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<strong>Dow</strong> Corning Proprietary<br />

Revised April, 2004<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong><br />

Photodefinable Spin-On<br />

Silicone<br />

Properties and Processing Procedures<br />

Introduction<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> is a silicone<br />

formulation which can be photopatterned<br />

and cured using standard microelectronics<br />

processing techniques. The silicone material<br />

is prepared in mesitylene with a solution<br />

viscosity of 450 cP. The standard method for<br />

application of <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> is<br />

by spin coating although other methods of<br />

application (such as spray coating and<br />

extrusion coating) may also be applicable.<br />

Application, patterning and cure of <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> is accomplished in a<br />

simple six-step process that utilizes<br />

commercially available equipment. Updated<br />

information on the processing of the <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> materials is available<br />

from your local <strong>Dow</strong> Corning<br />

representative.<br />

Material Properties<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> can be solvent cast<br />

to form free standing monoliths or spincoated<br />

onto substrates to form sub 50 µm<br />

thick films. The mechanical properties of<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> thin film (20 µm)<br />

and bulk samples (~ 2 mm thickness) are<br />

listed in Table 1 for samples cured at 250°C<br />

for 30 minutes.<br />

The room temperature modulus of <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> has been measured by a<br />

continuous stiffness (CSM) nanoindentation<br />

technique on spin-coated thin films. Figure 1<br />

shows a typical modulus vs. displacement<br />

curve for a 20 µm thick film of <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> cured at 250°C for 30<br />

minutes. The plot shows the change in the<br />

modulus as the indenter tip penetrates into<br />

the film surface up to a maximum<br />

penetration depth of 2200 nm.<br />

Modulus (GPa)<br />

1<br />

Mechanical Property Value<br />

Nanoindentation Modulus (MPa) 301<br />

Nanoindentation Hardness<br />

(MPa)<br />

9.5<br />

Film Residual Stress on Si<br />

Wafer (MPa)<br />

2.6<br />

Bulk Modulus (MPa at 25°C) 160<br />

Bulk Tensile Strength (MPa) 6.0<br />

Bulk Elongation (%) 37.6<br />

CTE (ppm/°C) 236<br />

Table 1. Mechanical properties of <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong>.<br />

0.8<br />

0.7<br />

0.6<br />

0.5<br />

0.4<br />

0.3<br />

0.2<br />

0.1<br />

0<br />

0 500 1000 1500 2000 2500<br />

Displacement Into Surface (nm)<br />

Figure 1. Modulus vs. displacement curve<br />

for <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> (frequency =<br />

75 Hz).<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> provides a low<br />

modulus, low stress film after cure with a<br />

film surface modulus of approximately 300<br />

MPa. The increase in modulus with indenter<br />

displacement into the film is due an<br />

increasing substrate effect with penetration.<br />

The dimensional change of <strong>Dow</strong> Corning ®<br />

<strong>WL</strong>-<strong>5150</strong> as a function of temperature is<br />

shown in Figure 2. A linear expansion is<br />

observed throughout the temperature region<br />

of –100 to 300°C.<br />

The thermal stability characteristics of <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> cured at 250°C for 30<br />

minutes are listed in Table 2. Good thermal<br />

stability and modulus retention have been<br />

demonstrated to a temperature of 300°C.


<strong>Dow</strong> Corning Proprietary<br />

Revised April, 2004<br />

Dimension Change (µm/m)<br />

1e+5<br />

8e+4<br />

6e+4<br />

4e+4<br />

2e+4<br />

0<br />

-100 -50 0 50 100 150 200 250 300<br />

Figure 2. Dimension change vs. temperature<br />

for <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong>.<br />

Condition Weight Loss (%)<br />

Isothermal at<br />

1.9<br />

250°C/60 minutes<br />

Isothermal at<br />

3.5<br />

300°C/60 minutes<br />

Dynamic to 250°C<br />

1.0<br />

(10°C/minute)<br />

Dynamic to 300°C<br />

1.7<br />

(10°C/minute)<br />

Table 2. Thermal stability characteristics for<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong>.<br />

