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Published 10/17/2016
Copyright © 2016 SAE International
doi:10.4271/2016-01-2287
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ABSTRACT
Mobile source emissions standards are becoming more stringent and particulate emissions from gasoline direct injection (GDI) engines
represent a particular challenge. Gasoline particulate filter (GPF) is deemed as one possible technical solution for particulate emissions
reduction. In this work, a study was conducted on eight formulations of lubricants to determine their effect on GDI engine particulate
emissions and GPF performance. Accelerated ash loading tests were conducted on a 2.4L GDI engine with engine oil injection in
gasoline fuel by 2%. The matrix of eight formulations was designed with changing levels of sulfated ash (SASH) level, Zinc
dialkyldithiophosphates (ZDDP) level and detergent type. Comprehensive evaluations of particulates included mass, number, size
distribution, composition, morphology and soot oxidation properties. GPF performance was assessed through filtration efficiency, back
pressure and morphology. It was determined that oil formulation affects the particulate emission characteristics and subsequent GPF
performance.
CITATION: Shao, H., Lam, W., Remias, J., Roos, J. et al., "Effect of Lubricant Oil Properties on the Performance of Gasoline Particulate
Filter (GPF)," SAE Int. J. Fuels Lubr. 9(3):2016, doi:10.4271/2016-01-2287.
during the vehicle service life.[10], [11], [12] Ash can be derived The effects of the experimental oil formulation compositions on the
from various sources, including lubricant oil, engine wear particles GPF performance, chemistry, and composition of particulates
and other secondary sources.[9], [13] Lambert et al. found out that produced are addressed.
approximately 50 wt% of the collected ash was non-lubricant derived
in their work to understand ash accumulation in GPFs over significant
mileage.[14] The results indicate that the exhaust gas backpressure EXPERIMENTAL
did increase with mileage accumulation and ash loading, but did not
lead to significant decrease in fuel economy. In the meanwhile, as the
1. Experimental Setup
significant contributor of ash, lubricant additive has been investigated Engine Setup
for its impact on ash formation and according influence on DPF/GPF A 2.4 L 4-cylinder, naturally aspirated, production GDI spark-ignition
performance. It was found that ash, taken from filters of 100,000 mile engine was used in this work. The engine geometry and specifications
run vehicle, enhanced soot oxidation reactivity at simulated tight are given in Table 1. This engine is basically operated at homogenous
contact and loose contact conditions.[15] The impact of ash on and stoichiometric charge conditions. The engine was mounted on a
backpressure has been studied by many researchers on GPF/DPF.[16] 112 kW blower-cooled AC dynamometer for speed control and torque
Researchers also found that an ash membrane can effectively prevent measurements. In this work, the certified Tier 2 EEE fuel and
soot from entering into the porous network of the filter wall. This can experimental style additive formulation in conventional motor oil
contribute to the reduction of the overall pressure drop compare to with an SAE grade of 5W-20 were used.
the no-ash case.[17]
Table 1. Engine geometry and specification
It has been a logical development to apply catalyzed GPF (c-GPF) for
GDI engines since the optimized design and robust formulation can
simultaneously reduce gaseous emissions while PM emissions are
well controlled.[18] In order to ensure the satisfactory performance of
c-GPF over full useful life (FUL), the interaction between lubricant-
derived ash and c-GPF (both the catalyst washcoat and substrate)
needs to be understood. This fundamental understanding will help for
the c-GPF system development and lubricant formulation
optimization. Early investigations show that the ratio of Ca to ZDDP
is critical in the degree of deactivation: when the ratio is low,
amorphous zinc-phosphate glasses and other zinc and/or phosphorus
compounds deposited on the surface of catalyst washcoat reduce
GPF Test Setup and Procedure
porosity of the coating.[19] Another study indicates that phosphorus,
A partial flow exhaust system was built to test prototype bench-scale
which has higher diffusion coefficients than zinc, calcium and
GPFs (2” in diameter and 6” in length) at a wide range of flow rates
magnesium, can penetrate deep into the washcoat, facilitating
(0 - 40 kg/hr) at the same steady state engine condition. Figure 1 (a)
deactivation process.[20] As the deactivation of three-way catalyst
shows the schematics of the partial flow GPF setup. The flow rate to
(TWC) is obvious with the inclusion of P derived from engine oil,
the GPF is controlled by two flow control valves at the main exhaust
low volatility engine oils have been developed to reduce P impacts on
pipe and the partial flow exhaust pipe. The pressure drop and
catalysts.[21]-[22] The main concern for the impact of ash level is
temperatures across the filter were measured, and the particulate
that the non-combustible ash deposits trapped in the channels of the
number and mass filtration efficiencies were calculated by measuring
filter may potentially increase backpressure over the filter and further
the particulate number and mass of upstream and downstream of the
affect its performance.[23] Earlier experience from DPF work
filter. The compressed air and air heater (6 kW) were connected to the
indicates that detergents have significant contribution to the ash
partial flow exhaust pipe at the GPF inlet, which allows cold air and
accumulation in the channel.[24] But the effect largely depends on
hot air (max. 600˚C @ filter inlet) test for pressure drop measurement
the system design, detailed oil formulation and operating condition.
