Spherical Boron Nitride Fillers For High Performance Thermal Greases

Arun Gowda*, Sara N. Paisner, and Sandeep Tonapi

GE Global Research Center
One Research Circle, Niskayuna, NY 12309.
*gowda@research.ge.com
Paulo Meneghetti, Paul Hans, and Gregory Strosaker
GE Advanced Ceramics
22557 West Lunn Road, Strongsville, OH 44149.
Ashwini Acharya, Kaustubh Nagarkar, and K. Srihari
Electronics Manufacturing and Research Services
Department of Systems Science and Industrial Engineering
State University of New York at Binghamton, Binghamton, NY 13902.

Abstract conventional single crystal hexagonal BN, the agglomerates

Highly efficient thermal interface materials (TIMs) have are more isotropic in nature. To illustrate this, silicone-based
become necessary to effectively manage the increasing heat thermal pads with 40 volume percent (vol%) of hexagonal
generated at the silicon level with every new generation of BN and with 40 vol% of spherical BN were fabricated and
microprocessors. Typically, TIMs consist of polymers that their thermal conductivities compared using a laser flash
are highly loaded with thermally conductive fillers. Boron thermal diffusivity instrument. Thermal pads with
nitride (BN) fillers have been employed as a thermal hexagonal BN showed an in-plane thermal conductivity of
conductive filler for TIMs for decades. However, 5.7 W/mK and a through-plane conductivity of 0.8 W/mK,
conventional boron nitride fillers were largely anisotropic in while pads with spherical BN showed an in-plane thermal
nature. A novel spherical BN filler is presented as an conductivity of 6.4 W/mK and a through-plane conductivity
isotropic thermally conductive filler for TIMs and the of 6.4 W/mK. Such isotropic spherical BN are studied in
thermal and reliability performance characteristics of this paper, which focuses on their application in thermal
spherical BN filled high thermal performance greases will greases. Different spherical BN fillers were incorporated
be described. into silicone resins to form thermal greases. The thermal and
reliability performance of these greases were characterized
1. Introduction using a laser flash thermal diffusivity instrument and
Typical fillers for thermal interface materials (TIMs) different accelerated reliability tests. A discussion of the
include a variety of metal and ceramic fillers. Depending on characteristics of thermal greases using spherical BN fillers
the type of application, an electrically insulating (ceramic) is presented in this paper.
or electrically conducting (metallic) filler is utilized in the
TIM. Alumina, zinc oxide, and boron nitride are typical
ceramic fillers, while silver and aluminum are the
predominant metallic fillers used in TIMs. Table I provides
a comparison of the representative properties of different
fillers for TIMs - boron nitride (BN), aluminum nitride
(AlN), alumina (A1203), silica (NiO2), zinc oxide (ZnO),
nermal Conductivity 300 260 30 1.4 54 430 235
w/m-&)
V
silver (Ag), and aluminum (Al) [1,2]. Dielectric Constant 3.9 8.8 9.7 3.8 9.9
Single-crystalline hexagonal boron nitride (BN) is the
typical BN filler used in TIMs. Heat is transported through Volume Resistivity 1 -+15 io+14 io+14 1o0+4 10+7 10-6 0o-6
boron nitride by phonons. A perfect BN crystal possesses (ohm-cm) __
two principal conductivities - one, parallel to the hexagonal Coefficient of <1 4.4 6.7 0.5 0.7 19 23
axis and the other, the basal plane conductivity, Expansion (ppm/K) <1 . . . I 92
perpendicular to this axis. Thermal conductivity in the plane Knoop Hardness 1 1 1200 1500 500 387 260 180
parallel to the hexagonal axis is much greater than the
thermal conductivity along the perpendicular axis. When Specific Heat (J/kg-K 794 734 798 689 523 235 900
highly filled into polymers to form TIMs, the BN platelets 250C)
typically orient themselves such that the high thermal Theoretical Density 2.25 3.26 3.98 2.2 5.64 10.5 2.7
conductivity plane is perpendicular to the ideal heat transfer (g/cc)
path. This results in a system that does not fully utilize the wote: Ine values shown in the table are approximations based on available
AT, .0

inherent high thernal conductivity of BN. data from various sources and may vary from actual performance
In this paper, a unique spherical agglomerate of boron depending on variables in composition, processing, etc.
nitride crystals is studied as a filler for TIMs. Compared to

