Spin-Valve Fabrication

SPIN-VALVE FABRICATION
Tcnicas de Micro e Nanofabricao - Prof. Susana Freitas
08-07-2011
IST 2Sem - 2010/2011 Grupo Em&M&M
Step 1- Al2O3 Deposition (500) *

* Steps not done; the
500
sample was supplied.
Sample enter the machine the day before
Ink lines on the calibration sample for measurements *
Electrical insulator
Machine: UHV2
Deposition
rate (/s)
Exposure
time (s)
RF Power
(W)
RF
Frequency
(Hz)
Pressure
(Torr)
Ar Flow
(sccm)
0.2
2500
200
811
2,4x10-7
45
Measurements/Tests:
1.
Profilometry (film thickness): ink lines wiped off

with acetone; sample cleaned (IPA+H20) and
dried (air jet) *
2.
Elipsometry (film thickness + refractive index):

calibration with the alignment of the 2 beams
(reflected and refracted) with calibration
sample, before sample.
Step 1- Ellipsometry Results
Refraction index
Thickness ()
1st point
1,633
567
2nd point
1,633
560
Consistent results for refraction index (same value)

Smal diferences in thickness (non uniform deposition rate over all
wafer)
Deviation to target thickness (500 ): real deposition rate
expected deposition rate
SV O que uma Spin-Valve? - 1

4
Bias Current
t
L
Figura: GMR - variao da resistncia com o campo magntico externo
External H
SV O que uma Spin-Valve? - 2

5
Grfico: Resposta desejada MR vs H ext
Figura: Exemplo de aplicao deteco de markers

magnticos
Variao da resistncia com H externo

Zona linear permite determinar H externo com biasing do aparelho
sensor magnetorresistivo
Step 2- Spin Valve (231 ) deposition - 1

6
Preparation: No preparation needed.

Responsible: Prof. Susana Freitas
Machine: Nordiko 3000
Method: Ion-beam deposition
Antes de mais, porqu a N3000?

Figura: resultados esperados aps
deposio
Nordiko 3000 Algumas consideraes

7
Mquina usada em duas etapas do processo

Elevada versatilidade e fiabilidade (em operao intensa desde 1998)
Componentes principais:
-
Fontes de ies por RF
Canho de deposio e auxiliar
Neutralizadores
Sample holder
Obturador
man permanente (~40 Oe, rodado de 40)
Alvos
Protector dos alvos (um sempre exposto)
Sistema de vcuo
Sistema de carregamento das amostras
Figura: esquema do interior e componentes da

N3000
Nordiko 3000 Vantagens

8
Inmeras:
-
Totalmente automatizada vrios batches com diferentes camadas
Escolha de diferentes alvos versatilidade
Monitorizao detalhada das condies do processo (inmeros controlos)
No obriga a expor a amostra aos plasmas dos canhes
Boa uniformidade na energia dos ies energia para o substrato controlada
Funcionamento a baixas presses preveno de contaminantes

Fail-safes garantem pausa no processo quando parmetros se afastam dos
intervalos tolerados atravs do obturador e sua re-estabilizao
Permitem:
-
Filmes homogneos, densos e uniformes ( 2% numa wafer de 6 pol)
Reduzido stress no filme (ies no incidem na amostra)
Taxas de deposio controlveis

9
Layer
SV stucture
Material
1
2
3
4
5
6
Buffer Layer
Ta
NiFe
CoFe
Cu
CoFe
IrMn
Free Layer
Spacer Layer
Pinned Layer
Exchange
Layer
Ta
Deposition Thickness Exposure

rate (/s)
()
time (s)
0.15
20
133.33
0.24
28
116.67
0.205
20
97.56
0.31
18
58.06
0.205
20
97.56
0.23
65
282.61
0.15
60
400.00
231
1185.80
Total
Tabela: recapitulao das camadas a depositar e tempos de deposio
Amostras de calibrao:
1) Lamela de vidro para medio de propriedades
magnticas VSM e GMR
2) Lamela de vidro para etch stop-point no passo 5

deposio

10
Colocao da amostra e lamelas (2 amostra de

calibrao irrelevante):
Colar com fita cola todas as amostras wafer (esta
invertida na mquina para minimizar deposio
de contaminantes estranhos)
Wafer base
Receita utilizada: SV22

