• Journal of the Korean Ceramic Society
• /
• v.38 no.1
• /
• pp.34-38
• /
• 2001

Hot filament CVD 방법에서 가스압을 증가시키는 방법을 사용하여 nanocrystalline 다이아몬드 막을 합성하였다. 메탄-수소 혼합가스를 사용하고 메탄함량, 유량, 기판온도합성시간은 각각 4%, 100sccm, 110$0^{\circ}C$, 10시간으로 일정하게 유 였다. 합성 변수로서 가스압을 40 Torr에서 300 Torr 구간에서 변화시켰다. High-resolution SEM으로 막 표면의 형상을 관찰하고, TEM, XRD, micro-Raman spectroscopy를 사용하여 합성된 막의 구조 및 특성을 분석하였다. 합성된 다이아몬드 막은 압력이 높아짐에 따라 mocrocrystalline 다이아몬드 막에서 점진적으로 nanocrystalline 다이아몬드 막으로 변화해갔으며, 가스압에 다라 비다이아몬드 상의 량이 증가하였다. 증착속도는 microcrystalline 다이아몬드 막이 형성되는 구간에서는 압력에 따라 1.1~1.3 $\mu\textrm{m}$/h까지 증가하다가 nanocrystalline 다이아모느 막이 형성되는 구간에서는 압력에 따라 감소하였다. 감소하였다.

• Journal of the Korean institute of surface engineering
• /
• v.42 no.5
• /
• pp.216-219
• /
• 2009

A surface acoustic wave (SAW) filter structure was fabricated employing $4{\mu}m$ thick nanocrystalline diamond (NCD) and $2.2{\mu}m$ thick ZnO films on Si wafer. The NCD film was deposited in an $Ar/CH_4$ gas mixture by microwave plasma chemical vapor deposition method. The ZnO film was formed over the NCD film in an RF magnetron sputter using ZnO target and $Ar/O_2$ gas. On the top of the two layers, copper film was deposited by the RF sputter and inter digital transducer (IDT) electrode pattern (line/space : $1.5/1.5{\mu}m$) was defined by the photolithography including a lift-off etching process. The fabricated SAW filter exhibited the center frequency of 1.66 GHz and the phase velocity of 9,960 m/s, which demonstrated that a giga Hertz SAW filter can be realized by utilizing the nanocrystalline diamond thin film.

• Journal of the Korean institute of surface engineering
• /
• v.50 no.5
• /
• pp.352-359
• /
• 2017

The growth of nanocrystalline diamond films on a p-type poly silicon substrate was studied using microwave plasma chemical vapor deposition method. A 6 mm thick poly silicon plate was mirror polished and scratched in an ultrasonic bath containing slurries made of 30 cc ethanol and 1 gram of diamond powders having different sizes between 5 and 200 nm. Upon diamond deposition, the specimen scratched in a slurry with the smallest size of diamond powder exhibited the highest diamond particle density and, in turn, fastest diamond film growth rate. Diamond deposition was carried out applying different DC bias voltages (0, -50, -100, -150, -200 V) to the substrate. In the early stage of diamond deposition up to 2 h, the effect of voltage bias was not prominent probably because the diamond nucleation was retarded by ion bombardment onto the substrate. After 4 h of deposition, the film growth rate increased with the modest bias of -100 V and -150 V. With a bigger bias condition(-200 V), the growth rate decreased possibly due to the excessive ion bombardment on the substrate. The film grown under -150V bias exhibited the lowest contact angle and the highest surface roughness, which implied the most hydrophilic surface among the prepared samples. The film growth rate increased with the apparent activation energy of 21.04 kJ/mol as the deposition temperature increased in the range of $300{\sim}600^{\circ}C$.

• Journal of the Korean institute of surface engineering
• /
• v.44 no.4
• /
• pp.131-136
• /
• 2011

A kinetic study has been made for the growth of nanocrystalline diamond (NCD) particles to a continuous thin film on silicon substrate in a microwave plasma chemical vapor deposition reactor. Parameters of deposition have been microwave power of 1.2 kW, the chamber pressure of 110 Torr, and the Ar/$CH_4$ ratio of 200/2 sccm. The deposition has been carried out at temperatures in the range of $400\sim700^{\circ}C$ for the times of 0.5~16 h. It has been revealed that a continuous diamond film evolves from the growth and coalescence of diamond crystallites (or particles), which have been heterogeneously nucleated at the previously scratched sites. The diamond particles grow following an $h^2$ = k't relationship, where h is the height of particles, k' is the particle growth rate constant, and t is the deposition time. The k' values at the different deposition temperatures satisfy an Arrhenius equation with the apparent activation energy of 4.37 kcal/mol or 0.19 eV/ atom. The rate limiting step should be the diffusion of carbon species over the Si substrate surface. The growth of diamond film thickness (H) shows an H = kt relationship with deposition time, t. The film growth rate constant, k, values at the different deposition temperatures show another Arrhenius-type expression with the apparent activation energy of 3.89 kcal/mol or 0.17 eV/atom. In this case, the rate limiting step might be the incorporation reaction of carbon species from the plasma on the film surface.