The weight loss profile for <strong>Dow</strong> Corning ®<br />

<strong>WL</strong>-<strong>5150</strong> is shown in Figure 3 for a sample<br />

cured at 250°C for 30 minutes.<br />

Weight Percent Remaining<br />

102<br />

100<br />

98<br />

96<br />

94<br />

92<br />

90<br />

88<br />

86<br />

84<br />

82<br />

80<br />

0<br />

0 20 40 60 80 100 120<br />

Time (minutes)<br />

600<br />

500<br />

400<br />

300<br />

200<br />

100<br />

Figure 3. Thermal weight loss for a<br />

250°C/30 minute cured <strong>Dow</strong> Corning ® <strong>WL</strong>-<br />

Temperature (°C) (°C)<br />

Percent Transmittance<br />

Cured films of <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong><br />

show excellent optical transparency down to<br />

a wavelength of 220 nm. The UV-visible<br />

spectrum for a 24 µm thick 250°C cured<br />

film on a quartz substrate is shown in Figure<br />

4.<br />

The electrical properties and moisture<br />

absorptivity for <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong><br />

are listed in Table 3.<br />

100<br />

90<br />

80<br />

70<br />

60<br />

50<br />

40<br />

30<br />

20<br />

10<br />

0<br />

100 200 300 400 500 600 700 800 900<br />

Wavelength (nm)<br />

Figure 4. UV-visible spectrum for a cured<br />

film of <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong>.<br />

Electrical Property Value<br />

Dielectric Constant (1 MHz) 3.2<br />

Dissipation Factor (1 MHz) 0.007<br />

Leakage Current (A/cm 2 ) 1 x 10 -11<br />

Breakdown Voltage (V/cm) 3.9 x 10 5<br />

PCT Moisture Absorption (%) 0.24<br />

Table 3. Electrical properties and moisture<br />

absorptivity for <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong><br />

measured on monolithic specimens.<br />

Material Shipping and Storage<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> is shipped cold<br />

with blue ice at a temperature of<br />

approximately 5°C. If the solution arrives at<br />

its destination warm please contact your<br />

local <strong>Dow</strong> Corning representative. Upon<br />

receipt the solution should be immediately<br />

stored at a temperature of –15°C. Prior to<br />

use the solution should be allowed to<br />

equilibrate to room temperature.<br />

<strong>5150</strong> sample analyzed under helium. During use <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> should<br />

not be allowed to remain at room<br />

2


<strong>Dow</strong> Corning Proprietary<br />

Revised April, 2004<br />

temperature for more than 3-4 days to<br />

maintain good performance.<br />

Material Waste Handling<br />

In disposing of <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> or<br />

rinse and developing solvents containing<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> it is important that<br />

these do not come into contact with basic<br />

materials (including ammonia, alkyl amines,<br />

ammonium hydroxides, alkyl ammonium<br />

hydroxides, metal hydroxides) as well as<br />

oxidizing metals and oxidizing agents.<br />

These in combination with water can result<br />

in the evolution of hydrogen gas from the<br />

composition. Consult the MSDS provided<br />

for additional information on materials<br />

waste handling.<br />

Processing<br />

A step-by-step summary of processing for<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> is presented<br />

schematically in Figure 5 and in Table 4.<br />

1<br />

Spin Coat<br />

2<br />

Soft Bake<br />

3<br />

UV Exposure<br />

4<br />

Post Exposure Bake<br />

5<br />

Solvent Develop<br />

6<br />

Hard Bake (Cure)<br />

Figure 5. Application, patterning and cure<br />

process steps for <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong>.<br />

