• Korean Journal of Materials Research
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• v.9 no.8
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• pp.837-842
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• 1999

The Ta/TaN multilayer structure with repeating layers of a poly-crystalline Ta layer of high ductility and a TaN layer of high hardness is expected to exhibit toughness. This paper reports the results on the hardness and the adhesion strength of Ta/TaN multilayers and compositional gradient Ta/TaN layers deposited on the high speed steel substrate by reactive sputtering as a function of annealing temperature. The TaN film deposited with the $N_2$/Ar ratio of 0.4 in the reactive sputtering process exhibits the highest crystallinity, and the highest hardness and the results of scratch test of the Ta/TaN multilayers. The hardness and adhesion strength of the Ta/TaN multilayers becomes deteriorated with increasing the annealing temperature in the heat treatment right after depositing the layers. Therefore, post-annealing treatments are not desirable in the case of the Ta/TaN multilayers from the standpoint of mechanical properties. Also the hardness of Ta/TaN multilayers increases with decreasing the compositional modulation wavelength, but the adhesion property of the layers is nearly independent of the wavelength. On the other hand, the compositional gradient Ta/TaN film exhibits the highest hardness and the value of scratch test for the post-annealing temperatures of 20$0^{\circ}C$ and 40$0^{\circ}C$, respectively. This tendency of the compositional gradient Ta/TaN films differs from that of the Ta/TaN multilayers.

• Journal of the Korean Magnetics Society
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• v.15 no.4
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• pp.226-230
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• 2005

In this research, magnetic properties and annealing effects of the spin valve structures were investigated, which have Ta underlayer deposited with Ar and $N_2$ gas mixture. Also, TaN underlayer as a diffusion barrier and the substrate were investigated. The structure of the spin valve was Si($SiO_2$)/Ta(TaN)/NiFe/CoFe/Cu/CoFe/FeMn/Ta. Deposition rate was decreased and resistivity and roughness of the TaN films were increased as the $N_2$ gas flow was increased. The XRD results after high temperature annealing showed that Silicides were created in Si/Ta layer, but not in Si/TaN layer. Magnetoresistance ratio (MR) and exchange coupling field ($H_{ex}$) were decreased when the $N_2$ gas flow was increased over 4.0 sccm. The MR of the spin valves with Ta and TaN films deposited with up to 4.0 sccm of $N_2$ gas flow was increased about $0.5\%$ until the annealing temperature of up to $200^{\circ}C$ and then, decreased. TaN film deposited with 8.0 sccm of $N_2$ gas flow showed twice the adhesion of the Ta film. The above results indicate that with 3.0 sccm of $N_2$ gas flow during the Ta underlayer deposition, the magnetic properties of the spin valves are maintained, while the underlayer may be used as a diffusion barrier and the adhesion between the Si substrate and the underlayer is increased.

• Applied Microscopy
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• v.50
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• pp.7.1-7.10
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• 2020

Tantalum nitride (TaN_x) thin films were grown utilizing an inductively coupled plasma (ICP) assisted direct current (DC) sputtering, and 20-100% improved microhardness values were obtained. The detailed microstructural changes of the TaN_x films were characterized utilizing transmission electron microscopy (TEM), as a function of nitrogen gas fraction and ICP power. As nitrogen gas fraction increases from 0.05 to 0.15, the TaN_x phase evolves from body-centered-cubic (b.c.c.) TaN_0.1, to face-centered-cubic (f.c.c.) δ-TaN, to hexagonal-close-packing (h.c.p.) ε-TaN phase. By increasing ICP power from 100 W to 400 W, the f.c.c. δ- TaN phase becomes the main phase in all nitrogen fractions investigated. The higher ICP power enhances the mobility of Ta and N ions, which stabilizes the δ-TaN phase like a high-temperature regime and removes the micro-voids between the columnar grains in the TaN_x film. The dense δ-TaN structure with reduced columnar grains and micro-voids increases the strength of the TaN_x film.

• Journal of Surface Science and Engineering
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• v.38 no.2
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• pp.65-68
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• 2005

The effect of crystal orientation and microstructure on the mechanical properties of $TaN_x$ was investigated. $TaN_x$ films were grown on $SiO_2$ substrates by ultrahigh vacuum unbalanced magnetron sputter deposition in mixed $Ar/N_2$ discharges at 20 mTorr (2.67 Pa) and at $350^{\circ}C$. Unlike the Ti-N system, in which TiN is the terminal phase, a large number of N-rich phases in the Ta-N system could lead to layers which had nano-sized lamella structure of coherent cubic and hexagonal phases, with a correct choice of nitrogen fraction in the sputtering mixture and ion irradiation energy during growth. The preferred orientations and the micro-structure of $TaN_x$ layers were controlled by varing incident ion energy $E_i\;(=30eV\~50eV)$ and nitrogen fractions $f_{N2}\;(=0.1\~0.15)$. $TaN_x$ layers were grown on (0002)-Ti underlayer as a crystallographic template in order to relieve the stress on the films. The structure of the $TaN_x$ film transformed from Bl-NaCl $\delta-TaN_x$ to lamellar structured Bl-NaCl $\delta-TaN_x$ + hexagonal $\varepsilon-TaN_x$ or Bl-NaCl $\delta-TaN_x$ + hexagonal $\gamma-TaN_x$ with increasing the ion energy at the same nitrogen fraction $f_{N2}$. The hardness of the films also increased by the structural change. At the nitrogen fraction of $0.1\~0.125$, the structure of the $TaN_x$ films was changed from $\delta-TaN_x\;+\;\varepsilon-TaN_x\;to\;\delta-TaN_x\;+\;\gamma-TaN_x$ with increasing the ion energy. However, at the nitrogen fraction of 0.15 the film structure did not change from $\delta-TaN_x\;+\;\varepsilon-TaN_x$ over the whole range of the applied ion energy. The hardness increased significantly from 21.1 GPa to 45.5 GPa with increasing the ion energy.

