• Journal of the Korean Society for Nondestructive Testing
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• v.33 no.2
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• pp.129-137
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• 2013

A force calibration of a nanoindenter and a 3D morphology observation of indenters were carried out in this study. A microbalance calibrated with standard weights was used for measuring the loads generated by a nanoindenter. The indentation load could be calibrated from the ratio of measured and generated loads and the first contact load also could be detected from the microbalance data. By analyzing atomic force microscopy images of two indenters, curvature radii of apexes were determined by $19.71{\pm}3.03$ and $1043.94{\pm}50.91$ nm, respectively, for the nearly new indenter A and the severly worn indenter B. Corresponding bluntness depths were estimated by 1.22 and 64.56 nm for the both indenters by overlapping their profiles on the perfect pyramidal shape. In addition, nanoindentation curves obtained from a fused silica reference material with the both indenters showed a depth difference corresponding to the bluntness depth difference along the indentation depth axis. By shifting amounts of the bluntness depths along the horizontal axis, whole nanoindentation curves overlapped on themselves and resulted in nanohardness values consistent within 1.11 % without considering the complex indenter area function of each indenter.

• Journal of the Korean Vacuum Society
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• v.18 no.5
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• pp.346-351
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• 2009

Due to the decrease of line width and increase of the integration level of the device, it is expected that 'Bottom-up' method will replace currently used 'Top-down' method. Researches about 'Bottom-up' device production such as Nanowires and Nanobelts are widely held on. To utilize these technologies in devices, properties of matter should be exactly measured. Nano-indenters are used to measure the properties of nano-scale structures. Additionally, Nano-indenters provide AFM(Atomic Force Microscopy) function to get the image of the surface and get physical properties for exact position of nano-structure using this image. However, nano-indenter tips have relatively much bigger size than ordinary AFM probes, there occurs considerable error in surface image by Nano-Indenter. Accordingly, this research used 50nm Berkovich tip and 1um $90^{\circ}$ Conical tip, which are commonly used in Nano-Indenter. To find out the surface characteristics for each kind of tip, we indented the surface of thin layer by each tip and compared surface image and indentation depth. Then, we got image of 100nm-size structure by surface scanning using Nano-Indenter and compared it with surface image gained by current AFM technology. We calculated the errors between two images and compared it with theoretical error.

• Proceedings of the Korean Vacuum Society Conference
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• 2015.08a
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• pp.176.1-176.1
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• 2015

본 연구는 플라즈마 건식 식각 후 박막의 물성 특성 변화 측정에 Nano-Indentation 분석 기법을 도입하였으며, 식각 후 박막 표면 강도를 nano 영역에서 측정하여 박막 표면의 damage 분석에 적용하여 물리적인 해석을 시도하였다. 하지만 기판의 대면적화로 인하여 반도체 공정에 사용되는 기판은 300 mm로 증가하였고 이로 인하여 플라즈마 건식 식각에서 대면적에 대한 균일도 향상 연구를 진행 중에 있다. 이 연구에서는 플라즈마 건식 식각 후 박막의 균일도를 Nano-indenter 측정 결과를 기반으로 Weibull 분포 해석을 통하여 정량적인 균일도를 측정하고자 하였다. 플라즈마 건식 식각을 위하여 플라즈마 소스는 Adaptively Coupled Plasma (ACP)를 사용하였고 식각 후 TEOS $SiO_2$ 박막 표면을 분석하기 위하여, 시료 평면의 x, y 축에 대하여 각각 $20{\mu}m$로 indent 각 지점을 이격하여 동일한 측정 조건에서 Nano-indenter를 이용하여 박막 표면의 강도를 측정하였다. 측정된 결과는 Weibull 분포를 활용하여 정량화하였다. 결과에 의하면 플라즈마 소스의 bias 파워가 300 W 일 때 균일도가 가장 높은 29.84로 측정되었고, 150 W 일 때 가장 낮은 8.38로 측정되었다. 식각 전 TEOS $SiO_2$ 박막의 Weibull 분포에 의한 균일도가 17.93으로 측정됨을 기반으로 ACP 플라즈마 소스의 식각 조건에 따라 TEOS $SiO_2$ 박막의 균일도가 상대적으로 변함을 정량적으로 분석할 수 있었다.