0-7803-9578-6/05/$20.00 .2005 IEEE 683 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.
2. Spherical Boron Nitride Filler 3. Experimental Details
There have been few attempts to produc e spherical BN
powder. Since the morphology of BN is inherently Spherical BNgreaseformulations
hexagonal, spherical particles have to be produced via Thermal greases containing different loadings of the four
secondary processing of BN platelets. Glei man et. al. [3] spherical BN fillers (Table II) were formulated in a 1000 cP
synthesized spherical BN by melting BN iri a microwave- silicone resin. Loading levels ranging from 10 weight
powered, atmospheric pressure nitrogen plasma. Lodyga et percent (wt%) to approximately 50 wt% were tested. The
al. [4] prepared spherical shape BN bound together by an thermal performance (in-situ thermal conductivity and
-al
organic binder via spray drying. Such spherit BN particles
were utilized in grease formulations and th eir thermal and
thermal resistance) was measured for each grease
formulation.
reliability characteristics are also reported hearein. Thermalperformance measurement ofgreases
Table II gives the details of the four sphe !rical
that were utilized. Two different partic le sizes were
BN fillers A laser flash thermal diffusivity instrument was utilized
to measure the in-situ thermal performance of the grease
primarily studied - 55-65 micron BN (PT) C60)
micron BN (PTX25). A coating was also applied on the
and 25-30 layers. Fixtures were developed that enabled the testing of
the greases between two interfaces under a load. The laser
surface of PTX60 and PTX25 fillers to obta in PTX60S and flash thermal diffusivity method and the grease fixture are
PTX25S. The coating promotes the interacti on between the described below.
filler and resin systems, leading to reduced' viscosities. Fig. The in-situ, or effective thermal resistance ofthe greases,
1 and Fig. 2 show representative Scai
Microscopy (SEM) images of PTX60 ani I PTX25. The mning Electron was measured using a three-layer 'sandwich' sample. The
grease was applied between two 8 mm x 8 mm substrate
lower particle size of PTX25 enables th inner bondline coupons (silicon, aluminum) to obtain an aluminum-grease-
thicknesses in TIMs. silicon sandwich. The aluminum coupon that represents the
heat sink material had a gold chromate conversion layer on
idied the surface. The unpolished backside of the silicon was
ice Sur1
7 il placed in contact with the grease. The three-layer samples
were coated with graphite before placing them into the
Coating sample holder of the laser flash thermal diffusivity
PTX60 55-65 20/90 0.4 5. 5 one
None equipment. A specific pressure was then applied on the
grease layer. One side of the sample was subjected
PTX25 25-30 10 /40 0.3 7 None uniformly to a single flash from a laser. The thermal
PTX60S 55-65 20/90 0.4 5. 5 S-Coating response of the opposite side of the sample was monitored
PTX25S 25-30 10/ 40 0.3 7 -S-Coating using a liquid nitrogen-cooled InfraRed (IR) detector. From
the measured time response, the thermal diffusivity of the
sample can be calculated [5,6]. For additional information
on the laser flash thermal diffusivity method, refer to
[5,6,7,8]. Fig. 3 is a schematic of the laser flash thermal
diffusivity instrument. For a known bondline thickness
(BLT), the thermal diffusivity of the TIM layer is extracted
from the apparent diffusivity (diffusivity of the sandwich).
This is possible, since the thermal properties (specific heat
capacity and thermal diffusivity) and the densities of the
other layers can be measured independently. A software
macro associated with the laser flash diffusivity system
determines the total thermal resistance of the grease layer,
Fig. 1: SEM image of PTX60 spherical BN agglomertes using a method developed by Lee [8]. The thermal
resistance determnined using this method includes the bulk
(intrinsic) thermal resistance of the grease and the contact
resistances at the grease-substrate interfaces.
Shown in Fig. 4 is a schematic of the fixture that was
utilized for thermal performance measurements using the
laser flash thermal diffusivity instrument. The sample holder
can be removed from the laser flash diffusivity instrument
and subjected to reliability tests, thus enabling the samples
to be un-disturbed between thermal measurements before
and after reliability testing. Different pressures can be
Fig. 2: SEM image of PT applied on the grease layers by varying the torque applied to
agglomerates the bolts.

