T.C
FIRAT ÜNİVERSİTESİ FEN BİLİMLERİ ENSTİTÜSÜ
TERMAL BUHARLAŞTIRMA METODU İLE BAKIR ESASLI
ŞEKİL HAFIZALI ALAŞIM ÜRETİLMESİ
Ayşe TEKATAŞ Yüksek Lisans Tezi Fizik Anabilim Dalı
Yrd. Doç. Dr. Canan AKSU CANBAY 2013
T.C
FIRAT ÜNİVERSİTESİ FEN BİLİMLERİ ENSTİTÜSÜ
TERMAL BUHARLAŞTIRMA METODU İLE BAKIR ESASLI ŞEKİL HAFIZALI ALAŞIM ÜRETİLMESİ
YÜKSEK LİSANS TEZİ Ayşe TEKATAŞ
(102114106)
Anabilim Dalı: Fizik Programı: Genel Fizik
Tez Danışmanı: Yrd. Doç. Dr. Canan AKSU CANBAY
T.C
FIRAT ÜNİVERSİTESİ FEN BİLİMLERİ ENSTİTÜSÜ
TERMAL BUHARLAŞTIRMA METODU İLE BAKIR ESASLI ŞEKİL HAFIZALI ALAŞIM ÜRETİLMESİ
YÜKSEK LİSANS TEZİ Ayşe TEKATAŞ
(102114106)
Tezin Enstitüye Verildiği Tarih : 14.08.2013 Tezin Savunulduğu Tarih : 26.08.2013
Tez Danışmanı: Yrd. Doç.Dr. Canan AKSU CANBAY Diğer Jüri Üyeleri: Prof. Dr. Fahrettin YAKUPHANOĞLU
II hocam Yrd. Dr. Dr. Zuhal arkada -Efrahim BAP-FF.12.14 2013
... II ...III ... IV SUMMARY ... V ... VI ... VIII ... X ... 1 ... 2 ... 2 ... 3 ... 3 ... 4 2.3. ... 4 ... 6 ... 6 ... 6 ... 8 11 ... 12 ... 13 ... 13 ... 15 rasyonu ... 16 ... 18 3.7.1.Ka ... 19 ... 19 ... 24 4.MATERYAL VE METOT ... 27 4.1 Materyal ... 27 4.2. Metot ... 29 4.2.1. EDX Analizleri ... 29 4.2.2.X- ... 29
III ... 30 ... 32 alorimetri (DSC) ... 33 ... 35 5. BULGULAR 34 5.1. EDX Analizleri 35 5.2. X- 39 lemler 41 5.3.1. Cu-Al- ... 42 ... 44 5.4.1 Cu-Al- ... 45 5.5. Cu-Al- ... 48 ... 50 ... 55 KAYNAKLAR 57 ... 63
Cu-Al-Ni
a ve ince filmin; EDX analizi,
X-
Al
-belirlendi.
--
-Al-i . Fakat ince filmde bu
ir miktarda malzeme belirlenirken ince filmde bu
Cu-V
SUMMARY
Production of Copper Based Shape Memory Alloy By Thermal Evoporation Method In this study, Cu-Al-Ni shape memory alloy produced by the method of thermal evaporation. Initially in this experimental process, determined Cu-Al-Ni shape memory alloy was obtained using electroslag remelting method. Then, the obtained alloy ingots was cut to small pieces, and coated on the silisium as a thin film with thermal evaporation method. After this experimental method, thermal and structural characteristics of the alloy and thin film obtained by thermal evaporation process were analyzed. EDX analysis, X-ray diffraction, metallographic methods, differential scanning calorimetry (DSC) and differential thermal analysis (DTA) of the alloy and thin film was used in this analysis.
At the end of the observations, the reflection planes of both Cu-Al-Ni alloy and the thin film obtained by the method of thermal evaporation of this alloy determined by X-ray measurements. The owned structures of the alloy and thin film were examined by metallographic analysis and SEM observations. The start and finish temperatures of characteristic austenitic and martensitic phase of the alloy and thin film was determined. As a result of differential thermal analysis measurements, in high-temperature and low-temperature region regular and irregular phase transitions were determined in the structure of the alloy and the thin film.
Obtained data were evaluated at the end of the experimental process. Accordingly, for the purpose of this thesis, Cu-based Cu-Al-Ni shape memory alloy was obtained by the method of thermal evaporation. The martensitic structures were observed in the alloy, but these observations could not be observed in thin film. While austenitic, martensitic phase
observed in thin film. This is because very small amount of the material was coated on the Si substrate in the thin film by thermal evaporation method. Although the eutectoid point determined in TG / DTA measurement of the alloy, this analysis could not be made for thin film.
Keywords: Cu-based shape memory alloy, thermal evaporation, structural analysis, the characteristic transformation temperature.
