Applied Mechanics and Materials Submitted: 2017-08-07

ISSN: 1662-7482, Vol. 873, pp 20-25 Revised: 2017-08-09

doi:10.4028/www.scientific.net/AMM.873.20 Accepted: 2017-08-17
© 2017 Trans Tech Publications, Switzerland Online: 2017-11-15

Metallographic Determination for Porosity of Zirconia Ceramic Knives

Ge-Ping BI1,a, Wen-Hua TAN1,b and Ai-Jin MA2,c*
1
China National Quality Supervision and Inspection Center for Knife, Scissors and Domestic Metal
Tool, Yangjiang 529539, China
2
China National Institute of Standardization, Beijing, 100191, China
a
bigeping@sina.com, b415925053@qq.com, cmaaj@cnis.gov.cn

Keywords: Ceramic, Porosity, Metallographic determination

Abstract. Porosity has many effects on performance of ceramic knife including sharpness,
durability, etc, the metallographic detection for porosity of food contact ceramic knife was
established in this study. By compared the relation of sharpness, durability and porosity, Calculated
quantitative metallographic of porosity, and established the standard atlas of metallographic sample,
the porosity was detected. The results showed that not only the <0.5% porosity could be detected,
and the opening, the closing porosity would be detected quickly and accurately at the same time. It
could be used in optimizing process and monitoring quality and safety of food contact ceramic
knife.

Introduction
Zirconia ceramic knives are made through sintering material whose main component is zirconia.
It has advantages of high sharpness, high wear resistance, good chemical corrosion resistance, etc.,
it is widely used in developed countries or regions like Japan, USA and European countries, etc.,
and China has many enterprises manufacturing high performance ceramic knives. The performance
of ceramic knives is dictated by their microstructure. Due to the characteristics of zirconia ceramic
manufacturing technique, there are inevitably pores in zirconia ceramic and the ratio of pore volume
to total volume of zirconia ceramic is porosity. Pores in ceramic knives can be classified into open
pores and closed pores while porosity can be classified into closed porosity and apparent porosity
[1]. Porosity, size, quantity and distribution of pores are important content in microstructure of
zirconia ceramic and are also import indicators determining performance of zirconia ceramic. The
porosity of ceramic knifes is closely related to their functional performance and mechanical
performance while lower porosity, smaller pores, more globular pores and more uniform
distribution of pores means better performance of zirconia ceramic knives. Besides, in case of
contact with food, it is difficult to remove the residuals in pores which will bring adverse influence
on food safety. Consequently, porosity is an important indicator to assess performance of zirconia
ceramic knives. At present, porosity of ceramic is usually determined using Archimedes method [2]
in the world. This method is only applicable to determining ceramic with porosity of 0.5%-10% and
it can only be used to determine apparent porosity and is incapable of determining closed porosity;
Additionally, the specimen treatment period and determining period is long; What’s more, for the
specimen with identical mass, if surface area of the specimen is increased (pulverized), the apparent
porosity will increase and the testing result tends to be every easily influenced by the surface area of
the specimen. During the research of determining porosity of zirconia ceramic knives, the author
finds that determining porosity of zirconia ceramic knives using metallographic method solves the
problem that closed porosity and apparent porosity lower than 0.5% cannot be determined, and
provides an important means to control quality of zirconia ceramic knives, which is important for
quality control and technique improvement of ceramic material.

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 Applied Mechanics and Materials Vol. 873 21

