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Thin Solid Films 340 (1999) 1±6

Letter

Fabrication of diamond microstructures for microelectromechanical


systems (MEMS) by a surface micromachining process
Rajeshuni Ramesham
Jet Propulsion Laboratory, California Institute of Technology, 4800 Oak Grove Drive, M/S 125-152, Pasadena, CA 91109, USA
Received 30 July 1998; accepted 28 August 1998

Abstract
Selective polycrystalline diamond thin ®lm has been grown on a silicon dioxide/silicon substrate using high pressure microwave plasma-
assisted chemical vapor deposition from a gas mixture of methane and hydrogen at a substrate temperature of 9508C. A simple process ¯ow
has been developed to fabricate diamond microstructures such as diamond beams and cantilever beams using surface micromachining and
photolithography for the ®rst time. Scanning electron and optical microscopy has been used to characterize the surface micromachined
diamond microstructures. q 1999 Elsevier Science S.A. All rights reserved.
Keywords: Diamond; Microstructures; Beams; Bridges; Cantilever beams; Selective deposition

1. Introduction their process technology to fabricate the MEMS devices is


necessary for high temperature applications where silicon
Growth of polycrystalline diamond ®lms using micro- may not be applicable at temperatures greater than 1508C.
wave plasma-assisted chemical vapor deposition (CVD) MEMS devices may have a use in monitoring a wide variety
has received signi®cant interest in recent years for potential of parameters such as temperature, accelerations, ¯ow rates,
microelectromechanical (MEMS) applications since it has pressures, vibrations, surface wear rates, ¯uid contaminants,
unique chemical and physical properties. Diamond growth position sensing, etc.
at pressures of 10±760 Torr has been achieved by several A novel method was reported earlier to selectively
groups [1±6]. It is necessary to ultrasonically damage the deposit polycrystalline CVD diamond on a silicon surface
silicon dioxide/silicon substrate to enhance the nucleation and further demonstrated the fabrication of diamond micro-
density of diamond to achieve a pinhole-free continuous structures such as cantilever beams (single-side supported),
layer of diamond [7]. In order to facilitate application of bridges (double-side supported), and membranes (four-side
diamond ®lms for MEMS, a surface micromachining tech- supported) using anisotropic chemical etching of solution
nique has been developed for the ®rst time in this paper to [8]. This technique involves the protection of the silicon
fabricate diamond microstructures such as bridges and surface by using low pressure chemical vapor deposited
cantilever beams. (LPCVD) silicon nitride from attacking the front side of
MEMS is a microelectronics fabrication approach to the silicon wafer by hot KOH chemical solutions. The etch-
miniaturize the electromechanical sensor devices and inte- ing rate of silicon is , 1 mm/min in KOH solution at 608C.
grate with the integrated circuit (IC) fabrication processes. The method is relatively cumbersome such as cleaning the
MEMS devices may have a signi®cant application in auto- wax and any other masking materials, which are used to
motive, displays, printers, ¯uid thrusters, analytical instru- protect the silicon surface. The etching of silicon substrate
ments, communications, biomedical, and the aerospace in KOH solution is anisotropic in nature. Salvadori et al. [9]
industry. Operation, reliability, sensitivity, and stability of have reported the fabrication of free-standing diamond
smaller, lighter, and cheaper MEMS devices is very critical membranes using an `O' ring instead of mask materials.
in any chosen application, particularly under extreme shock This approach certainly does not allow the de®ned dimen-
and ambient temperature conditions. These MEMS devices sions of the microstructures for sensor applications. Nogu-
should be built in along with other semiconductor devices chi et al. [10] have reported the fabrication of diamond
using integrated semiconductor fabrication technologies. membranes using KOH solutions for X-ray lithography
New material such as silicon carbide and diamond and masks. Deng and Ko [11] have shown that the diamond-

0040-6090/99/$ - see front matter q 1999 Elsevier Science S.A. All rights reserved.
PII: S 0040-609 0(98)01370-4
2 R. Ramesham / Thin Solid Films 340 (1999) 1±6

low z. In contrast with wet bulk micromachining only the


wafer thickness limits the feature height.
Microscale movable mechanical pin joints, springs,
gears, sliders, sealed cavities, and many other mechanical
and optical components have been fabricated using surface
micromachining of poly-silicon. Analog devices have
commercialized ADXL-50, a 50-g accelerometer that was
developed using surface micromachining for activating air-
bag deployment. Texas Instruments' Digital Micromirror
Device is also based on surface micromachining.
In this paper, we describe a process ¯ow combined with
conventional photolithography and our technique of selec-
tive deposition of diamond over silicon dioxide/silicon
substrate to fabricate diamond beams and cantilever
beams for microelectromechanical device applications
using a surface micromachining approach. This is only
possible since we can grow diamond over the silicon diox-
ide/silicon substrate. We have used an approach of selective
Fig. 1. X-ray microfocus photograph of the diamond membranes over a
silicon substrate using reactive ion etching and an aluminum mask.