• Proceedings of the Korean Vacuum Society Conference
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• 2015.08a
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• pp.177.2-177.2
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• 2015

Nano-mechanics 연구는 기판의 나노표면에 대하여 indenter tip을 직접 인가하여 측정함으로써 기존 분광학 연구에서는 불가능했던 박막의 기계적 특성 연구가 가능하다. 그러나 박막분석 특성상 박막의 표면, 기판 또는 하부 박막에 의한 영향으로 인해 박막의 고유한 물성특성 연구에 제약이 있다. 박막 표면에 의한 영향인 표면효과는 nano-indentation을 실행 할 때 tip의 압입으로 발생되는 표면의 스트레스로 인해 표면 변형이 나타나는 현상이다. 반면에 하부 박막과 기판에 의한 오류는 nano-indentation 실행 시 tip의 압입 깊이가 깊어질수록 하부박막 또는 기판과 가까워지기 때문에 박막 고유의 특성이 아닌 하부박막과 기판에 의한 영향이 같이 나타나는 현상이다. 이러한 오류를 최소화 하고자 많은 연구에서는 박막의 강도에 따라 nano-indentation의 실행 깊이를 박막 총 두께의 최소7%에서 최대 50%까지 삽입하는 방법을 도입하였다. 이를 기반으로 본 연구는 Zirconium nitride (ZrN) 박막의 증착된 두께 깊이만큼 nano-indentation 분석을 실행 하였으며 박막 고유의 nano-mechanics 특성을 연구 하였다. ZrN 박막은 hard coating 분야에 많이 사용되는 물질로 박막 고유의 hardness를 연구하는 것이 큰 의미가 있다. 연구 결과 모든 박막은 두께 30% 깊이 측정에서 박막 표면과 기판효과가 최소화된 박막의 물성 측정이 가능 하였고, 증착 시 질소를 0.5, 1, 2 sccm 흘려준 박막들은 총 두께 30% 깊이에서 hardness가 각각 23.2, 8.6, 18 GPa이었다. 따라서 nano-indenter 측정 시 유효한 측정 깊이에서 측정을 실시하는 것이, 박막의 물성분석에 있어서 대단히 중요함을 확인 하였다.

• Journal of the Microelectronics and Packaging Society
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• v.26 no.4
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• pp.95-100
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• 2019

Nanoindentation has been widely used for evaluating mechanical properties of nano-devices, from MEMS to packaging modules. Residual stress is also estimated from indentation tests, especially the Knoop indenter which is used for the determination of residual stress directionality. According to previous researches, the ratio of the two stress conversion factors of Knoop indentation is a constant at approximately 0.34. However, the ratio is supported by insufficient quantitative analyses, and only a few experimental results with indentation depth variation. Hence, a barrier for in-field application exists. In this research, the ratio of two conversion factors with variation in indentation depth using finite elements method has been attempted at. The magnitudes of each conversion factors were computed at uniaxial stress state from the modelled theoretical Knoop indenter and specimen. A model to estimate two stress conversion factor of the long and short axis of Knoop indenter at various indentation depths is proposed and analyzed.

• Transactions of the Korean Society of Mechanical Engineers A
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• v.37 no.12
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• pp.1503-1512
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• 2013

In this study, we proposed an indentation evaluation method for fracture toughness using cohesive finite element simulations. First, we examined the effect of material properties (yield strain, Poisson's ratio, and elastic modulus) on crack size during Vickers indentation and then generated a regression formula that explains the relations among fracture toughness, indentation load, and crack size. We also proposed another indentation formula for fracture toughness evaluation using the contact size a and E/H (H: hardness). Finally, we examined the relation between the crack size and the indenter shapes. Based on this, we can generate from the formula obtained using the Vickers indenter a formula for an indenter of different shapes. Using the proposed method, fracture toughness is directly estimated from indentation data.

• Geomechanics and Engineering
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• v.30 no.4
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• pp.345-352
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• 2022

When rock burst occurs, the damaged coal, rock and other fragments can be ejected to the roadway at a speed of up to 10 m/s. It is extremely harmful to personnel and mining equipment, and seriously affects the mining activities. In order to study the energy evolution characteristics, especially kinetic energy, in the process of rock mass failure, this paper first analyzes the energy changes of the rock in different stages under uniaxial compression. The formula of the kinetic energy of rock sample considering the energy from the indenter of the testing machine is obtained. Then, the uniaxial compression tests with different stiffness ratios of the indenter and rock sample are simulated by numerical simulation. The kinetic energy U_d, elastic strain energy U_e, friction energy U_f, total input energy U and surface energy U_θ of crack cracking are analyzed. The results show that: The stiffness ratio has influence on the peak strength, peak strain, U_d, U_e, U_θ, U_f and U of rock samples. The variation trends of strength, strain and energy with stiffness are different. And when the stiffness ratio increases to a certain value, if the stiffness of the indenter continues to increase, it will have no longer effect on the rock sample.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.11a
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• pp.39-39
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• 2003