and complete soot oxidation. Reproducibility of this technique has
Ito et al. reported that there is no interaction or phase change of ash
been checked and gives representative results. For accelerated ash
components and cordierite material was observed during an extensive
loading, lube oil was sprayed into the fuel supply line at a controlled
c-GPF field test up to 160,000 km. [18]
rate by using a solenoid valve in connection with a pulse generator to
the lube oil in gasoline fuel by 2 wt. %, which allows about 1 g/L of
Generally, there is a trade-off relationship between backpressure, PN
ash loading in 1 hour at 1250 rpm - 25% load with 1 % sulfated ash
filtration efficiency, soot/ash loading.[25] Therefore, oil formulation
lube oil.
as a whole shall be investigated in order to be compatible with GPF/
DPF application while delivering desired performance to engine
system operation. Here, an accelerated ash loading condition is
achieved by direct engine oil injection into the combustion chamber.
Shao et al / SAE Int. J. Fuels Lubr. / Volume 9, Issue 3 (November 2016)
The GPF test procedure was designed for efficient and fair 2. Exhaust Emissions Measurements
comparison of GPF performance after ash loading, as shown in Soot mass concentration was measured using a high-sensitivity
Figure 1 (b). Every new filter was pre-treated in hot air (550˚C) photo-acoustic sensor (AVL 483 micro soot sensor). For partial flow
before the test. Clean filter pressure drop (without soot) was first measurements of particulate number and size distribution, a scanning
measured cold (room temperature) air, and the clean filtration mobility particle sizer (SMPS, TSI Model 3936) with a condensed
efficiency was measured under steady state engine condition of 1250 particle counter (CPC, TSI Model 3022A) was used after exhaust
rpm - 25% and flow rate of 15 kg/hr. Accelerated ash loading was emissions were diluted by a fine particle sampler (Dekati FPS-4000).
conducted to target lube oil consumption, followed by complete soot The raw emissions were sampled from the exhaust pipe through the
oxidation with hot air (550˚C). In the complete soot oxidation heated stainless steel probe and subsequently diluted in two stages, a
process, the hot air kept flowing at 20 kg/hr until the measured perforated tube for the primary dilution and an ejector pump for the
pressure drop change gets smaller than 0.05 kPa/10 min. The engine secondary dilution. The temperatures of the sampling probe, primary
condition was maintained at 1250 rpm - 25% and fuel was doped by dilution air were controlled at 350°C in this study. The actual dilution
2 wt. % in the accelerated ash loading. After ash loading, soot was ratio was calculated based on measuring the CO2 concentrations
completely oxidized with hot air (550˚C) to measure clean filter before and after dilution using an infrared CO2 analyzer (California
pressure drop and filtration efficiency after ash loading. In this study Analytical Instruments, Inc., Model 200).
this procedure was repeated twice for each lube oil sample, at target
lube oil consumptions of 61 g and 122 g, and the pressure drop and
filtration efficiency changes at earlier ash loading were compared for 3. Characterization Tools
different lube oil additive formulation.
Thermogravimetric Analysis (TGA)
A TGA instrument (TA Instruments Q50) was used to evaluate
volatile organic fraction (VOF) and oxidation reactivity of GDI PM
collected on Teflon® filters. Each PM sample scraped from a filter
was loaded in a platinum pan of 9.85 mm diameter and 1.68 mm
height. Each sample of 1 - 1.5 mg was thermally treated under N2 at
600°C for 100 minutes and then, isothermal oxidation was performed
at the same temperature with 8% O2 in N2.
