THE AMERICAN SOCIETY OF MECHANICAL ENGINEERS

345 E. 47th St, New York, N.Y. 10017 96-GT-446

The Society shall not be responsible for statements or opinions advanced in papers or discussion at meetings of the Society or of its Divisions or ,
Sections, or printed in its publications. Discussion Is printed only If the paper Is published in an ASME Journal. Authorization to photocopy
material for internal or personal use under circumstance not falling within the fair use provisions of the Copyright Act is granted by ASME to
libraries and other users registered with the Copyright Clearance Center (CCC) Transactional Reporting Service provided that the base fee of
$0.30 per page Is paid directly to the CCC, 27 Congress Street, Salem MA 01970. Requests tor spacial permission or WU( reprocittion should be ad-
dressed to the ASME Technkal Publishing Dscanment

Copyright 0 1998 by ASME NI Rights Removed Printed In USA

DEVELOPMENT AND FABRICATION OF CERAMIC GAS TURBINE COMPONENTS

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

11111111111111111101111
Koichi Tanaka, Sazo Tsuruzono,
Toshifumi Kubo and Makoto Yoshida
R&D Center, Kagoshima
Kyocera Corporation
Kokubu, Kagoshima, Japan

ABSTRACT thermal efficiency. For example, the thermal efficiency of the

Kyocera has been developing various ceramic components for small sized engines under 500kW is 15 20% • which hinders

gas turbines, under the Ceramic Gas Turbine (CGT) Project funded their popularity. In order to improve the thermal efficiency, it is

by the Japanese Government. This project has set a turbine inlet necessary to increase the turbine inlet temperature (TIT). There
temperature (III) of I350 °C as a final target. are, however, some difficulties for increasing the TIT when metal

For 1350°C ITT, we have developed a new silicon nitride components are used. For example, it is difficult to apply the

material SN281, which has high stress rupture strength at elevated internal cooling systems because of the size limitation of

temperatures up to 1500 °C. This material has excellent oxidation components. For this reason, ceramic components have been

resistance as well, actively investigated as tmcooled beat resistive components for

We have also developed improved sintering and inspection high thermal efficiency gas turbine engines.

technologies for the use of SN281 as engine components. We are Ceramic gas turbines (CM) have advantages such as the use of

able to fabricate rotors and nozzles of the gas generator turbine uncooled components, energy saving, low emissions and,

(GM) in good agreement with design geometry requirements, by neecOess to say, high thermal efficiency. A 300 kW class COT

optimizing sintering conditions. Small defects were also project, which is administered by the New Energy and Industrial

siccessfully detected by microfocus X-ray radiography. The Technology Development Organization (NED)) and sponsored

SN281 rotors have attained 120% of design rotating speed at by the Ministry of International Trade and Industry (MITI), is

room temperature being carried out in Japan". The project deals with developments

of three fferent type engines. They are CGT301, 302 and 303.

INTRODUCTION The development of CGI301 has been reported elsevAtere 2).

The advantages for gas turbines include small size, light weight, Kyocera has been supplying various kinds of ceramic

high output power, mtdti-fuels capability, low emissions, low components for the last two programs. C. 02 is the

noise and low v i brati on. However its only shortcoming is its low development of ceramic components for the stationary type

Presented at the International Gas Ttubine and Aeroengine Congress 8r Exhibition

Birmingham, UK — June 10-13, 1996
regenerative two - shaft ceramic gas turbine for cogeneration, SN252. SN281 shows excellent oxidation resistance. Details of

which is conducted in cooperation with Kawasaki Heavy the characteristics of this material are given below.

Industries, Ltd. (KHI) 3). CG1303 is the development of the

ceramic components for the mobile type regenerative two - shaft ELEiLIRAL.SThala111

ceramic gas turbine for electric power generation, which is The flexural strengths were measured according to JIS R 1601

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

conducted in cooperation with Yanmar Diesel Engine Co., Ltd and 1604. Figure 1 shows the as-machined flexural strength of
(yDE) 4).
SN281 and SN252 up to 1500 °C. The strength of SN281 is

In 1995, engine tests at 1200 °C (midterm target of 111), were 861MPa at room temperature, 606MPa at 1400 °C and 546MPa at

successfully carried out in uncooled systems 3). All these ceramic 1500°C. The room temperature strength is about 40% higher than

components were made of SN252. This SN252 had been that of SN252. At high temperatures the flexural strength of

developed formerly as a high strength silicon nitride, with use up SN281 is much higher than that of STC52. The higher strength

to 1371 °C. For a final target of 1350 °C TIT, a new material with can be attributed to two reasons. One is the fine grain structure

high fast fracture strength and high stress rupture strength at of the matrix. The grain growth has been restrained as a result of

temperatures above 1350 °C is required. Oxidation resistance is controlling the a -4$ phase transformation of silicon

also important for the material, since a long duration time is nitrides). The other is a grain boundary phase with higher melting

necessary for the final COT engine. point as because of optimized sintering additive composition.

