• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.103.1-103.1
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• 2017

Nanocrystalline HfN coatings were prepared by reactively sputtering Hf metal target with N2 gas using a magnetron sputtering system operated in DC and ICP (inductively coupled plasma) condition with various powers. The effects of ICP power, ranging from 0 to 200 W, on the coating microstructure, corrosion and mechanical properties were systematically investigated with FE-SEM, AFM, potentiostat and nanoindentation. The results show that ICP power has a significant influence on coating microstructure and mechanical properties of HfN coatings. With the increasing of ICP power, coating microstructure evolves from the columnar structure of DC process to a highly dense one. Average grain size and nano hardness of HfN coatings were also investigated with increasing ICP powers.

• Journal of the Korean institute of surface engineering
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• v.53 no.2
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• pp.67-71
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• 2020

For deposition technology using plasma, it plays an important role in improving film deposited with high ionization rate through high density plasma. Various deposition methods such as high-power impulse magnetron sputtering and ion-beam sputtering have been developed for physical vapor deposition technology and are still being studied. In this study, it is intended to control plasma using inductive coupled plasma (ICP) antennas and use properties to improve the properties of Hafnium nitride (HfN) films using ICP assisted magnetron sputtering (ICPMS). HfN film deposited using ICPMS showed a finer grain sizes, denser microstructure and better mechanical properties as ICP power increases. The best mechanical properties such as nanoindentation hardness of 47 GPa and Young's modulus of 401 GPa was obtained from HfN film deposited using ICPMS at ICP power of 200 W.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.56 no.2
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• pp.349-354
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• 2007

In this work, we investigated etching characteristics of $HfO_2$ thin film and Si using inductive coupled plasma(ICP) system. The ion energy distribution functions in an ICP system was analyzed by quadrupole mass spectrometer(QMS) with an electrostatic ion energy analyzer. The maximum etch rate of $HfO_2$ thin film is 85.5 nm/min at a $BCl_3/(BCl_3+Ar)$ of 20 % and decreased with further addition of $BCl_3$ gas. From the QMS measurements, the most dominant positive ion energy distributions(IEDS) showed a maximum at 20 % of $BCl_3$. These tendency was very similar to the etch characteristics. This result agreed with the universal energy dependency of ion enhanced chemical etching yields. And the maximum selectivity of $HfO_2$ over Si is 3.05 at a $O_2$ addition of 2 sccm into the $BCl_3/(BCl_3+Ar)$ of 20 % plasma.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.22 no.5
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• pp.448-454
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• 2009

Hydrogen was produced from water plasma excited in high frequency (HF) inductively coupled tubular reactor. Mass spectrometry was used to monitor gas phase species at various process conditions, Water dissociation rate depend on the process parameters such as ICP power, $H_{2}O$ flow-rate and process pressure, Water dissociation percent in ICP reactor decrease with increase of chamber pressure, while increase with increase of ICP power and $H_{2}O$ flow rate. The effect of $CH_4$ gas addition to a water plasma on the hydrogen production has been studied in a HF ICP tubular reactor. The main roles of $CH_4$ additive gas in $H_{2}O$ plasma are to react with 0 radical for forming $CO_x$ and CHO and resulting additional $H_2$ production. Furthermore, $CH_4$ additives in $H_{2}O$ plasma is to suppress reverse-reaction by scavenging 0 radical. But, process optimization is needed because $CH_4$ addition has some negative effects such as cost increase and $CO_x$ emission.

• Analytical Science and Technology
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• v.26 no.6
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• pp.375-380
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• 2013

Ammonium biflouride ($NH_4HF_2$) digestion was studied for germanium analysis in rock and sediment by inductively coupled plasma mass spectrometry (ICP/MS). QLO-1 and SDO-1 are used for reference materials from USGS. Sediment, basalt and ball clay for GeoPT were chosen as real samples. The loss of germanium in open vessel digestion was well known which can be caused by easy transformation to volatile compounds. But ammonium bifluoride digestion could suppress loss of germanium in open vessel digestion. Germanium recovery was not influenced by hydrogen peroxide with ammonium bifluoride digestion. Furthermore, the new method was simple and rapid in germanium analysis by ICP/MS. MDL(method detection limit) was 0.015 ${\mu}g/g$ and germanium recovery was 106~128%.

• Analytical Science and Technology
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• v.27 no.6
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• pp.352-356
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• 2014

Various studies have been done to improve the properties of the steel by adding boron to the steel. Some studies have reported on the analysis of the boron in steel by AAS (atomic absorption spectrometry), ICP-OES(inductively coupled plasma-optical emission spectrometry), ICP-MS (inductively coupled plasma/mass spectrometry). The volatile loss of boron of steel in sample digestion and the separation procedure for avoiding matrix effect by high concentration of iron are difficulties for determination of boron in steel. The method to determine boron in steel by ICP-MS was developed without volatilization of boron in sample digestion step with $HNO_3-NH_4HF_2$ digestion method, and the additional separation process for avoiding matrix effect. Complete decomposition of steel with $HNO_3-NH_4HF_2$ digestion method, and boron determination by ICP-MS in the matrix of high concentration of iron were possible. Quantitative recoveries of boron in certified standard steel by new method in this study were 103 to 111%, and the relative standard deviation is less than 5%. The method detection limit was $1.17{\mu}g/g$.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.477-477
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• 2008