• Journal of the Korean Vacuum Society
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• v.3 no.2
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• pp.190-197
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• 1994

본 연구에서는 DC magnetron 스퍼터링법을 이용하여 고정밀, 고저항 저항체 박막으로 TaNx film을 제조하였을 때 형성될 수 있는 화합물 중 TaN0.1, TaN0.8과 TaN 박막의 Rs와 TCR특성을 평가하 고 film층의 우선방향성을 XRD를 이용하여 판명한 뒤 저항체의 Rs와 TCR에 미치는 영향을 조사하였 다. TaN0.1 박막이 35$\Omega$/$\square$의 면저항값과 안정된 TCR값을 나타내는 것을 알수 있었다. 두께50~200nm 의 TaN0.1과 Alumina 기판 사이에 정(+)의 TCR을 갖는 약 50nm의 Cr층을 증착하였을 때 Rs는 180$\Omega$/ $\square$ 과 TCR는 20ppm/$^{\circ}C$인 적층박막을 제조할 수 있었다. TaN0.1, TaN0.8 과 TaN 시편에서 화합물 형성 에 따른 Ta의 결합에너지를 ESCA를 이용하여 조사하였다. 이상의 연구결과로부터 TaN0.1 film이 TaNfilm 보다 고정밀, 고저항 박막 저항체 제조에 있어 우수한 전기저항 특성을 가지며 Cr 중간층 형성 으로 TCR이 $\pm$ppm/$^{\circ}C$정도로 안정된 고정밀 다층 저항체 박막을 형성할 수 있었다.

• Korean Journal of Materials Research
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• v.21 no.2
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• pp.95-99
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• 2011

The microstructure and Cu diffusion barrier property of Ta-Si-N films for various Si and N compositions were studied. Ta-Si-N films of a wide range of compositions (Si: 0~30 at.%, N: 0~55 at.%) were deposited by DC magnetron reactive sputtering of Ta and Si targets. Deposition rates of Ta and Si films as a function of DC target current density for various $N_2/(Ar+N_2)$ flow rate ratios were investigated. The composition of Ta-Si-N films was examined by wavelength dispersive spectroscopy (WDS). The variation of the microstructure of Ta-Si-N films with Si and N composition was examined by X-ray diffraction (XRD). The degree of crystallinity of Ta-Si-N films decreased with increasing Si and N composition. The Cu diffusion barrier property of Ta-Si-N films with more than sixty compositions was investigated. The Cu(100 nm)/Ta-Si-N(30 nm)/Si structure was used to investigate the Cu diffusion barrier property of Ta-Si-N films. The microstructure of all Cu/Ta-Si-N/Si structures after heat treatment for 1 hour at various temperatures was examined by XRD. A contour map that shows the diffusion barrier failure temperature for Cu as a function of Si and N composition was completed. At Si compositions ranging from 0 to 15 at.%, the Cu diffusion barrier property was best when the composition ratio of Ta + Si and N was almost identical.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2001.05b
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• pp.79-83
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• 2001

In order to compare the barrier properties of Ta-N/Si(001) with those of Ta-N/Ta/Si(001), we studied structural properties of films grown by RF magnetron sputtering with various $Ar/N_2$ ratios. To evaluate the barrier properties, the samples were annealed in a vacuum chamber. Ex-situ x-ray scattering measurements were done using an in-house x-ray system. With increasing nitrogen ratio in Ta-N/Si(001), the barrier property of Ta-N/Si(001) was enhanced, finally failed at $750^{\circ}C$ due to the crystallization and silicide formation. Compared with Ta-N/Si(001), Ta-N/Ta/Si(001) forms silicides at $650^{\circ}C$. However it does not crystallize even at $750^{\circ}C$. With increasing nitrogen composition in Ta-N/Ta/Si(001), the formation of tantalum silicide was reduced and the surface roughness was improved. To observe the surface morphology of Ta-N/Ta/Si(001) during annealing, we performed an in-situ x-ray scattering experiment using synchrotron radiation of the 5C2 at Pohang Light Source(PLS). Addition of Ta layer between Ta-N and Si(001) improved the surface morphology and reduced the surface degradation at high temperatures. In addition, increasing $N_2/Ar$ flow ratio reduced the formation of tantalum silicide and enhanced the barrier properties.