Molecular dynamics (MD) simulation was performed to study the stress induced grain boundary migration caused by the interaction of dislocations with a gain boundary. The simulation was carried out in a Ni block (295020 atoms) with a ∑ = 5 (210) grain boundary and an embedded atom potential for Ni was used for the MD calculation. Stress was provided by indenting a diamond indenter and the interaction between Ni surface and diamond indenter was assumed to have a fully repulsive force to emulate a faction free surface. Results showed that the indentation nucleated perfect dislocations and the dislocations produced stacking faults in the form of a parallelepiped tube. The parallelepiped tube consisted of two pairs of parallel dislocations with Shockley partials and was produced successively during the penetration of the indenter. The dislocations propagated along the parallelepiped slip planes and fully merged onto the ∑ = 5 (210) grain boundary without emitting a dislocation on the other grain. The interaction of the dislocations with the grain boundary induced the migration of the grain boundary plane in the direction normal to the boundary plane and the migration continued as long as the dislocations merged onto the grain boundary plane. The detailed mechanism of the conservative motion of atoms at the gram boundary was associated with the geometric feature of the ∑ = 5 (210) grain boundary.

• Proceedings of the KSME Conference
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• 2000.11a
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• pp.256-261
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• 2000

In this study, we derived work-hardening exponent using continuous indentation test technique. Continuous indentation test technique is a powerful method to evaluate mechanical properties, such as hardness, modulus, ${\sigma}-{\varepsilon}$ curves and etc. It has many merits conventional indentation test has. The relationship between true stress and mean contact pressure and between strain and indentation depth were derived. While the indenter pushes the materials, the region around the indenter is deflected elastically. It is called elastic deflection. And pile-up phenomenon related to plastic deformation around the indenter increased the contact depth, and sink-in phenomenon decreases. So we calibrated contact depth change by considering elastic deflection and pile-up/sink-in. Using calibrated contact depth we redefined the relationship between true stress and mean contact pressure and between strain and contact depth. Through these relationship we could derive work-hardening exponent by analyzing load-depth curves. And it showed good agreement with tensile test results.

• Proceedings of the Korean Vacuum Society Conference
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• 2014.02a
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• pp.354.1-354.1
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• 2014

Hafnium nitride (HfN) 박막은 고온에서의 안정성과 낮은 비저항 그리고 산소확산에 대한 억제력을 가지고 있기 때문에 확산방지막으로 많은 연구가 진행 되고 있다. 현재까지 진행된 대부분의 연구는 HfN 박막의 전기적인 특성과 구조적인 특성에 대한 것이었고 다양한 연구 결과가 보고되었다. 하지만 기존의 연구들은 박막의 nano-electrotribology 특성에 대한 연구가 부족하여 박막 적층 공정시 요구되는 물성에 대한 연구가 절실하다. 따라서 본 연구에서는 HfN 박막의 증착조건 및 열처리조건에 따른 nano-electrotribology 특성 변화를 확인하고자 하였다. HfN박막은 rf magnetron sputter를 이용하여 Si 기판위에 Hf target으로 질소 유량을 변화시키며 증착하였고 가열로에서 $600^{\circ}C$와 $800^{\circ}C$로 20분간 열처리를 실시하였다. 열처리한 박막과 as-deposited 상태의 박막을 nano-indenter를 통하여 나노기계 전기적인 특성을 분석하였다. nano-indenter는 박막에 인가된 stress와 탄성계수(elastic modulus), 표면경도(surface hardness)와 같은 특성을 직접적인 tip 접촉을 통하여 in-situ로 분석할 수 있는 장비이다. 실험결과 HfN박막을 $600^{\circ}C$로 열처리 한 경우 표면경도가 16.20에서 18.59 GPa로 증가하였다. 표면경도의 증가는 열처리 시 박막내에 compressive stress가 생성되었기 때문이라고 생각된다. 그러나 $800^{\circ}C$로 열처리 한 경우 표면경도가 16.93 GPa로 감소하였는데 이는 표면균열 발생으로 인한 stress relaxation 때문인 것으로 생각된다. 증착 시 주입되는 질소의 유량과 열처리 온도는 HfN박막의 기계적 안정성에 영향을 미치는 중요한 요소임을 본 실험을 통해 확인하였다.