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Density of Silicon Nit_ride Ceramics ....._. Krzysztof J. Cios and Leszek M. Sztandera. = University of Toledo. Toledo, Ohio and. George Y. Baaklini and Alex Vary.
NASA

Technical

Memorandum

106049

7,a3

Fuzzy Sets Predict F!exural Strength and Density of Silicon Nit_ride Ceramics ..... _

Krzysztof University

J. Cios and Leszek of Toledo

M. Sztandera

=

Toledo, Ohio and George Y. Baaklini and Alex Vary Lewis Research Center .... Cleveland,

Ohio

May 1993

r T7

(NASA-TM-I06049) PREOICT FLEXURAL DENSITY OF SILICON (NASA)

23

N93-27270

FUZZY SETS STRENGTH AND NITRIDE CERAMICS

Uncl

p

G3/24

fiJ/ A

as

0169404

__

I

m

__

n

_

It

FUZZY

SETS

PREDICT FLEXURAL OF SILICON NFrRIDE Krzysztof

J. Cios

and

STRENGTH CERAMICS

Leszek

University

AND

DENSITY

M. Sztandera

of Toledo

Toledo,

Ohio

43606

and George National

Y. Baaklini

Aeronautics Lewis

and

and Research

Cleveland,

Alex

Space

Vary

Administration

Center

Ohio

44135

SUMMARY

In this strength time,

work

we utilize

and

density

sintering

time,

Flexural

strength

modulus

of

Celsius

are

utilized

to build

exceed

3.3%,

11.34%

obtained

These

the

randomness

bars

the

and

6Y

are

such

fuzzy

as ceramics, variables

of manufacturing

7.1%,

networks,

that

The

of flexural

are

as an input

to the fuzzy

used

of the and

system.

135

operator

maximum

Data tested

and

Hamming

error

with

system.

273 Si3N 4

at 1370

for

the

of milling

from

bars

test

as compared

degrees

distance

density

errors

of

are

does 1.72%

not and

respectively. sets

theory

especially

and

predictions variables

mean

model.

make

Processing

parameters

Generalized

neural

and

ceramic.

temperature

strength

demonstrate

nitride

output

predictive

by using

to evaluate

pressure

at room

flexural

processing

silicon

the

study.

fuzzy

theory

nitrogen

tested

this

for

sets

sintering

density

in

materials,

between

and

rupture

results

designing

of NASA

and

used

fuzzy

can be incorporated for

parameters,

assessing like

into the

more

strength,

complex

which

process

of

relationships

are

governed

by

processes.

INTRODUCTION

High savings,

engine reduced

improvements to

leave

temperatures

weight,

and

for automotive

50 percent

*On sabbatical

operating

over

current

from the University

made

environmental engines

engine

of Toledo

with

benefits. structural

technology.

and NASA

possible

Resident

Estimates ceramic

Structural

Research

by ceramics

in energy

potential

efficiency

of

components

ceramics

Associate

will result

range

such as silicon

at Lewis

Research

Center.

from carbide

30

and

silicon

their

nitride

relatively

light

high-temperature when

mass

fracture parts

strength.

toughness

discrete

Therefore

fabrication and

only

physical

and

ceramic regarding

the

through

improved

expended

fabrication

reliable

structural

Scatter

scatter

silicon

work

a

silicon

nitride

Lewis

Research

strongly

nitride

affected temperature, processing procedures.

to by

and

taken

shorten

may the

metal

to

Current bulk

performance

NDE

[1].

available

regarding

time

engine

attributed

methods

the

that

material's

technology may

minimize

help

low

containing

affect

to

inexpensive

processing.

information

good

relatively

many

ceramics

(N'DE)

N'DE

be

and

during

information

be

and

generally

By incorporating

of ceramics

powder

variables

Center

a

obtained occurence

reduce

needed

into

be their

to

the

effort

to develop

sintering

conditions

were

trials

varied

conditions

processing time,

grinding

time,

21

batches

and

based

on

feedback

improved

of

during

strong,

3].

work

evident

Based at

NASA

The

investigation

of one

from

strength

radiography and

2

reduced

From

research

and density

the

gradients

sintered

silicon

a program

was

strength

relationships

as

described. to obtain

variables

position.

The

of powder

silicon

scatter.

Space

LeRC,

furnace

or exclusion

were

during

sintering

inclusion

material

that

upon

gradient-flexural

and

occuring

Aeoronautics

it was

[2,

contact,

a design/reliability

fabrication.

National

variables.

setter

of an extensive

of

concomitant

the

from

inhomogeneities

and

LeRC)

density

drawback

and

characterization

powder

In [4], the results

at

(NASA

sintering

overpressure, were

defects

compositions

investigate

and

nitrogen

to

is a great

composition

upon

systematically sintering

with

provide

are

adversely

evaluation

Thus,

pro_am

X-radiographic

involving

structures

can

can

attributed

nitride

dependent

preliminary

undertaken

produce

steps

procedures.

is

of

were

frequently

so

properties

processing

Administration

introduced

that

can

replacing

toughness

program,

that

that

of

ceramics.'

