A 3D Printed Superconducting Aluminium …A 3D Printed Superconducting Aluminium Microwave Cavity...

4
A 3D Printed Superconducting Aluminium Microwave Cavity Daniel L. Creedon, 1 Maxim Goryachev, 2 Nikita Kostylev, 2 Tim Sercombe, 3 and Michael E. Tobar 2, a) 1) School of Physics, University of Melbourne, Parkville, Victoria 3010, Australia 2) ARC Centre of Excellence for Engineered Quantum Systems, University of Western Australia, 35 Stirling Highway, Crawley WA 6009, Australia 3) School of Mechanical and Chemical Engineering, University of Western Australia, 35 Stirling Hwy, Crawley 6009, Australia (Dated: 2 June 2016) 3D printing of plastics, ceramics, and metals has existed for several decades and has revolutionized many areas of manufacturing and science. Printing of metals in particular has found a number of applications in fields as diverse as customized medical implants, jet engine bearings, and rapid prototyping in the automotive industry. Whilst many techniques can be used for 3D printing metals, they commonly rely on computer controlled melting or sintering of a metal alloy powder using a laser or electron beam. The mechanical properties of parts produced in such a way have been well studied, but little attention has been paid to their electrical properties. Here we show that a microwave cavity (resonant frequencies 9.9 and 11.2 GHz) 3D printed using an Al-12Si alloy exhibits superconductivity when cooled below the critical temperature of aluminium (1.2 K), with a performance comparable to the common 6061 alloy of aluminium. Superconducting cavities find application in numerous areas of physics, from particle accelerators to cavity quantum electrodynamics experiments. The result is achieved even with a very large concentration of non-superconducting silicon in the alloy of 12.18%, compared to Al-6061, which has between 0.4 to 0.8%. Our results may pave the way for the possibility of 3D printing superconducting cavity configurations that are otherwise impossible to machine. Superconducting cavities are commonly used to trap and store resonant microwave radiation and reduce losses, allowing devices with very high quality factor (Q), nar- row bandwidth and long storage times 1 . Such cavities are essential for many physics applications, including par- ticle accelerators 2 , ultra-sensitive motion/displacement sensing 3 , precise frequency stabilisation 4 and testing fun- damental physics. In particular tests of the speed of light and the constancy of fundamental constants 4–6 as well as the search for hidden sector particles, which are dark matter candidates 7–10 depend on such cavities. More re- cently they have been applied to cavity quantum electro- dynamics (CQED) experiments to house qubit devices and provide a reduced density of states to radiate into, vital for the success of such experiments. The use of these cavities allows enhanced coherence times 11 and may even serve as a quantum memory. Superconducting cavities are often precision-machined from extremely high purity aluminium or niobium at great cost and investment of time in achieving optimal surface preparation. The use of highly pure aluminium is not always neces- sary, as the standard 6061 aluminium alloy allows very high mechanical Q-factors, and was used in the past for large scale acoustic resonant-mass gravitational wave detectors 12 . The alloy has been shown to become super- conducting, allowing microwave quality factors on the order of 10 6 to be achieved 13 . An analysis by Reagor et al. 13 shows that limitations in quality factor are de- pendent on dielectric losses from the oxide layer lining the interior of the cavity, as well as damping from finite residual surface resistance, both effects being dependent a) Electronic mail: [email protected] on the spatial distribution of the choice of mode excited in the cavity. With the rise in popularity of 3D printing in recent years, it is now fast and inexpensive to manufacture parts from metallic powders, commonly an aluminium alloy with a high concentration of silicon to allow effec- tive laser melting. To investigate whether 3D printed aluminium-silicon cavities exhibited superconductivity, a simple resonant microwave cavity was designed in a cylindrical configuration. The cavity was modelled using COMSOL Multiphysics finite element analysis software, and the geometric factor for the modes computed using: G = ωμ 0 RRR | - H | 2 dV RR | - H | 2 dS (1) where ω is the (angular) eigenfrequency of the mode, μ 0 is the vacuum permeability, and - H is the magnetic field component of the mode. The geometric factor is a cavity parameter which is independent of the cavity size and wall losses, and is related to the intrinsic quality factor of the cavity through the surface resistance R S : Q 0 = G R S (2) Two versions of the cavity were created, differing only in the location of the probe mounts, as seen in Fig. 1, with the internal dimensions of 20mm diameter and 30mm height remaining nominally the same. The cav- ities were 3D printed using a Selective Laser Melting process, performed on a Realizer SLM 100 (ReaLizer GmbH, Germany), which was equipped with a fibre laser (λ=1.06μm) having a maximum power of 200 W at the arXiv:1604.04301v2 [physics.ins-det] 1 Jun 2016

Transcript of A 3D Printed Superconducting Aluminium …A 3D Printed Superconducting Aluminium Microwave Cavity...