684 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.
 grease layers and significantly reduce test times. Several
LN2 Cooled accelerated tests for thermal greases have been reported in
IR Detector the literature [11]. Three types of reliability tests were
performed in the current research - air-to-air thermal
cycling, high temperature storage, and mechanically induced
pump-out. Table III gives the conditions for the reliability
tests that were performed.
Sample
For thermal cycling and high temperature storage tests,
the grease fixture shown in Fig. 4 was utilized to measure
_ Laser Optics the thermal performance of the greases before and after
reliability testing. The thermal cycling was performed for
t Laser Flash 1000 cycles using a -50 to 150°C, 20 minute thermal cycle.
High temperature storage was performed at 150°C for 200
Fig. 3: Laser flash setup for diffusivity measurements hours.

F F

3-lae Thermal
-su to
150°C, Grease In-situ thermal
Cycling 1000 fixture resistance, 0.10 MPa I
cycles conductivity
High 150'C, 200 Grease In-situ thermal
Collar Temperature hou°Cure resistance, 0.10 MPa
Laear 1 mm)
Storage hours fixture conductivity I
Bolts Mechanical 0.1
0.
Hz,
z
Cooling
chuck- Junction
At 100
125 gm,
gim,
Cycling 1500
cycles grease-die temperature and 150 gm
thermal
_ ._ n ITop view
Fig. 4: Grease thermal measurement fixtures
Chiu et al. [10] developed an accelerated mechanical test
method to evaluate the pump-out performance of thermal
Reliability assessment of thermal greases greases. This test method simulated the squeezing action on
Thermal greases typically offer better thermal the thermal grease that is created during a traditional thermal
performance and reduced manufacturing cycle times in power cycle. The frequency of cycling in the accelerated
comparison to other thermal interface material options. mechanical test method is in the order of hundreds of cycles
Thermal greases, however, are susceptible to a variety of per hour, which makes this test much faster than a
failure mechanisms during their service life. Two main traditional power cycling test.
causes for increases in thermal resistance of a grease layer In this study, spherical BN grease samples were
are, grease pump-out and grease dry-out. The powering up subjected to the accelerated mechanical test that was set up
and powering down of a device cause relative motion using an Instront Universal Testing Machine. As shown in
between the die and the heat spreader, which tends to Fig. 5, the test vehicle was a thermal test die mounted on a
squeeze the thermal grease out of the interface gap. This FR-4 board. The thermal die was 6.35 mm x 6.35 mm in
phenomenon is referred to as "pump-out" and results in size and had a thickness of 600 microns. The thermal die
increased thermal resistance due to loss of grease material incorporates a resistive heating element and a serial five-
from the interface [9,10]. Grease "dry-ouf' occurs due to diode temperature sense network [12]. The diode network
the separation of the filler from the polymer matrix at voltage as a function of junction temperature was measured
elevated temperatures. The polymer matrix tends to according to "JESD51-1 - Integrated Circuit Thermal
preferentially flow out of the interface and result in 'drying- Measurement Method" standard [13]. The thermal die
out' of the thermal grease. This also results in an increased assembly was fixed to the actuator base of the Instron and a
in-situ thermal resistance of the material [9]. liquid-cooled chuck was connected to the fixed head. The
Traditional power cycling is a direct method of coolant temperature was set at 300C.
determining the ability of a grease layer to provide a reliable Greases were subjected to 1500 cycles using this
interface throughout the operating life of the device. accelerated mechanical test. The frequency of cycling was
However, power cycling tests can be time consuming and 0.1 cycles/sec, which translates to 360 cycles per hour. The
costly, especially when screening multiple greases during bondline thickness of the grease was varied from 100 jim to
the design stage of a microelectronic package [10]. 150 jnm. The junction temperature of the thermal die was
Accelerated reliability tests that simulate the stress measured every 500 cycles at bondlines of 100 gim, 125 jim,
conditions observed in power cycling can be used to screen and 150 pm. A higher frequency of cycling and between

685 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.
different BLTs is possible with this setup. All the greases
were tested by powering the thermal die to the same level.
PTX60 filled greases (A-series formulations). Similarly,
Table V and Fig. 8 show thermal performance results for
PTX25 filled greases (B-series formulations), Table VI and
Fig. 9 show thermal performance results for PTX60S filled
greases (C-series formulations), and Table VII and Fig. 10
show thermal performance results for PTX25S filled greases
(D-series formulations).