This

on

low

because

resistance,

properties

toward

development

research

in mechanical

standpoint.

materials

in strength

uniformity.

components shock

cracks

also

and

defects

in a materials

and and

but

thermal

move

non-destructive

properties

of

variation

also

flaws

hot-section

nonstrategic

anomalies

to have

technology

source

of

inclusions,

discrete

materials

and

in strength

procedures

mechanical

oxidation

wide

microstructural

detect

engine

a large-scale

scatter

it is essential

not

their

as voids,

for

consist

precluded

The

such

variations

excellent

However,

ceramics.

cost-effective

candidates

They

have

defects

density

leading

weight,

produced.

with

can

are

nitride

were powder

wet-sieving composition

Sintering/processing high-density These

previous

uniform results,

in turn, were used in neural systems[5], and are usedin this paper to study the viability of using fuzzy sets for predicting strength and density, speeding the optimization of the manufacturingprocess,and for comparingfuzzy systemswith neural systems. In this work we are interested in finding whether it is possibleto utilize fuzzy systemsto help in the material developmentprocessof advancedceramics.Fuzzy systemsare good in function approximation, and if the trend could be easily noticed as to which variable contributesmost for the increaseof a desiredoutput parameter,say strength, then this may help in speedingup the processof manufacturingand optimizing a new material. Material developerscan easily notice suchchangesfor a few variablesbut it becomesvery difficult to do so for a large number of variables.From the data collected by Sandersand Baaklini [4], we selectedonly three input variables,namely, milling time of the composition powder, the sintering time of the modulus of rupture test bars, and the nitrogen pressure employed during sintering. From the output variables,flexural strengthand density were selected.The rationale for using only the above mentioned variables is that there were not enough training pairs (outputs associatedwith inputs) for all the variablesused in the experimental work [4]. In this paper, relationshipsbetweenthe milling time, sintering time and nitrogen pressureand the resultantstrengthand densityare establishedby using fuzzy systems.Fuzzy set results arecomparedwith thoseobtainedusing radial basisfunction neural network [5]. BASICS

Randomness

is not

mathematical became 11].

the

gradual class

was

to be known

Essentially,

which

transition than

membership

defined In the

for

as fuzzy set

abrupt, rather

dealing

sections

form

in which

to formulate set theory.

theory

between

to be susceptible next

only

developed

fuzzy

rather

methodology

this

tool

the

OF FUZZY

provides

than with

the

source

the presence phenomena

to analysis

we provide

basic

uncertainty and

deal

reveals

with

other

It was first introduced

membership and

SET THEORY

a natural and

of random that

by

are

conventional

definitions

paper.

3

of

is the

variables.

vague,

of the

the

published

the

fuzzy

classes

In other too

mathematical set theory

sixties

of uncertainty

absence

imprecise,

strict

In

[10,

problems

in

of objects

is

of sharply words,

defined

it renders

a

or too

ill

complex approaches which

a and

by Zadeh

to manipulating

nonmembership

of imprecision

forms

and

approach

itself.

are

[7, 9]. used

in

Definition

of Fuzzy

Let

R be

collection

Sets

the

of items

set

of reals

of interest.

defined

by a membership

interval

on the real

line.

Note

that

the

Then

U -> {0, 1}, where

the

gA : U ->

the fuzzy

subset

of discourse

element

A of U can

0 and

subset

[0, 1] denotes

be expressed

or grade

be considered

{0, 1} is the set of values

set)

the

which

is a

A of U is closed

unit

as:

g. [0,1]}.

to as the degree

set B can

(crisp

of U. A fuzzy

[0, 1], where

I.tA(u)

gA is referred

non-fuzzy

universe

u be a generic

{gA(u)/u;uEU,

value

a classical

Let

U be

function

A= In this case,

and

of membership

as a binary

1 rather

than

characteristic

of u in A. function

an interval.

Support Let

A be a fuzzy

memberships

subset

in A

of U. The

support

P.A ( U ), are positive. Supp(A)=

of A, Supp(A), That

is the set of elements

in U whose

is,

{ u /u e U,

gA ( u ) > 0}.

Normality A fuzzy That

subset

A is normal

is, the supremum

As an example

let us consider of U, and the

Then

subset

Much

less

Note the

a crisp

set

the items

above

itemizing

( _ A ( U ) ) = 1.

of U, called

which

U, where

sign " + " is used "much

have

zero

here

it is subnormal.

U =

value

+ 0.6/5

1 +

to express

less than 5", may

5 = 1/1 + 1/2 + 1/3 +1/4

that

Fuzzy

Let

than

if Sup

over U is unity; otherwise,

are elements a fuzzy

if and only

... +

10, where

membership

be expressed

+ 0.4/6

in the grade

2 +

+ 0.3/7

(union)

1, 2, ..., 10 in the

set.

as: + 0.1/8.

of membership

have

been

ignored

in

expression.

operations

A and

operations

B be fuzzy for fuzzy

subsets

of a crisp

set U, with membership

sets follow:

4

functions

gA and

I.tB. Major

Complement The complementof a fuzzy subsetA of a crisp setU, denotedA', is definedby A'=

_., (1-ktA(u))/u,ueU, U

where

_

is used

as a convenient

notational

form.

Union The

union

of A and

B, denoted

A k..)B = _ U

Ak.JB,

(Max

is defined

by

[_A(U),I.tB(U)])/U,

ueU.