Parmetros da receita:
Positive
Grid (V)
Set point
Read out
1200
1174.5
Beam
Negative
Current
Grid (V)
(mA)
300
22
291.25
21.88
Xe
Substrate
Subrotation
Flow
Inclination
(rpm)
(sccm)
()
2.4
15
80
2.45
n/a
n/a
Rotao e inclinao do substrato maximizam uniformidade
Janela de visualizao durante o processo
Testes iniciais VSM

11
VSM vibrating sample magnetometer
Estudo das propriedades magnticas da amostra:

Voltagem induzida nas pickup coils proporcional ao
momento magntico da amostra, mas independente do
campo externo aplicado.
Esquema de funcionamento
Mquina: DMS Model 880
Software auxiliar para operao e

obteno de resultados
Testes iniciais VSM resultados 1

12
Along Easy-Axis - zoomed in
Signal on X direction, Moment [emu]
Along Easy-Axis
-4
1.6x10
-4
1.4x10
-4
1.2x10
-4
1.0x10
-5
8.0x10
-5
6.0x10
-5
4.0x10
-5
2.0x10
0.0
-5
-2.0x10
-5
-4.0x10
-5
-6.0x10
-5
-8.0x10
-4
-1.0x10
-4
-1.2x10
-4
-1.4x10
-4
-1.6x10
-4
1.4x10
-4
1.2x10
-4
1.0x10
-5
8.0x10
-5
6.0x10
-5
4.0x10
-5
2.0x10
0.0
-5
-2.0x10
-5
-4.0x10
-5
-6.0x10
-1500
-1000
-500
500
1000
1500
-60
-50
-40
-30
-20
-10
Applied Field [Oe]
10
20
30
40
50
60
Applied Field [Oe]
Campo externo > 0: fcil alinhamento da free layer com a pinned layer mximo momento
Campo externo < 0: contra a pinned layer surge o exchange field e, depois, histerese
Campo externo < 0 intenso: a pinned layer virada pelo campo intenso
Testes iniciais VSM resultados 2

13
Perpendicular to easy-axis
-4
1.6x10
-4
1.4x10
-4
1.2x10
-4
1.0x10
-5
8.0x10
-5
6.0x10
-5
4.0x10
-5
2.0x10
0.0
-5
-2.0x10
-5
-4.0x10
-5
-6.0x10
-5
-8.0x10
-4
-1.0x10
-4
-1.2x10
-4
-1.4x10
-4
-1.6x10
-1200 -1000 -800 -600 -400 -200
200
400
600
800 1000 1200
Applied Field [Oe]
Free layer alinha-se rapidamente com campo externo
Pinned layer eventualmente tambm se alinha para campos mais

intensos
Testes iniciais - GMR

14
GMR giant magnetorresistance
Estudo das propriedades magnetorresistivas

fundamentais para o funcionamento das SVs:
Resistance [Ohm]
Resistance along easy-axis - zoomed in

29.8
29.6
29.4
29.2
29.0
28.8
Aparato experimental para GMR
28.6
28.4
28.2
28.0
27.8
-35 -30 -25 -20 -15 -10
-5
10
15
20
25
30
35
Applied Filed [Oe]
Resultado obtido: MR=6.15% (valor de referncia para testes finais)
Pormenor 4-point probing
Step 4 1st lithographic process SV grid

patterning
4.1) Preparation
Vapour priming:
Samples enter chamber >30 min before resist
coating
25 min @ 130 C (vacuum: 10Torr 1Torr)
5 min @ 130 C (HDMS flow; 4/6 Torr)
Resist coating:
Bake 60 sec @ 120 C
Cool 30 sec @ air
Dispense photoresist 5 sec @
800 rpm (1,5m)
Spin 40 sec @ 2,5k rpm 5
sec @ 1,6k rpm
Clean photoresist {wafer
border} 2 sec @ 1k rpm
Bake 60 sec @ 87C
Improves
resist
adherence!!
Step 4 1st lithographic process