• Journal of the Korean institute of surface engineering
• /
• v.46 no.1
• /
• pp.29-35
• /
• 2013

The effect of DC bias on the growth of nanocrystalline diamond films on silicon substrate by microwave plasma chemical vapor deposition has been studied varying the substrate temperature (400, 500, 600, and $700^{\circ}C$), deposition time (0.5, 1, and 2h), and bias voltage (-50, -100, -150, and -200 V) at the microwave power of 1.2 kW, working pressure of 110 torr, and gas ratio of Ar/1%$CH_4$. In the case of low negative bias voltages (-50 and -100 V), the diamond particles were observed to grow to thin film slower than the case without bias. Applying the moderate DC bias is believed to induce the bombardment of energetic carbon and argon ions on the substrate to result in etching the surfaces of growing diamond particles or film. In the case of higher negative voltages (-150 and -200 V), the growth rate of diamond film increased with the increasing DC bias. Applying the higher DC bias increased the number of nucleation sites, and, subsequently, enhanced the film growth rate. Under the -150 V bias, the height (h) of diamond films exhibited an $h=k{\sqrt{t}}$ relationship with deposition time (t), where the growth rate constant (k) showed an Arrhenius relationship with the activation energy of 7.19 kcal/mol. The rate determining step is believed to be the surface diffusion of activated carbon species, but the more subtle theoretical treatment is required for the more precise interpretation.

• Journal of the Korean institute of surface engineering
• /
• v.47 no.2
• /
• pp.75-80
• /
• 2014

Nanocrystalline diamond(NCD) films on steel(SKH51) has been investigated using SiC interlayer film. SiC was deposited on SKH51 or Si wafer by RF magnetron sputter. NCD was deposited on SiC at $600^{\circ}C$ for 0.5~4 h employing microwave plasma CVD. Film morphology was observed by FESEM and FIB. Film adherence was examined by Rockwell C adhesion test. The growth rate of NCD on SiC/Si substrate was much higher than that on SiC/SKH51. During particle coalescence, NCD growth rate was slow since overall rate was determined by the diffusion of carbon on SiC surface. After completion of particle coalescence, NCD growth became faster with the reaction of carbon on NCD film controlling the whole process. In the case of SiC/SKH51 substrate, a complete NCD film was not formed even after 4 h of deposition. The adhesion test of NCD/SiC/SKH51 samples revealed a delamination of film whereas that of SiC/SKH51 showed a good adhesion. Many voids of less than 0.1 ${\mu}m$ were detected on NCD/SiC interface. These voids were believed as the reason for the poor adhesion between NCD and SiC films. The origin of voids was due to the insufficient coalescence of diamond particles on SiC surface in the early stage of deposition.

• Journal of the Korean institute of surface engineering
• /
• v.46 no.2
• /
• pp.68-74
• /
• 2013

For the coating of diamond films on WC-Co tools, a buffer interlayer is needed because Co catalyzes diamond into graphite. W and Ti were chosen as candidate interlayer materials to prevent the diffusion of Co during diamond deposition. W or Ti interlayer of $1{\mu}m$ thickness was deposited on WC-Co substrate under Ar in a DC magnetron sputter. After seeding treatment of the interlayer-deposited specimens in an ultrasonic bath containing nanometer diamond powders, $2{\mu}m$ thick nanocrystalline diamond (NCD) films were deposited at $600^{\circ}C$ over the metal layers in a 2.45 GHz microwave plasma CVD system. The cross-sectional morphology of films was observed by FESEM. X-ray diffraction and visual Raman spectroscopy were used to confirm the NCD crystal structure. Micro hardness was measured by nano-indenter. The coefficient of friction (COF) was measured by tribology test using ball on disk method. After tribology test, wear tracks were examined by optical microscope and alpha step profiler. Rockwell C indentation test was performed to characterize the adhesion between films and substrate. Ti and W were found good interlayer materials to act as Co diffusion barriers and diamond nucleation layers. The COFs on NCD films with W or Ti interlayer were measured as less than 0.1 whereas that on bare WC-Co was 0.6~1.0. However, W interlayer exhibited better results than Ti in terms of the adhesion to WC-Co substrate and to NCD film. This result is believed to be due to smaller difference in the coefficients of thermal expansion of the related films in the case of W interlayer than Ti one. By varying the thickness of W interlayer as 1, 2, and $4{\mu}m$ with a fixed $2{\mu}m$ thick NCD film, no difference in COF and wear behavior but a significant change in adhesion was observed. It was shown that the thicker the interlayer, the stronger the adhesion. It is suggested that thicker W interlayer is more effective in relieving the residual stress of NCD film during cooling after deposition and results in stronger adhesion.