like carbon (DLC) may be used as friction-reducing coating


materials for MEMS applications. Houston et al. [12] have
reported the use of diamond-like carbon ®lm to passivate the
silicon surfaces to reduce stiction in microelectromechani-
cal devices. Stiction is one of the most dif®cult problems
that are being experienced by the MEMS research commu-
nity. Aslam and Schulz [13] have reported the selective
diamond nucleation technology employing electroplated
chromium as a mold during diamond deposition for micro-
electromechanical applications. Ramesham et al. [14] have
reported a process ¯ow combined with conventional photo-
lithography and reactive ion etching of silicon to fabricate
diamond membranes for MEMS applications. Fig. 1 shows
the microfocus X-ray photograph of diamond membranes
fabricated using this process such as bulk micromachining
process. To our knowledge there are no reports pertinent to
surface micromachining of diamond to fabricate diamond
microstructures for possible MEMS applications.

1.1. Surface micromachining

Bulk micromachining means that three-dimensional


features are etched into the bulk of crystalline and non-crys-
talline materials. In contrast, surface micromachined
features are built up, layer by layer, on the surface of a
substrate such as a single crystal silicon substrate. Dry etch-
ing or selective deposition de®nes the surface features in the
x±y plane and wet etching releases them from the plane by
undercutting.
The nature of the deposition processes involved deter-
mined the very ¯at surface micromachined features. The Fig. 2. Schematic diagram of the fabrication of diamond microstructures
low-pressure chemical vapor deposited polycrystalline (diamond beams and cantilever beams) for MEMS by selective diamond
diamond ®lms generally are only a few microns high with deposition and surface micromachining processes.
R. Ramesham / Thin Solid Films 340 (1999) 1±6 3

Fig. 3. Scanning electron micrographs of (a) morphology of the diamond thin ®lm, (b) typical morphology of the backside of the fabricated diamond ®lm with
a cross-section and (c) backside of the diamond morphology with the diamond ®lm not completely covering the silicon substrate.

deposition of diamond over silicon dioxide/silicon substrate damaged by ultrasonic agitation for 15±60 min in metha-
to fabricate diamond microstructures for the ®rst time to nol containing diamond particles. The ultrasonically
achieve a possible enhancement in the yield of diamond damaged SiO2 was then photolithographically patterned
MEMS devices. and partially chemically etched in the opening of the
photoresist using a solution of buffered oxide etch
(BOE) in order to smooth the surface so that no diamond
2. Experimental growth would result. The photoresist was removed with a
commercial stripper solution, and the resist residue was
A commercially available microwave plasma-assisted
removed with a commercial stripper solution, and the
CVD system (ASTeX, Woburn, MA) was used in our
resist residue was removed with oxygen plasma (¯ow
experiments to grow polycrystalline diamond thin ®lms.
rate: 40 sccm, 300 W, 1±2 min).
The schematic diagram of the polycrystalline diamond
² The silicon dioxide was photolithographically patterned
growth system and growth process details are described in
and hard baked with the photoresist at 150±2008C for 1±2
earlier publications.[7,8,15±17].
h. The sample was ultrasonically agitated for 15±60 min
Starting substrates were mirror-smooth ®nished n- or p-
in methanol containing diamond particles and the photo-
type, (100) oriented single crystal silicon wafers with a
resist was stripped with commercial stripper solution.
resistivity of , 20 V cm. Cleaned silicon wafers were
The substrate was eventually cleaned in an oxygen
thermally oxidized to a thickness of 1±1.5 mm. Selectivity
plasma (¯ow rate: 40 sccm, 300 W, 1±2 min). This
of diamond thin ®lms on silicon dioxide was achieved by the
approach resulted in selectively damaged patterns of sili-
following two distinct processes described below.
con dioxide so as to yield diamond growth only there.
² The complete surface of the oxidized silicon wafer was
4 R. Ramesham / Thin Solid Films 340 (1999) 1±6

Fig. 4. Scanning electron micrographs of (a) top view of diamond bridge, (b) top view of diamond cantilever beam and (c) backside of diamond ®lm membrane
fabricated using anisotropic chemical etching of the silicon substrate.