Intersection The

intersection

of A and

B, denoted

A CkB,

is defined

by

A (-'IB = _.,(Min[_A(U),p.B(u)])/u,ueU. U The

union

connective

Examples

corresponds "AND",

of the

to the and

the

operations

connective

operation

defined

"OR",

of complementation

above

follow:

Let U={

1, 2, 3,4,

5, 6, 7 },

and

A = 0.8/3

+ 1/4 + 1/5 + 0.6/6,

and

B = 0.7/3

+ 1/4 + 0.5/6.

Then A k..)B A _ A'

= 0.8/3

+

1/4+

1/5 + 0.6/6,

B -- 0.7/3

+

1/4 +

0.5/6,

= 1/1 + 1/2 + 0.2/3

+ 0.4/6

while

+ 1/7.

5

the

intersection corresponds

corresponds to negation.

to the

AGGREGATION

Aggregation

operations

combined

into

a

on

single

set.

fuzzy

sets

In

general,

OF

are

FUZZY

SETS

operations any

by

which

aggregegation

several

operation

fuzzy

is

sets

are

by

the

defined

function

h'[0,1]"410,1]

for some

n >

2. When

set A by operating

In order

Axiom

on the

to qualify

axiomatic

applied

as

1. Boundary

membership

an

requirements,

which

2. For

any pairai

additional

the fact Axiom

This

that

a noticeable Axiom

4.

equally

element

h must

the essence

of the

an aggregate

fuzzy

of U in the aggregated

satisfy

at

least

the

notion

of aggregation:

sets.

following

two

axioms they

.... ,0)=

0

are

usually

and

h(1,1

.....

e [0,1land

1.

bi e [0,1],ifai

nondecreasing

employed

1)=

>

bi for alli,

then

in all its arguments.

to characterize

aggregation

operations

despite

are not essential:

guarantees change

function.

that in the

h is a symmetric

an infinitesimal

variation

in any

argument

of h does

not produce

aggregate. function

in all its arguments,

that

is, the

aggregated

sets

are

important.

fuzzy

associativity arguments.

express

that is, h is monotonic

We can easily on

function,

, bi ,whereai

3. h is a continuous

axiom

of each

on U, h produces

conditions

h ( ai ) >- h ( bi ),

Two

sets def'med

grades

aggregation

h(O,O

Axiom

to n fuzzy

sets.

see that Although

provides Hence,

fuzzy they

a fuzzy

unions are

mechanism unions

and

and

intersections

defined

for

for

extending

intersections

6

qualify

only

two their

can

be

as aggregation

arguments, definition viewed

their to

as

any

special

operations property

of

number

of

aggregation

operationsthat are symmetric, usually continuous,and required to satisfy some additional boundary conditions. As a result of these additional requirements,the standard max and min operationsrepresentboundariesbetweenthe averagingoperationsand the fuzzy unions and intersections,respectively. There are severalclassesof averagingoperations[8, 9]. One of them that coversthe entire interval between the rain and max operationsconsistsof generalizedmeans.This class of operations will be usedin this paper. It is defined asfolows: 1 ha ( al , a2 , ....

an)=

(

aT+

a_ +n ""+

a_

)

-6

f

where

a

is a parameter

In our

application

consequently,

by which

we used

different

_x =

it represents

means

2. Function

are distin_ished,

ha clearly

a pararneterized

class

and

satisfies

o_ E R

Axioms

of continuous

and

\

_ (x _ 0 ).

1 through

symmetric

4, and,

aggregation

operations.

A METHOD

The were

fuzzy

tested

system

was built

at room

temperature

temperature, pressure listed

18 yielded

in Table

In order the

system

number

removed

from

into

the

of training

in the

ability

from

the 70

vectors

data. %

for

test

data

and

test

batch the

data

training set. This data

sets

was which

evaluate network

data

set

then

30

sintering

which

are

repeated

7

[4].

of the the

Thus,

testing. for

labeled

5 times

and

in Table

predictions.

number

values

6Y25

divided

into

number

6Y25

in order

as combinations

room

nitrogen

combination

batch

Batch

the

I. Also

we needed

output

optimium

which

°C.

predictions,

the error

the

listed

bars

C. For

time,

at 1370

pseudo-randomly

% for

were

system

to predict

represents

were and

fuzzy

of rupture

at 1370

for 9 combinations

then

available

tested

time,

densities

in the

of the

were

milling

densities

and

273 Si3N4 modulus

which

and

number

The

from

of

confidence

test

this

variables

approximately

our

and

PREDICTION

bars

strengths

strengths

known

as

135

combinations

to determine

6Y25,

the data

and

composition

I are the

interested

processing

pairs

the

using

particularly

inserted

different

using

FOR

to have A through

a

to test We

were

for

batch

for

the

was

first

ratio was

of then

5 different E (Table

Room temp Batch #

Number of

Millingtime,

specimen

[hr]

'6Y1B

30

24

6Y2B

30 15

24 100

15 15

300 100

14 19

300 ..... 24

10 10 10 10 15

100 100 100 100 100

15

100 100

6Y11 6Y12 6Y13 6Y14 6Y1516 6Y17 6Y18 6Y19 6Y20 6Y23 6Y24A 6Y24B 6Y25 6Y26A 6Y26B 6Y28 1370C Batch # 6Y9B 6Yll 6Y12 6Y13 6Y14 6Y1516 6Y17 6Y18 6Y25

Table

15 10

2.5 2.5 2.5

r

300

Actual strength, [MPa] 556

Nitrogen pressure, [MPa] 2.5 2.5

532 490

,

!