• Journal of the Korean institute of surface engineering
• /
• v.46 no.4
• /
• pp.145-152
• /
• 2013

The growth behavior of nanocrystalline diamond (NCD) film has been studied for three different substrates, i.e. bare Si wafer, 1 ${\mu}m$ thick W and Ti films deposited on Si wafer by DC sputter. The surface roughness values of the substrates measured by AFM were Si < W < Ti. After ultrasonic seeding treatment using nanometer sized diamond powder, surface roughness remained as Si < W < Ti. The contact angles of the substrates were Si ($56^{\circ}$) > W ($31^{\circ}$) > Ti ($0^{\circ}$). During deposition in the microwave plasma CVD system, NCD particles were formed and evolved to film. For the first 0.5h, the values of NCD particle density were measured as Si < W < Ti. Since the energy barrier for heterogeneous nucleation is proportional to the contact angle of the substrate, the initial nucleus or particle densities are believed to be Si < W < Ti. Meanwhile, the NCD growth rate up to 2 h was W > Si > Ti. In the case of W substrate, NCD particles were coalesced and evolved to the film in the short time of 0.5 h, which could be attributed to the fact that the diffusion of carbon species on W substrate was fast. The slower diffusion of carbon on Si substrate is believed to be the reason for slower film growth than on W substrate. The surface of Ti substrate was observed as a vertically aligned needle shape. The NCD particle formed on the top of a Ti needle should be coalesced with the particle on the nearby needle by carbon diffusion. In this case, the diffusion length is longer than that of Si or W substrate which shows a relatively flat surface. This results in a slow growth rate of NCD on Ti substrate. As deposition time is prolonged, NCD particles grow with carbon species attached from the plasma and coalesce with nearby particles, leaving many voids in NCD/Ti interface. The low adhesion of NCD films on Ti substrate is related to the void structure of NCD/Ti interface.

• Journal of the Korean institute of surface engineering
• /
• v.48 no.6
• /
• pp.297-302
• /
• 2015

Nanocrystalline diamond(NCD) coated aluminium plates were prepared and applied as heat sinks for LED modules. NCD films were deposited on 1 mm thick Al plates for times of 2 - 10 h in a microwave plasma chemical vapor deposition reactor. Deposition parameters were the microwave power of 1.2 kW, the working pressure of 90 Torr, the $CH_4/Ar$ gas ratio of 2/200 sccm. In order to enhance diamond nucleation, DC bias voltage of -90 V was applied to the substrate during deposition without external heating. NCD film was identified by X-ray diffraction and Raman spectroscopy. The Al plates with about 300 nm thick NCD film were attached to LED modules and thermal analysis was carried out using Thermal Transient Tester (T3ster) in a still air box. Thermal resistance of the module with NCD/Al plate was 3.88 K/W while that with Al plate was 5.55 K/W. The smaller the thermal resistance, the better the heat emission. From structure function analysis, the differences between junction and ambient temperatures were $12.1^{\circ}C$ for NCD/Al plate and $15.5^{\circ}C$ for Al plate. The hot spot size of infrared images was larger on NCD/Al than Al plate for a given period of LED operation. In conclusion, NCD coated Al plate exhibited better thermal spreading performance than conventional Al heat sink.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.23 no.2
• /
• pp.86-92
• /
• 2013

$SF_6/O_2$ inductively coupled plasmas were employed to texture Si surface as a pretreatment for nanocrystalline diamond film growth. It was found that the $SF_6/O_2$ plasma texturing provided a very wide process window where normalized roughness values in the range of 2~16 could be obtained. Significantly improved nucleation densities of ${\sim}6.5{\times}10^{10}cm^{-2}$ compared to conventional mechanical abrasion were achieved after seeding for the textured Si substrate.