Page 1: A 3D Printed Superconducting Aluminium …A 3D Printed Superconducting Aluminium Microwave Cavity Daniel L. Creedon,1 Maxim Goryachev, 2Nikita Kostylev, Tim Sercombe,3 and Michael

A 3D Printed Superconducting Aluminium Microwave CavityDaniel L. Creedon,1 Maxim Goryachev,2 Nikita Kostylev,2 Tim Sercombe,3 and Michael E. Tobar2, a)1)School of Physics, University of Melbourne, Parkville, Victoria 3010, Australia2)ARC Centre of Excellence for Engineered Quantum Systems, University of Western Australia, 35 Stirling Highway,Crawley WA 6009, Australia3)School of Mechanical and Chemical Engineering, University of Western Australia, 35 Stirling Hwy, Crawley 6009,Australia

(Dated: 2 June 2016)

3D printing of plastics, ceramics, and metals has existed for several decades and has revolutionized many areasof manufacturing and science. Printing of metals in particular has found a number of applications in fields asdiverse as customized medical implants, jet engine bearings, and rapid prototyping in the automotive industry.Whilst many techniques can be used for 3D printing metals, they commonly rely on computer controlledmelting or sintering of a metal alloy powder using a laser or electron beam. The mechanical properties ofparts produced in such a way have been well studied, but little attention has been paid to their electricalproperties. Here we show that a microwave cavity (resonant frequencies 9.9 and 11.2 GHz) 3D printedusing an Al-12Si alloy exhibits superconductivity when cooled below the critical temperature of aluminium(1.2 K), with a performance comparable to the common 6061 alloy of aluminium. Superconducting cavitiesfind application in numerous areas of physics, from particle accelerators to cavity quantum electrodynamicsexperiments. The result is achieved even with a very large concentration of non-superconducting silicon inthe alloy of 12.18%, compared to Al-6061, which has between 0.4 to 0.8%. Our results may pave the way forthe possibility of 3D printing superconducting cavity configurations that are otherwise impossible to machine.

Superconducting cavities are commonly used to trapand store resonant microwave radiation and reduce losses,allowing devices with very high quality factor (Q), nar-row bandwidth and long storage times1. Such cavities areessential for many physics applications, including par-ticle accelerators2, ultra-sensitive motion/displacementsensing3, precise frequency stabilisation4 and testing fun-damental physics. In particular tests of the speed of lightand the constancy of fundamental constants4–6 as wellas the search for hidden sector particles, which are darkmatter candidates7–10 depend on such cavities. More re-cently they have been applied to cavity quantum electro-dynamics (CQED) experiments to house qubit devicesand provide a reduced density of states to radiate into,vital for the success of such experiments. The use of thesecavities allows enhanced coherence times11 and may evenserve as a quantum memory. Superconducting cavitiesare often precision-machined from extremely high purityaluminium or niobium at great cost and investment oftime in achieving optimal surface preparation.

The use of highly pure aluminium is not always neces-sary, as the standard 6061 aluminium alloy allows veryhigh mechanical Q-factors, and was used in the pastfor large scale acoustic resonant-mass gravitational wavedetectors12. The alloy has been shown to become super-conducting, allowing microwave quality factors on theorder of 106 to be achieved13. An analysis by Reagoret al.13 shows that limitations in quality factor are de-pendent on dielectric losses from the oxide layer liningthe interior of the cavity, as well as damping from finiteresidual surface resistance, both effects being dependent

a)Electronic mail: [email protected]

on the spatial distribution of the choice of mode excitedin the cavity.

With the rise in popularity of 3D printing in recentyears, it is now fast and inexpensive to manufactureparts from metallic powders, commonly an aluminiumalloy with a high concentration of silicon to allow effec-tive laser melting. To investigate whether 3D printedaluminium-silicon cavities exhibited superconductivity,a simple resonant microwave cavity was designed in acylindrical configuration. The cavity was modelled usingCOMSOL Multiphysics finite element analysis software,and the geometric factor for the modes computed using:

G =ωµ0

∫∫∫|−→H |2dV∫∫

|−→H |2dS

(1)

where ω is the (angular) eigenfrequency of the mode,

µ0 is the vacuum permeability, and−→H is the magnetic

field component of the mode. The geometric factor isa cavity parameter which is independent of the cavitysize and wall losses, and is related to the intrinsic qualityfactor of the cavity through the surface resistance RS :

Q0 =G

RS(2)

Two versions of the cavity were created, differing onlyin the location of the probe mounts, as seen in Fig.1, with the internal dimensions of 20mm diameter and30mm height remaining nominally the same. The cav-ities were 3D printed using a Selective Laser Meltingprocess, performed on a Realizer SLM 100 (ReaLizerGmbH, Germany), which was equipped with a fibre laser(λ=1.06µm) having a maximum power of 200 W at the

arX

iv:1

604.