In order to achieve the final target, we have developed a new

silicon nitride material, SN281. SN281 has been developed with 1 000
the aim of improving the heat resistance and oxidation resistance o_ 900
800
of the grain boundary phase. As a result of research and 700
cs) 600
development. SN281 has high strength at elevated temperatures 500
400
up to 1500°C and oxidation resistance equal to that of silicon .
300
carbide. In this paper, we will present characteristics of SN281,

engine component fabrication technologies developed for

9 200
100
0
1 • SN281
• SN252

200 400 600 800 1000120014001600

SN28I, reproducibility of design geometries, inspection of
temperature (C)
components and results of proof testing gas generator turbine
Figure 1. As-machined flexural strength
(GG1) rotors.

THE CHARACTERISTICS OF SN281 Figure 2 shows the as-processed flexural strength. The strength

Two points are improved for 5N281; fine grain size structure and of SN281 is 657MPa at room temperature, 537MPa at 1400 °C and

oxide type grain boundary phase with a high melting point. For 470MPa at 1500 °C. The room temperature strength is about 40%

the SN281 we have achieved higher strength than SN252 up to higher than that of SN252. The reason for the high strength is

1500 °C. SN281 has better creep resistance than SN252. The considered to be low surface roughness which is caused by

fracture toughness of S1C81 is equal to or higher than that of restraint of Si02 decomposition during the sintering.

2
 1000
Ca. 900 1000
Nam nuts tint
X 800 700 811.1M1 MI 111.111 SIBIU
ma tairsinintani
W1111
.c 700
15) 600 amt. „ 500 Mi MIT 11111fi 1114
a)
• 500
111 is Mill 'il

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

u,
s 400
4t- 300
300 Il• SN28 II
3 200
x
a' 100
0
1 • 5N281
• SN252

200 400 600 800 1000120014001600

• 5N252( t 1371t)
11111 11 1 1 11
100
temperature (t) 0.0010.0 0.1 1 0 100 1000
Figure 2. As-processed flexural strength failure time (hr)

Figure 4. Stress rupture at 1400t .

STRFSS RUPTURE AND CRFFP RATE.

The stress rupture at 1200 °C and 1400 °C are shown in Figure 3

i o-4 —,===
and Figure 4, respectively. The characteristics were measured INIMNIN•1=11
.;

according to JIS R 1612. The allowable stress for 100hr with no

creep rate ( /hr)
10-s
failure is 550M1'a at 1200 °C and 450MPa at I400 ° C. These

strengths are 150 200 MPa higher than those of SN252. 1 o6

1000
700 lliEfilarF lo-7
; below detection knit ;

a. 500 INFingi 104

F' mit liii

100 ZOO 400 600 1000
stress (MPa)
300
V_ • SN281 Figure 5. Creep rate
• SN2S2 • SN281 at 1400t

100
11 • SN2S2 at 1400t
o SN281 at 1200t
0.0010 01 01 1 10 100 1000
o SN252 at 1200t
failure time (hr)

Figure 3. Stress rupture at 1200t resistance of SN281 is considered to be about 200 °C higher than

that of SN252 in the result.

Figure 5 shows the creep rate of SN281 and SN252. The creep

rate at 1200 ° C of SN281 is lower than detection limit and creep EBACILIREMICENESS

deformation was hardly observed The creep rate at 1400 °C is Fracture toughness measured by the SEPH method is shown in

approximately the same as that of 5N252 at 1200 °C The heat Figure 6. It was measured according to JIS R 1607 at room

temperature and JIS R 1617 at high temperature in N2. It is

3
 •

6.2MPa • m 1/2 at room temperature and is the same as that of 10

SN252. It is 0.8MPa • m than that of SN252 at 1400 °C 1==ara:::
...=LITAN;
niunniuuu
SINC81 preserves high fracture toughness up to high temperature. 111111•1111111M1•1111111
This phenomenon may be explained from the higher melting
Ennui
imaminnue.
••11••••01
point of grain boundary phase than that of SM252.