4.2) Mask Exposure
DWL 2.0 (Lasarray) laser
Helium-Cadmium {120mW;
442nm}; filtered to 30/50%
laser power
Exposure energy adjusted
according to substrate
material reflectivity
Inverted mask
4.3) Development
Resist development:
Bake 60 sec @ 120 C
Cool 30 sec @ air
Water spray and rinse 1 sec @ 500
rpm
Dispense developer 5 sec @ 500
rpm
Developent 60 sec @ 0 rpm
Rinse with H2O 20 sec @ 1k rpm
Dry 30 sec @ 3,5k rpm
Step 4 1st lithographic process Mask

details
SV dims: 2,5x10 m
Cross frame dims: 100x100 m

SV frame dims: 3610x800 m
Step 4 1st lithographic process

Problems in mask exposure!
1st Lithography
Problem!
But it is reversible
2nd
Lithography
OK!
Step 5 Ething SV grid patterning
Nordiko 3000 (Ion-beam milling system)

Basic pattern definition on SV
10% over-etch= 231 x (1+0,1)= 254,1
Etch rate
(/s)
1
Beam
current
(mA)
29-31
Power
(W)
65
Thickness Etching
()
time (s)
254,1
254,1
Declination
Rotation
Speed (rpm)
70
12
Etching steps:
1. Estabilizao do canho
2. Etch
3. End-etch
Note: last 30 seconds with +1W (power) ensure there is no
under-etch
Step 5 Nordiko 3000 Ion beam (milling) system

Example of dry etch (physical
process)
Advantages (vs wet etch):
Better process control
Easily repeated
Low residues/waste
Anisotropy (allows patterns
design)
Step 5 Result
Perfect!
Step 6 - Resist Strip

Ultra-sounds machine + heated water bath
i. Samples inside crystallizer with micro strip 2001;
ii. Crystallizer in bain-marie for, at least 2h, alternated with 5 min
in ultrasounds;
iii. Cleaning with IPA distilled water air jet (drying);
iv. Optical inspection of residues on the sample.
Step 7 - 2nd Lithographic process - SV

AlSiCu contacts
23
7.1) Preparation
Vapour priming:
Samples enter chamber >30 min before

resist coating
25 min @ 130 C (vacuum: 10Torr
1Torr)
5 min @ 130 C (HDMS flow; 4-6 Torr)
Resist coating (SVG - coating track):
Bake 60 sec @ 120 C

Cool 30 sec @ air
Dispense photoresist 5 sec @ 800 rpm
(1,5m)
Spin 40 sec @ 2,5k rpm 5 sec @ 1,6k
rpm
Clean photoresist {wafer border} 2 sec @ 1k
rpm
Bake 60 sec @ 87C
IST-TMN-2S 10/11- Emanuel Antunes, Manuel Nascimento, Miguel Leito
~2x2.5m for
contact-SV overlap

AlSiCu contacts Mask Details
24
7.2) Mask Exposure

Helium-Cadmium
{120mW; 442nm}; filtered
to 30-50% laser power
Exposure data:
Layer: Layer_2
Layer inversion: non-inverted
Layer colour: green
Conversion name: g1linhas
Focus: 70
Energy: File 30

AlSiCu contacts - Development
25
7.3) Development
Resist development (SVG Development track):
Bake 60 sec @ 120 C

Cool 30 sec @ air
Water spray and rinse 1 sec @ 500 rpm
Dispense developer 5 sec @ 500 rpm
Developent 60 sec @ 0 rpm
Rinse with H2O 20 sec @ 1k rpm
Dry 30 sec @ 3,5k rpm

AlSiCu contacts Post-development pics.
26
Bom alinhamento
entre a 1 e 2
litografia!
27
IST-TMN-2S 10/11- Emanuel Antunes, Manuel Nascimento,

Miguel Leito
Step 8: AlSiCu contact lines deposition (3000 )

28
Machine: Nordiko 7000
Deposition
Parameters
Pressure
(mtorr)
Ar Flow
(sccm)
N2 Flow
(sccm)
Power
(W)
Voltage
(V)
Current
(A)
Deposition
Rate [/s]
Time
(s)
Soft sputter
Etching
50
RF1=60
RF2=40
~3/60 to 4/60
60
Al98.5Si1Cu0.5
3000
50
2k
400
38
60+20
Ti12.5W50(N37.5)
150
50
10
500
433,5
1,2
27
The initial soft sputter etching removes the first atomic layers
of the formed tantalum oxide, in order to improve the
electrical contact between Ta and AlSiCu.
The Nitrogen gas injected during the TiW deposition dopes
the TiW forming TiWN, giving a better resilience to corrosion.
IST-TMN-2S 10/11- Emanuel Antunes, Manuel Nascimento, Miguel
Leito