Material and Method

Material and Reagents. The zirconia ceramic knives are provided by Jiaozuo Weina Science &
Technology Co., Ltd., Kyocera of Japan, Keteng Industry and Trade Co., Ltd. of Yangdong County
of Yangjiang City, Yangjiang Kingdouble Precision Ceramic Knives Manufacturer LTD, Leci
Cutting Tools Co., Ltd of Yangodng District of Yangjiang City, Ganzhou Jinghuan Rare Earth
Materials Co., Ltd., Shandong Zibo Huachuang Fine Ceramics Co., Ltd., Guangdong Jialeer
Tableware and Kitchenware Co., Ltd. and Yangjiang Goldenhorse Industrial Co., Ltd. The cutting
medium is quartz sand paper.
Instruments and Equipments. Blade sharpness and edge retention tester using paper, Guangzhou
Yilang Mechanical and Electrical Equipment Co., Ltd, Yangjiang Supervision Testing Institute of
Quality & Metrology; Metallographic microscope, Leica of Germany; Quantitative and
semiquantitative image analyzing software, Beijing Hengzhiyou Science and Technology
Development Center; High precision electronic density hydrometer, Dongguan Hongtuo
Instruments Co., Ltd.
Method.
Sharpness and edge retention determining of ceramic knives. Keep the cutting edge of
ceramic knife to be tested upward and fix it on the knife fixture and use additional weight to apply
50N pressure to press the cutting medium to the cutting edge. Keep the cutting medium still, use a
motor to drive the knife fixture so as to make the knife reciprocate at a speed of 50mm/s and thus to
cut the cutting medium while the cutting stroke is 40mm, and repeat cutting back and forth for
60 rounds. Obtain the vertical height drop of cutting medium in every cutting stroke through
sensors, and obtain the test data through computer statistics. The cutting depth sum of the first 3
cutting rounds is the sharpness of the ceramic knife while the cutting depth sum of all the 60 cutting
rounds is the edge retention of the ceramic knife.
Determining porosity of ceramic knifes through metallographic method. Take 100mm2~
400 mm2 specimen from the ceramic knife and use epoxy to mosaic it into a metallographic
specimen. Use 400 meshes, 500 meshes, 600 meshes, 800 meshes and 1000 meshes abrasive paper
to grind the specimen successively and then use W0.5 abrasive paste to polish the specimen
mechanically. Purge the specimen and blow-dry it and then carry out bright field observation for the
pores in the ceramic knife as well as their characteristics while the amplification factor is 50 times,
100 times, 200 times and 500 times. Use digital photograph system to collect images when
observing the pores and their characteristics. Open the collected images of pores and their
characteristics in quantitative and semiquantitative image analyzing software and modify the
scale-plate according to images' amplification factor. Fill the pores in the image with color, then
extract the pores, and carry out quantitative analysis for the pores.
Determining apparent porosity of ceramic knives through boiling method. Take specimen
from the ceramic knife while the area of specimen shall not be lower than 0.4 cm3. Dry the
specimen at 110 °C±5 °C for 10h, cool it to room temperature and weigh it, and the dry weight m1
of the ceramic knife is got. Immerse the specimen into slightly boiling water and boil it for 4h, then
cool it to room temperature and immerse it into water to weigh it, and the buoyant weight m2 of the
ceramic knife is got. Measure the temperature of water, take the ceramic knife specimen out from
water, use a piece of gauze to dry the outer surface of the ceramic knife, weigh the specimen
immediately, and the wet weight m3 of the ceramic knifes is got. The cloth for moisture absorption
shall be soaked completely in water and wrung to be dry so as to prevent it from absorbing water in
pores of the specimen.
The apparent porosity of the ceramic knives is calculated as formula (1) while the result is
corrected to two decimal places
m3  m1
x  100%
m3  m2 (1)
where, x is apparent porosity; m1 is dry weight of the ceramic knife; m2 is buoyant weight of the
ceramic knife; m3 is wet weight of the ceramic knife.
22 Advanced Materials, Structures and Mechanical Engineering IV

Result and Analysis

Porosity Analysis of Ceramic Knives. Determining through boiling method, for 1# ceramic knife
specimen, the mean dry weight is 12.1678g, the mean buoyant weight is 10.1688, the mean wet
weight is 12.1702, and the calculated apparent porosity is 0.12%. Because boiling method can only
be used to determine apparent porosity higher than 0.5%, the porosity of 1# ceramic knife measured
using boiling method is not accurate.
Fig. 1 is the metallographic image of 1# ceramic knife specimen when determining porosity of
ceramic knives through metallographic method. From Fig. 1, it can be seen that there are pores with
various size which distribute in a ceramic knife and the pores have many shapes, such as circular
shape, ellipse, flat shape, trapezoid, polygon, etc. The pores have no obviously non-uniform
distribution on the surface and in the core in the whole field of view. Fig. 1d shows that parts of big
pores are formed by gathered small ellipse pores. Carry out quantitative analysis for Fig. 1b of 100×
pores image, the total measured area is 0.57mm2, the pores quantity is 165, the pores quantity in
unit area is 288, the relative shape factor of pores is 0.78, and the maximum relative shape factor is
0.99 while the minimum shape factor is 0.32. The mean area of pores is 5.20×10-5 mm2, the mean
equivalent diameter is 6.82×10-3 mm while the maximum equivalent diameter is 31.95×10-3 mm,
and the calculated porosity is 1.5%.

a.50×; b.100×; c.200×; d.500×

Fig. 1 Metallograph of ceramic knife.
Fig. 2 is the metallographs of 2#, 3#, 4#, 5#, 6#, 7# ceramic knife specimens for determining
porosity through metallographic method (100×). From the results, it can be concluded that the
porosity is 0.06%, 0.1%, 0.3%, 0.5%, 1.0%, 1.5% respectively.
 Applied Mechanics and Materials Vol. 873 23

a. 2#; b. 3#; c. 4#; d. 5#; e. 6#; f.7#

Fig. 2 Metallograph of ceramic knife.
Porosity's Influence on Sharpness of Ceramic Knives. From Fig. 3, it can be concluded that the
sharpness of ceramic knives is 100 mm when porosity < 0.1% while sharpness decreases to 50 mm,
which is an obvious decrease, when porosity > 0.5%. When porosity ≥1%, the sharpness remain
basically at 30 mm. It means that porosity has great influence on sharpness of ceramic knives when
porosity < 0.5% while ceramic knives' porosity has mild influence on the sharpness of ceramic
knives when porosity ≥1%.

Fig. 3 Relation of durability and porosity.