579 684 746 664 646

Actual density_ [g /cm "q 3.12 3.18 3.23 3.25 3.24

1 2

2.5 5

2 1.5

5 5

608

3.24 3.22 3.23 3.21

1.5 2 1.25

5 5 5

570 650 631

3.22 3.22 3.24

1.25 2 2

3.5 3.5

3.26 3.26

5

586 619 714

3.28

15 15 10

100 ..... 100 100

1 1 2

3.5 5 5

479 503 671

3.20 3.18 3.21

29

24 100

1 1

2.5 2.5

383 444

300 100

1

2.5 2.5

416 406 425 402

3.12 3.23 3.25

13 14 15 14 20 10 10 10

I: Strength/Density sintering

Sintedng time, [hr]

conditions.

2.5

300 24

2

100 100 300

2 1.5 2

,r

at room

temperature

and

439 458 467

5 5

1370

C for

different

processing

3.24 3.24 3.22 3.23 3.21 3.28

and

Table

!I: Selected

batch

Room

numbers

Training

Temp.

B

A

for 70% and 60% training

sets..A through

Sets 70%

Traininq

C

D

E

w

*

}

*

*

I

*

I

*

I I I

"

A

8

E

Sets 60%

C

D

E

Batch 13o. r.

L

6YIB

I

6Y2B

I

6Yll

I

6Y12 6Y13 ! 6Y14 [

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6Y15 6Y16 6Y17

6Y_8

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6Y25

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6Y26A

6Y2e8 6Y28



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II). This

entire

training

process

a training

created.

Batch

batch

placed

data

composition

input

and

(nitrogen support

using

a ratio

of approximately

pressure,

sintering

elements

60 % data

used

for

elementwise,

and

membership

grades fuzzy

shown

shown

input

that

UI

we

fuzzy

sets

grinding

C. was

%) except

sole

made

vector.

6Y25

Finally,

predictions

density).

The

grades

repeated

for 70%

variables

sets

for each

for

was all the

the

for

while

every

of generalized and

60%

respectively.

The

Thus,

appropriate

models

parameters,

and

for the

Different of

were

for nitrogen

of the

input

ones

have

were

formed

sets

of

for

The

resulting

the

the

temperature

for

sintering

for

normalized

for the room

formed

their

to produce

membership

pressure,

of support

were

operation

data

(21

output

of prediction.

mean

material

values

fuzzy

step

of silicon

three

memberships

training grades

of 21 batches batch

are defined

time)

and

by means

sets

processing

IV,

VI.

(100

set as the

and

42 fuzzy

input and

1370

and

set

and

strength

combined

output

1370

flexural time

C are strength

and

grinding

parameters.

a measure

the

The time,

fuzzy

V and

as the

as the

between

The

in Tables

density

sets).

normalization

were

sets.

in Tables

After

the

data

to establish

and

numbers

the outputs.

(flexural

temperature

batch

in the test data

sintering

formed

fuzzy

room

placed

representing

was

of all the

in a training

21 output

of two

resulting

was

we do not know

collected

nitride

time

repeated

set consisting

6Y25

were

for which

The

and

data

number

numbers

vectors

are

then

and 40 % for testing.

Next,

the

was

actual

similar and

to Hamming

generalized

distance

fuzzy

sets

is proposed

of input

to calculate

parameters.

The

the

difference

measure

is defined

by:

ucS

where

S is an interval

in R, and

thenD(A,B/R)= Nextl from

the

values the

combination

B are

fuzzy

subsets

on S. In the case

when

S = R,

D(A,B).

the k-fraction

of the

generalized

for flexural

method

A and

grades strength

is depicted A with

70%

measure,

of memberships and densit3r,

on

where

Fig.

training

1. As at the

k e (0, of the

k was chosen an example room

1), is either

output

us consider

temperature.

10

parameters.

to be 0.1. The let

added

The

to or subtracted This

graphical 6Y12

generalized

results

in the

explanation test

batch

input

fuzzy

of from set

Generalized input fuzzy set

Actual input fuzzyset l.t

_t

Supp mt Generalized

output

st

p

fuzzy

set

Supp mt

Dissimilarity measure

Predicted

st

output

p

fuzzy

set

_t i

I

/

> Supp

Supp s

s

d

I'he generalized input fuzzy set consists of grades ol _embership obtained by generalized mean operation 3erformed on normalized values of input parameters: milling :ime, sintering time, and pressure (note that these fuzzy sets :lifter for different combinations of training data). The actual nput fuzzy set represents normalized values of a parficulat nput. The dissimilarity measure based on Hamminc :listance concept is then employed, that is, the elementwise :lifferences are summed up. k- fraction of the measure is :hen added to the grades of membership of the generalizec _utput fuzzy set ( a fuzzy set obtained by generalized meat _peration performed on normalized values of outpul 3arameters: strength and density), resulting in the predictec _utput fuzzy set. The grades of memberships of the latte_ are compared then with the actual ones obtained b normalization of the values of a particular output.