- Calibration samples
29
Callibration samples:
Deposited over piece one
big piece of glass,
marked with pen marker
lines to be used for two
tests:
Perfilometry
Resistivity
measurements

30
Profilometry - Dektak 3030 ST

Film thickness via profilometry. Acetone aided lift-off of the pen stripes is applied to produce
the required steps for measurement
Five measurements were taken in different places, all steps were well defined ensuring a
nice precision. The Dektak 3030 ST has a sensitivity of about 200.
t1[]
t2[]
t3[]
t4[]
t5[]
Average []
Average [m]
3235 23.2
3216 42.2
3139 119.2
3592 333.8
3109 149.2
3258.2 333.8
0.32582 0.03338
As we can see the film is quite uniform and the total thickness is close to the
intended 3150 (covered by the error bar).

31
Resistivity Measurements:
With the aid of a diamond-tip a stripe of AlSiCu is defined by scratching two parallel
lines, which limit a rectangular area of AlSiCu used to calculate resistivity together
with current and voltage measurements obtained in the GMR bench via the probe
tips.
Distance between scratched lines: d = 31091 m (measured using the profilometer)
Distance between Voltage probes: L = 3162.8 200 m (measured using the dicing
microscope software ruler - 200m error bar)
I
I = 10 mA (stable no error bar)

V = 1.3775 0.0005 mV
=R t d /L = 4.4118 0.2834 ..cm
Reference value:
Al98.5SiCu0.5 =5.36 ..cm //Al =4 ..cm
L
t
d
Step 9 AlSiCu pads Lift-off via Resist Strip

32
Ultra-sounds machine + heated water bath

i. Samples inside crystallizer with micro strip 2001;
ii. Crystallizer in bain-marie (65C) for over 2h, alternated with 5 min in ultrasounds
(sometimes >15min);
iii. Cleaning with IPA distilled water air jet (drying);
iv. Optical inspection of residues on the sample .
Step 10 - SiO2 Passivation Layer Deposition (2000)

33
Machine: Alcatel UHV Sputtering system
Preparation: Insert sample >8h prior to deposition for

primary vacuum.
Calibration samples: 2 Si pieces to be deposited
alongside our sample, one with marker lines:
to be used in measurements indicated below
used as calibration in Step 12 (RIE stop-point)
Deposition conditions:
Thickness()
RF Power (W)
Pressure (mTorr)
Ar flow (sccm)
Time
2000
140
3.15
20
1h30m

- Calibration Sample Measurements - Perfilometry
34
1. Profilometry - Dektak 3030 ST (SiO2 film thickness): ink lines are wiped off
with acetone, then sample is cleaned, dried and put into the profilometer to
measure the thickness of the film.
Height ()
Large dispersion of the results in relation to each other.
The deposition rate is never perfectly uniform across all

sample
Even to the naked eye we can see some slight differences in

the shade of the film colour.
Measured
Average
2502
2456
2043
2618
2404.75 361.75
error ~ 15% of the average value
2. Ellipsometry (film thickness + refraction

index): the sample is put into the
ellipsometer after calibrating the machine
via alignment of the reflected/refracted
beams with calibration sample. Parameters
used: pattern 91, program 9.

- Calibration Sample Measurements - Ellipsometry
35
2. Ellipsometry (film thickness + refraction index): the sample is put into the
ellipsometer after calibrating the machine via alignment of the reflected/refracted
beams with calibration sample. Parameters used: pattern 91, program 9.
Refractive index
1.54
1.48
1.49 0.04
1.48
1.48
Thickness ()
2236.00
2236.00
2224.33 23.33
(DD)
2201.00
()
(NR)
(NR)
249.87
270.12
()
(NR)
(<20)
17.56
25.25
NR, the results were not

registered; DD: the
machine didnt display
the values
Refraction index: Values close to each other, except the first one. This could probably be because the
deposition wasnt uniform all over the wafer, leading to a result a little further away from the others. and
are in a very high line density zone > small deviation in the measurement of and yield a wide range
for the refractive index results.

