PROOF OF CONCEPT THIN FILMS AND MULTILAYERS TOWARD ENHANCED FIELD - - PowerPoint PPT Presentation

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PROOF OF CONCEPT THIN FILMS AND MULTILAYERS TOWARD ENHANCED FIELD - - PowerPoint PPT Presentation

PROOF OF CONCEPT THIN FILMS AND MULTILAYERS TOWARD ENHANCED FIELD GRADIENTS IN SRF CAVITIES Rosa A. Lukaszew , Douglas B. Beringer, William M. Roach, College of William and Mary , Williamsburg, Virginia, USA Grigory V. Eremeev, Charles E. Reece,


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SLIDE 1

PROOF OF CONCEPT THIN FILMS AND MULTILAYERS TOWARD ENHANCED FIELD GRADIENTS IN SRF CAVITIES

Rosa A. Lukaszew, Douglas B. Beringer, William M. Roach,

College of William and Mary, Williamsburg, Virginia, USA

Grigory V. Eremeev, Charles E. Reece, Anne-Marie Valente-Feliciano,

Thomas Jefferson National Accelerator Facility [TJNAF], Newport News, Virginia, USA

Xiaoxing Xi,

Temple University, Philadelphia, Pennsylvania, USA

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SLIDE 2

Nb SRF cavities

  • The choice of Nb for superconducting cavities has been dictated by

the requirement of having a material with a high lower critical field Bc1 and a large energy gap D to prevent vortex dissipation and provide a low surface resistance Rs caused by thermally-activated quasiparticles at T << Tc and w << D,

  • Rs = (Aw2/T) exp(-D/T) + Ri where Ri is a small temperature

independent residual resistance and A depends on SC parameters and w and T

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SLIDE 3
  • Significant improvement could be

achieved if a Nb cavity is coated with a multilayer consisting of alternating superconducting S layers with higher Bc, and dielectric I layers

  • The S layer has thickness d < l , and

therefore can remain in the Meissner state at fields much higher than Bc1 bulk due to the increase of the parallel Bc1 in a thin film, while the insulating layer (~15 nm) is needed to prevent Josephson coupling between the SC layers.

  • Such structure would be particularly

efficient in the case of elliptical cavities where the magnetic field is concentrated well inside the cavity and is parallel to the surface.

  • A. Gurevich, Appl. Phys. Lett. 88, 012511 (2006).

The Gurevich model

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SLIDE 4

Thin film geometry  Bc1 enhancement  Multilayer shielding

Image: CERN Accelerator School

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SLIDE 5

Our experimental approach and methods

  • In order to test the Gurevich

model we have investigated the effect of microstructure and morphology on the superconducting properties

  • f Nb thin films deposited
  • nto different ceramic
  • surfaces. In particular we

studied a-plane sapphire and (001) MgO.

  • We have also investigated

Nb, NbN, NbTiN and MgB2 based S/I/S trilayers.

  • We monitored the

microstructure of the films, the morphology of the surface and the superconducting properties as well as the DC and RF transport properties.

  • We explored several aspects

in the thin film deposition parameters-space, such as growth rate, substrate temperature during growth, annealing treatments, etc.

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SLIDE 6
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SLIDE 7

Thin film growth onto various different surfaces

  • Growth on sapphire, magnesium
  • xide and copper surfaces
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SLIDE 8

Nb growth on a-plane sapphire

  • Nb can grow epitaxially on a-plane sapphire, with Nb(110)//Al2O3(11-20)

* RRR values for niobium thin films is highly dependent on thickness [1]. S. A. Wolf et al., J. Vac. Sci. Tecnol. A 4 (3), May/June 1986 [2] G. Wu et al., Thin Solid Films, 489 (2005) 56-62

Group Nb film thickness (nm) RRR Lukaszew 600 97

  • S. A. Wolf [1]

600 82

  • G. Wu [2]

235 50.2* Comparison of RRR values obtained by different groups:

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SLIDE 9

Early stages of growth

1 10 100 0.29 0.30 0.31 0.32 0.33 0.34 0.35 0.36

0.23 2.3 23

Nb thickness (nm)

Lattice parameter (nm) Nb atomic layers

bulk Nb bcc

[111]Nb ll[0001]Al O

2 3

[1120]Nb ll [0001]Al O

2 3

a

hcp Nb bcc Nb hcp+bcc Nb

a

  • Using

Reflection high energy electron diffraction (RHEED), we

  • bserved

a hexagonal Nb surface structure for the first 3 atomic layers followed by a strained bcc Nb(110) structure and the lattice parameter relaxes after 3 nm.