Fig.

1.

A graphical

explanation

of the method

used

11

Actual

d

output

fuzzy

set

I-t

Supp s

for fuzzy

set prediction.

d

consists of grades of membershipobtained by generalizedmean operation performed on normalized values of input parameters:milling time (mt), sintering time (st), and pressure (p). In this particular case the fuzzy set with the support of (mt, st, p) has grades of membership0.44, 0.73, and 0.82, respectively (Table III). Note that generalizedinput fuzzy setsdiffer for different combinationsof training data. The actual-input fuzzy set represents normalizedvaluesof the 6Y12 batch input, that is, a fuzzy set with supportof (mt, st, p) with gradesof membership1, 0.5, 0.5, respectively.The dissimilarity measurebasedon Hamming distance is then employed, that is, the elementwise differences between grades of membershipof actual and generalizedinput fuzzy sets are summed up. In this particular case the dissimilarity measureis 0.01. The k-fraction of the measure,which is 0.001 when k=0.1, is then added to the gradesof membershipof the generalizedoutput fuzzy set. The generalized output fuzzy set, obtained by generalized mean operation performed on normalized values of output parameters,strength(s) and density (d), has in this casegrades of membership0.82 and0.99, respectively,as shown in Table III. Addition of the k-fraction of dissimilarity measureresults in the predicted fuzzy set with gradesof membership0.821 and 0.991, respectively.The latter are then comparedwith the actual gradesof membership obtained by normalizationof the values of the 6Y12 batch output 0.781 and 0.99i, resulting in error of 4% for the strength and perfect prediction of density for the batch under consideration.

RESULTS

The

method

strength

and

prediction detailed

density

of the results

100%

ones

6Y25

Table

of

data.

the

for

and the

batch. 30%

optimum

E are

Table

data

variables. 6Y25.

room

sets

are

chosen and

listed

in Table

VIII

obtained

to predict

in Table

Resultant

strengths

reason

12

for 70%

made

being

C, II.

(A).

6Y25

and

densities fuzzy

as

well

Table

and

strength

selected

of the flexural

The

training,

for

is that

values

1370

the first combination

predictions

The

randomly

temperature

set, for

shown

shows

DISCUSSION

to predict

training

the results

XI

batch

in

The test

X shows

sintering

was used

samples

A through

training.

processing

above

batch

for the

for combinations 60%

described

AND

new are systems

as

VII

overall

shows results

in Table

and

for

IX for

density

combinations lower

than

are

bounded

using of the as

wasproven in our other work [6]. With 40% test data at room temperature,the strength and density values were predicted with an averagepercentageerror of less than or equalto 7.1% and 2.8%, respectively.When the slightly smaller test set of 30% was used,the averagepercentageerrors for strengthand density droppedslightly to less than or equal to 5.7% and 2.4%, respectively.Similar results were obtained for the 1370 °C data (Tables XII-XV). With 40% test data the average percentageerrors for strength and density were less than or equal to 5.4% and 3.3%, respectivelylWith 30% test data thesevalues were 4.6% and 2%, respectively.For 1370°C, prediction of the 25th batch was perfect (0% error) for all combinationsof 30% test data and even for all combinations of 40% test data, for both strength and density. So, even using only

60%

of the

data

The

reason

parameters. crisp

set

with

all

for

training,

for that

the

model

is that

membership

was

the fuzzy

functions

able

to exactly

set representing

equal'1

(it

predict

25th

the 25th

batch

reaches

batch

output

is actually

maximum

in

all

a

input

parameters). The

information

sintering that

and

obtained

in Tables

processing

variables

for

where

6Y25

sintering

time

can

sintering

time

of 2 hours,

strength 467

of 462.86

MPa,

materials

be used.

MPa

viewpoint.

sintered

grains,

which

can

temperature loss

pressure

required

strength

or density.

turned for

out

parameters.

to prevent

was

also

some

They

were

the

makes

with

large,

times

may

and

to find

thus

lead were

was

the

triples

of

not not

tried.

and

to have

room

and

1370

input

parameters (300,

more

of input

sense

1.75,

that

a

from

growth

to high

and

actual

beyond

that

on

either

parameters

which

In addition,

maximal

5 ), (300,

the

columnar

influence

the

of

powder,

resistant

C temperatures. gave

a

for 6Y25

pressure great

lower

predict

value

as

hours,

in a coarser

grain

Nitrogen

combination

p):

and

randomly-oriented

toughness

found

( mr, st,

13

results

to exaggerated

optimal

for both

combinations following

This

of

dense

of 250

sets

the

microstructure

fracture

time

fuzzy

also

and

pressure

less than

time

as for 6Y25

other

slightly

of 50 hours.

of higher

nitrogen

the

combinations

as strong

a milling

milling

decomposition

used

same

C

a

sintering

to evaporation,

to be the

1370

yield

using

shorter

the ceramics

Long

due

system

the

make

creep.

material

will

Namely,

almost

of 5 MPa,

This is only time

may be other

or lower

XVI,

pressure

in milling

there

material

time

in Table

a nitrogen

that

produce

grinding

can be obtained.

processing

suggests

will

shorter

and

a reduction

when

that

For example,

but with

which

The

XI and XVI

output

2, 4.5),

and

Table

III:

The

resulting

temperature

fuzzy

sets,

for 70%

Table

B C

.0.82 0.82 0.82

D E

0.83 0.79

IV: The

resulting

temperature

A B C D E

Table¥:

The

A B C I

D E

Pressure

0.99 0.99

0.50 0.49

0.69 0.75

0.80 0.79

0.99 0.99

0.49 0.39

0.67 0.76

generalized

mean

operation,

0.82

. 1

0.77 0.79

for the room

training.

