ASTM RR-C28-1004 1996
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24
September
1996
Committee
C28
on
Advanced
Ceramics
Subcommittee
C28.01
on
Mechanical
Properties
and
Performance
Research
Report
C28-1004
Interlaboratory
Study
to
Establish
Precision
Statements
for
ASTM
C1327,
Standard
Test
Method
for
Vickers
Indentation
Hardness
of
Advanced
Ceramics
ASTM
International
100
Barr
Harbor
Drive
West
Conshohocken,
PA
19428-2959
tf&^A-Vk
r
/99ir-
CIM7BC,
DEVELOPMENT
OF
CERAMIC
HARDNESS
REFERENCE
MATERIALS
J
/
/
R.
J.
GETTINGS,
G.
D.
QUINN,
A.
W.
RUFF,
and
L.
K.
IVES
Ceramics
Division,
NIST,
Gaithersburg,
MD
20899,
USA
Hardness
is
a
frequently
measured
material
characteristic
of
advanced
ceramics
Measurement
accuracy
\s
often
unknown,
and
uncertainties
of
20%
are
not
unusual.
To
remedy
this,
two
standard
reference
matenaU
(SRMs)
with
certified
hardness
values
of
nominally
15
GPa
are
under
development
at
NIST.
A
cobalt-bonded
tungsten
carbide
was
selected
for
the
Vickers
standard,
and
a
hot
isostatically-pressed
silicon
nitride
was
selected
for
the
Knoop
hardness
standard.
Prototype
SRMs
were
developed,
measured,
and
tested
f«
jepeataWity
and
reproducibility
of
their
hardness
numbers,
and
for
conformance
to
ASTM
standards.
These
SRMs
will
facilitate
testing
procedures
leading
to
higher
accuracy
and
precision.
1.
INTRODUCTION
Hardness
is
a
characteristic
of
ceramics
that
is
frequently
measured
for
materials
science
research
or
materials
engineering
and
characterization
purposes.
The
indentation
method
and
load
used
depends
upon
the
application.
For
research
purposes,
Vickers,
Knoop,
or
Berkovich
indenters
are
used,
typically
with
loads
from
0.01
to
9.8
N.
Rockwell
and
Brinell
indenters
are
rarely
used
for
ceramics
research,
but
are
widely
used
for
engineering
characterization.
Approximately
60%
of
worldwide
published
ceramic
hardness
values
are
Vickers,
with
loads
usually
up
to
about
9.8
N,
35%
are
Knoop,
the
majority
of
which
are
at
0.98
N,
and
5%
are
Rockwell
The
high
hardness
of
ceramics
is
important
for
cutting
tool,
and
wear
and
abrasion
applications.
1
The
difficulty
in
obtaining
accurate
and
precise
hardness
readings
is
often
not
appreciated.
Hardness
is
proportional
to
the
square
of
the
diagonal
length
of
the
indentation,
so
any
error
in
length
measurement
is
doubled
in
the
hardness
number.
Accurate
readings
require
a
low
overall
uncertainty
and
bias
in
this
length
measurement.
There
is
insufficient
space
in
this
paper
to
detail
all
of
the
factors
which
contribute
to
the
experimental
uncertainty
and
bias
in
hardness
measurement;
the
reader
is
referred
to
several
review
articles
for
specifics.
2
-
10
Diamond
indenter
geometry,
machine
vibration
and
operator
subjectivity
are
among
the
important
contributing
factors.
A
recent
Versailles
Advanced
Materials
and
Standards
(VAMAS)
round-robin
study
reported
an
uncertainty
of
10-15%
or
higher
in
the
hardness
measurement
of
two
aluminas."
One
of
the
four
primary
conclusions
of
the
round-robin
was
that
there
is
a
clear
need
for
hardness
reference
materials
for
ceramics
with
hardness
greater
than
10
GPa.
Progress
on
the
development
of
two
such
standard
reference
materials
(SRMs)
is
the
subject
of
this
report.
Z
GENERAL
Vickers
and
Knoop
micro-
and
macrohardness
machines
make
an
impression,
or
indentation,
and
enable
the
operator
to
measure
its
diagonal
lengths
with
an
attached
optical
microscope.
Most
current
ceramic
related
hardness
standards
specify
a
9.8
N
(1
kg)
indentation
load,
which
straddles
the
miaohardness
and
macrohardness
ranges.
4
At
lower
loads
there
are
problems
arising
from
the
load
dependence
of
hardness
4
-
6
-
9
and
measurement
uncertainty,
due
to
the
small
indentation
size.
Cracking
at
the
indentation
is
a
problem
at
higher
loads.
In
general,
it
is
desirable
to
make
as
large
an
indentation
as
possible
to
reduce
measurement
uncertainties,
without
causing
)
excessive
cracking
that
will
interfere
with
the
measurement.
Most
structural
ceramics
where
hardness
is
important
have
hardness
numbers
in
the
10-20
GPa
range.
The
prototype
V.ckers
and
Knoop
SRMs
now
under
development
will
be
indented
with
a
9.8
N
or
19.6
N
load
and
will
have
a
nominal
hardness
of
15
GPa.
