و و SSnn--PPbb--CCddتأثري إضافت اإلندٌىم على اخلىاص الفٍسٌائٍت و املٍكانٍكٍت للسبائك املنصهرة تأثري إضافت اإلندٌىم على اخلىاص الفٍسٌائٍت و املٍكانٍكٍت للسبائك املنصهرة

SSnn--PPbb--BBii املتصلبت بسرعت فائقتاملتصلبت بسرعت فائقت

إعداد

سىزان خلف محدان علً الغامدي سىزان خلف محدان علً الغامدي األقسام العلمية - لكية الرتبية /جامعة طيبة / احملارض بقسم الفزيايء

حبث مقدم إىل قسم الفزيايء للحصول عىل درجة دكتوراه الفلسفة يف العلوم

(جوامد عامة ) ختصص فزيايء جتريبية

: إرشاف

حممد بشري عبد القادر كرمان . د. ا حممد بشري عبد القادر كرمان . د. الكية املعلمني ابملدينة املنورة سابقاً – أس تاذ فزيايء اجلوامد التجريبية

لكية الرتبية األقسام العلمية

جدة

جامعة املكل عبد العزيز

ـ ه1429جامد اثين

م 2008 يونيو

EEffffeecctt ooff IInnddiiuumm AAddddiittiioonn oonn tthhee PPhhyyssiiccaall aanndd tthhee MMeecchhaanniiccaall PPrrooppeerrttiieess ooff RRaappiiddllyy SSoolliiddiiffiieedd

SSnn--PPbb--CCdd aanndd SSnn--PPbb--BBii FFuussiibbllee AAllllooyyss

Prepared by

SSUUZZAANN KKHHAALLAAFF HHAAMMDDAANN Lecturer in Physics Department

/Science section Taiba University/Girls College of Education /Medina Monawara

A dissertation Submitted To Department in Partial Fulfillment of the Requirement for the Award of the

Ph.D Degree

in Physics (Experimental Solid State Physics)

Supervised by PPrrooff.. DDrr.. MMOOHHAAMMMMEEDD BBAASSHHIIRR KKAARRAAMMAANN

Professor of Experimental Solid State Physics Teachers College in Medina Monawara

GIRLS COLLEGE-Science Sections

KING ABDULAZIZ UNIVERSITY

JEDDAH

Rٌajab1429H

June2008G

المستخلص

(Fusible Alloys)

SnPbCdInSnPbBiIn

SnPbCdSnPbBi SnPbCdInSnPbBiIn

16

SnPbCd(20-x)In x

SnPbBi(20-x)Inx

Abstract

The most important type of alloy, which is used in most industrial applications, is a fusible alloy. Fusible alloys

are used in many electronics applications as solder materials to connect parts that have apposite influence when

temperature arise such as in the access to measure and determine matters, such as those on kitchen ovens. The

Stopwatch in the kitchen oven starts and stops on specific times according to the determined time set. This is a tool

that determines the timing of the power that starts the internal engine.

These alloys should hold certain properties such as low melting temperature; at the same times alloys are

capable of returning to normal status when used upon reoccurrence. Alloys rarely lose their properties if used in any

process; however, alloys have the ability to be used in any other time frame without loosing their special

characteristics.

Therefore, solder alloys are nonferrous alloys that have melting point bellow 450oK. In electronics the solder

alloys must have low melting temperature, low resistivity and high strength.

All these facts encouraged us and raised our interest to plan and organize researchable project to reach the

goal in industrializing alloys that melt at low temperature with specific properties special. The scientific base for this

goal initiates the preparation and comprehension of scientific concepts about the development of new alloys which

are sensitive to temperature and also has sophisticated properties. This helps future research to acquire and develop

scientific prediction to produce such alloys.

A new fusible alloys is presented In this study, based on the Sn-Pb-Cd-In and Sn-Pb-Bi-In systems, with

substantially improved structure, mechanical, thermal and electrical properties over those of the classical solder

alloys. The presented dissertation has been divided into four parts:

1- Introduction and literature survey:

Present the main scientific framework for the chapters which follows. The concepts of fusible alloys are

reviewed. Scientific concepts deal with the structural aspects to provide qualitative and quantitative explanation for

such concepts as solid solutions, eutectic mixture, solidification, quenching and rapid solidification, cooling rate,

and structural characteristics of rapid solidification which is produced from melting and rapid solidification

techniques.

2- Theoretical considerations: This part is concerned with the theoretical framework. It highlights the important aspect in the design and the

evaluation of various fusible materials. It is presented as an aid to help in understanding important concepts such

as, lattice parameters, electrical parameters, Fermi parameters, thermal calculations, thermal diffusivity, elastic

moduli, hardness measurements, internal friction, and cooling rates. Most of the physical formulas represents a

review of mathematical techniques which is used in this dissertation including scientific notations.