  • RHEED images for the hexagonal

phase at the third atomic layer. Patterns repeat every 60 deg. 0 deg 30 deg 60 deg

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SLIDE 10

Susceptibility AC measurements

  • The thinner Nb film exhibits two

steps in the χ’ susceptibility transition accompanied by two peaks in the χ’’ susceptibility due to strained Nb layers at the interface.

  • Growth on a-plane sapphire

initially follows a hexagonal surface structure to relax the strain and to stabilize the subsequent growth of bcc Nb(110) phase.

  • Such initial layers affect the

superconducting properties of the films and these effects must be taken into account in the design of multilayers.

0.0 0.1

  • 1

0.0 0.1

  • 1

7 8 9 10

0.0 0.2

7 8 9 10

  • 1

''

'

600 nm 100 nm

Temperature (K) Temperature (K)

30 nm

χ(ω)= χ’(ω)+i χ’’(ω)

Strain Effects on the Crystal Growth and Superconducting Properties of Epitaxial Niobium Ultrathin Films, C. Clavero, D. B. Beringer, W.

  • M. Roach, J. R. Skuza, K. C. Wong, A. D. Batchelor, C. E. Reece, and R. A. Lukaszew, Cryst. Growth Des., 12 (5), pp 2588–2593 (2012)
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SLIDE 11

400 nm

( a ) 30 nm Nb

. 200 nm

( c ) 600 nm Nb

200 nm

( b ) 100 nm Nb

500 10 00 10 20 30

30 nm 100 nm heigth (nm) distance (nm) 600 nm Al O [0001]

2

3

Al O [1100]

2 3

( d )

N b [ 1 1 ] Nb [001]

50 nm

Biaxial anisotropy is observed for thicknesses up to 100 nm while uniaxial anisotropy is observed. For thicker films

Subsequent growth

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SLIDE 12

Nb growth on (001) MgO

  • Nb can also be

epitaxially grown on (001) MgO surfaces.

  • Unexpected findings:

We have found that depending on the deposition conditions it is possible to tailor different epitaxial possibilities.

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SLIDE 13

RHEED images for Nb(110) on MgO

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SLIDE 14

Scaling of surface features

RRR = 46.5 RMS = 6.51 nm 50 nm 600 nm

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SLIDE 15

Nb (001) on MgO

14.29 nm 0.00 nm

400nm RRR = 165 RMS = 4.06 nm

>200 RRR values!

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SLIDE 16

RHEED beam along MgO [100] MgO out of box MgO annealed at 600 °C 30 nm Nb

Nb (001) on MgO

RHEED beam along MgO [110] 100 nm Nb MgO out of box MgO annealed at 600 °C 30 nm Nb 100 nm Nb

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SLIDE 17

30.00 nm 0.00 nm

1.0µm

RMS = 2.90 nm

10.00 nm 0.00 nm

400nm

10.00 nm 0.00 nm

200nm

RMS = 1.21 nm RMS = 1.08 nm

  • D. B. Beringer, W. M. Roach, C. Clavero, C. E. Reece, and R. A. Lukaszew, "Roughness analysis applied to niobium thin films

grown on MgO(001) surfaces for superconducting radio frequency cavity applications," Phys. Rev. ST Accel. Beams 16, 022001 (2013).

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SLIDE 18

4 5 6 7 8 9 10

  • 0.2

0.0 0.2 0.4 0.6 0.8 1.0 " Temperature (K)

  • 1.0
  • 0.8
  • 0.6
  • 0.4
  • 0.2

0.0 4 5 6 7 8 9 10 '

SQUID characterization

Tc = 9.2 K! Possible loss due to interfacial strain

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SLIDE 19

38.5 39.0 55 56

Nb(110) Nb(200)

Intensity (arb. u.) 2 (deg)

RHEED indicates film with high degree of (001) texture

XRD confirmed RHEED results:

Nb-based trilayer

MgO (100) 250 nm Nb 15 nm MgO 30 nm Nb

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SLIDE 20
  • Antoine et al [1] using SQUID magnetometry as well as

third harmonic analysis to validate SQUID magnetometry measured the vortex penetration field

  • n multilayered samples and demonstrated field

enhancement.

  • In our work, we measured hysteresis loops as well as

trapped moments that appear after application and removal of the applied field, following the work of C. Bohmer et al. [2]

[1] C. Z. Antoine, S. Berry, S. Bouat, J.-F. Jacquot, J.-C. Villegier, G. Lamura, and A. Gurevich, Phys.