- Calibration Sample Measurements - Ellipsometry
36
2. Ellipsometry
Thickness:
Close to 2000 with some deviation > deposition rate isnt constant in the UHV sputtering
system, but also because, as we have seen in the refractive index, and are in a very high
line density zone, making it difficult to determine accurately the thickness of the film.
The ellipsometer used has a good resolution up to 1000, and is unreliable for values higher.
Successive variations in thickness propagate through layers, increasing the non-uniformity of the
last layer.
Profilometer and elipsometer

measurements are in agreement.
IST-TMN-2S 10/11- Emanuel Antunes, Manuel

Nascimento, Miguel Leito
Step 11 - Lithographic process 3 - pads

exposure 1
37
11.1) Preparation
Vapour priming:
Samples enter chamber >30 min before

resist coating
25 min @ 130 C (vacuum: 10Torr
1Torr)
5 min @ 130 C (HDMS flow; 4-6 Torr)
Resist coating (SVG - coating track):
Bake 60 sec @ 120 C

Cool 30 sec @ air
Dispense photoresist 5 sec @ 800 rpm
(1,5m)
Spin 40 sec @ 2,5k rpm 5 sec @ 1,6k
rpm
Clean photoresist {wafer border} 2 sec @ 1k
rpm
Bake 60 sec @ 87C

deposio

exposure 2
38
11.2) Mask Exposure

Helium-Cadmium
{120mW; 442nm}; filtered
to 30-50% laser power
Pad dims.: 220x180m
Exposure data:
Layer: Layer_3
Layer inversion: non-inverted
Layer colour: blue
Conversion name: g1pads
Focus: 70
Energy: File 30
Vista geral e detalhes da mscara.

exposure 3
39
Fotografias de microscpio
Diferena ntida de cor: com resist e sem resist.

Nota-se um alinhamento quase perfeito entre camadas e litografias.
DWL bem sucedido
Step 12 RIE Contact Pads Exposure

40
Machine: LAM
Pre-treatment: None needed
Calibration: Use the calibration sample prepared
on Step 10 to evaluate etching stop-point
Deposition settings:
Etching rate ~ 10 /s .
To ensure perfect contact pads exposure a 10% over-etch limit is applied.
Etching depth: 2200 220s total time to ensure 10% o.e.

Because there is little risk of the reactive plasma etching the AlSiCu (despite the
chance of the TiWN being slightly attacked by the plasma) we proceeded with two
runs of 150s -> 3000 of SiO2 could be etched, which copes with the maximum
2618 value measured for the film thickness

41
It's better to do more runs of lesser time, than one run exceeding 150s as
the sample will be heated and that could harden the photo-resist making it
worse for resist-strip (He refrigerates wafer).
Flow values: Ar : 200sccm (Physical component)

CF4: 100sccm (CF4 + SiO2 > SiF4 + CO2)
Pressure in chamber: 140mTorr

42
Measurements: Use of GMR test bench in order to confirm total removal of SiO2
over the contact pads (full exposure of contacts). Verification of proper SV
operation with GMR measurements.
quasi-linear MR transfer curve
Resistance [Ohm]
Pre chip one SV resistance along easy axis
MR= 5.78%
111
110
109
108
characteristic to this sort of SV

device with these dimension
OK!
107
106
105
104
-150
-100
-50
50
100
Applied Filed [Oe]
Although this is only one SV of the 144 fabricated, we can conclude that the
fabrication process was successful, and the pads are well exposed as
inspected optically.
Step 13- Dicing
Photoresist is not removed (helps protect the samples)

Sample placed on adhesive plastic sheet
Cut
Samples retrieved with help of tweezers (BE CAREFUL!!)
Step 14- Resist Strip

(Step equal to Step 6)
Step 15 Encapsulamento e Wire Bonding

45
Responsvel: Eng. Jos Bernardo

Mquina: Kulicke and Seffa (including microscope)
Processo:
- Amostras coladas a um chip carrier genrico (cola rpida).
- Utilizao de uma agulha com fio de solda de 25 m e ultra-sons.
1. Agulha solda contacto ao chip;
2. Mantendo o fio esticado, solda a outra ponta ao pad da SV correspondente;
3. Corte do fio.
Parmetros de controlo:
Fora aplicada agulha;
Tempo de contacto para a soldadura;
Regulao da potncia de ultrasons.
Consultar parmetros no computador prximo (registo emprico de parmetros
pticos para tipos de chip carriers e de amostra)
Step 16 Testes finais das SVs - I