• Korean Journal of Materials Research
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• v.28 no.4
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• pp.241-246
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• 2018

$TaN_x$ film is grown by plasma enhanced atomic layer deposition (PEALD) using t-butylimido tris(dimethylamido) tantalum as a metalorganic source with various reactive gas species, such as $N_2+H_2$ mixed gas, $NH_3$, and $H_2$. Although the pulse sequence and duration are the same, aspects of the film growth rate, microstructure, crystallinity, and electrical resistivity are quite different according to the reactive gas. Crystallized and relatively conductive film with a higher growth rate is acquired using $NH_3$ as a reactive gas while amorphous and resistive film with a lower growth rate is achieved using $N_2+H_2$ mixed gas. To examine the relationship between the chemical properties and resistivity of the film, X-ray photoelectron spectroscopy (XPS) is conducted on the ALD-grown $TaN_x$ film with $N_2+H_2$ mixed gas, $NH_3$, and $H_2$. For a comparison, reactive sputter-grown $TaN_x$ film with $N_2$ is also studied. The results reveal that ALD-grown $TaN_x$ films with $NH_3$ and $H_2$ include a metallic Ta-N bond, which results in the film's higher conductivity. Meanwhile, ALD-grown $TaN_x$ film with a $N_2+H_2$ mixed gas or sputtergrown $TaN_x$ film with $N_2$ gas mainly contains a semiconducting $Ta_3N_5$ bond. Such a different portion of Ta-N and $Ta_3N_5$ bond determins the resistivity of the film. Reaction mechanisms are considered by means of the chemistry of the Ta precursor and reactive gas species.

• Journal of the Korean Magnetics Society
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• v.5 no.5
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• pp.601-605
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• 1995

Magnetic properties of FeTaN and FeTaC films deposited by DC magnetron reactive sputter were investigated, and correlated with their microstructures. The optimum magnetic properties of Hc : 0.25 Oe, Bs : 14.5 kG, and ${\mu}'$ : 4000 (5MHz) are observed in the $Fe_{78.8}Ta_{8.5}N_{12.7}$ film, and Hc : 0.25 Oe, Bs : 14.5 kG, and ${\mu}'$ : 2700 (5MHz) in the $Fe_{75.6}Ta_{8.1}C_{16.3}$ film. In both FeTaN and FeTaC films with minimum grain size show the best soft magnetic properties. Thermal stability of the soft magnetic properties of FeTaN is found to be higher than FeTaC for similar compositons. TaN and TaC particles form to retard the growth of $\alpha$-Fe grains. TaN particles in FeTaN show higher efficiency in retarding the grain growth during heat treatments resulting the higher thermal stability, compared to TaC particles in FeTaC films.

• Korean Journal of Materials Research
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• v.7 no.10
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• pp.877-883
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• 1997

Ar 및 Ar과 $N_{2}$ 분위기하에서 rf 마그네트론 스퍼터링방법으로 Ta-AI과 Ta-AI-N합금막을 제조하였다. Ta-7.9at.% AI계열, Ta-26.7 at% AI게열과 Ta-45.4at.%AI계열에 Ar에 대한 질서유량비로 26%까지 질소를 첨가하여 Ta-AI-N박막을 증착한후, 300-$600^{\circ}C$온도 구산에서 열처리 전후의 구조 및 전기적 특성과 열적안정성을 통하여 레지스터의 적용가능성을 조사하였다. 구조 및 조성 분석은 X-선 회절과 Rutherford Backscattering Spectrometry(RBS)로 관찰하였고 열적안정성은 4단자법(four point probe method)을 이용한 저항변화를 통하여 측정하였다. 순수 Ta에 AI을 첨가하면 확장된 $\beta$($\beta$-Ta)N 합금박막에서 가장 열적안정성이 우수하게 나타났던 질소첨가 범위는 Ta $N_{hcp}$또는 TaN/ sub fcc/또는 Ta $N_{fcc}$와 비정질과의 혼합상순으로 상천이를 나타내었다. Ta-AI-N 합금박막에서 가장 열적안정성이 우수하게 나타났던 질서첨가 범위는 Ta-26.7at. % AI계열의 경우 19-36at.% $N_{2}$구간이었고, Ta-45.5at.% AI계열의 경우는 30-45at.%구간이었다. Ta-AI합금박막은 질소가 첨가되지 않아도 열처리 온도 및 시간에 따라 약 10% 이내의 비교적 작은 저항변화를 보여 열적안정성이 우수하지만 질소를 첨가하여 Ta-AI-N합금박막을 형성시킬경우, 증착된 상태에서 이미 큰 비저항을 나타내었고 열처리 동안 3%이내의 매우 작은 저항변화를 나타내었기 때문에 레지스터용 재료로써 열적안정성에 대한 잠재력이 크다.