3<br />

The process consists of six general process<br />

steps to arrive at a cured patterned film. The<br />

target thickness is approximately 22 µm.<br />

Process Step Standard Conditions<br />

1. Spin Coat<br />

a) Spread<br />

b) Spin<br />

c) Edge Bead<br />

500 rpm/10 sec.<br />

500-2500 rpm/30 sec.<br />

1500 rpm/30 sec.<br />

2. Soft-bake Hot Plate<br />

110°C/120 seconds<br />

3. UV Exposure i-line or Broadband<br />

1000 mJ/cm 2<br />

4. Post-exposure<br />

Hot Plate<br />

Bake<br />

150°C/120 sec.<br />

5. Development Stoddard Solvent<br />

Automated<br />

Development Process<br />

(see Step 5 comments)<br />

6. Hard Bake Oven (Air, N2 or<br />

vacuum)<br />

150°C/120 min. or<br />

180°C/60 min. or<br />

250°C/30 min.<br />

Table 4. Processing conditions for <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong>.<br />

Step 1. Coating Process<br />

Surfaces for coating <strong>Dow</strong> Corning ® <strong>WL</strong>-<br />

<strong>5150</strong> should be free of surface impurities<br />

prior to coating. It is recommended that the<br />

spin-coaters used to deposit the solutions be<br />

equipped with a backside rinse capability<br />

and bowl exhaust. The coater should also be<br />

equipped with two dispense heads, one for<br />

dispensing <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> and a<br />

second for dispensing a solvent for edge<br />

bead removal.<br />

Depending on the size of the substrate<br />

approximately 8-10 mL of <strong>Dow</strong> Corning ®<br />

<strong>WL</strong>-<strong>5150</strong> is applied to a wafer in either<br />

static or dynamic dispense modes. The<br />

wafer speed is then set to 500 rpm for 10<br />

seconds to allow the solution to spread<br />

across the wafer. The speed is then increased<br />

to achieve a uniform film coating across the<br />

wafer. A speed of 1500 rpm is<br />

recommended to achieve a film thickness of


<strong>Dow</strong> Corning Proprietary<br />

Revised April, 2004<br />

approximately 22 µm after full processing<br />

(completion of steps 1-6). Expansion of the<br />

spin speed range between 500 and 3000 rpm<br />

allows for final fully processed film<br />

thicknesses ranging from 40 to 15 µm<br />

respectively. During the spin step it is<br />

recommended that a backside rinse be<br />

implemented to eliminate polymer string<br />

(cotton candy) formation at the wafer edge.<br />

Edge bead removal is conducted by spinning<br />

the wafer at speeds not faster than the spinon<br />

speed and applying mesitylene or a<br />

Stoddard type of solvent (such as Air<br />

Products Negative Resist Developer ® ) to the<br />

topside of the wafer to remove the bead<br />

formed at the wafer edge. The solvent can<br />

be applied using a dispenser or manually by<br />

syringe.<br />

Step 2. Soft-bake<br />

After coating, the film produced from <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> is subjected to a low<br />

temperature bake to remove residual solvent.<br />

The standard process is to heat the wafer on<br />

a hotplate to a temperature of 110°C for a<br />

period of 2 minutes. After the soft-bake the<br />

film will remain tacky; however, the<br />

tackiness can be reduced by further heating<br />

the film on a hotplate at a temperature of<br />

110°C for up to 5 minutes.<br />

It may be desirable to perform an oven<br />

rather than hotplate soft-bake. Any oven<br />

process will need to be optimized to the<br />

equipment used. If such an approach is used<br />

it is important that the coatings remain in a<br />

horizontal rather than vertical orientation to<br />

avoid a downward flow of the material on<br />

the substrate.<br />

Step 3. UV Exposure<br />

UV-light exposure of films prepared from<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> causes the<br />

activation of a photo-sensitive compound in<br />

the formulation that results in selective<br />

cross-linking (setting) of the UV-light<br />

exposed regions during the post-exposure<br />

bake (Step 4). As the photoactivation and<br />

subsequent cross-linking takes place in the<br />

light exposed regions, dissolution and<br />

4<br />

removal of the non-cross-linked regions in<br />

Step 5 results in a negative image of the<br />

original photomask. Films prepared from<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> can be exposed to<br />

