4.

Materials and Device Characterization

0156

IN-SITU HEATED DEPOSITION OF PARYLENE TO ENHANCE PORE

PENETRATION INTO PDMS
Dongyang Kang1, Sanae Matsuki2 and Yu-Chong Tai1
1
California Institute of Technology, USA
2
Northeastern University, USA

This paper presents a novel approach of implementing in-situ heating to facilitate the diffusion and penetration
of parylene coatings into PDMS, demonstrating enhanced pore sealing capability of parylene deposited at elevated
temperature.
In-situ heated deposition has proven useful to improve parylene-on-parylene adhesion[1], and has led to the
thorough investigation of deposition temperature effects on thermal, structural and mechanical properties of Parylene
C[2]. This pore-sealing feature of parylene deposition has also been used to coat porous materials to reduce gas or
moisture permeation. For examples, parylene-caulked PDMS was promising for long-term pneumatic balloon
actuator[3], and parylene coatings onto porous ultralow-k interlayer dielectrics was used to prevent precursor
penetration during subsequent metallorganic deposition[4]. However, these demonstrations only used parylene coated
at room temperature (RT). The hypothesis is that the surface mobility of parylene monomer is strongly dependent on
temperature so the pore sealing capability should be enhanced at elevated deposition temperature. This paper then
investigates the pore sealing capability of parylene at elevated deposition temperature, and for the first time, verifies
this by experiments.
We built a closed-loop temperature control system inside a parylene coater (SCS PDS 2035CR) as in Figure 1.
PDMS (Sylgard 184, Dow Corning) were molded in a small Petri dish and cured at 70C for 75 minutes. Parylene N,
C, D and HT (SCS products) were then coated on the PDMS for studies. Each parylene was first deposited at RT onto
three pieces of PDMS. Two of the three samples were then thermally annealed at 80C in convection oven for 8 hours,
and at 180C in vacuum oven (to prevent oxidation) for 8 hours, respectively. A fourth PDMS sample was then coated
with parylene by deposition at 80C. The parylene penetration profile into PDMS was then characterized using
secondary-ion-mass spectrometry (SIMS) (IMS 7f-GEO, CAMECA). SIMS sputter-etches the surface into the depth
and measures specific atomic species distribution simultaneously, therefore parylene depth profiling curves were
obtained (Figures 2 and 3). For mechanical adhesion tests, PDMS were spin-coated on silicon wafers and cured,
followed by Parylene C deposition at RT and at 85C, respectively. Then the samples were cut into 8mm wide strips
and mounted on a tensile testing machine (Q800, TA Instruments) to perform the 180 degree peeling tests (Figure 4).
The depth profiles from Figures 2 and 3 demonstrated that in-situ heating did significantly increase the
penetration depths of all parylene types except Parylene D. In addition, post-deposition thermal annealing also
promoted penetration, but only in a limited way. The adhesion strength can be evaluated using the equation =

/
[2 +
], where R is the adhesion strength, F the peeling force, w the width of the testing strips, and t and E the

2
thickness and Youngs modulus of parylene layer[5]. The ratio of the adhesion strength for deposition at 85C to that
at RT was found almost equal to the ratio of their peeling forces, around 1.6. The data support the hypothesis that insitu heated deposition is a very effective means to enhance the pore sealing capability of parylene deposition.
Finally, to produce visual evidence of enhanced parylene penetration for deposition at elevated temperature,
Parylene C films were deposited at RT and at 85C onto porous glass (Vycor 7930). The glass substrates were then
dissolved completely in buffered HF solution and the bottom sides (i.e., interface sides) of the Parylene C samples
were examined under scanning electron microscope (SEM) (ZEISS 1550VP). The SEM images in Figure 5 did verify
that much more densely packed Parylene C micro-structures were found for samples deposited at 85C than at RT.
Figure 6 then concludes our hypothetical molecular caulking mechanism at different temperatures.
Word count: 599
Submitting author: Dongyang Kang, California Institute of Technology, 1200 E. California Blvd., MC136-93,
Pasadena, CA 91125; Tel: +1-626-395-3885; E-mail: dkang@caltech.edu
References
[1] D. Kang, J. H. Chang, J. Y. H. Kim, and Y. C. Tai, NEMS 2012, pp. 226-229.
[2] D. Kang, A. Standley, J. H. Chang, Y. Liu, and Y. C. Tai, MEMS 2013, pp. 389-390.
[3] S. Sawano, K. Naka, A. Werber, H. Zappe, and S. Konishi, MEMS 2008, pp. 419-422.
[4] C. Jezewski, C. J. Wiegand, D. X. Ye, A. Mallikarjunan, D. L. Liu, C. M. Jin, et al., Journal of the Electrochemical
Society,151(2004), pp. F157-F161.
[5] K. Kendall, Journal of Physics D-Applied Physics, 8(1975), pp. 1449-1452.

Figure 1. Parylene CVD process with in-situ heating. The heater and
the thermocouple are placed inside the vacuum chamber, but
connected to the exterior components of the controller through
electrical feedthroughs.

1.61m PA-N
surface layer

(a)

1.41m PA-C
surface layer

(b)

(c)
(d)
Figure 3. Comparison of the SIMS depth profiling data for
conventional room temperature deposition, post-deposition thermal
annealing at 80C and 180C for 8 hours, and in-situ heated
deposition at 80C for each parylene. (a) Parylene N; (b)Parylene
C; (c) Parylene D; (d) Parylene HT.
~25m-thick and 8mm-wide
Parylene C surface layer

PDMS substrate
after top layer
Parylene C film
was peeled off

(a)
(b)
Figure 4. (a) A picture of a testing sample. Parylene C film is peeled
off from PDMS substrate at constant speed of 160m/min. (b) 180
peeling test curves for Parylene C prepared by conventional RT
deposition versus by in-situ heated deposition at 85C.

0.34m PA-HT
surface layer
0.21m PA-D
surface layer

(c)

(d)

Figure 2. SIMS data for the depth profiling of atomic species 12C,
28Si, 35Cl and 19F. Parylene N, C, D and HT were deposited into
PDMS at 80C. Note that 12C profile represents Parylene N (a), 35Cl
profile represents Parylene C (b) and Parylene D (c), and 19F profile
represents Parylene HT (d). 28Si represents PDMS.

(a)

(b)

Figure 5. SEM images of the released sides (i.e. the interface sides)
of Parylene C after the porous glass (Vycor 7930) was dissolved
completely in BHF. (a) Parylene C film deposited at RT, and (b) at
85C.

Figure 6: Hypothetical parylene caulking mechanism. (a) Substrate

porous material, such as porous glass and PDMS, (b) parylenecoated porous material, (c) RT CVD deposition, and (d) in-situ
heated deposition.