Table IV. Thermal performance of PTX60 filled grease

Powered Die

PCB Assembly A-1 PTX60 10.0 22.8 1.64 13.83

Attached to Base A-2 PTX60 15.0 29.0 2.44 11.88
Base with A-3 PTX60 20.0 32.4 3.74 8.67
Vertical t A-4 PTX60 25.0 31.4 3.99 7.87
Movement A-5 PTX60 30.0 50.2 5.26 9.78
A-6 PTX60 35.0 52.6 5.39 9.82
Fig. 5: Grease mechanical cycling test A-7 PTX60 45.0 56.4 5.12 11.17
A-8 PTX60 50.0 52.0 3.66 14.35
4. Thermal Performance of Spherical BN Greases A-9 PTX60 54.2 49.2 3.60 13.78
Thermal greases at different filler loadings were A-10 PTX60 57.2 116.2 4.69 25.20
formulated with each of the four spherical BN fillers
described in Table II with a 1000 cP silicon fluid. The
smaller sized PTX25 showed relatively higher viscosities | * Resistance (nmme2KW) * Conduclivfty (W/rnK)
(Fig. 6) than the PTX60 and PTX60S due to the larger 16.00 -
surface area of the smaller PTX25. Formulations with the PTX60
surface modified PTX60S showed lower viscosities than 14.00-
with unmodified PTX60 at similar loading levels. The 12.00
viscosities of PTX25S formulations are currently being 10.00
measured. Phase separation was observed within hours of
blending for grease formulations with less than 25 wt%/o 8.00 -
loading of spherical BN. 6.00-
4.00
100000
2.00 ,
e 80000 PTXBOS 0.00
0 0.0 10.0 20.0 30.0 40.0 50.0 60.0
X. 60000- PTXO*
Spherical BN Loading (wt%.)
o 40000
Fig. 7: In-situ thermal conductivity and resistance vs.
>20000 i PTX60 filler loading in greases
0
0.0 10.0 20.0 30.0 40.0 50.0 PTX60, PTX25, and PTX25S showed the lowest thermal
resistance and highest thermal conductivity when filled at
wt%spherical BN the 30-40 wt% loading level. At loadings of spherical BN
filler greater than 45 wt%, the in-situ thermal conductivity
Fig. 6: Viscosity of Spherical BN filled grease formulations tended to decrease and the in-situ thermal resistance tended
to increase. This was due to the increase in BLT as well as
Table IV gives the thermal performance characteristics an increase in the interfacial thermal resistance. The high
of ten different grease formulations that use PTX60 as the viscosities of the highly filled formulations do not provide
filler (Al-AIO). The filler loading ranges were from 10 wt% as intimate a contact with the interfacing surfaces as
to 57.2 wt%. The BLT for the various formulations when compared to the lower viscosity, more flowable greases.
measured under a pressure of 0.20 MPa is also given in the
table. Fig. 7 plots the in-situ thermal resistance and the in-
situ thermal conductivity versus the filler loading for the

686 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.
 Table V. Thenral perfonnance of PTX25 filled grease
*Resistance (nrtn2KiW) U Conducti%ity (W/nK)I
30.00
PTX60S
25.00
B-l 10.0 3.6 0.35 9.92 20.00
B-2 PTX251 15.0 17.2 2.43 7.21
15.00 - -
""0
B-3 PTX25 20.0 9.0 1.28 7.06 ir
B4
B-5
PTX25
PTX25
25.0
30.0
14.0
27.0
2.33
4.34
5.98
6.27
10.00
tO.OO- w
~w - w m& , --t-
B-6 PTX25 35.0 26.2 3.65 7.26 5.00~ J

B-7 PTX25 40.0 35.4 4.31 8.21

0.00I
B-8 PTX25 45.0 32.4 3.62 8.96 0.0 10.0 20.0 30.0 40.0 50.0 60.0
B-9 PTX25 50.0 33.8 3.63 9.31
Spherical eN Loading (wt%)
B-10 PTX25 52.0 60.0 4.62 13.13
Fig. 9: In-situ thermal conductivity and resistance vs.
PTX60S filler loading in greases
0 Resistance (r2K/W) U Conducity (W/lK)
12.00 Table VII. Thermal performance of PTX25S filled grease
PTX25 fnrn,illafnnc
10.00

