Surface Modification Technologies XIII - Proceedings of the Thirteenth International Conference Held in Singapore

354 Pages·1999·40.922 MB·354\354

by  Sudarshan, T. S., Khor, K. A., Jeandin, M. (Eds.)

Surface Modification
Technologies XIII
Proceedings of the Thirteenth International Conference on
Surface Modification Technologies
held in Singapore
September 07-10, 1999
Editors (Proceedings).
T. S. Sudarshan
Materials Modification Inc.
2929-P1, Eskridge Road
Fairfax, VA 22031
K. A. Khor
School of Mechanical & Production Engineering
Nanyang Technological University
Singapore 639798
M. Jeandin
Ecole des Mines de Paris
Centre des Materiaux P.M.FOURT
B.P.87, 91003 Evry Cedex, France
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THE-INSTITUTE-Or:
MATERIAIS
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Copyright? 1999
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Library of Congress Cataloging-in-Publication Data.
ASM International
Surface Modification Technologies, Volume 13
Includes bibliographical references and index.
ISBN 0-87170-648-2
ASM International"
Materials Park, OR 44073-0002
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Contents
Foreword '" ix
Hard Materials 1
Surface Oxidation of Steels at Low Oxygen Pressures and Elevated Temperatures,
and its Impact on Gas Nitriding 3-11
BRIGITTEHAASE,MICHELESTILES,and JUANDONG
Effect of Ar Ion Bombardment on the Surface Layer of Ion Nitrided Cr-Mo Low Carbon Steel 13-19
K.P. KHOO,R.I. URAO,I.Y. OSHIMA,and K.Y. TERAKADO
Influence of Sputtering Parameters on Residual Stress of CoCrTaPt Magnetic Thin Film Coating 21-26
Y.H. LEE, L. Lu, and J.P. WANG
Analysis of Structure and Properties of Diamond Like Carbon Films by Ion Beam Deposition
ZHUPINGCHEN, AyO OLOFINJANA,and JOHNBELL ..................•.••...•....... ;.......•...................•••.....................•.........•........•..••.... 27-32
Microscopic Observation of Corrosion of Amorphous Carbon Coated Magnetic
Recording Disks with CrN Interlayer 33-39
SAMZHANG,M.1. TAN, X.T. ZENG,I. ANNERGREN,H. XIE, P. HING, and W.L. NG
Diamond Coating on WC-Co Tools 41-44
00.0 •••• 0•••••••••• 0••••••••••••••••••••• 0. 0••••••••• 0•••••••••• o.0••••••••••••••••••••••••••••• o••••••••••••••••••••••••••••••
JIANZHOU,RUNZHANGYUAN,JIANHUAWANG, BINGCHUMEl, and WEIHUAYu
Growth of SiCN Films by Magnetron Sputtering 45-52
J. WEI, Y. GAO,D.H. ZHANG,P.HING, and Z.Q. Mo
Formation of ~-C3N4 Grains by Sputtering 53-58
J. WEI and P. HING
Potential of Duplex Treatment: Combining Plasma Nitriding with Carbon Nitride Films 59-69
Y.Q. Fu, N.L. LOH, B.B. YAN,J. WEI, and P. HING
The Influence of FEP Additions on the Properties of WC-Co Coatings Obtained by
Detonation Spray Coating .. 71-81
o••••••••••••• 0•••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••••
D. SEN,K.R.C. SOMARAJU,D. SRINIVASARAo, and G. SUNDARARAJAN
Nucleation and Growth of Polycrystalline Diamond Particles on Ceramic Substrates by Microwave Plasma CVD 83-90
K. INDERJEET,S. RAMESH,and C.K. CHAKRABARTY
Lasers/Surface Melting 91
Sintering Behavior of Nano-Ceramic Coatings 93-101
J.TH.M. DE HOSSON,J. HOOIJMANS,and R. POPMA
Laser Surface Hardening of Steel by Low Power CO" Laser 103-107
NISARAHMAD,KHALILAHMADQURESHI,S. ATHARAB~ASJAFFRI,and MEHBOOBSARWAR
Electrodeposition and Evaluation of Modified Surfaces 109
An Instrument for Measuring Instantaneous Value of Internal Stress of Electrodeposit 111-119