  • Rev. ST Accel. Beams, vol. 13, p. 121 001, 2010; C. Z. Antoine, S. Berry, M. Aurino, J.-F. Jacquot, J.- C.

Villegier, G. Lamura, and A. Andreone, IEEE Trans. Appl. Supercond., vol. 3, p. 2601, 2011; [2] C. Böhmer, G. Brandstätter, and H. W. Weber, Supercond. Sci. Technol. 10 A1 (1997).

SQUID magnetometry

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SLIDE 21

4 5 6 7 8 9 0.0 0.2 0.4 0.6 0.8 1.0 " Temperature (K)

  • 1.0
  • 0.8
  • 0.6
  • 0.4
  • 0.2

0.0 4 5 6 7 8 9 '

  • 6000 -4000 -2000

2000 4000 6000

  • 0.02

0.00 0.02

4 K

Long Moment (emu)

Field (Oe)

SQUID characterization

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SLIDE 22

Nb on Cu (111)

  • Growth at room temperature and annealing at

350 ºC leads to the crystallization of Nb islands in a hexagonal surface structure, even though Nb is expected to growth tetragonal (110).

3.30 Å 0.00 Å

3.3 Å

0 Å

Cesar Clavero, Nathan P. Guisinger, Srivilliputhur G. Srinivasan, and R. A. Lukaszew, “Study of Nb epitaxial growth

  • n Cu(111) at sub-monolayer level”, J. Appl. Phys. 112, 074328 (2012).
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SLIDE 23

Nb films on Cu (001) surfaces

(a) RHEED pattern for Nb(110)/Cu(100)/Si(100) along the Si[100] and Si[110] azimuths. (b) A representative 2 µm x 2 µm AFM scan for Nb films on the Cu template. Possible Nb/Cu(100) epitaxy:

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SLIDE 24

SC properties for different growth T

  • The films grown at 150 °C have

a very sharp transition from the superconducting state to the normal state that begins at ~9 K while films grown at RT have a much more gradual transition.

  • Our results suggest that an

increased deposition temperature of Nb onto Cu leads to films with higher crystalline quality (grain size) and thus improved superconducting properties (HC1).

Niobium thin film deposition studies on copper surfaces for superconducting radio frequency cavity applications, W. M. Roach, D. B. Beringer, J. R. Skuza, W. A. Oliver, C. Clavero, C. E. Reece, and R. A. Lukaszew, Phys. Rev. ST Accel. Beams 15, 062002 (2012).

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SLIDE 25

Nb films on Cu

Substrate RRR Single crystal Cu (100) 129 Cu (110) 275 Cu (111) 242 Polycrystalline Cu fine grains 150 Cu large grains 289

Nb films with quality comparable to high RRR bulk Nb (as used for SRF cavities) have been produced both on single crystal and polycrystalline Cu substrates with energetic condensation via ECR (electron cyclotron resonance) at

  • Jlab. SRF measurements are in progress.

Hetero-epitaxial relationships between Nb and Cu verified.

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SLIDE 26

Other possible SC thin films for the SIS model

NbN, MgB2, etc.

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SLIDE 27

Growth Procedure for NbN Films Partial Pressure Series

All NbN films are ~200 nm thick based on XRR/Profilometry

MgO (001) ~400 nm NbN

600 °C (40 V) for 1 hour 600 °C growth

3 nm MgO

RT growth

~1-2 ML Mg

600 °C growth 600 °C (40 V) for 30 min

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SLIDE 28

Compare Surface Morphology of Nb and NbN similar films

0.0 0.5 1.0 1.5 2.0 5 10 15 20 25

Nb(110) Nb(100)

Height (nm)

Distance (m)

NbN

400nm

400nm 400nm

NbN Nb(100) Nb(110)

RMS Roughness for comparable film thickness: NbN <1 nm Nb(100) 1.21 nm Nb(110) 2.45 nm

  • D. B. Beringer, W. M. Roach, C. Clavero, C. E. Reece and R. A. Lukaszew, “Roughness analysis applied to niobium thin films

grown on MgO(001) surfaces for superconducting radio frequency cavity applications” accepted for publication in Phys. Rev. ST Accel. Beams (2012).