3- Experimental techniques :

The experimental techniques involve the preparation of a series of ternary and quaternary alloys SnPbCd,

SnPbBi, SnPbCdIn, SnPbBiIn fusible alloys, of different compositions . These alloys have been rapidly solidified by

melting using melt spinning technique.

The measurements of the structural, electrical, thermal and mechanical properties are measured using, X-ray

diffraction analysis, scanning electron microscope, dynamic resonance technique, Vickers's microhardness test,

electrical measurements, and differential scanning calorimeter.

In the present work sixteen alloys were prepared in two groups as follows:

4- Experimental results and discussions:

It has been divided into two parts, the first deals with group SnPbCd(20-x)Inx and the second with the group

SnPbBi(20-x)Inx . Each group was investigated and studied in a systematic manner.

This study is not only for research purposes but also to highlight the uniqueness of physical properties of these

fusible alloys. Studying the alloys properties will not be only beneficial to solid state physics researchers but will

also benefit those in technical/practical domains. This is related to the significance of the special characteristics of

the alloys that connect the infrastructures of the alloy to metallic substances properties.

فهرس المحتويات

انصفحت املىضىع أأإجاسة انزسانت ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

بباملستخهص ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

ددشكز وتقذيز ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

وواحملتىياث ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

ي ي قائمت األشكال ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

ررقائمت اجلذاول ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

املقذمت و املسح املزجؼي: انفصم األول واهلذف من انزسانت واهلذف من انزسانت املقذمت و املسح املزجؼي: انفصم األول

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25 ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ15

27 ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ16

27 ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ17

31 ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ18

32 ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ19

انصفحت املىضىع 11035

111

42

112 51

11357

11471

االػتباراث اننظزيت : انفصم انثاني االػتباراث اننظزيت : انفصم انثاني 2173

2279

23 80

2481

2583

26 87

26188

27 94

2896

29 100

انتقنياث املؼمهيت: انفصم انثانث انتقنياث املؼمهيت: انفصم انثانث 31 103

32108

انصفحت املىضىع 33 111

34 117

35117

351118

36 122

37 125

38129

ػزض اننتائج و مناقشتها : انفصم انزابغ ػزض اننتائج و مناقشتها : انفصم انزابغ 41 134

42(Sn-Pb-Cd) 137

421 137

421 137

421 170

422177

423186

424197

43(Sn-Pb-Bi) 214

431 214

421 214

421 254

432262

انصفحت املىضىع 433271

434280

298 االستنتاجاث ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

304املقرتحاث و انتىصياث ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

305املزاجغ ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

aقائمت انزمىس وانىحذاث ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ (1)مهحق

cبطاقاث حتهيم حيىد األشؼت انسينيت ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ (2)مهحق

lانسرية انذاتيت ـــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ (3)مهحق

Aمهخص بانهغت االجنهيشيت ــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــــ

Summary

The most important type of alloy, which is used in most industrial applications, is a

fusible alloy. Fusible alloys are used in many electronics applications as solder materials to

connect parts that have apposite influence when temperature arise such as in the access to

measure and determine matters, such as those on kitchen ovens. The Stopwatch in the

kitchen oven starts and stops on specific times according to the determined time set. This is

a tool that determines the timing of the power that starts the internal engine.

These alloys should hold certain properties such as low melting temperature; at the

same times alloys are capable of returning to normal status when used upon reoccurrence.

Alloys rarely lose their properties if used in any process; however, alloys have the ability to

be used in any other timeframe without loosing their special characteristics.

Therefore, solder alloys are nonferrous alloys that have melting point bellow 450oK.

In electronics the solder alloys must have low melting temperature, low resistivity and high

strength.

All these facts encouraged us and raised our interest to plan and organize

researchable project to reach the goal in industrializing alloys that melt at low temperature

with specific properties special. The scientific base for this goal initiates the preparation

and comprehension of scientific concepts about the development of new alloys which are

sensitive to temperature and also has sophisticated properties. This helps future research to

acquire and develop scientific prediction to produce such alloys.

A new fusible alloys is presented In this study, based on the Sn-Pb-Cd-In and Sn-Pb-

Bi-In systems, with substantially improved structure, mechanical, thermal and electrical

properties over those of the classical solder alloys. The presented dissertation has been

divided into four parts:

1- Introduction and literature survey:

Present the main scientific framework for the chapters which follows. The concepts of

fusible alloys are reviewed. Scientific concepts deal with the structural aspects to provide

qualitative and quantitative explanation for such concepts as solid solutions, eutectic

mixture, solidification, quenching and rapid solidification, cooling rate, and structural

characteristics of rapid solidification which is produced from melting and rapid

solidification technique.