K.S. RAJAM,INDIRARAJAGOPAL,and S.R. RAJAGOPALAN
The Effect of Pad Dimension on Growth of Flip Chip Electroless Nickel/Electroplated Solder Bump 121-126
K\vANG-LuNGLIN and HUEy-RuE TSAI
vi Surface Modification Technologies XIII
Crater Wear Mechanisms of TiN Coated High Speed Steel Tools 127-133
C.Y.H. LIM, S.C. LIM, and K.S. LEE
Parametric Impact on the Microstructure and Wear Behavior of Laser Surface Alloyed Iron Boride Layers 135-144
S.M. SHARIFF,G. SUNDARARAJAN,and S.V. JOSHI
Evaluation of The Abradable Performance of Clearance Control Coatings 145-150
B. VENKATARAMANJ,.K.N. MURTHY,and CH.V. SUBBARAO
Rapid Tools with High Quality Surface Finish and Strength Using High-Temperature Epoxy
Resin and Electroless Nickel Plating 151-156
FRANCISE.H. TAY,E.A. HAIDER,M. RAHMAN,lY. LEE, and TEDDYE.H. ONG
Thermal Spray Techniques 157
Morphology of Oxide in Thermal Sprayed Metal Coatings 159-168
KENJIMURA~MI, NAOYAFUJITA,YUKOHANATATE,SHIN'ICHIROADACHI,and HIDEONAKAJIMA
Thermal Shock Testing of Plasma Sprayed Discs 169-176
Y. Lu, H.W NG, and K.A. KHOR
The Effect of Top Coat Sintering on Ceramic Spallation in Plasma-Sprayed Thermal Barrier Coatings 177-182
J.A. THOMPSON,W. JI, and T.W. CLYNE
Comparison of Computer Modeling and Measurements in Plasma Spraying ofNi and Al0 183-188
2 3
Yu. BORISOV,I. KRIVTSUN,A. MUZHICHENKO,E.E. LUGSCHEIDER,and U. ERm
A Process Control Methodology for
D.C. Plasma Spraying 189-193
C.~. ANG, H.W. NG, S.C.M. Yu, and Y.C. LAM
A Comparative Study of the Performance of Two Diverse
Detonation Spray Systems 195-205
P. SARAVANANK, .R.C. SOMARAJU,D. SRINIVASARAo, V. SELVARAJANS,.V. JOSHI,and G. SUNDARARAJAN
Nitride Coatings 207
Surface Oxidation of Aluminum Nitride Thin Films 209-215
YOSHIHISAWATANABE,YUJI HARA, TAKESHITOKUDA,
NOBUAKIKITAZAWA,and YOSHIKAZUNAKAMURa
Deposition of AIN Films by RF Reactive Magnetron Sputtering: Effect of Processing Parameters 217-224
J.C. OLIVEIRA,A. CAVALEIRO,and M.T. VIEIRA
Evaluation of Modified Surfaces 225
Characterization of Gas and Liquid Nitrocarburizing Microstructure and
its Influence on Wear and Mechanical Properties 227-233
NURIALLORCA-IsERN, FRANCISCOBORREGO,GUILLERMOGONZALEZ,and MONTSERRATESPANOL
Microstructure and Mechanical Properties of PVD WC/C Coatings 235-240
NJ.M. CARVALHO,A. VAN DER BORDEN,J.TH.M. DE Hesson, and AJ. HUIS IN'T VELD
Characterization of Sol-Gel Derived PZT Films Prepared at Low Temperatures 241-246
KUN'ICHI MIYAZAWA,JUNYAYANO, MASASHIKAGA, YOUSUKEITO, KUNIOITO, and RYUTAROMAEDA
The Stability of Aluminide Coatings on Ni-Based Superalloy In-738 in Electrochemical Hot Corrosion Test 247-251
M. SAREMI,M. ZAMANI,and S. KHALICHI
SrI/face Modification Technologies XIII vii
Transparent Conducting Coatings: Applications, Materials, and Deposition Techniques .............................................. 253-256
S.H. KESHMIRI, M.M. BAGHERI MOHAGHEGHI, S. OJAGHI SHIR-MARD, and
MAHMOOD REZAEE ROKN-ABADI
Calculation of the Adhesive Strength by Using the Fracture Mechanical Test Methods ................................................ 257-261
H. SAUER and H. WEIB
Influence of the Pulse Duration on the Application of Laser Shock Technique for
the Debonding of Coating ................................................................................................................................................ 263-268
M. BOUSTIE, E. AUROUX, J.P. ROMAIN, and D. BERTHEAU
Gelling-Induced Autophobicity Effects in Multi Layered Sol-Gel Coating Systems ..................................................... 269-275