Porosity's Influence on Edge Retention of Ceramic Knives. From Fig. 4, it can be concluded that
the edge retention of ceramic knives is 1000 mm when porosity < 0.1% while the edge retention
decrease to 500 mm when porosity > 0.5%, decreasing by 50%. The edge retention remains
basically at 400 mm when porosity ≥ 1%. It means that porosity has great influence on the edge
retention of ceramic knives when porosity < 0.5% while ceramic knives' porosity has mild influence
on the edge retention of ceramic knives when porosity ≥ 1%.
24 Advanced Materials, Structures and Mechanical Engineering IV

Fig. 4 Relation of sharpness and porosity.

Conclusion
The porosity of zirconia ceramic knives has great influence on the sharpness and edge retention
of ceramic knives. From the perspective of safety, residuals may accumulate in pores while
residuals may breed bacteria, which is harmful to human's health. Thus, determining porosity of
ceramic knives is more important.
For the identical 1# zirconia ceramic knife specimen, the testing results of metallographic
method and boiling method in porosity determination are 0.12% and 1.5% respectively and the
results of these two methods differs greatly. The main reason is that the principles of these two
methods are different. Metallographic method is based on stereology principle and phase volume
percentage in 3D space is determined through 2D parameters measured and calculated for ground
surface of metallographic specimens. Boiling method is based on Archimedes principle, it uses
Archimedes to measure volume and high-precision balances to measure weight, and then calculate
the apparent porosity while it is incapable of determining closed porosity.
For whether ceramic products or powder metallurgical products, the nature of porosity is the
same. If metallographic method is to be used to determine porosity of zirconia ceramic, the most
widely used metallographic method is atlas comparison method. Establish standard series atlas at
first, in which every map's porosity is determined through quantitative metallographic calculation,
and the 6 maps in Fig. 2 series are established using this method. Use metallographic microscope to
observe the shape and feature of pores in a specimen, and compare it with standard atlas and thus
get the porosity of the specimen. The advantage of this method is that quick determination of
porosity of specimens can be achieved and complicated quantitative analysis can be avoided.
Using metallographic method to determine porosity can remedy the disadvantage of ISO 18754
standard, and its main advantage is that it can determine the porosity in case of pores existing
without restriction of porosity value. For example, Fig. 2a is the photograph of pores in zirconia
ceramic knife with porosity of 0.04%; Both open porosity and closed porosity can be determined;
The specimen treatment period and determining period are short; The testing result is independent
of surface area of the specimen. Size, shape and distribution of pores, impurities and structure
defects due to raw material of ceramic and resulted from technological process like profiling,
sintering, etc. can also be determined when porosity is determined, which provides more
information for technological process research and control of ceramic.
To ensure the results accuracy and consistency of metallographic method in determining porosity
of zirconia ceramic, the following content shall be also specified for standard metallographic
determination method of porosity. The establishment of standard atlas: the amplification factor of
atlas shall be definite. Pores belong to microstructure and the testing results in case of different
amplification factors differ greatly. The amplification factor shall be determined according to size,
quantity and distribution of pores while atlas shall reveal the basic characteristics of pores in
zirconia ceramic knives. If amplification factor is too high, the area of field of view is too small and
 Applied Mechanics and Materials Vol. 873 25

the representativeness of pores is not sufficient. If amplification factor is too low, the pores included
in statistics and to be calculated are small and the quantity of pores is large. Specifications for
preparing specimens: metallographic specimens are usually taken from the area with the highest
porosity while the detecting area is usually 10 mm×10 mm or has diameter of Ø10 mm. Specimens
are prepared by processing them through coarse grinding, fine grinding, polishing, etc. and
specimen which can be observed with microscopes is obtained. GB/T 13298 can be referred to for
specimen preparation. Specifications for determining process: Because products failure usually
originates from the area with microdefects and the pores in zirconia ceramic in contact with
compact food belong to one kind of structure defects, the area with the worst defects of pore in the
field of view shall be chosen to determine the porosity. Observe the whole specimen in low
amplification factor at first to identify the area with the worst pore defects, then observe it in the
amplification factor of the standard atlas, compare it with the standard atlas to determine which map
is the closest one to it, and then report the porosity of this map as the porosity of this specimen.
Meanwhile, report impurities and defects found in the whole field of view when observing the
specimen in the determining report.
Metallographic method can determine the porosity lower than 0.5% when used for determining
porosity of zirconia ceramic in contact with food. It is a quick and effective method, which can also
determine the size, shape and distribution of pores as well as impurities and microstructure defects
and can provide more information for technological process research and control of zirconia
ceramic. Besides, the accuracy and consistency of testing result can be ensured through
standardization of specimen sampling and preparing as well as determining process and
standardization of standard atlas.

References
[1] Materials and articles in contact with foodstuffs-Cutlery and holloware-Part 5: specification for
sharpness and edge retention test of cutlery ISO 8442-5:2004, Switzerland: International
Organization for Standardization.
[2] Fine ceramics (advanced ceramics, advanced technical ceramics) -Determination of density and
apparent porosity ISO 18754:2003, Switzerland: International Organization for Standardization.