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

.7172;7811
■IIMMMINE•3 • 514252

100 1000
exposure time (hr)

Figure 8. Change of weight gain at 1500t

• $•28
• 514252
has not shown any weight gain at temperatures lower than 900 °C
200 400 600 800 moo two loco ism
temperature (t) Above 1000°C, the weight gain increases with rising
temperature. The oxidation rate is approximately equal to that of
Figure 6. Fracture toughness by SEPB
method silicon carbide. The high oxidation resistance of S14281 is due to
the grain boundary phase being an oxide and not containing any
nitrogen.
OaDATIONEESISMUCE The flexural strength at room temperature after oxidation is
The weight gain after oxidation at 800 °C •-••• 1500°C in air for shown in Figure 9. The strength of SM252 decreases after

100hr is shown in Figure 7. The change of the weight gain at exposure to oxidation with noticeable oxidation weight gain. On
1500°C is shown as a function of time in Figure 8. The test
specimens were not subjected to heat treatment at all to 200
2 180
investigate the exact oxidation resistance of the material. SN281
19 160

10 j,t 140
8 120
o 1 111111-11•11=1•111-- 47,100
5 80
-4

cn
c 60
01 94281
13 40
a) as Nal
raras -a 20 -0- SN2S2
001 OMMinnn 0 I
• 514281 800 900 1000 100 1200 1300 1400 1500
:et
0.001
-5-

- - - -L • 5144252 oxidation temperature (t)

800 900 1000 1100 1200 1300 1400 1500
oxidation temperature (t) Figure 9. Flexural strength after oxidation for
100hr
Figure 7. Weight gain after oxidation for
100hr

4
the other hand the strength of SN281 increases after exposure to Apart from material characteristics, geometric precision is also
oxidation, at all temperatures. The healing effect of oxidation an important consideration in effectively utilizing ceramics as
may overcome strength degradation by grinding damage. gas turbine components. It is especially important to make the
sintered parts in accordance with design geometry requirements.

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

ARP U CATION OF 5N281 FOR CERAMIC GAS TURBINE since the blades of rotors and nozzles are cEfficult to machine after
COM PCNDITS sintering.
FABRICATION PROCFSS FOR CFRAMIC GAS TURRINF Ceramics shrink 30 •••• 60% by volume during sintering. Also
CohrfinallibaS ceramics are deformed by their own weight or subjected to surface
Figure 10 shows the fabrication process for ceramic turbine decomposition during sintering. SN281 uses sintering adcitives
rotors and nozzles. Silicon nitride powier and sintering add ti ves with a higher melting point than those used in SN252 thereby
are weighed and the mixture milled f or 48hr. The mixture is dried reducing the deformation caused by weight for SN281
and the binder is added. The mixture is molded by slip casting. components. It is expected that the deformation by
The green bocfies are dried, dewaxed and densified in a controlled decomposition reaction is smaller because the change of
atmosphere sintering process. The sintered bodes are machined composition during sintering is restrained. Consequently, it is
into their final component shape After machining, heal easy to predict the exact shrinkage or deformation and to restrain
treatment and inspection are carried out. The heat treatment is the deformation for SN281. Modification of molds is still
performed in order to heal the grinding damage necessary, however.

RAW MATERIALS OD GOT Intocs

SILICON NITRIDE POWDER SINTERING ADDITIVES
The car rotor of CGT302 is shown in Figure 11. This is a large
MILLINGI
axial rotor whose cE omelet is 146mm and blade length is 12mm.
(SLIP PREPARATION I
i Figure 12 compares measured and design values of blade profile
ISLIP edam
[DRTINGI tolerance for SN252 and SN281. The difference between the

IDEWAXINGj desi gned and measured value is maximtzn 0.4mm for Sht252. On

ISINTERINGI the other hand, the measured difference of sN281 is maximum

IMACIOIING I +0.16mm. The design tolerance range varies from -0.1 -- +0.2mm
!NEAT TREATMENq and sN281 shows good agreement with the drawing requirements.
I FINAL INSPECTION I

Figure 10. Fabrication process for ceramic turbine (hi GOT nozzle assembly
rotors and nozzles The GUT nonde assembly of Ca 302 is shoat in Figure 13. It
has 21 nozzle segments and they are bound with SiC fiber 3).
Figure 14 shows the measured result of the nozzle geometry.
IMPROVFMFNT OF flFrIMFIRICAI PRPCISION TIC TO The difference between the designed and measured value is
SinthictlEadgiLaC maximum 0.3mm for SN252. On the other hand, the measured

5
 GGT nozzle segment

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

Figure 11. GGT rotor of CGT 302

—0.40 GGT nozzle assembly

—0.10 Figure 13. GGT nozzle assembly of
GGT 302

—025--0.30 0.15
—.0.10 I 0.10
SN252 SN281

Figure 12. Measured results of GGT

rotor blade geometry 0.08

—measured value
----designed value 0.17
SN252 SN281
clifference of SN281 is maximum +0.15trun. The target tolerance
is -0.1 ^- +0.2mm and SN281 shows good agreement with designed
Figure 14. Measured results of GGT
nozzle blade geometry
geometry.
—measured value
----designed value
INSPECTION
Improvements in the precision of nondestructive inspection is components whose defects were detected by the microfocus X-ray
crucial to making high quality components. It is difficult for the radiography were eliminated before the proof testing.
conventional X-ray radiography to detect the defects of thick
components such as rotors. The detection limit is improved by a PROOF TEST OF rriT 10 , ROTOR

microfocus X-ray radiography. Figure 15 shows the X-ray film of Proof test of rotors made of SN281 were carried out to evaluate
the rotor by the microfocus X-ray radiography. The white speck the fabrication process. Figure 16 shows the maximum principal
is a pore that developed during molding. The size of the speck is stress distribution of the COT 302 rotor at a proof speed of
about 0.1nun and the thickness of the rotor is 25mm. The COT 91.200rpm. This figure was obtained using the finite element
method (FEM). The proof speed is defined as 120% of design