48
- Montagem experimental descrita anteriormente mas usando o adaptador

para chips.
Chip SV testings resistance along easy axis - #2
Resistance [Ohm]
Resistance [Ohm]

105
104
103
98
97
96
102
95
101
94
100
93
99
92
-100
-50
50
MR=5.97%
Comportamento esperado.
100
Applied Filed [Oe]
-100
-50
MR= 5.81%
Histerese indesejada.
50
100
Applied Filed [Oe]
Step 16 Testes finais das SVs - II

49
- Montagem experimental descrita anteriormente mas usando o adaptador

para chips.
Resistance [Ohm]
Resistance [Ohm]

106
105
104
103
116
115
114
113
102
112
101
111
110
100
109
99
108
-100
-50
50
100
-100
-50
50
Applied Filed [Oe]
MR= 6.09%
100
Applied Filed [Oe]
MR= 5.98%
Agradecimentos
50
O
g r u p o
EM&M&M (pela
ordem inversa na
foto) agradece a
todos os que
ajudaram estes
( a i n d a )
nanoengenheiros
d u r a n t e a
c a d e i r a .
FIM

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SPIN-VALVE FABRICATION

Tcnicas de Micro e Nanofabricao - Prof. Susana Freitas

IST 2Sem - 2010/2011 Grupo Em&M&M

Step 1- Al2O3 Deposition (500) *

Profilometry (film thickness): ink lines wiped off

Elipsometry (film thickness + refractive index):

Step 1- Ellipsometry Results

Consistent results for refraction index (same value)

SV O que uma Spin-Valve? - 1

Figura: GMR - variao da resistncia com o campo magntico externo

SV O que uma Spin-Valve? - 2

Grfico: Resposta desejada MR vs H ext

Figura: Exemplo de aplicao deteco de markers

Variao da resistncia com H externo

Step 2- Spin Valve (231 ) deposition - 1

Preparation: No preparation needed.

Antes de mais, porqu a N3000?

Nordiko 3000 Algumas consideraes

Mquina usada em duas etapas do processo

Fontes de ies por RF

Canho de deposio e auxiliar

man permanente (~40 Oe, rodado de 40)

Protector dos alvos (um sempre exposto)

Sistema de carregamento das amostras

Figura: esquema do interior e componentes da

Nordiko 3000 Vantagens

Totalmente automatizada vrios batches com diferentes camadas

Escolha de diferentes alvos versatilidade

Monitorizao detalhada das condies do processo (inmeros controlos)

No obriga a expor a amostra aos plasmas dos canhes

Boa uniformidade na energia dos ies energia para o substrato controlada

Funcionamento a baixas presses preveno de contaminantes

Filmes homogneos, densos e uniformes ( 2% numa wafer de 6 pol)

Reduzido stress no filme (ies no incidem na amostra)

Taxas de deposio controlveis

Step 2- Spin Valve (231 ) deposition - 2

Deposition Thickness Exposure

Tabela: recapitulao das camadas a depositar e tempos de deposio

Figura: resultados esperados aps

Step 2- Spin Valve (231 ) deposition - 3

Colocao da amostra e lamelas (2 amostra de

Receita utilizada: SV22

Rotao e inclinao do substrato maximizam uniformidade

Janela de visualizao durante o processo

Testes iniciais VSM

VSM vibrating sample magnetometer

Estudo das propriedades magnticas da amostra:

Mquina: DMS Model 880

Software auxiliar para operao e

Testes iniciais VSM resultados 1

Signal on X direction, Moment [emu]

Signal on X direction, Moment [emu]

Applied Field [Oe]

Applied Field [Oe]

Testes iniciais VSM resultados 2

Signal on X direction, Moment [emu]

800 1000 1200

Applied Field [Oe]

Free layer alinha-se rapidamente com campo externo

Pinned layer eventualmente tambm se alinha para campos mais

Testes iniciais - GMR

GMR giant magnetorresistance

Estudo das propriedades magnetorresistivas