0.7235 400 and ion and electron microscopy. MCP treatment with high secondary electron emission film leads to a substantial, 0.95 y 0.789x 0.7235 R² = 0.9975 400 8-50X, gain increase over commercial lead glass MCPs. These devices exhibited extended lifetime and required a 0 90 0.95 le 350 , Å reduced scrubbing dose for preconditioning to stabilize gain. This treatment can be used to revive aged MCPs. 0 85 0.90 cyc 300 ess, 0.85 Å/c Conclusion 250 kne 0.80 e ,Å Conclusion 250 hick 0.75 Rate 200 Th 0.70 h R ALD th b h i fM O d t td i l l til d li id M i Bi (Di 150 ilm 0.65 wth ALD growth behavior of MgO was demonstrated using a novel volatile and liquid precursor, Magnesium Bis(Di- b l idi ) Th M O fil hd d bl l l fC dN b h d ll f Al 100 150 Fi 0 60 0.65 row secbutylacetamidinate). The MgO films had undetectable levels of C and N, but showed a small amount of Al as 100 0 55 0.60 G a contaminant. Films exposed to air form a self-limiting hydroxide layer. Electrical measurements indicate the 50 0.55 film is a good insulator with a dielectric constant of 8-10. Application of MgO to Arradiance microchannel plate 0 0.50 amplifiers showed a substantial improvement in performance over existing commercial MCPs. 0 0 100 200 300 400 500 600 200 225 250 275 300 0 100 200 300 400 500 600 Cycle Number Growth Temp, °C Rf Film thickness determined using spectroscopic ellipsometer . Å References Growth rate is relatively stable over the temperature range of 225 Index of refraction=1.74; Extrapolated growth rate = 0.8Å/cycle. References – 275°C. Examination of of a larger temperature range is No growth delay on UV-ozone treated Si. 1 Atomic Layer Deposition of MgO Using Bis(ethylcyclopentadienyl)magnesium and H2O; B B Burton D N currently underway. Atomic Layer Deposition of MgO Using Bis(ethylcyclopentadienyl)magnesium and H2O; B. B. Burton, D. N. Goldstein and S M George J Phys Chem C 2009 113 1939–1946 Goldstein, and S. M. George, J. Phys. Chem. C 2009, 113, 1939–1946 printed by printed by t i www.postersession.com
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