Su NEE TAN, XIANTING ffi'lG, and BART FOKKINK
Posters ............................................................................................, ................................................... , ................. 277
Adhesive Wear Resistance of HVOF Sprayed Cu Based Alloy Coating ........................................................................ 279-290
MITSUMASA SASAKI, TOMOKO MIYAZAKI, TADAOKI ARAKAWA, and RYOICHI URAO
Preparation of Fluorinated Amorphous Carbon Nitride Films by Magnetron Sputtering .............................................. 291-298
HARUO YOKOMICHI
Acoustic Emission Evaluation of Plasma Sprayed Functionally Graded Thermal Barrier Coatings ............................. 299-306
L. Fu, K.A. KHOR, H.W. NG, and T.N. TEO
Wear and Friction of Diamond Coatings Deposited on Pure Titanium ........................................................................... 307-315
Y.Q. Fu, N.L. LOH, B.B. Y AN, C.Q. SUN, and P. HING
Improvement of Interfacial Structure of Diamond Coating on Ti by
Duplex Surface Engineering ............................................................................................................................................ 317-323
BlBo Y AN, NEE LAM LoH, YONGQING Fu, CHANG Q. SUN, and PETER HING
Wear Resistance of Three Chromium-Based Coated JIS SKD61 Tool Steels ................................................................ 325-331
LIU-Ho CHIU, CHIH-Fu YANG, and PING-MING LIU
Effect of Surface Modification on Room Temperature Tensile Properties of
Fe-18AI and Fe-18AI-5Cr Alloys .................................................................................................................................... 333-337
Lru-Ho CHIU, PEE-YEw LEE, and CHIEH-LuNG CHANG
Reactive Plasma Spray of Nickel Aluminide Coatings from Elemental Ni and Al Powders ......................................... 339-344
SACHIO OKl, TETsuRou KIMATA, AKIRA lKENAGA, and MAKOTO KAWAMOTO
Surface Microstructure Effects of Single Crystal Tungsten After Nd: YAG Laser Irradiation ....................................... 345-351
Yun KAWAKAMI, SHINYA SASAKI, and EIICHI OZAWA
Surface Modification of PTFE by Plasma Treatment ..................................................................................................... 353-358
C. LIU, S.M. GREEN, R.D. ARNELL, A.R. GIBBONS, L. REN, and J.TONG
Effects of an Additive on the Corrosion Performance of
Electroplated Zinc on Different Alloy Steels .................................................................................................................. 359-365
HYUNG-JOON KIM
Subject Index ................................................................................................................................................................... 367-370
Author Index .................................................................................................................................................................. 378-383
Hard Materials
Surface Oxidation of Steels at Low Oxygen
Pressures and Elevated Temperatures, and its
Impact on Gas Nitriding
Brigitte Haase
Hochschule Bremerhaven
An der Karlstadt 8, D-27568 Bremerhaven, Germany
Michele Stiles and Juan Dong
Institut fOrWerkstofftechnik
Badgasteiner Str. 3, D-28359 Bremen, Germany
Abstract When this layer isformed spontaneously near room temperature, it
is also thinner than 10nm.