Sayfa No ... 9 ... 10 ... 11 ... 15
ik reaksiyon sonucu meydana gelen fazlar ... 19
... 20 Cu- ... 21 Cu-Al- ... 22 -Al- ... 23 -Al- ... 23 ... 27 Sistemi ... 28 ince film ... 28 31 a) P ey,b) P ... 31
. -60A, Shimadzu TA-60 WS TG/DTA ... 33
... 33
1.Cu-Al- 36
2. Cu-Al- ... 38
Cu-Al- - difraksiyon deseni ... 39
Cu-Al-Ni ince filminden elde edilen X- ... 40
Cu-Al- - ... 41
a) b) c) ... 42
VII a) b) 43 ... 43 Cu-Al- ... 44 Cu-Al- 45 Cu-Al- .... 45 Cu-Al- 46 ... 46 Cu-Al-Ni i ... 47 .Cu-Al- a) b) ... 48 ... 51 Cu-Al- ... 50 ... 51 ... 52 Af-As ... 52 Af-Ms ... 53
Sayfa No
Tablo 1. ... 7
Tablo 2.Cu- ... 24
Tablo 3. Cu-Al- ... 47
X
Af :Martensit austenit
As
a0
bcc
bct :Cisim merkezli tetragonal d :Entalpi :Entropi fcc fct hkl Mf : Ms : T Tc T0 Tm :Maksimum pik
Metal
sonra ya sahip olan
martensit , artensit kristal materyal . Cu-Bu etki;stentler,
-1] sahipken deformasyona -rmasyonunu ve [4]; 1) Martensitik faz, 2) az durumunda,
lenmeler ve dislokasyonlardan kaynakl gereklidir [5]. termal D 2.2.1. s i nsit
4 s martensit -- tekrar anafaz 6]. 2. Martensitik s emine 7]. tler (Ms s - s - s s - Bu tip termoelastikmart -Zn ve In-8 tlerin de itler olarak [9].
it
-Al-Ni. Au-Cd. Ni-Ti. Fe-Pt ve Fe-Mn-Si
,
metal ailesidir.
ellikler sayesinde tekstillerde
AuCd
-titanyum (NiTi 10].
--Cd,Cu-Zn-Al,Cu-Al- -Ti,Mn-Cu ,Ni-Mn-Ge) dem ve bunlardan Ni-Ti ve Cu-Zn-Al
Tablo 1. 4].
Kimyasal histerizisi
Ag-Cd 44-49 %Cd -190~-50 15
Au-Cd 46.5-50%Cd 30~100 15
Cu-Al-Ni 14-14.5 %Al 3-4.5 %Ni -140~100 35
Cu-Sn -120~30 Cu-Zn 38.5-41.5 %Zn -180~-10 10 Cu-Zn- az %X -180~200 10 In-Ti 18 -23%Ti 60~100 4 Ni-Al 3 6-38%Al -180~100 10 Ni-Ti 49-51%Ni - 50~110 30 Fe-Pt yak.-130 4 Mn-Cu 5-35 %Cu -250~180 25 Fe-Mn-Si 32 %Mn, 6 %Si -200~150 100 -titanyum(
3].Nitinol (nikel- -Ti) yada
-
-4]. 50/50 atomik o
-mekanik
, tabaka ve
n 6].
8 malzemelerdir[14 l etkisidir[15 Fiziksel hareketlilik uygulamala mekanik .
a korur, fakat deforme edilirse uygun 7].
1 deki gibi 8].
10 nokta (molek [19]. bir de austenit . 2. -20]. 3.2 de verilen grafikte; T h Ms: Mf As: Af [14, 20]. un [19]. s ta k Martensit %
f -%50 martensit h) gecikme olarak s ve Af f nin s f 20 3.3). 3. [21]. 20]. Austenit Deformasyon Martensit
12 veya - dioksit veya 4 -1010 mikro [18,19].
3.5.2. isi veya pres [22]. madde gibi [23]. -5 10-6 Kaplanan u teknikler; metallerden(Mo,W,Ta), oksitlerden(Al2O3,SiO2,M2 ;
14
,
4. [26]. -6 Tor n -teknikte lazer Sarmal Kablo
kablo sepeti aliminyum pota
Metal hazneli
Metal yatak
16
l edile
atomlar, vakumlu ortamda hareket edip, substrat (alt tabaka)
-elektri
-OMVPE(Organometallic Vapor Phase E 7].
3.6.
Uzun periyotlu
-fa )
0-[1]
1 ,62
8,29].
Elektron-tipi, tipi ve tipidir,
-1 1
].