8.00
14.12
6.00-
D-2 PTX25SI 15.0 14.2 1.22 11.74
4.00 D-3 PTX25S 20.0 18.4 1.77 10.39
D-4 PTX25S 25.0 25.2 2.66 9.52
2.00- D-5 PTX25S 30.0 28.3 2.71 10.47
0.00 D-6 PTX25S 35.0 32.2 2.85 11.39
0.0 10.0 20.0 30.0 40.0 50.0 60.0 D-7 PTX25S 40.0 32.2 2.66 12.10
Sphwrical BN Loading (wt%/,) D-8 PTX25S 45.0 34.4 2.65 12.99
Fig. 8: In-situ thermal conductivity and resistance vs. D-9 PTX25S 50.0 41.8 2.73 15.27
PTX25 filler loading in greases D-10 PTX25S 54.2 145.2 3.69 39.82

Table VI. Thermal performance of PTX60S filled grease

formulations RResistance (rnrn2K/W) * Conductvity (W/mK)
18.00
PTX25S
16.00 A
14.00
U-l PTXA60 10.0) I19.8 2.07 1 9.58
12.00
C-2 PTX60S 15.0 27.0 2.93 9.55
31.6 3.05 10.50
10.00
C-3 PTX60S 20.0
4.27 12.38 8.00
C4 PTX60S 25.0 52.6
C-5 PTX60S 30.0 51.0 3.98 12.94 6.00
C-6 PTX60S 35.0 56.2 3.97 14.17 4.00
C-7 PTX60S 40.0 65.6 4.56 14.38 2.00
C-8 PTX60S 45.0 73.4 4.40 16.65 0.00
C-9 PTX60S 50.0 152.0 6.19 24.62 0.0 10.0 20.0 30.0 40.0 50.0 60.0
C-10 PTX60S 54.2 451.6 8.32 54.07 Spherical BN Loading (wt%)
Fig. 10: In-situ thermal conductivity and resistance vs.
PTX25S filler loading in greases

687 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.
 The PTX25 and PTX25S filled greases resulted in lower
BLTs at similar loadings than the PTX60 and PTX60S filled
greases, due to their smaller average particle size. Several
formulations showed in-situ thenmal resistances lower than
10 mm2K/W and thennal conductivities greater than 4
W/mK at modest loadings of spherical BN filler. However,
these values are presented as a representation of the
behavior of spherical BN in silicone resins for grease
formulations. Grease formulation optimization (resin,
additives, surface functionalization, etc.) and testing
parameters (contact pressure, temperature, interface
characteristics, etc.) can have a significant impact on the
overall in-situ perfonnance of thennal greases [14].
Fig. 11 shows the in-situ thermal conductivity and
resistance, BLT, and viscosity of grease formulations with
35 wt%/o of the different spherical BN fillers. The PTX25
and PTX25S formulations show lower BLTs than the
PTX60 and PTX60S formulations. The S-coated PTX60S
filler showed lower viscosity than the uncoated PTX60 filler
(3700 kP vs. 7400 kP). The S-coated fillers showed slightly
lower thermal perfonnance than the uncoated spherical BN
fillers. Optimization of the silicone resin and the surface
coating on the spherical BN fillers, however, may enable
reduced viscosity without negatively affecting thermal
perfonnance.
Air-to-air thermal cycling (AA TC)
The changes in thermal resistance, thennal conductivity,
and BLT of greases G-1, G-2, and G-3, after 1000 thenmal
cycles, is shown in Table VIII. The measurements were
done on greases sandwiched between aluminum and silicon
surfaces, under a pressure of 0.10 MPa. There was a
reduction in thermal resistance observed upon thermal
cycling (statistically significant, p value < 0.05) most likely
due to the combination of a reduction in BLT and increased
wetting of the mating surfaces by the greases. The viscosity
of thenmal greases reduced significantly at elevated
temperatures, thus enhancing the wetting of surfaces, and
consequently reducing interfacial thermal resistance. For
example, grease G-l showed a 45% reduction in viscosity
upon heating from 25 C to 100 C.
To detennine the effect of wetting perfonrance on
greases upon subjecting them to elevated temperatures,
grease samples, in a fixture were measured at room
temperature, subjected to 10 minutes at 150 C, then
measured again at room temperature. (This is equivalent to
one cycle through the maximum temperature used for high
temperature storage and thermal cycling). The thermal
resistance of the samples was observed to reduce by 7-12%
after only one thenmal cycle.