4. Oil Matrix
Eight (8) fully formulated experimental engine oils of SAE 5W-20
viscosity grade were prepared according to the 3-factor, 2-level
matrix design shown in Figure 2. The three factors are chemical
properties of the engine oil: SASH, phosphorus level from ZDDP,
and alkaline earth metal type from detergents. Treating levels of
(b). test procedure ZDDP and detergent for each matrix oil were varied accordingly in
order to meet target SASH and P values. Other essential components,
Figure 1. GPF test setup and procedure such as dispersant, antioxidant, friction modifier and viscosity
modifier, were treated at constant levels for all oils. The base oils
used in this work are of Group III base stock as categorized by API in
API 1509 EOLCS Appendix E publication.
Shao et al / SAE Int. J. Fuels Lubr. / Volume 9, Issue 3 (November 2016)
Some physical and chemical properties of the eight oils are shown in According to the profile, calculated compositions of VOF, soot and
Table 2. Actual measured SASH and P results, which are slightly ash were summarized in Table 3. It is noted that the N2 pretreatment
deviated from targeted low and high levels of the matrix design, are for 100 minutes was not enough to remove all the volatile parts for
deemed within acceptable ranges for this study. the Oil B and Oil E cases, which have high Ca and Mg contents with
low ZDDP contents. Therefore, these samples would expect to
contain higher VOFs than those in the table when the pretreatment
time is longer, which was avoided for fair comparisons in this work.
Apparently, the composition of PM is largely affected by oil
formulation. For the same ZDDP level, high SASH oil produces
relatively less soot compared to the low SASH one, regardless of the
metal type. For example, using Oil B (low ZDDP, high Ca) has very
low normalized soot percentage (18.6%), while Oil A (low ZDDP,
low Ca) has much higher normalized soot percentage (43.2%).
Similar difference is seen between Oil C (29.4%) and Oil D (63.0%),
Oil E (33.3%) and Oil F (66.6%), Oil H (51.8%) and Oil G (54.7%).
For the same ZDDP and SASH level, calcium-based oils (A, B and
C) produce relatively less soot than magnesium-based oils (F, E and
H accordingly). This is largely due to calcium being a better soot
oxidation catalyst than magnesium. The difference between Oil D and
Figure 2. Oil matrix design
Oil G is unexpected, which requires further examination. The
Table 2. ICP/SASH analysis of oil samples difference in PM composition from this work is primarily due to the
oil chemistry and its participation in the combustion process. As
being a conventional anti-oxidant additive, ZDDP hinders the
oxidation process, which can increase the normalized soot percentage
in total PM emissions. For detergent, metal type and concentration
can affect the combustion and oxidation of PM. In details, Ca
improves the combustion better than Mg. For the same metal type,
higher concentration of detergent leads to lower normalized soot
production rate, while leaving high total ash level.
RESULTS
TGA Results
TGA was used to determine the composition of PM and its oxidation
trends with different oil formulations. Figure 3 is the PM TGA
production profile, in which three distinctive stages are shown for all
the test oils. Time starts when the pan is still at room temperature,
and it takes 1 hour for the temperature of the pan ramp to reach
600°C. Volatile organic fraction (VOF) removal takes place in N2
environment at 600°C for about 100 minutes. Afterwards, 8% O2 is
introduced to the system (balanced with N2) for oxidation while the
temperature is kept at 600°C. The remaining unburned part is Figure 3. PM TGA production profile
attributed to ash. Since our energy dispersive X-ray spectroscopy
Table 3. PM samples composition from TGA measurement (weight percent %)
(XEDS) analysis coupled with TEM and scanning electron
microscope (SEM) did not indicate the presence of engine wear
metals (data was not included), ash contributions were ascribed to
solely additive elements in engine oils. Obviously, the weight loss,
both the relative amount and the rates, is largely affected by lubricant
formulation.