patterned UV-light using a mask aligner or a<br />

stepper. Due to the surface tackiness of the<br />

films after soft-bake direct contact of the<br />

films with the UV exposure equipment<br />

components must be avoided. For UV-light<br />

exposure using a mask aligner a typical<br />

proximity gap of 20-40 µm is used. It is<br />

recommended that the UV-light exposure be<br />

conducted using either i-line or broadband<br />

radiation. The sensitivity of the films to g-<br />

and h-line radiation is low and exposure at<br />

these wavelengths is not recommended. The<br />

standard dose of broadband UV-light from a<br />

medium pressure Hg lamp for films with a<br />

thickness of 15 to 40 µm is 1000 mJ/cm 2 .<br />

Doses in the range of 600 to 1000 mJ/cm 2<br />

can be used but may result in slightly<br />

reduced film retention. Exposure to doses<br />

lower than 600 mJ/cm 2 will result in low or<br />

no film retention.<br />

Step 4. Post-Exposure Bake<br />

Following Step 3 it is necessary to subject<br />

the film to a post UV-light exposure bake.<br />

Omitting this step will result in the complete<br />

removal of both the irradiated and nonirradiated<br />

portions of the film during the<br />

development step. It is during this step that<br />

the UV-light irradiated portions of the film<br />

undergo a cross-linking process rendering<br />

those areas insoluble in the developing<br />

solvent. The standard condition for the postexposure<br />

bake is placement of the substrate<br />

onto a hotplate at 150ºC for a period of at<br />

least 90 seconds and not exceeding 180<br />

seconds. The standard hot-plate exposure is<br />

150ºC for 120 seconds. Exposure of the film<br />

to a temperature of 150ºC for periods longer<br />

than 180 seconds can result in a significant<br />

increase of film residue (scumming) in the<br />

non-exposed regions. Exposure at 150ºC for<br />

periods less than 90 seconds can result in<br />

insufficient cross-linking and a significant<br />

reduction in the final film thickness after<br />

development.


<strong>Dow</strong> Corning Proprietary<br />

Revised April, 2004<br />

Step 5. Development<br />

The solvent used to develop the negative<br />

image in the film is a Stoddard type of<br />

solvent such as Negative Resist Developer ®<br />

(NRD) that is available from Air Products.<br />

This solvent can be used as both developer<br />

and rinse solvent (Step 1). Alternatively,<br />

mesitylene has also shown to be a good<br />

development solvent for <strong>Dow</strong> Corning ®<br />

<strong>WL</strong>-<strong>5150</strong>. After the post UV-light exposure<br />

bake (Step 4), the negative image pattern<br />

can be developed by the following process<br />

using an automated coater with two dispense<br />

heads, one for NRD and one for IPA:<br />

1. 15-second static dispense of NRD to coat<br />

the wafer.<br />

2. 10 second dynamic dispense (200 rpm)<br />

of NRD to rinse wafer.<br />

3. 60 second NRD puddle.<br />

4. 10 second NRD dynamic rinse at 500<br />

rpm.<br />

5. 10 second NRD dynamic rinse at 1000<br />

rpm.<br />

6. 10 second IPA dynamic rinse at 1000<br />

rpm.<br />

7. 30 second spin dry at 3000 rpm.<br />

During development a portion of material in<br />

the exposed regions is removed in addition<br />

to the non-irradiated regions. This results in<br />

the post-developed film having a final<br />

thickness less than the original thickness<br />

achieved after the soft-bake step. The<br />

percentage of the final film thickness<br />

relative to the thickness after the soft-bake<br />

step (Step 2) is referred to as the film<br />

retention. The film retention for fully<br />

processed (Steps 1-6) films from <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> is in the range of 80 to<br />

90 percent with the higher values obtained<br />

for the thicker films.<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> is an organic<br />

solvent developable film. Water or aqueous<br />

alkali types of developers cannot be used.<br />

Step 6. Hard Bake<br />

The objective of the hard bake is to<br />

complete the film cure process resulting in<br />

5<br />

CSM Modulus (MPa)<br />

maximization of the cure level and<br />

mechanical properties. Curing of <strong>Dow</strong><br />

<strong>Corning®</strong> <strong>WL</strong>-<strong>5150</strong> films is a result of an<br />