Table VIII. Thermal performance after thermal cycling

16.0
*I cducnUttY (WV/mr) * Resistance (rm^2KJW) OViscosity (kP)
.~~~~~~Ps 10X tbrnL .. .es5
BLT 56 pm
14.0 _
12.0 -
~~~BLT 26 prn BLT 32 pmn
,.,.B;~~~~in BLT(%): S.ifiWS
G-l 35.8 10.55 0.00 14.67
G-2 41.6 13.69 6.15 10.30
G-3 46.4 17.25 8.61 10.46

High temperature storage (HTS)

The change in thermal perfonrance and BLT of G-l, G-
G0.0
PTXOD PTXSOS PTX25 PTX25S
2, and G-3 when subjected to high temperature storage is
shown in Table IX. Upon testing aluminum-grease-silicon
Greass Loaded to 35wt% samples in the grease fixture (0.10 MPa), a significant (p
Fig. 11: In-situ thennal conductivity and resistance, BLT, value < 0.05) reduction in thermal resistance was observed.
and viscosity of grease formulations with 35 wt%/o spherical The average resistance of the grease layers dropped by 7-
BN filler 14%. The drop in thermal resistance was likely due to a
combination of BLT reduction and increased wetting at the
mating surfaces.
5. Reliability of Spherical BN Filled Greases Table IX. Thermal perfonnance after high temperature
Three types of reliability tests were performed in the storage
current research - air-to-air thermal cycling, high
temperature storage, and mechanically induced pump-out.
The details of the reliability tests are given in Table III.
Three new greases were formulated using 35.8 wt%/o (G-1),
41.6 wt%/o (G-2), and 46.4 wt%/o (G-3) spherical BN filler in
silicone resins, based on the preferred loading limits that G-l 35.8 9.81 1.49 9.34
were observed in the studies discussed in previous sections. G-2 41.6 8.27 3.14 7.29
The measurement pressure that was used for the reliability G-3 46.4 9.49 1.73 8.25
tests was 0.10 MPa. The previous sections report values
obtained at 0.20 MPa.

688 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.

Accelerated mechanical pump-out testing
Thermal grease layers were subjected to a pumping
action using the test setup described in Fig. 5. The BLT of
the greases was varied from 125 gim to 125 ± 25 ,um.
Junction temperatures of the thermal die were monitored at
BLTs of 100 pun, 125 pun, and 150 jim. The change in
junction temperature of thermal die using greases G-1 and
G-3 at a bondline of 125 gm is shown in Fig. 12. The
junction temperature for both G-1 and G-3 increased by a
similar extent with mechanical cycling. The junction
temperature increased by 3°C for G-1 and 4°C for G-3 after
1500 cycles.
Comparing thermal results from the two cycling methods
(grease fixture vs. accelerated mechanical pump-out
apparatus) showed the mechanical pump-out apparatus to be
a harsher test method. In the fixture-based thermal cycling,
the thermal resistance dropped for all greases whereas in the
mechanical pump-out test the junction temperature
increased, indicating an increase in thermal resistance. Note,
however, that the BLTs for the two methods were different.
For the fixture-based test, the pressure on the grease layers
was applied consistently across the three materials, allowing
the viscosity and filler characteristics to dictate the resulting
BLT. By contrast, using the Instron(g) based test, similar
bondlines were maintained for all the greases. In addition,
the grease fixtures allow a reduction in BLT when the
viscosities of the greases reduce at elevated temperatures. In
the Instrong based test, the BLT is maintained constant
throughout the test.
oo-
00~~~~~~~~
86 - Nitride in a Microwave-powered, Atmospheric Pressure
0 84 "~~~~
0 No. 6, 2002, pp. 3429-3440.
0 82 - 4. Lodyga, D., Tereshko, J.W., Sane, A., and Fox, T., "Low
80 - Viscosity Filler Composition of Boron Nitride Particles
E of Spherical Geometry and Process", United States
i 78 -
0 76 - G-3
o~ 74 -
0
c "Measurements of Adhesive Bondline Effective Thermal
72-
70-
0 250 500 750 1000 1250 1500 1750
Cycles
Fig. 12: Junction temperature change on mechanical cycling
6. Summary and Conclusion
Thermal greases with significantly lower thermal