0.81 0.82 0.79 0.79

0.99 0.99 0.99 0.99

sets,

after

Milling time 0.45 0.53

Sintering time 0.72

Pressure 0.82

0.72 0.73 0.70 0.75

0.85 0.79 0.82 0.77

0.53 0.42 0.41

generalized

mean

operation,

for

1370

C

training.

Milling time 0.61

0.91 0.93

Density 0.99 0.99 0.99

0.92 0.92

0.98 0.99

0.62

Strength 0.92

for the room

Sint.ering time 0.73

Density 0.99

for 70%

operation,

Milling time 0.44

Strength 0.82

fuzzy

mean

Density 0.99

sets, after

for 60%

resulting

temperature

fuzzy

generalized

training.

Strength A

after

0.60 0.47 0.24

14

I. Sintering time 0.65 0.71 0.74 0.74 0.55

Pressure 0.71 0.71 0.79 0.79 0.61

......

Table

VI: The

resulting

temperature,

sets, after

for 60%

E

VII:

Predicted

Density 0.98 0.99 0.99 0.98 0.98

room temperature

6Y2B 6Y12 6Y17 6Y18 6Y24A 6Y25

Overall

Combination

operation,

Sintering time 0.68

0.65 0.26 0.26 0.67

"0.74 0.78 0.68 0.56

with 70%

training,

0.74 0.74 0.84 0.74 0.63

Combination

Actual

Predicted Density, g/cm2.93 3.26 3.27 3.23 3.28

537 602

1 4

646

633

608 586 714

614 604 686

2 1

3.23 3.21

3 4 3

3.26 3.28

for room

Pressure

% Error

532 579

results

for 1370 C

Milling time 0.65

Density, cj/cm _ 3.12 3.25

AveraQe Error

VIII:

mean

strength

Predicted Actual Strength, MPa Strength, M Pa

Batch Number

Table

generalized

training.

Strength 0.93 0.93 0.94 0.93 0.91

A B C D

Table

fuzzy

temperature,

A % Error

6 0

3.25

1 2 0

i|

70% training

Strength - % error for 6Y25

A

Strength - average % error for all test vectors 2.2

Density - % error for 6Y25

4

Density - average % error for all test vectors 2.0

B C D E

3.0 7.0 6.2 10.0

4 4 3 7

2.8 3.6 1.6 2.0

0 0 0 0

Combined Average % error

5.7

4.4

2.4

0

15

0

....

Table

IX: Overall

results

Combination

Table

60% training

Strength- % error for 6Y25

Density oaverage % error for all test vectors

A B

2.7 6.0

4 6

.2.5 4.3

C D E

7.3 10.5

4 7

3.6 2.2

0 0

9.0 7.1

7 5

1.3 2.8

0

X: Prediction

Batch Number

Xl:

for 6Y25

density

and strength

716

714

Prediction

of selected

temperature Milling Time, hr

strength

''

processing

Densit,_,, g/cm_ .... 3.28

and

and density,

sintering

....

temperature,

Actual

_0.3

Density - % error for6Y25

training

Predicted

% Error

Density/, g/cm_ 3.28

0

variables

100 % plus 6Y25

100%

0 0

for

optimum

room

training

Nitrogen Pressure, MPa 3

Predicted Strength, MPa 596

Predicted Density, g/cm 3 3.15

1.5 1.5 1.75 1.5

3 3

604 611

3.18 3.21

4

634 619

3.28

1.5 1.75

4 4

634 649

300

1.5

4

649

300 300

.1.75 2

4

656 686

15C; 175 200 200 250 250 250

Sintering Time, hr

at room

% Error

Actual Predicted Strength, MPa Strength, MPa

6Y25

Table

temperature,

Strength- average % error for all test vecto rs

CombinedAverage % error

o

for room

1.5

t6

3.25 3.28 3.28 3.28 3.28 3.28

Table

Xil:

Predicted

6Yll 6Y156Y16 6Y25 Average Error I

Xlll-

Batch Number

395 426

11 6

467

467

0 5.7

for 6Y25

density

and strength

Actual Predicted Strength, MPa Strength, MPa 467

XlV:

Overall

% Error

444 402

Prediction

6Y25

Table

at 1370 °C with 70% training,

Predicted Actual Strength, MPa Strength, MPa

Batch Number

Table

strength

results

467

% Error

0

Combination

Actual

Predicted

Density,, _cm_ 3.23

Density, g/cm3.04

3.22

3.25

3.28

3.28

A % Error

6 1 0 2.3

at 1370 °C with 100% training Actual

Predicted

% Error

Density, .... g/cm _ 3.28

Density, g/cm V 3.28

0

for 1370 °C, 70% training

Combination

Strength- average % error for all test vectors

Strength - % error for 6Y25

Density- average % error for all test vectors

Density - % error for 6Y25

A B C D

8.5 6.5 1.0 2.5

0 0 0 0

3.5 1.5 3.0 0.5

0 0 0 0

E

4.5

0

1.0

0

4.6

0

2.0

0

Density - % error for 6Y25

Combined Average % error

Table

XV:

Overall

Combination

results

for 1370 °C, 60% training

Strength - % error for 6Y25

A B

Strength - average % error for all test vectors 6.3 4.3

0 0

Density- average % error for all test vectors 5.7 4.3

C D E

3.3 6.3 6.7

0 0 0

3.0 0.7 2.7

0 0 0

Combined Average % error

5.4

0

3.3

0

17

0 0

Table XVI: Prediction of selected processing and sintering variables for optimum density and strength at 1370 °C with 100 % plus 6Y25 training Sinterincj Time

MillingTime 150 175

Nitrogen Pressure 4 4

1.5 1.5 1.5

200

4 5

200 200 250

1.5 1.75

300 300

1.5

5 5 4

1.5 1.75 2

5 5 5

30,0 300

Predicted Strength 425 430 434

Predicted Density 3.18 3.21 3.25 3.28

444 448

3.28 3.28

462 453

3.28

462 467 467

3.28 3.28 3.28

Average error

12

%

- RBF

60%

70%

Room

temperature

60%

70%

8

- FS

0

Fig. 2

Average

errors

(RBF)

and

in predicting

fuzzy

sets

60%

%

using

radial

basis

function

neural

network

(FS).

Average error

strength

1370 C

60%

70%

70%

3

2

0 Room Fig. 3

Average (RBF)

errors and

in predicting

fuzzy

sets

temperature density

using

(FS).

18

1370 C radial

basis

function

neural

network

(270,

2, 5).

The and

results

show

property

processing learning based

control.

the

host

pressure,

fact

whereas

microstructure,

and

with

neural

less

precise

Fig.

3) which

are

on

due

Developers

data

existing

between

the

and

to be applicable and

for

density

nitride. than

predicting time, on

sets with fuzzy

processing

variables

and

strength.

sintering

pore

This

time

and

morphology,

on

defects.

that

in the

development

those

sets

variables

manufacturing density

obtained

are

superior

and

strength

process.

was

modelled

previously in modeling (Fig.

The

2 and

more

better

(in

precise terms

of

networks. and composite

the

processing

will

help

to capture

in a manufacturing

process,

This

variations

processing

of ceramics

relationships.

the

modeling

strength

to milling

fuzzy

[5] indicates

found

dependent

causing

process

the

predicting

related

by using

the same

was

successful

additionally

of failure

for both speed

for silicon

more

is directly

obtained

system

features

is

and

consequently

was

strength

presence

shorten

former

density

to statistical

between neural

as input

density

results

relationships

using

and

on the

networks

relationship error)

bulk

fuzzy

and

tool

optimize

The

parameters

bulk

be a powerful

help

materials.

flexural

of the

can

should

variables

that

the

Comparison

logic

processing

predicting

to the

set theory

ceramic

processing

In general, due

fuzzy

Fuzzy

of emerging

on three

was

that

can

by

structures

utilizing

fuzzy

sets

imprecise

relationships

the

to capture

be seen

latter as the

can achieve

alternative

and

better

neural

which

strength

networks

are due

and density,

in

tandem.

to unavoidable

more

precise,

although

to the

Taguchi

method

still

The

variations

very

complex,

[12].

CONCLUSIONS

Fuzzy and

sets

density,

pressure.

theory and

The

combinations by The fuzzy

are

three

learned

the

maximum sets

the

of the

calculating

was applied

error

to learn

processing

relationships processing

errors for

superior

on

relationships

variables: were

for

variables.

The

reliability

data

encompassing

test

neural

was

7.1%,

networks

and

time,

predicting

for

exist

density

between

sintering strength

of these

either

in capturing

19

that

milling

used

strength to

the

30%

vague

time, and

or 40% 3.3%.

strength

and

nirogen

density

predictions

it was

the

was

for

validated

of available It was

relationships

new

data.

found

that

between

the

processingvariablesand strength.However, for density which is more directly related to the input variables,neural networksgave better results. Summarizing, developers of structural ceramics and ceramic composites, may utilize computational paradigms of fuzzy sets and neural networks to optimize the desired parametersand to shortenthe processingand manufacturingcycle:

ACKNOWLEDGEMENT

The LeRC,

authors

would

like to thank

for thoughtful

Mr. William

A. Sanders

from

Ceramics

Branch,

NASA

discussions.

REFERENCES [1] Klima SAMPE

S. J. and

[2] Klima [3]

Baaldini

Quarterly,

Vol.

S. J., NDE

Baaklini,

G.:

for Heat

N'DE

for Gas

Turbines

[4]

W.

and

with

the

Strength

Proceedings, [5] Cios Ceramic

A.

Vol.

and

Engine

and

Baaldini

and

Process

Power,

Vol.

G.

Correlation 1986.

G. Y., Vary and

Testing,

Predicts Gordon

A. and Tjia Related

and

[7] Cios

K. J., Shin

Stenosis,

IEEE

[8]

G.

I., and

Computer

J. and Cliffs,

Folger

T.