addition cure mechanism that does not<br />

involve the evolution of cure by-products.<br />

This feature results in negligible shrinkage<br />

(~ 2%) and low stress after cure. The<br />

standard cure process for <strong>Dow</strong> <strong>Corning®</strong><br />

<strong>WL</strong>-<strong>5150</strong> films is 250ºC for 30 minutes in<br />

an oven. The cure atmosphere can be air,<br />

nitrogen or vacuum. No heating or cooling<br />

ramps are necessary to bring the films to the<br />

cure temperature. Films can also be cured at<br />

a temperature of 180ºC for 60 minutes. The<br />

final modulus as a function of cure condition<br />

is shown in Figure 6 for 250ºC/30 minute<br />

and 180ºC/60 minute cures and well as a<br />

third condition of 180ºC/60 minutes<br />

followed by 3 excursions to 260ºC for 1<br />

minute each.<br />

400<br />

300<br />

200<br />

100<br />

0<br />

250°C/<br />

30 min<br />

180°C/<br />

60 min<br />

180°C/1 hr +<br />

3 x 260°C/1 min.<br />

Figure 6. CSM modulus against cure<br />

condition for <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong><br />

films.<br />

Lithographic Process Performance<br />

The lithographic performance for fully<br />

processed 20 µm thick films of <strong>Dow</strong><br />

Corning ® <strong>WL</strong>-<strong>5150</strong> is summarized in Table<br />

5. The results were generated for films<br />

processed using a mask aligner and standard<br />

process conditions for steps 1 through 6.<br />

Key performance features include good<br />

resolution down to 15 µm sized pads, a<br />

sidewall slope of 60º and minimal shrinkage<br />

during cure.


<strong>Dow</strong> Corning Proprietary<br />

Revised April, 2004<br />

Process Property Value<br />

Film Thickness Range 15 to 40 µm<br />

Minimal Feature Size 15 µm<br />

Aspect ratio (ht/w)


<strong>Dow</strong> Corning Proprietary<br />

Revised April, 2004<br />

films cured at 180°C for 1 hour can be<br />

removed by immersion for approximately 40<br />

minutes, and films cured at 250°C for 30<br />

minutes can be removed by immersion for<br />

approximately 90 minutes. Following film<br />

removal, the substrate should be washed<br />

with IPA and water.<br />

<strong>Dow</strong> Corning ® <strong>WL</strong>-1975 cannot be used as<br />

a developing solvent for Step 5 as it will<br />

remove the entire film.<br />

Rework of <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong> films<br />

can results in the evolution of trace amounts<br />

of hydrogen gas requiring good ventilation<br />

for processing. Please consult the MSDS<br />

provided with <strong>Dow</strong> Corning ® <strong>WL</strong>-1975 for<br />

additional details.<br />

Plasma and Reactive Ion Etch Processing<br />

Films derived from <strong>Dow</strong> Corning ® <strong>WL</strong>-<br />

<strong>5150</strong> contain silicone and as a result are<br />

sensitive to O2 and air plasmas. Excessive<br />

exposure to these plasmas may cause the<br />

films to crack. O2 and air plasmas at low<br />

exposure dose may be used to increase the<br />

surface energy of the films to improve the<br />

adhesion and wettability to other electronics<br />

materials.<br />

Following processing and cure,<br />

films derived from <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong><br />

may leave a small amount of polymer<br />

residue on the surface of the developed<br />

regions of the substrate. This residue is not<br />

visible to the eye and is typically less than<br />

2000 Å thick. To remove this unwanted<br />

material a reactive ion etching process may<br />

be used. As <strong>Dow</strong> Corning ® <strong>WL</strong>-<strong>5150</strong><br />

contains silicone it is not desirable to use a<br />

pure O2 etch. An etching gas combination of<br />

SF6/O2 is recommended with an optimum<br />

SF6 level of 50 percent. After SF6/O2 etch, a<br />

water wash is recommended to avoid<br />

contamination of the substrate. Additionally,<br />

CF4/O2 gas systems have been demonstrated<br />

as an effective etch system. Please ask your<br />

local <strong>Dow</strong> Corning representative for the<br />

latest detailed results in etching processes.<br />

7

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