Shao et al / SAE Int. J. Fuels Lubr. / Volume 9, Issue 3 (November 2016)
Figure 4 presents the soot oxidation only profile and the normalized oil case as indicated in Figure 6 (c), primary particles were found to
remaining soot mass indicates the soot oxidation rate with using be less spherical with rough surface due to attached nanoparticles for
different lubricant oil in ash loading. Similar to PM examination, oil oil additions as shown in Figure 7 (b) and Figure 8(f). Soot
formulation has significant influence on the soot oxidation rate. aggregation degree is relatively lower than the case when no oil is
Figure 5 is based on calculating soot oxidation rate from TGA injected, and mostly fragmented and amorphous as shown in Figure
analysis. Overall, high SASH oils give faster soot oxidation rate, for 8(c). It is postulated that the presence of oil combustion products can
both ZDDP level. However, the effect of calcium-based oils is much assist the suppression of soot formation and oxidation of soot
greater than that of magnesium-based ones. Therefore, soot control, aggregates, as presented in.[26] The effects will be manifested at
from generation to passive regeneration, is desired for the efficient lower soot emission rates and reduced size. Previous TGA results
operation of GPF. already provided the information of PM composition. Some
crystalized or amorphous metal components (Ca, P or Mg) are
present in the aggregate or as single particles.
Figure 6. TEM of PM collected at 1250 rpm, 25% load (no oil case as a
baseline)
Figure 4. Soot oxidation profile for the oxidation portion of TGA experiment
TEM Results
TEM was performed for the PM collected through the gravimetric
sampling system. While TEM images of no oil case were shown in
Figure 6 as a baseline, the results for Oil B and Oil E were shown in
Figure 7 and Figure 8 respectively. Images (a) through (c) were
observed on carbon-coated grid, while (d) through (f) was observed
on lacey carbon-coated grid with larger magnification for
nanostructure examination. For carbon-coated grid, the whole particle Figure 8. TEM of PM collected at 1250 rpm, 25% load (Oil E)
distribution can be collected on the TEM grid for morphological
examination. Compared to no oil case, the most particles for oil
additions are observed to be nanoparticles, about 5-25 nm. While
primary particles appeared to be spherical with smooth surface for no
Shao et al / SAE Int. J. Fuels Lubr. / Volume 9, Issue 3 (November 2016)
Ash Loading and Backpressure Among four high SASH oils, Ca-based detergent oils (oil B and oil
Figure 9 is the result of ash loading rate after two stages, with oil C) experience an earlier transition from bed filtration to cake filtration
consumption amount at 61g and 122 g respectively. High SASH oils than Mg-based detergent oils (oil E and oil H). This can be related to
(B, C, E and H) have about twice amount of ash loading as of those the composition or particle size of PM altered by doping with
low SASH oils (A, D, F and G) for the same amount of aging time. It different lubricant oil formulations. Although further work needs to
has to be noted that the ash loading is solely calculated based on oil be done to characterize the composition of combustion products with
consumption rate, which means the loss in cylinder and exhaust different oil formulation, the results imply that filtration mode
system is not taken into consideration in this work. The primary transition can be controlled by changing oil formulation, which in
reason to use this calculation method is because early stage of ash turn determines the backpressure rising rate. This chemistry impact
loading, up to 4 g/L, was mainly focused in this study, while the real on filtration mode transition can potentially affect GPF application
ash loading in the GPF vehicle was reported to be 20 - 30 g/L after and its performance under real-world operating conditions.
about 100,000 miles run, and the actual weighing of such low ash
loading incurred measurement errors. Undoubtedly, actual collection
rate is certainly much lower than presented, but this calculation still
allows reasonable and noticeable comparison among different
lubricant oils as intended in the scope of work here.