At elevated temperatures, i.e., during the heating inanitriding
Low alloy steels arecovered with athin oxide layer containing furnace to 500 or 600°C, oxide layers tend to grow fast when
Fe0 at the metal and Fe0 at the solid/atmosphere interface. It oxygen ispresent, even atlow partial pressures. The result isoxide
3 4 2 3
can be shown by means ofmodern surface analysis that these layers layers that, which are at least one order of magnitude thicker than
are usually less than 10nm thick. The formation ofFe0 isheld to oxide layers formed atroom temperature, their thickness depending
3 4
be a precondition for the formation of Fe203, the latter being not only on oxygen partial pressure but also on kinetic parameters,
responsible for corrosion protection and the slight passivity ofiron such asheating rate and time.
and low alloy steels. Experimental investigations were carried out to study the
Passivity canbesignificantly increased byincreasing chromium formation of oxide layers at different temperatures and oxygen
concentration, i.e., in the case of stainless steels with chromium partial pressures, and their impact on subsequent nitrogen uptake
contents exceeding 13wt.%. Stainless steels form anoxide layer at in an ammonia atmosphere. The objective ofthe investigation was
the surface in which chromium oxides (i.e., Cr203) are enriched. to explain contradictory and irreproducible results in practical gas
Surface Modification Technologies XIII
Edited by T.S. Sudarshan, K.A. Khor, and M. Jeandin
© ASM International, Materials Park, Ohio, 1999 3
4 Haase, Stiles, and Dong
Table 1.Properties of the Iron Oxides2,3,4
Phase Structure 02-Lattice Formation Properties
Fel_xO FCC (NaCI) FCC >570°C Antiferromagnetic
F~04 Inverse-Spinel Vacuum Heat Treatment Highly Conductive,
FCC
Magnetite (AlMg04) of y-F~03 Antiferrimagnetic
2
a-Fez03 Heat Treatment of
Corundum (Al0 HDP Antiferromagnetic
Haematite 2 3) y-F~03 in Air
y-F~03 Cautious Oxidation of
Spinel FCC Ferrimagnetic
Maghemite F~04
nitriding and, more generally, in heterogeneous surface treatment very different crystal structure and electrical properties. When
processes in gas atmospheres at elevated temperatures. 'Y-Fe203is heat-treated at high temperature and made to
undergo the transition to a-Fe0 it appears to lose almost
1.0Introduction 2 3,
all of its sensitivity regarding reductive gases. This is the
reason for Fe203not having attracted much attention asagas
Real surface modification processes at elevated sensor.'
temperatures take place in reactors or furnaces, which are Surface oxidation ofiron occurs atelevated temperatures
heated toreaction temperature during aperiod, which depends even at low oxygen partial pressure. Oxide layers formed at
onthe type and supplier ofthe reactor. In contrast tonitriding 300°C are easily one order of magnitude thicker than oxide
reaction conditions, heating parameters are usually not well layers formed at RT, even after short oxidation times. Real
defined. Reactions occurring during heating can influence world reactors and furnaces are likely to contain sufficient
theresult ofthe surface modification process, especially when oxygen for oxide layer formation, especially during heating
the process is controlled kinetically and by the composition to reaction temperature. This makes it probable that
ofthe furnace gas atmosphere, heating time and rate influence thermochemical processes at elevated temperatures have to
surface composition.' A reaction likely to occur in the deal with the reactivity ofiron oxide layers rather than that of
presence of oxygen during heating is surface oxidation. A metal iron (steel).
surface modification process, which may be influenced by Inthe case ofgas nitriding ofstainless steels, the problem
prior surface oxidation, isthe gas nitriding process, consisting of passive oxide layers is well known. The composition of
of ammonia dissociation and nitride formation at steel high-chromium steel oxide layers is rich with chromium
surfaces. Gas nitriding usually takes place in ammonia at oxides, thus preventing notonly corrosion but alsothereaction
temperatures between 500 and 580°C. with ammonia to form iron and chromium nitrides.