-karakterize edilir. Dealey ve Corn
tipindedir. 1,42 < e/a < 1,45 elektro-atom ve
martensit plaklarda ve kusursu ].
rinde kalorimetrik ve ].
s ve Mf
-18 . V -mevcuttur. 1, martensit ort yoktur[28,31]. 3.7. ].
olarak malzemede meydana gelen
iziksel ederek daha 3.7.1. a) S b) 3.5
5. sonucu meydana gelen fazlar [33].
c) Peritektik reaksiyon;
da
3.7.2
kopar, ikin
20
ki -
-Al ikili 5
-
--faz ( -faz (fcc) dir. Bu nedenle
-MS nin
-Al sistemlerinde 2
-termoelastikmar rli olarak
-[36].
7.Cu- 37]. e, verir. -Al-3.8 -Al-Ni ve Cu-Al- 3.9 3.10 Bu den 37,38,39].
22
9. -Al-Ni 41].
24
3.8
sahiptir. s rumunda 40,41].
ve korozyona
metaldi 42].
CuZn,CuAl,CuSn ve CuSn martensitik
termoelastik . Ve tavlama
, Al Ni,Be,Zn ve Mn
yla ince taneli hale getirilir[43].
CuAlNi, CuAlMn, CuZnAl
; CuAl alt .CuAl
fazda [44]. idir v CuAl i 5]. 2 Bu nedenle Ni,Mn ve Be ilavesi Cu ve Al 43,46]. -faz Cu-ana gelir [46,47]. s s Bu s
26
4.MATERYAL VE METOT 4.1 Materyal - -Al-diyagr e homojen 12-24 V and ( ) -faz getir te 4x10-5 ). film haline get
-Al-Ni ve Cu-Al-Ni ince filminin ve termal 1. oran 2. -5 3. -4Malzemenin 5. da
28
2. ma Sistemi.
3. 4.2. Metot 4.2.1. EDX Analizleri - -Enerji dispersif
X-antitatif analizlerini verir [50
4.2.2.
X
-e -eld-e -edil-en Bu parametreler;
30 pozisyonu, parametreleri hesaplanabilir [51,52]. -mi [52]. - -DMAX II - a ( =1.5405 4.2.3. Malzemelerin optik mik 53
ikinci faz ve ikizlenmeler
num if yani
4.4. ikrograf.
dan
-10gr ( FeCl3-6H2O )-96 ml metanol
Nikon MA 200 Model optik mikroskob 4.4.)
32 5 .
53].
4.2.4
sebep olabilir. Termal analizde
54]. Bir numunenin
r
5].
mine
endotermiktir [56 Shimadzu TA-60
WS TG/DTA
atmosferinde
4.2.5
il
deney reaksiyon termodinamikleri, reaksiyon kinetikleri, reaksiyon
57].
s f
58]. 4.7'de
34
kil 4.6.Termal -60A, Shimadzu TA-60 WS TG/DTA.
bir fonksiyonu olarak faz
(1)
(2) ile verilir.
-Al-entalpilerini belirl Shimadzu DSC-60A )termal
4.2.6
(3)
m
ve R ise evrensel gaz sabitidir [59].
(4)
m i
5.BULGULAR 5.1. EDX Analizleri
Date:07/12/2012 13:07:04 HV:20.0kV Puls th.:11.58kcps El AN Series unn. C norm. C Atom. C Error [wt.%] [wt.%] [at.%] [%] --- Al 13 K-series 12.00 14.29 28.12 0.6 Ni 28 K-series 2.88 3.43 3.10 0.1 Cu 29 K-series 69.12 82.29 68.78 1.9 2 4 6 8 10 12 14 16 18 20 keV 0 5 10 15 20 25 30 35 40 cps/eV C u C u Al Ni Ni
--- Total: 84.00 100.00 100.00
Date:07/12/2012 13:07:35 HV:20.0kV Puls th.:11.80kcps El AN Series unn. C norm. C Atom. C Error [wt.%] [wt.%] [at.%] [%] --- Al 13 K-series 12.47 14.92 29.17 0.6 Ni 28 K-series 2.74 3.29 2.95 0.1 Cu 29 K-series 68.32 81.79 67.88 1.9 --- Total: 83.53 100.00 100.00 1. Cu-Al-EDX ana ). arak Cu-Al-Ni Cu-14,60 Al-2 4 6 8 10 12 14 16 18 20 keV 0 5 10 15 20 25 30 35 40 cps/eV C u C u Al Ni Ni
38
Date:07/12/2012 13:24:09 HV:20.0kV Puls th.:11.31kcps El AN Series unn. C norm. C Atom. C Error [wt.%] [wt.%] [at.%] [%] --- Al 13 K-series 4.68 5.58 7.47 0.3 Si 14 K-series 45.34 54.08 69.56 2.0 Ni 28 K-series 0.61 0.72 0.45 0.1 Cu 29 K-series 33.21 39.62 22.52 1.0 --- Total: 83.83 100.00 100.00 2 4 6 8 10 12 14 16 18 20 keV 0 5 10 15 20 25 30 35 40 cps/eV C u C u Al Ni Ni Si
Date:07/12/2012 13:24:40 HV:20.0kV Puls th.:11.31kcp El AN Series unn. C norm. C Atom. C Error [wt.%] [wt.%] [at.%] [%] --- Al 13 K-series 4.55 5.22 7.12 0.3 Si 14 K-series 45.17 51.81 67.93 2.0 Ni 28 K-series 0.83 0.95 0.60 0.1 Cu 29 K-series 36.63 42.01 24.35 1.1 --- Total: 87.18 100.00 100.00
2. Cu-Al-Ni ince fimine
-Al-Ni ekil 5.2). planan
Buna Si-40,81 Cu-5,4
Al-2 4 6 8 10 12 14 16 18 20 keV 0 5 10 15 20 25 30 35 40 cps/eV C u C u Al Ni Ni Si
40
5.2. X- Analizleri
3.Cu-Al-
-Cu- z
--fazdan
2 1(DO3/L21 l mada Cu-Al-Ni
-incelendi.