A
19.6
N
load
may
be
necessary
for
the
Knoop
SRM
in
order
to
keep
its
total
uncertainty
to
5%
or
less.
Requirements
for
certified
Vickers
and
Knoop
SRMs
are
listed
in
ASTM
E
384-89
12
and
ISO
640-1984
13
2.1
Indentation
Measurements
Skill,
experience
and
meticulous
care
are
necessary
to
accurately
measure
the
diagonal
lengths
of
Vickers
and
Knoop
impressions.
Although
most
microhardness
machines
can
measure
diagonals
to
0.1
or
0.2
pm,
in
practice,
the
resolution
of
indentation
tips
and
the
subjectivity
of
the
viewer
can
easily
lead
to
variabilities
in
V.ckers
of
up
to
±1
M
m
in
tip
location.
2
-
10
The
uncertainty
is
even
higher
for
Knoop
hardness
because
of
the
small
angle
between
the
impression
sides,
and
potentially
lower
viewing
contrast
levels.
On
the
other
hand,
the
overall
uncertainty
is
offset,
compared
to
V.ckers,
due
to
the
greater
length
(-2.8X)
and
smaller
amount
of
cracking
inherent
in
Knoop
impressions.
Optical
resolution
limits
affect
both
V.ckers
and
Knoop
(but
especially
the
latter)
indentation
length
measurements.
4
^'
14
As
the
numerical
aperture
(NA)
of
the
lens
decreases,
lower
resolution
leads
to
an
underestimate
of
the
diagonal
length.
This
error
is
estimated
to
be
X/2(NA)
for
Vickers
impressions,
and
7X/2(NA)
for
Knoop,
where
X
is
the
wavelength
of
light.
For
a
typical
microscope
having
a
40X,
0.65
NA
objective
lens,
the
calculated
correction
for
green
light
(X=0.55
jim)
is
0.4
^m
for
V.ckers
and
3
M
m
for
Knoop.
These
are
significant
numbers.
This
correction
is
incorporated
in
two
ASTM
Knoop
standards;
one
for
glass
and
glass
ceramics,
15
and
one
for
ceramic
whitewares,
16
but
is
not
used
in
others.
12
An
alternate
measurement
procedure
that
does
not
involve
corrections
for
optical
effects
uses
a
scanning
electron
microscope
(SEM).
In
the
past,
the
uncertainty
in
SEM
magnification
inhibited
accurate
length
evaluation,
but
a
calibration
technique
has
been
developed
at
N1ST
to
address
the
issue.
The
higher
resolution
and
magnification
capability,
as
well
as
the
possibility
of
attaining
higher
accuracy,
prompted
NIST
to
use
SEM
microscopy
for
the
SRM
measurement
3.
MATERIALS
A
number
of
commercially
available*
advanced
ceramics
were
evaluated
for
their
suitability
as
hardness
SRMs.
The
materials
had
to
have
a
fully
dense,
very
fine-grained
(-1
/im),
uniform
microstructure,
and
be
opaque,
to
avoid
complications
of
poor
optical
contrast
that
are
typical
of
translucent
or
transparent
ceramics.
Some
of
the
materials
tested
had
elongated
grains,
which
when
indented,
gave
a
ragged
or
uncertain
appearance
to
the
resulting
impression
(see
Figure
la).
These
irregular
edges
are
a
consequence
of
fracture
or
displacement
of
individual
grains
along
the
impression
boundary.
Therefore,
for
a
polycrystalline
ceramic
SRM,
it
is
imperative
that
the
grams
be
equiaxed
and
as
fine
as
possible.
3.1
Materials
Selection
It
was
difficult
to
find
a
suitable
Vickers
SRM
prototype
material
Most
ceramics
cracked
at
the
indentation
tips
under
a
9.8
N
load
to
the
degree
that
it
interfered
with
the
diagonal
measurement.
A
tungsten
carbide
with
"Certain
commercial
equipment,
instruments,
or
materials
are
identified
in
this
paper
to
speofy
adequate
y
the
expeSeTalTocSure
Such
identification
does
not
imply
recommendation
or
endorsement
by
the
National
XTe
ol
Stands
and
Technology,
nor
does
it
imply
that
the
materials
or
equipment
.denUfied
are
necessanly
the
best
available
for
the
purpose.
摘要：
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ASTM RR-C28-1004 1996 是美国材料与试验协会发布的一项关于耐火材料测试与性能评估的标准参考文件。该标准规范主要涉及耐火砖、耐火浇注料及高温陶瓷等材料在极端热环境下的物理与化学性能测试方法，包括抗热震性、体积稳定性、高温强度及耐腐蚀性等关键指标。1996版为其重要修订版本，适用于冶金、玻璃、水泥及化工等高温工业领域。遵循此标准有助于确保耐火材料在实际应用中的安全性与耐久性，同时为工程设计与质量验收提供权威依据。该规范对从事耐火材料研发、生产及质量控制的专业技术人员具有重要参考价
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