A.,

for

1987,

Ceramics,

Nitride,

Structural

Ceramic

R. E., Radial and

1992,

1984. Ceramics.

Basis

Density,

and

Sintering

Engineering

Function International

L.,

Using

24:3,

Fuzzy

Sets,

1988.

2O

of

Variables and

Science

Network

Learns

Advances

in

submitted.

Boundness and Equivalence of Fuzzy IEEE Transactions on Fuzzy Systems,

Vol.

Journal

pp. 263-266.

of Processing

Strength

Breach,

Goodenday

Magazine,

of Structural

TM-86949,

Control 109,

Silicon

K. J. and Sziandera L. M., Artificial Neural Networks,

Englewood

Y.,

Radiography

[6] Cios Forward

Klir

NASA

of

Processing

Characterization

Ceramics,

7, No. 7-8, pp. 839-860,

K. I., Baaklini

Nondestructive

Nondestructive 1986, pp. 13-19.

Reliability

Engineering Sanders

G. Y.,

17, No. 3,

Fuzzy

1991,

Sets

to Diagnose

Systems and Feed 1992, submitted. Artery

Coronary

pp. 57-63.

Uncertainty,

and

Information,

Prentice

Hall,

[9]

Sztandera

Department Columbia, [10]

L.M.,

of MO,

Zadeh

Michie

L.,

Zadeh

[12]

McEntire

J. E.,

and

Turbine Contractors' PA,

1990,

Electrical 1990. A Theory

D., and

[11]

Spatial

Mikulich

L., Fuzzy

sets,

Relations and

Engines,

Computer

C. L.,

Willey,

of

the

Component

27th

Society

of

pp. 341-349.

21

an of

1979, pp.

M.S.

Thesis,

Missouri-Columbia,

9, in Hayes

I. K.,

149-194.

1965. E., Yeckley Development

Automotive Automotive

Image,

Intelligence,

York,

D. N., Bright

Nitride

of

University

8, pp. 338-353,

A. P., Heichel

Meeting,

Subsets

Machine

New

Control,

Silicon

Proceedings

Coordination

Reasoning,

John

Information

Fuzzy

Engineering,

of Approximate L. I., Eds.,

B. J., Taglialavore

Quackenbush

Among

R. L., for

Technology Engineers,

Holowczak

Advanced

Gas

Development Inc.,

Warrendale,

i [-_::-4/_"_/ '"

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REPORT

DATE

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REPORT

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May 1993 4.

TITLE

AND

AND

DATES

Technical

SUBTITLE

5.

Fuzzy Sets Predict

Flexural

Strength

and Density

of Silicon

Nitride

COVERED

Memorandum

FUNDING

NUMBERS

Ceramics WU-506--01-50

AUTHOR(S)

Krzysztof

J. Cios, Leszek

M. Sztandera,

George Y. Baaklini,

and Alex Vary

8.

7. PERFORMINGORGANIZATIONNAME(S)ANDADDRESS(ES)

PERFORMING REPORT

National Aeronautics and Space Administration Lewis Research Center Cleveland, I 9.

Ohio

ORGANBATION

NUMBER

E-7794

44135-3191

SPONSORING/MONITORING

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SPONSORING/MONITORING AGENCY

National Aeronautics and Space Administration Washington, D.C. 20546-0001

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NASATM-106049

11. SUPPLEMENTARYNOTES Krzysztof J. Cios (on sabbatical leave from the University of Toledo and NASA Resident Research Associate at Lewis Research Center), Leszek M. Sztandera, University of Toledo, Toledo, Ohio 43606; George Y. Baaldini and Alex Vary, NASA Lewis Research Center. Responsbile person_ .G.eorge Y. Baaklini_ (216) 433-6016. 12¢ DISTRIBUTION/AVAILABILITY STATEMENT 12b. DIS_-RiBUTION CODE Unclassified

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ABSTRACT

(Maximum

24 and 38

200

words)

In this work we utilize fuzzy sets theory to evaluate and make predictions of flexural strength and density of NASA 6Y silicon nitride ceramic. Processing variables of milling time, sintering time, and sintering nitrogen pressure are used as an input to the fuzzy system. Flexural strength and density are the output parameters of the system. Data from 273 Si3N 4 modulus of rupture bars tested at room temperature and 135 bars tested at 1370 degrees Celsius are used in this study. Generalized mean operator and Hamming distance are utilized to build the fuzzy predictive model. The maximum test error for density does not exceed 3.3%, and for flexural strength 7.1%, as compared with the errors of 1.72% and 11.34% obtained by using neural networks, respectively. These results demonstrate that fuzzy sets theory can be incorporated into the process of designing materials, such as ceramics, especially for assessing more complex relationships between the processing variables and parameters, like strength, which are governed by randomness of manufacturing

processes.

15.

14. SUBJECTTERMS

SECURITY OF

NsN 7540-01-280-5500

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OF

22

Ceramics; Processing; Fuzzy logic; High-temperature Neural networks; Silicon nitride; Monolithic ceramics 17.

NUMBER

SECURITY

CLASSIFICATION

20.

UMITATION

OF

ABSTRACT

OF ABSTRACT

Unclassified Standard

Fo_m

Prescribed 298-102

by ANSI

298 Std.

(Rev. Z39-18

2-89)