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SLIDE 29

NbN films microstructure

2.6 2.8 3.0 3.2 3.4

26.5% 20.6% 14.7%

Intensity (arb. units)

qz (Å

  • 1
  • 1)

11.8% MgO(200)

-NbN(200)

5.9%

4.32 4.34 4.36 4.38 4.40 300 400 500 0.0 0.5 1.0 5 10 15 20 25 30 0.75 1.00 Bulk

(d) (c) (b)

c a

Spacing (Å)

(a)

Grain Size (Å) Misalignment () Mosaicity ()

N2 Partial Pressure (%)

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SLIDE 30

Residual Resistance Ratio

50 100 150 200 250 300 0.1 1 10

Resistivity (Ohm)

Temperature (K)

RRR = 1

10 15 20 1E-5 1E-4 1E-3 0.01 0.1 1 10

Resistivity (Ohm)

Temperature (K)

Resistive behavior for NbN differs from that of metals such as Nb. RRR=1 Is indication of very good quality film!

50 100 150 200 250 300 0.1 1 10

Resistivity (Ohm)

Temperature (K)

RRR = 165

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SLIDE 31

Superconducting Properties

  • 1

4 6 8 10 12 14 16 5 10 15 20 25 30 6 8 10 12 14 16 H = 50 Oe 26.5 % 14.7 %

Temperature (K) Susceptibility (arb. units)

5.9 %

(a) (b)

TC (K)

N2 Partial Pressure (%) H = 50 Oe Bulk

500 1000 1500 1 5.9% 11.8% 14.7%

Normalized Moment (arb. units)

Field (Oe)

  • W. M. Roach, J. R. Skuza, D. B. Beringer, Z. Li, C. Clavero, and R. A. Lukaszew, “NbN thin films for superconducting radio

frequency cavities”. Supercond. Sci.Technol. 25, 125016 (2012).

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SLIDE 32

MgB2 thin films

We have initiated investigations on MgB2 thin films.

40 60 80 100 120 140 1000 2000 3000 4000 5000 6000 7000 8000 9000 10000

Hc1 (Oe) Thickness (nm)

Theory

Falls apart due to surf. roughness

  • D. B. Beringer, C. Clavero, T. Tan, X. X. Xi,W.M. Roach, and R.
  • A. Lukaszew, "Thickness Dependence and Enhancement of

HC1 in Epitaxial MgB2 Thin Films," IEEE Trans. Appl.

  • Supercond. 23, 7500604 (2013).
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SLIDE 33

SIS layers

  • NbN-based, MgB2 based and

NbTiN-based trilayers

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SLIDE 34
  • 6000
  • 4000
  • 2000

2000 4000 6000

  • 0.0010
  • 0.0005

0.0000 0.0005 0.0010

Long Moment (emu) Field (Oe) Long Moment (emu)

T = 4.5 K

Hc1-NbN-based-Multilayer ~ 220 mT! Hc1-bulk Nb = 170 mT

NbN-based multilayer

MgO (100) 250 nm Nb 50 nm NbN 15 nm MgO

“Magnetic Shielding Larger than the Lower Critical Field of Niobium in Multilayers” W. M. Roach, D. B. Beringer, Z. Li, C. Clavero, and R. A. Lukaszew, IEEE Trans. Appl. Supercond. 23, 8600203 (2013).

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SLIDE 35

35 40 45 50 55 60 1 10 100 1000 10000 100000

Intensity (arb. units) 2 (deg)

-NbN (200)

MgO(200) Nb(200)

  • 0.00015
  • 0.00010
  • 0.00005

0.00000 4 6 8 10 12 14

NbN Transition Temperature (K) Long Moment (emu) Nb Transition H = 10 Oe

XRD SQUID

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SLIDE 36

35 40 45 50 55 60

MgO(200) MgB2(200) Nb(110) Intensity 2 (deg)

XRD characterization MgB2-based ML sample

MgO (100) 250 nm Nb 50 nm NbN 15 nm MgO

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SLIDE 37

XRD scan optimized on the MgB2(200) peak. The scan indicates that there are multiple MgB2 phases present, all strained 1st phase 3.4275 Å 2.7108% strain 2nd phase 3.4223 Å 2.8584% strain 3rd phase 3.4155 Å 3.0514 % strain Bulk 3.523 Å (2 = 51.863o)

53.0 53.5 54.0

Data 1st phase 2nd phase 3rd phase Cumulative fit MgB2(200) Intensity 2 (deg)

53.0 53.5 54.0

MgB2(200) Intensity 2 (deg)

XRD detail

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SLIDE 38

5 10 15 20 25 30 35

  • 0.00006
  • 0.00005
  • 0.00004
  • 0.00003
  • 0.00002
  • 0.00001

0.00000

Long Moment (emu) Temperature (K) H = 10 Oe

SQUID characterization

Tc ~ 30.2 K (recall that bulk Tc = 39K)

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SLIDE 39

SQUID measurements

Reference Nb penetration field ~ 1300 Oe; MgB2-based ML penetration field ~ 1700 Oe

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SLIDE 40

Surface impedance characterizations (SIC)

  • The ultimate performance test of

the films and multilayers for this application is a measurement of their surface impedance, Rs.