Metals are very sensitive to surface oxidation. Nearly all Consequently, high-chromium steels are not easily nitrided
metals and alloys are covered by athin oxide layer « 1anm) in ammonia. On the other hand, gas nitriding (not only) of
which is formed at room temperature. Metal alloys can be stainless steels has been reported to be possible owing to the
used asengineering materials because this oxide layer causes addition of small amounts of oxygen to the nitriding
passivity and prevents them from further oxidation and atmosphere. This oxygen addition is said to be responsible
corrosion. Oxide layers formed at steels are complex in for the formation of Fe304(magnetite), which promotes
nitrogen uptake and nitride formation/' See Ref.7-10 for more
structure and composition.
Three different iron oxides are stable at temperatures and deeper information ongas nitriding and nitrocarburizing.
between room temperature (RT) and nitriding temperature The influence of oxygen and of oxide layer formation
on nitrogen uptake regarding·nitriding inammonia was studied
of approximately 580°C; the Fe-II-oxide FeO (or Fe1_xO)is
experimentally. Itwastheaimoftheinvestigation tobring some
unstable at these temperatures and undergoes
light in the sometimes contradictory findings regarding the
disproportionation to form Fe and Fe304. Some information
formation ofiron and chromium oxides and their nitridability.
about the oxides isgiven inTable 1.2,3.4
There are two types of Fe203: a-Fe203, which has a
2.0 Methods
corundum-type crystal structure, and y-Fe203, which has a
spinel-type crystal structure. Conversion bet°ween these two
types and magnetite, spinel-type crystal Fe3 4is carried out Experiments were carried out with different steels. This
by processes of oxidation, reduction and transition. A report concentrates ontheresults ofonematerial, thehigh alloy
reversible oxidation-reduction process can be used toconvert stainless steel X4CrNi18-10 (SS304), composition asgiven in
between Fe304 and y-Fe203• The a andyphases ofFe203 have Table 2.
Surface Oxidation of Steels at Low Oxygen Pressures and Elevated Temperatures, and its Impact on Gas Nitriding 5
Table 2.Specimen Material
Composition, wt. % .
Material Heat Treatment
C Cr Ni Fe
X4CrNi18-10 ~0.07 17- 19 8.5 - 10.5 Balance Solution-annealed
Table 3.Oxygen Pressure in Various Atmospheres
Atmosphere Oxygen Air Nitrogen Ammonia Addition
p(02)lbar 1* 0.2* 1x 10-5** 1X 10-27**
'Measurement by mass spectrometry, "Measurement by oxygen sensor.
Table 4.Specimen Treatment in the Furnace: Heating and Nitriding
Heating Nitriding
Conventional N2P(02) = lO-5bar 580°C, K = 10,2 h
N
Pre-oxidation Air, 300°C, 30 min. 520oe, K = 10,_4 h
N
Oxidation Air, 5?0°C, 10min. -
Oxygen-Reduced N-33 vol.% NH3 580°C, K = 10,2 h
2 N
550°C, 20 min.
Oxygen-Reduced N2-33vol.% NH3
Nz-32.6 vol.% NH3, - 2.3 vol.% air
550°C, 60 min. 550°C, 60 min., N-33
Oxygen-Reduced N-33 vol.% NH3 2
2 Nz-32.6 vol.% NH3, - 2.3 vol.% air vol.% NH3, KN= 10
Prior to treatment in the furnace, the specimens were analysis depends onelement specific sensitivity factors, sothose
cleaned/degreased using acetone/ultrasound. Oxidation and error limits asgiven inTable 5are equally element specific.
nitriding were performed in an inert quartz reactor. The Depth profiling was done using an argon ion sputter
oxygen partial pressures in the various gas atmospheres are gun with a sputter current of 1 rnA. The sputtered surface
given in Table 3. area was 4 x 3mm. The sputter rate depends onthe materials;
Six different furnace processes were performed, with it is lower for ceramics and higher for metals. All depth
different oxygen partial pressures at different temperatures profiles have been calculated using the sputter rate of Si02,
i.e., 4 nml300 s. The sputter rate for steel is known to be
during heating and nitriding. These processes are described
slightly higher (5 nm/300 s). Though the examined
in Table 4.
specimens were covered with multi-component layers, the
Prior to heating, the furnace was flushed with nitrogen
sputter rates were assumed to be uniform. When sputtering
and then with nitrogen /hydrogen, until oxygen could not be
rough surfaces of composite materials, however, different
detected any longer by mass spectrometry. Heating to
sputter rates may increase the concentration error limit.
nitriding temperature took about 40 min.