6
 Photo Sonsor

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

microfocus conventional

Figure 17. System for the cold spin

Figure 15. X-ray film of the rotor by test
microfocus X-ray radiography

Figure 18. Photograph at the

359MPa fracture moment

permitted on any location on the component. The proof test

367MPa
reveals weak points in every step of the fabrication process such

as raw material, molding, sintering and machining.

Figure 17 is a schematic of the cold spin testing set up. A

ceramic rotor with metal shaft is suspended by a spindle in a

vacant chamber and is driven by an electrical motor until the

374MPa
370MPa failure occurs. Photographs at the instant of fracture are taken and

failure speed of the turbine rotor is measured by the system. At

Figure 16. Distribution of the
the moment when the sensor perceives fmctoanissions of the
maximum principal stress for MT
302 rotor at 91,200 rpm rotor, a strobe lamp flashes and the photographs at the failure are
6.7).
taken Fi gure 18 shows an example photograph at the fracture

speed. The maximum principal stress is 380MPa and high stress moment.

occurs throughout the disk. Therefore no critical defect is

7
 600 5) The SN281 rotors have attained proof speeds in excess of
91,20Orpm.
500
In order to commercialize ceramic gas turbines, long term
0 400
0
P2 durability tests need to be completed and cost reduction steps need
300
to be taken.

Downloaded from http://asmedigitalcollection.asme.org/GT/proceedings-pdf/GT1996/78767/V005T13A024/4465239/v005t13a024-96-gt-446.pdf by guest on 04 March 2024

200

? 100 ACKNOVVLEDGM ENT

The present study has been carried out under contract in a ceramic
25 50 75 100 125
rotating speed ( X 1,00Orpm) gas turbine program. The authors express deep appreciation to the
Agency of Industrial Science and Technology, New Energy and

Figure 19. Results of the cold spin test Industrial Technology Development Organization, Kawasaki

• SN281 Heavy Industries, Ltd., and Yanmar Diesel Engine Co., lid..
• 5N252
• 1200t CGT design rotating speed
o 1350t CGT design rotating speed REFERENCES
1) T. Mtaayarna, K Nagata, H. Abe, and H. Ogiyarna, 1995,
Figure 19 shows the proof test results of the car rotors Made of "Current Status of 300kW Industrial Gas Turbine R&D in Japan".
SN281. Four rotors attained the proof speed of 91,200rpra The ASME95-GT-445.
average burst speed of the rotors made of SN252 is below 2) M.Tatsuzawa, T.Taoka, T. Sakida, and S.Tanaka, 1995,
90,000rpm. The result shows the improvement of the material "Development of 300kW-Class Ceramic Gas Turbine (CGT301)
strength of SN281. Burst spin testing of the SN281 rotors is Engine System", ASME95-GT-201.
planned in the near future. 3) K Nisio, J. Fujioka, T. Tatsumi, and I. Talcehara, 1995,
"Development of 300kW Class Ceramic Gas Turbine (CG1302)",
SUM MARY ASME95-GT-264:
The new silicon nitride material SN281 has been developed by 4) M. Murota, I. Ohhashi, Y. Ito, and S. Aralcawa 199$,
optimization of sintering collations and grain boundary phase. "Research and Development of 300kW CI ass Ceramic Gas Turbine
514281 has also been applied for ceramic gas turbine components. (Development of The Static Ceramic Components for CGT 303)",
Results are summarized as follows. ASME95-GT-200.
1) 5/C81 has exhibitedhigher flexural strength and stress rupture 5) K Tanaka, M. Sato, Ni Yoshida, and K Koga, "The Sintering
strength at elevated temperatures up to 1500 °C than 511252. Process andCharacteristics of Silicon Nitride" 8th Kouonzairyo-
2) SN281 has excellent oxidation resistance. Kisotouronkai (Japan), (1988)18-22.
3) Geometrical precision of gas turbine components made of 6) M. Sasaki, T. lzumi, S. Achiwa, and T. Rob, 1. of the Gas
SN281 is better than that of S11252. Turbine Society of Japan, 13 (1985)28-35.
4) The detection limit of thick components has been improved by 7)M. FE ei, J. of the Gas Turbine Society of Japan, 21 (1993) 56-
rnicrofocus X-ray radiography. 61.