resistance (< 10 mm2K/W) are continually to being sought
to meet the requirements for high-performance
microelectronic thermal solutions. To develop new high
performance thermal greases, new thermally conductive
fillers are also being sought. Spherical BN offers the
advantages of isotropic high thermal conductivity, low
dielectric constant, and compressibility, which make it
suitable for a high thermal performance greases that require
electrically insulating properties.
The characteristics of four spherical BN materials,
PTX60, PTX60S, PTX25 and PTX25S, as fillers in thermal
greases, were explored through the use of thermal,
rheological, and reliability tests. Each filler was shown to
respond slightly differently in different rheological and
thermal tests. Grease formulations with spherical BN
particles asfillers showed thermal resistance below 10
mm2K/W and thermal conductivities greater than 4 W/mK at
modest filler loadings and testing pressures. The smaller
sized PTX25 and PTX25S yielded lower BLT greases which
may have applications in systems that require thinner grease
layers. Grease formulation optimization, interfacial
resistance reduction, addition of secondary fillers, and
optimized testing conditions, may result in dramatically
different, and potentially improved, thermal performance.
Acknowledgments
The authors acknowledge the assistance of David Esler
and Don Buckley of GE Global Research, Niskayuna, NY.
References
1. Gleiman, S., Chen, C., Datye, A., and Phillips, J.,
"Melting and Spheroidization of Hexagonal Boron
Nitride in a Microwave-powered, Atmospheric Pressure
Nitrogen Plasma", Joumal of Materials Science, Vol. 37,
No. 6, 2002, pp. 3429-3440.
2. Tummala, R., Fundamentals of Microsystems Packa2ing
McGraw Hill, NY, 2001.
3. Gleiman, S., Chen, C., Datye, A., and Phillips, J.,
"Melting and Spheroidization of Hexagonal Boron
Nitrogen Plasma", Journal of Materials Science, Vol. 37,
Patent 6713088, March 2004.
5. Campbell, R.C., Smith, S.E., and Dietz, R.L.,
Conductivity and Thermal Conductance using the Laser
Flash Method", 15th Annual IEEE Semiconductor
Thermal Measurement and Thermal Management
Symposium, San Diego, CA, 1999, pp. 83 - 97.
6. Campbell, R.C. and Smith, S.E, "Flash Diffusivity
Method: A Survey of Capabilities", Electronics
Cooling, Vol. 8, No. 2, 2002.
7. Netzsch Instruments, Microflash Operation and
Maintenance Manual, Burlington, MA, 2001.
8. Lee, H.J., 1975, "Thermal Diffusivity in Layered and
Dispersed Composites", Ph.D. Thesis, Purdue
University, West Lafayette, IN.
9. Viswanath, R., Wakharkar, V., Watwe, A., and
Lebonheur, V., "Thermal Performance Challenges from
Silicon to Systems", Intel Technology Joumal, Q3, 2000.

689 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.
10.Chiu, P-C., Chandran, B., Mello, M., and Kelly, K., "An
Accelerated Reliability Test Method to Predict Thermal
Grease Pump-Out in Flip-Chip Applications", Electronic
Components and Technology Conference, 2001.
1 1. Gowda, A., Esler, D., Nagarkar, K., Paisner, S.N.,
Tonapi, S., and Srihari, K., "Degradation of Thermal
Grease Interface Layers with Thermal Shock and High
Temperature Storage", SEMI-THERM 2005, San Jose,
CA, 2005.
12.Delphi, PST4-02 Thermal Test Die Data Sheet,
http://www.delphi.com/pdf/micro/testdie/PST402.pdf
13.EIA/JEDEC, "EIA/JESD51-1 - Integrated Circuit
Thermal Measurement Method", http://wwwjedec.org,
1995.Early, M., Lee, S., and Pellilo, M., "Thermal
Performance of Interface Materials in Microelectronics
Packaging Applications", International Packaging
Conference, San Diego, CA, USA, 1995, pp. 534-44.
14.Gowda, A., Nagarkar, K., Esler, D., Acharya, A.,
Paisner, S.N., Tonapi, S., and Srihari, K., "Influence of
Surface Characteristics on the In-situ Performance of
Thermal Greases", SMTA International, Chicago, IL,
2005.

690 2005 Electronics Packaging Technology Conference

Authorized licensed use limited to: University of Catania. Downloaded on November 30,2022 at 15:10:44 UTC from IEEE Xplore. Restrictions apply.