A
noklinik bir kristal simetriye sahip
4.Cu-Al-Ni ince filminden elde edilen X- -Al-filminin X az ektedir [35,36,61]. -
-42
Cu-Al-
-Cu-Al- -Al-Ni ince filminin tane (D) Debye-Scherer
63]; (1) - ), B Buna gore 5.3. 5.3.1.Cu-Al-B ekil da
(a)
(b)
(c)
5.6. ar a) 50
44
(a) (b)
7. a) b)
8.Cu-Al-Ni ince filminin
5.4. Diferansiyel DSC
Martensit s, Mf, As ve Af
-Al-Ni
5.4.1 Cu-Al-Ni
yon meydana gelir ve martensit austenit Burada
ise austenit
-Al-C/dak 5.9,5.10,5.11, C/dak. s Ms ve Mf C ve 54,45 C dir. tablo de 9.Cu-Al-Ni C/dakika .
46
10.Cu-Al-Ni 15 C/dakika .
12.Cu-Al- 35 C/dakika .
13.Cu-Al- 5, 15, 25 ve 35
48 Tablo 3. -Al-I ( C/dak.) As ( C) Af ( C) Amax ( C) Ms ( C) Mf ( C) Mmax ( C) (J/g) A M (J/g) 5 68,47 82,38 74,70 66,90 54,45 60,27 -8,19 8,69 15 71,36 90,29 79,05 70,88 40,06 58,97 -9,69 5,01 25 72,17 96,10 86,35 68,75 51,52 58,60 -8,99 5,65 35 59,16 118,83 90,16 69,84 45,07 58,33 -5,18 5,83 5.5. Cu-Al-Ni C/dakika s f C
14.Cu-Al-Ni ince filminin 15 C/ dakika DSC
( C/dak.) C) C) C) (J/g) 15 129,10 141,34 122,95 -0,56 (a) (b) .Cu-Al- a) b)
Cu-Al-50
on enerjisi ise 116,33kJ/mol- -Al-5.6. 2(B2) 1(DO3/L21 iz Cu-Al- -2 2(B2) 1(DO3/L21 DSC analizinde belirlendi [57]. 5. Cu-Al-2(B2) 1(DO3/L21 -Al-miktardaki mevcut 5.17 de
16.Cu-Al- .
17.Cu-Al-Ni ince filmin .
-Al-52
Austenite
-18.Austenite
19.
Af-As
Af-As
54
5.21 de f-Ms
6.
Martensitik n d y
uygulanan e
Martensitik fa
-austenit, faz ise martensittir.Martensit
a
artarkende martensit yap kaybolur.
olupCu-AI- EDX analizi kullan arak yap
u-Al-Ni -14,60
Al-3,36Ni olarak
-Al-Ni ince filmin EDX analizi
Si - 40,81 Cu-5,4 Al-0,83 Ni olarak hes
- difraktometresiyle DSC -Al-Ni I- numunelerin in .
56
Cu-Al-Ni lde edilen ince filmin
X-2
-Al-it (122),(0018),(128),(1210),(2010) ve
ir.Bu noklinik kristal
-Al-Ni a parametreleri;a=4,420 , b=5,260 37,89 it edildi.Belirlenen parametrelerine ve ba S edilen verilerlitera III-Metalografik Cu-Al-Ni al k Cu-Al- .6 neler Martensit varyantlar V-tipi martensi IV- Cu-Al--Al-Ni e ,15,25,35 C/dak
5C/dakika / austenit C iken
Cve 54,45 C
olarak belirlendi.Y As ve Af
V-Diferansiyel T
Cu-Al- n 20 C/
-Al-
-2(B2) 1(DO3/L21 Cu-Al- 2(B2) faz
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