Figure 10. Pressure drop changes with ash loading for eight different oil
samples (air @ SV=46,600 hr-1)
In general, the filtration starts from bed filtration to surface, and then
to cake filtration.[27][28] As the porous structure of bed and surface Figure 11. Pressure drop changes with Ca(Mg)/ZDDP ratio for eight different
are filled with soot and ash, a sharp increase in backpressure is oil samples (air@SV=46,600 hr-1)
observed. After the surface pores are filled, it experiences the
transition from bed to cake filtration, where the pressure rise becomes Besides the ash loading amount, it is observed that the ratio between
mild. The duration of each stage and transition timing can be affected detergent metal and ZDDP plays important role in backpressure rise
by both the properties of GPF, the characteristics of PM that enter (Figure 11). When this ratio is in the low range (area 1), the pressure
into GPF, as well as the operating condition of GPF. The properties of drop increase is negligible. As the ratio moves to the middle range
the GPF include the geometry, porosity and pore size. The (area 2 and area 3), the pressure drop increase depends on the total
composition, amount, size and mobility of PM certainly affect how SASH of the oil, i.e. higher SASH level leads to elevated
soot and ash are trapped and transported. In addition, temperature, backpressure increase. For high ratio range (area 4), moderately high
flow rate and oxygen concentration, which are determined by engine pressure drop increase is observed regardless of the total SASH of the
operation, shall play an important role in actual operations. oil. Through the comparison of four different areas, it indicates that
Shao et al / SAE Int. J. Fuels Lubr. / Volume 9, Issue 3 (November 2016)
not only SASH level in the oil, but also the ratio between detergent
metal and ZDDP affects the pressure drop increase. Some explanation
could be that the oil chemistry will determine the ash formation, and
its interaction with soot as well as the substrate. However, this
requires further examination of the chemistry composition and
morphology on the deposited substrate.
Figure 12 shows the results of size-based particulate emissions before Figure 13. Size-based PN filtration efficiency for Oil H (different ash loading)
and after GPF at equal ash loading i.e., 122 g oil consumption for low
The relationship between filtration efficiency and ash loading rate
SASH oil and 61 g oil consumption for high SASH oil. Apparently, in
was presented in Figure 14 and Figure 15 for PN and soot
the presence of an efficient GPF, particulate emission rates are largely
respectively. At zero ash loading point, PN filtration efficiency ranges
reduced after the exhaust passes through GPF although there is
from 82 to 88%, and soot filtration efficiency starts even lower (70 to
significant difference in engine-out particulate emission with using
88%) and more spread. This filtration efficiency quickly increases to
different oils.
above 95% soon after mild amount of ash is loaded. This significant
improvement in filtration efficiency is attributed to the build-up of
ash layer. For the real-world application, the vehicle equipped with
GPF will have different levels of filtration efficiency with mileage
accumulation and oil consumption. In specifics, only moderate
filtration efficiency can be achieved in the break-in period where not
enough cake has been built. This can be improved soon after the cake
is built, and the filtration efficiency can be maintained at satisfactory
level until the severe plugging occurs.
• Engine oil injected into the fuel supply line can differentiate
the impact of various lubricant oil formulations on GPF
performance.
• Particulate composition, morphology and emission rates are
highly dependent on lubricant oil formulation.
• Calcium-based detergent promotes higher soot oxidation rate.
• Higher SASH oil level increases the ash loading and GPF back
pressure.
• Oil formulation chemistry determines the transition from
Figure 15. Soot Filtration efficiency with eight oils (different ash loading) bed filtration to cake filtration. Oil formulated with Ca-based
detergent experienced an earlier transition compared to Mg-
Besides the common trend of filtration efficiency vs. ash loading,
based one for higher SASH oil.
differentiation among eight oil samples are also noted. Figure 16
summarized the filtration efficiency and pressure drop response • Ash loading increase the backpressure, but filtration efficiency
(backpressure drop change per ash loading) with eight oils. For low is a more complex phenomenon. Filtration efficiency is more
SASH oils, those of higher metal/ZDDP ratio (oil A and oil F) have effective with a small amount of ash accumulation.
elevated filtration efficiency than the ones with lower ratio (oil D and
oil G). Additional difference is reflected in pressure drop response; oil It is learned from this work that oil formulation plays an important
A and oil F have slightly higher responses than oil D and oil G. This role in GPF performance through the effect on combustion and
impact is not well perceived when the total SASH is at higher range interaction of those combusted products with GPF. The oil matrix is
(oil B, oil E, oil C and oil H). However, pressure drop response is simple but well-defined, and the preliminary results certainly will
generally lower for low SASH oils. This is likely due to the fact that guide our future work on further in-depth understanding on the
the ash concentration in the flow dictates the deposition rate and impact of engine oil formulation on the performance of GPF and even
distribution of soot and ash in the filter, both in the pore and on the the whole vehicle system.
surface.
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Shao et al / SAE Int. J. Fuels Lubr. / Volume 9, Issue 3 (November 2016)
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