Surface composition was analyzed qualitatively and
3.0 Results
quantitatively using ESCA. The x-ray source was MgKa. The
detection limit in photoelectron spectroscopy depends on the
element examined but islower than 1at.%.Depth resolution is The composition of the clean stainless steel surface is
about 1nm but depends on surface roughness. Quantitative illustrated bythe XPS depth profile ofFigure 1.The specimen
6 Haase, Stiles, and Dong
50
eft 40
~
ctS
c
g
30 '-0
ctS -
~'- .•.•.•.. -
c \ .•.•.•.. -.•.•.•.. ..........•......
Qg) \ .....
20 \ .-.-._------.-
o "
o ==~~ ~~-------'-------------_ _ -.
cr:-~--::-::-:.:.:0::.:-:"::::
10
-------------------
o~--~----~--~----~--~----~--~----~--~--~
o
2 4 6 8 10
Depth, nm
Fig. 1: XPS depth profile of elements in a clean stainless steel surface.
Table 5_Error Limits for Quantitative Elemental Analysis
Element Specification Error Limit
N - 5%
0 20 at.% 2%
C Base Material 10%
iscovered by athin sorption layer rich with carbon and oxygen detected throughout the analyzed depth of 300 nm, surface
(1 nm), and an oxide layer containing iron and chromium hardness of the ammonia-treated specimen (385 HVO.5) is
oxides. Oxygen was found throughout the analyzed depth of slightly higher than the substrate hardness (320 HVO.5).There
10 nm. No chromium enrichment could be detected at the was little nitrogen uptake considering the high chromium
surface. content ofthe base material, and the thickness ofthe nitrogen
After preoxidation inairfor 30min, surface composition containing layer is low, despite the relatively long nitriding
has not changed significantly, as can be concluded from the time of2h.Disregarding nitrogen content, the depth profiles
depth profiles of Figure 2. Carbon-rich sorption and oxide ofthe conventionally nitrided specimen resemble the profiles
layers can still be found, their overall thickness is of Figure 2.
approximately 10 nm. Chromium enrichment did not occur A zone of 150 nm depth is depleted of iron whereas
at this temperature. chromium isenriched; besides, alotofoxygen isfound. Using
However, surface composition is affected strongly after element peak analysis, it can be shown that chromium and
10 min of oxidation in air at 570°C, as shown in Figure 3. the remaining iron are bound as oxides, so that a thick
Oxygen was detected throughout the analyzed depth of chromium oxide layer was formed atthis temperature, which
70 nm, chromium concentration is enhanced whereas there hasprevented themetal from nitrogen uptake andhas hindered
is an iron depletion. The affected zone is thicker than 70 nm chromium nitride formation, owing to the thermodynamic
and exceeds the oxide layers formed at lower temperatures stability of chromium oxide. Chromium nitride formation,
byroughly one order ofmagnitude. Up toadepth ofmore than however, isessential for the high surface hardness ofnitrided
30nrnthe oxide layer consists mainly ofchromium oxides. high chromium stee1.
The concentration profiles of Figure 4 were obtained This severe oxidation could have occurred only between
when the stainless steel was nitrided conventionally i.e., 300 and 580°C, before ammonia was introduced into the
heated innitrogen tonitriding temperature of580°C, followed reactor. Thus a relatively small partial pressure of oxygen
by the ammonia heat treatment. Although nitrogen can be (less than 10-5 bar, see Tables 3 and 4)-is responsible for