For more than three decades, the gate dielectrics in CMOS devices are $SiO_2$ because of its blocking properties of current in insulated gate FET channels. As the dimensions of feature size have been scaled down (width and the thickness is reduced down to 50 urn and 2 urn or less), gate leakage current is increased and reliability of $SiO_2$ is reduced. Many metal oxides such as $TiO_2$, $Ta_2O_4$, $SrTiO_3$, $Al_2O_3$, $HfO_2$ and $ZrO_2$ have been challenged for memory devices. These materials posses relatively high dielectric constant, but $HfO_2$ and $Al_2O_3$ did not provide sufficient advantages over $SiO_2$ or $Si_3N_4$ because of reaction with Si substrate. Recently, $HfO_2$ have been attracted attention because Hf forms the most stable oxide with the highest heat of formation. In addition, Hf can reduce the native oxide layer by creating $HfO_2$. However, new gate oxide candidates must satisfy a standard CMOS process. In order to fabricate high density memories with small feature size, the plasma etch process should be developed by well understanding and optimizing plasma behaviors. Therefore, it is necessary that the etch behavior of $HfO_2$ and plasma parameters are systematically investigated as functions of process parameters including gas mixing ratio, rf power, pressure and temperature to determine the mechanism of plasma induced damage. However, there is few studies on the the etch mechanism and the surface reactions in $BCl_3$ based plasma to etch $HfO_2$ thin films. In this work, the samples of $HfO_2$ were prepared on Si wafer with using atomic layer deposition. In our previous work, the maximum etch rate of $BCl_3$/Ar were obtained 20% $BCl_3$/ 80% Ar. Over 20% $BCl_3$ addition, the etch rate of $HfO_2$ decreased. The etching rate of $HfO_2$ and selectivity of $HfO_2$ to Si were investigated with using in inductively coupled plasma etching system (ICP) and $BCl_3/Cl_2$/Ar plasma. The change of volume densities of radical and atoms were monitored with using optical emission spectroscopy analysis (OES). The variations of components of etched surfaces for $HfO_2$ was investigated with using x-ray photo electron spectroscopy (XPS). In order to investigate the accumulation of etch by products during etch process, the exposed surface of $HfO_2$ in $BCl_3/Cl_2$/Ar plasma was compared with surface of as-doped $HfO_2$ and all the surfaces of samples were examined with field emission scanning electron microscopy and atomic force microscope (AFM).

• Journal of the Korean Chemical Society
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• v.41 no.8
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• pp.399-405
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• 1997

We examined the determination of trace amount of germanium in rocks and sediments by hydride vapor generation-ICP-AES. Germanium is formed volatile compounds with various types of acid reagents, but volatilizing of germanium was decreased in the presence of $H_3PO_4$. Sediments and rocks can be dissolved by mixed acids of $HF-HNO_3-H_3PO_4$ without volatilizing loss of germanium in open digestion system and it was possible to determine germanium by hydride generation-ICP-AES without further sample treatment. Detection limit of Ge is reached to 0.08 ppb under the condition of 5M $H_3PO_4$ and 1% $NaBH_4$ as a supporting acid and a reducing reagent, respectively. The measured values by hydride generation-ICP-AES agreed well with the reference values of SRMs as well as the values determined by solution nebulization-ICP-MS.

• Corrosion Science and Technology
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• v.22 no.6
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• pp.393-398
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• 2023

Properties of hafnium nitride (HfN) coatings are affected by deposition conditions, most often by the sputtering technique. Appropriate use of different magnetron sputtering modes allows control of the structural development of the film, thereby enabling adjustment of its properties. This study compared properties of HfN coatings deposited by direct current magnetron sputtering (dcMS), mid-frequency direct current magnetron sputtering (mfMS), and inductively coupled plasma-assisted magnetron sputtering (ICPMS) systems. The microstructure, crystalline, and mechanical properties of these HfN coatings were investigated by field emission electron microscopy, X-ray diffraction, atomic force microscopy, and nanoindentation measurements. HfN coatings deposited using ICPMS showed smooth and highly dense microstructures, whereas those deposited by dcMS showed rough and columnar structures. Crystalline structures of HfN coatings deposited using ICPMS showed a single δ-HfN phase, whereas those deposited using dcMS and mfMS showed a mixed δ-HfN and HfN_0.4 phases. Their performance were increased in the order of dcMS < mfMS < ICPMS, with ICPMS achieving a value of 47.0 GPa, surpassing previously reported results.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2010.06a
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• pp.382-382
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• 2010

The etch characteristics of the $HfAlO_3$ thin films and selectivity of $HfAlO_3$ to $SiO_2$ in $Cl_2/BCl_3$/Ar plasma were investigated in this work. The maximum etch rate was 108.7 nm/min and selectivity of $HfAlO_3$ to $SiO_2$ was 1.11 at $Cl_2$(3sccm)/$BCl_3$(4sccm)/Ar(16sccm), RF power of 500 W, DC-bias voltage of - 100 V, process pressure of 1 Pa and substrate temperature of $40^{\circ}C$. As increasing RF power and DC-bias voltage, etch rates of the $HfAlO_3$ thin films increased. Whereas as decreasing of the process pressure, those of the $HfAlO_3$ thin films were increased. The chemical reaction on the surface of the etched the $HfAlO_3$ thin films was investigated with X-ray photoelectron spectroscopy (XPS).