  • We note that Rs can be written as:

Rs = RBCS (T) + Ri, where RBCS = (Aw2/T) exp[-D/(kBT)]

Note: Rs decreases strongly for higher-Tc materials with larger superconducting gap Δ = 1.86Tc, implying that materials with Tc > 20K, could have the RBCS at 4.2 K comparable to RBCS of Nb at 2K. However, small Rs also implies small residual resistance Ri and no nodes in the superconducting gap, which rules out the d-wave high-Tc cuprates for which Rs ∝ T2

  • JLab’s SIC system is uniquely

capable of making temperature- dependent RF surface impedance measurements on 2inch-sized thin film samples.

  • Summary of 2 inch samples

studied:

  • Nb thin films grown under various

conditions

  • Epitaxial MgB2 films
  • NbN-based trilayer on copper
  • NbTiN-based multilayers deposited
  • n sapphire
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SLIDE 41

Nb thin films grown under different conditions

Nb films were grown at Jlab at different T, and bias conditions, etc. using ECR

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SLIDE 42

MgB2 films epitaxially grown on sapphire

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SLIDE 43

At the SRF 2011 the surface impedance of a MgB2-based multilayer was reported, and the residual resistance was found ~ 181 W

MgB2 based SIS structure

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SLIDE 44

Samples grown on Cu substrates contained large grains (on the order of millimeters) that were visible to the naked eye. The surfaces of these samples are dominated by rough features as seen with SEM and optical microscopy. After annealing 10 nm of MgO and 60 nm of NbN were deposited (W&M).

NbN-based SIS samples deposited on Cu substrates

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SLIDE 45

SIC for NbN/MgO/Nb trilayer on Copper

We note that the residual resistance (Ri) around 2K is approximately 35 Ohm.

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SLIDE 46

2 3 4 5 6 1 10 100 1000 10000

NbN/MgO/Nb/Cu Nb/Cu-ECR70-360°C/360°C, -180V(7')+0V(23') Nb/Cu-ECR64-360C/360C, -180V (30') Large grain Niobium

RS(W) T(K)

SIC comparison of different thin film and ML samples

We notice that the residual resistance of these thin film samples is one order larger than that of bulk Nb around 2K but in general lower than that of MgB2-based ML samples.

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SLIDE 47

Cu

NbTiN AlN

Nb

NbTiN

AlN NbTiN N2/Ar 0.33 0.23 Total pressure [Torr] 2x10-3 2x10-3 Sputtering Power [W] 100 300 Deposition rate [nm/min] ~ 5 ~ 18 Thickness [nm] 10 100 Tc [K] N/A 14

NbTiN-based SIS structures on bulk Nb and Nb/Cu substrates

NbN-based multilayers have been very promising regarding magnetic shielding, but we note that this material suffers from a higher resistivity due to the presence of both metallic and gaseous vacancies randomly distributed while the ternary nitride NbTiN presents all the advantages of NbN and also exhibits increased metallic electrical conduction properties with higher titanium (Ti) percentage.

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SLIDE 48

We note that the residual resistance (Ri) around 2K is approximately 30 Ohm. We also distinguish two temperature regimes with transitions around 8.5 K and 14.5K, related to Nb and NbTiN respectively.

SIC for NbTiN/AlN/Nb trilayer on sapphire

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SLIDE 49

Conclusions

  • Trilayers incorporating NbN and following the “Gurevich

model” were shown to shield niobium in the pioneer work by Antoine et al. using SQUID magnetometry as well as third harmonic analysis.

  • By tailoring thin film growth parameters, and also using

SQUID magnetometry we were able to demonstrate shielding beyond the critical field of Nb also using NbN- based trilayers.

  • We have also demonstrated that other suitable

superconductors show promise for SRF applications, but further studies to optimize thin film deposition conditions must be undertaken in this case.

  • This work is supported by the Defense Threat Reduction

Agency (DTRA) under grant # HDTRA1-20- 1-0072.