2- Theoretical considerations:

This part is concerned with the theoretical framework. It highlights the important

aspect in the design and the evaluation of various fusible materials. It is presented as an

aid to help in understanding important concepts such as, lattice parameters, electrical

parameters, Fermi parameters, thermal calculations, thermal diffusivity, elastic moduli,

hardness measurements, internal friction, and cooling rates. Most of the physical formulas

represents a review of mathematical techniques which is used in this dissertation (thesis

only for master’s level at least in the North American system) including scientific notations.

3- Experimental techniques :

The experimental techniques involve the preparation of a series of ternary and

quaternary alloys SnPbCd, SnPbBi, SnPbCdIn, SnPbBiIn and fusible alloys, of different

compositions . These alloys have been rapidly solidified from( or by) melting using melt

spinning technique.

The measurements of the structural, electrical, thermal and mechanical properties

are measured using, X-ray diffraction analysis, scanning electron microscope, dynamic

resonance technique, Vickers's micro hardness test, electrical measurements, and

differential scanning calorimeter.

In the present work seventeen alloys were prepared in groups as follows:

Group(

1)

Group(

2)

1 SnPbCd

20

SnPbBi

20

2 SnPbCd

19.5In0.5

SnPbBi

19.5In0.5

3 SnPbCd

18In2

SnPbBi

18In2

4 SnPbCd

16.5In3.5

SnPbBi

16.5In3.5

5 SnPbCd

15In5

SnPbBi

15In5

6 SnPbCd

13In7

SnPbBi

13In7

7 SnPbCd

11.5In8.5

SnPbBi

11.5In8.5

8 SnPbCd

10In10

SnPbBi

10In10

4- Experimental results and discussions:

It has been divided into two parts, the first deals with group SnPbCd (20-x)In x and the

second with the group SnPbBi(20-x)Inx. Each group was investigated and studied in a

systematic manner.

The structure of the first group alloys was examined by X-ray diffraction

technique. It was observed in the cast-melt spun ribbons crystalline, and contains

multiphase, such as -Sn, -Pb and Bi-phase. It also contains intermetallic compounds:

Cd0.05Sn0.95, In0.2Sn0.8. The microstructure for alloys was also examined using scanning

electron microscope, and the results were correspondent with X-ray diffraction results.

The structure of the second group alloys was examined by the X-ray diffraction

technique. It was observed in the cast-melt spun ribbons crystalline, and contains

multiphase, such as -Sn, -Pb and Bi-phase. It also contains intermetallic compounds:

Pb7Bi3, PbBi, In3Sn, In0.2Sn0.8 The microstructure for alloys was also examined using

scanning electron microscope, and the results were correspondent with X-ray diffraction

results.

Electrical resistivity and the temperature coefficient of resistivity of the produced

alloys have been measured using the double-bridge circuit. The variation of room

temperature resistivity within concentration obeys the mixture law in case of a multiphase

alloy (i.e., the resistivity increases linearly with the volume fractions), but in the case of the

presence of intermediate phase the mixture law does not obey. This happens because of the

presence of intermetallic compounds.

Mechanical measurements have been carried out to characterize the structure;

elastic modulus and internal friction of these alloys are in melt quenched condition. It is

worth mentioning that there is a connection between microscopic and macroscpic

characteristics of alloys in two cases: . First one, when we were able to count microstrain

to connect electrical characteristics with mechanical ones. The second process, when we

were able to calculate dynamic yield stress and then the maximum sheer stress of the

mechanical characteristic.

Differential thermal analysis was carried out for all the alloys. Phase

transformation was observed for some alloys during fusion process. Some thermal

parameters have been calculated experimentally, such as: melting point, Solidus and

liquids, thermal diffusivity, Specific heat, and enthalpy.

Three specific samples of the new fusible alloys are described. SnPbCd18In2 -

SnPbCd16.5In3.5 - SnPbCd10In10, the eutectic precipitate morphology is refined by the

relatively small amount of indium addition and as a result, a suitable strength, and

ductility solder with significantly stability in its electrical conductivity with temperature is

obtained, The results showed that the addition of indium to the ternary SnPbCd system also

improves the material properties, and lowers the melting temperature of the electrical and

thermal properties.

Three specific samples of the new fusible alloys are described. SnPbBi18In2 -

SnPbBi11.5In8.5 - SnPbBi10In10 ,the eutectic precipitate morphology is refined by adding

relatively small amount of indium. As a result, a suitable strength, and ductility solder with

significantly stability in its electrical conductivity with temperature is obtained. The

experimental results showed that the addition of indium to the ternary SnPbBi system also

improves the material properties, and lowers the melting temperature of the electrical and

thermal properties.

This study is not only for research purposes but also to highlight the uniqueness of

physical properties of these fusible alloys. Studying the alloys properties will not be only

beneficial to solid state physics researchers but will also benefit those in technical/practical

domains. This is related to the significance of the special characteristics of the alloys that

connect the infrastructures of the alloy to metallic substances properties.

االقتراحات و التوصيات

1.

2.

3.

4.

5.

6.