The wafers were cleaned in acetone, methanol, deionized graphy, and ®nally developed the photoresist using devel-
(DI) water, and dried with nitrogen gas. A continuous ®lm oper solution. Finally, the patterned diamond/silicon
of polycrystalline diamond was usually obtained after 15± dioxide/silicon substrate was hard baked at 110±1208C for
20 h of growth. The growth rate of microwave plasma CVD 15± 20 min and buffer oxide etched (NH4H 1 HF) the
diamond is typically 1 mm/h. The typical deposition para- silicon dioxide, which is called a surface micromachining
meters were as follows: substrate temperature 9508C, process, to yield diamond microstructures. Fig. 2 shows the
methane ¯ow rate 3.6 sccm, hydrogen ¯ow rate 500 sccm, schematic diagram of the process ¯ow steps to fabricate the
deposition pressure 45 Torr (5:985 £ 102 kPa), forward diamond microstructures for MEMS by selective diamond
power 1200 W, re¯ected power 34 W, and the percent of deposition over silicon dioxide/silicon substrate and surface
methane in hydrogen 0.71%. Films grown under these micromachining of the silicon dioxide process using BOE.
conditions have been analyzed earlier by Raman spectro-
scopy and X-ray diffraction and they were con®rmed to be
diamond [16]. The X-ray microfocus photograph shown in 3. Results and discussion
Fig. 1 clearly demonstrates the transparency of diamond for
X-rays [18]. Fig. 3a is a SEM micrograph showing a typical morphol-
The silicon dioxide/silicon substrate was cleaned thor- ogy of as-grown diamond ®lm on a silicon substrate. The
oughly with various solvents after the selective CVD diamond morphology was found to be very good as we have
diamond growth over the silicon dioxide. The substrate reported earlier in the literature [7,8,15±17]. Our objective
was baked at 175±2008C for 15±20 min and later spin coated in this paper is to propose a method and demonstrate how to
the adhesion promoter and subsequently spin coated thick fabricate diamond microstructures using a surface microma-
photoresist (AZ products). The substrate was soft baked for chining process. Fig. 3b shows the scanning electron micro-
30 min, patterned the photoresist using optical photolitho- graph of the cross-section of diamond ®lm and its
R. Ramesham / Thin Solid Films 340 (1999) 1±6 5

Fig. 5. Optical photographs of the diamond beams and diamond cantilever beams fabricated using selective diamond deposition and subsequent surface
micromachining processes.

morphology on the backside of diamond thin ®lm. It is clear micromachining of silicon. Therefore, we have proposed a
from Fig. 3b that the scratch pattern was replicated over the surface micromachining process to fabricate diamond
back of the diamond thin ®lm. Scratch damage on the silicon microstructures such as beams and cantilever beams and
substrate was necessary to enhance the nucleation of not for membranes. This was only possible since we could
diamond. Fig. 3c shows the scanning electron micrograph grow diamond selectively over the thermally grown silicon
of the backside of the diamond ®lm morphology where the dioxide/silicon substrate [7].
diamond ®lm was not nucleated over the silicon substrate Fig. 5a,b shows the optical photographs of the selective
uniformly. Discontinuities in the diamond ®lm are very diamond grown over the silicon dioxide/silicon substrate
clear from Fig. 3c. This suggest an improvement in the and diamond microstructures such as beams and cantilever
surface pretreatment to enhance the nucleation density of beams obtained via the surface micromachining process.
diamond. The diamond cantilever beam may be seen on the extreme
Fig. 4a±c shows the scanning electron micrographs of the left of Fig. 5a. Fig. 5b is the magni®ed view of Fig. 5a in the
diamond microstructures such as beam, cantilever beam, diamond beam area. The edge of the silicon dioxide after
membranes, fabricated using selective diamond deposition BOE etching to release the diamond microstructures is clear
and bulk micromachining of silicon substrate. The technical from Fig. 5b. We have only shown proof of the concept to
details to fabricate the diamond microstructures are fabricate diamond microstructures for possible MEMS
provided in an earlier publication [8]. This approach is applications using the surface micromachining process
very good only when bulk micromachining is needed to and to our knowledge this is the ®rst report.
fabricate diamond microstructures. This is a very laborious
approach to fabricate microstructures for microsensors.
Black wax was used to mask the front or diamond side of 4. Summary
the silicon wafer and silicon nitride was used as a mask to
etch the silicon on the backside of the wafer to yield A process has been developed and demonstrated to fabri-
diamond microstructures. Cleaning the black wax is a cate polycrystalline diamond beams and cantilever beams
very dif®cult task and will reduce the yield substantially. on a silicon dioxide/silicon substrate using selective
The presence of small particles is very clear from Fig. 4a,b. diamond deposition and a surface micromahining process.
These microstructures were cleaned thoroughly. The Buffered oxide (BOE) etch has been used to etch silicon
diamond membrane is very clean since this micrograph dioxide under the selectively deposited polycrystalline
was taken from the backside of the membrane. In principle, diamond to yield diamond microstructures. This is the ®rst
it is possible to make diamond microstructures using bulk report of fabricating the diamond microstructures using
6 R. Ramesham / Thin Solid Films 340 (1999) 1±6

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