0430

1v2

[ph

ysic

s.in

s-de

t] 1

Jun

201

6

Page 2: A 3D Printed Superconducting Aluminium …A 3D Printed Superconducting Aluminium Microwave Cavity Daniel L. Creedon,1 Maxim Goryachev, 2Nikita Kostylev, Tim Sercombe,3 and Michael

2

FIG. 1. Photograph of several samples of the 3D printedcavity. The colour difference between the non-annealed andannealed samples is readily visible. (a) Cavity as-printed,(b) Cavity after annealing and having microwave probe holesdrilled and tapped and mating surfaces of lid and body ma-chined flat, (c) Cavity after annealing, machining, and pol-ishing.

part bed. Al-12Si (in wt.%) powder (d50 ∼ 38µm, TLSTechnik, Germany) was used. The exact composition ofthe powder is 12.18% silicon, 0.118% iron, 0.003% cop-per, with the balance consisting of aluminium. In con-trast, 6061 aluminium alloy typically contains maximumimpurity composition of 0.8% silicon, 0.7% iron, 0.15%copper and 1.2% magnesium. An inert, high purity argongas atmosphere was used during processing to minimiseoxidation. The laser scan speed and laser power were1000 mm/s and 200 W, respectively. The powder layerthickness was fixed at 50 µm and the scan spacing at 150µm, while the substrate was heated to 200◦C.

After printing, the cavities underwent further process-ing. In addition to being measured bare (as-printed),the internal surfaces of the cavity were also machinedsmooth, then wet sanded with 220, 600, and 1000 gritsandpaper, followed by polishing with a felt-tipped ro-tary tool and diamond paste at 1200, 1800, 3000, 14000,and 50000 grit. The cavity was wiped clean with acetonein between steps, and finally submerged in acetone in anultrasonic bath for 1 hour and thoroughly cleaned. Aschematic flow chart showing the fabrication process isgiven in Fig. 2. Microwave energy was coupled in andout of the cavity using small ‘loop’ probes consisting ofcoaxial microwave cable with the outer conductor and in-sulation stripped, and the center conductor formed backin a loop and soldered to the outer conductor.

The cavities were bolted to an OFHC (oxygen free highthermal conductivity) copper rod attached to the mixingchamber of a cryogen-free dilution refrigerator. This sys-tem is capable of achieving a base temperature of lessthan 20 millikelvin, and is necessary in order to cool thesamples below the known superconducting temperatureof 1.2 K for aluminium. The surface resistance of the cav-ity walls was then determined by converting, using thegeometric factor, from a direct measurement of the cav-

ity quality factor made with a vector network analyser(VNA). The VNA was connected to the cryostat usingcoaxial microwave cables which were thermally anchoredat each stage of the dilution refrigerator, and the cavitythen measured in transmission, with the weak outcom-ing signal amplified by a low-noise cryogenic microwaveamplifier situated at the 4K stage of the system. Mea-surements were first performed with the bare cavities (asprinted), followed by machining and polishing smooth theinternal surfaces of the cavities.

Coupling to the cavities such that the superconductingtransition could be measured posed a number of chal-lenges. Because the ratio of quality factor to couplingremains constant in such cavities, the probes must be pre-pared in such a way that the mode of interest is severelyundercoupled to the point of being unmeasurable at roomtemperature. In this way, the many orders of magnitudeincrease in coupling associated with the superconductingtransition still results in a very low-coupled mode wherethe quality factor is as close to intrinsic as possible, i.e.not loaded by the coupling probes. This also ensuresthat a reduced vibration sensitivity is achieved, as smalldisplacements of probes with coupling set close to unitycan result in very large change in coupling and thus de-tected amplitude. An insertion loss of -80 to -90 dB atthe peak of the mode at room temperature was foundto give good results. To achieve such low coupling, theloop probes were inserted in the wrong orientation inten-tionally - i.e. with the plane of the loop parallel to themagnetic field vector rather than perpendicular, resultingin an extremely small coupling to the mode.

In the cavity configuration selected, a number of modeswere found that could be coupled to. Modelling the

Cavity design

Machining & polishing of

interior surfaces

Acetonesonication

Anneal 770 K for 4 hours

3D printing by Selective Laser

Melting

Acetonesonication

FIG. 2. Simple flow chart showing an example of the fabrica-tion steps for the cavities described.

Page 3: A 3D Printed Superconducting Aluminium …A 3D Printed Superconducting Aluminium Microwave Cavity Daniel L. Creedon,1 Maxim Goryachev, 2Nikita Kostylev, Tim Sercombe,3 and Michael

3

0 50 100 150 200 250

Frequency offset (kHz) from 13.415,768,115 GHz

5

6

7

8

9

10

11

12

13Tr

ansm

issi

on c

oeffi

cien

t S21

(lin

ear m

agni

tude

)

x 10-3

Q = 1.433 million S21 dataFano fit

FIG. 3. An example of a Fano resonance fit to the transmis-sion coefficient of the TE1,1,2 mode below 100 mK in temper-ature, which is used to extract the resonance frequency andQ-factor.

Surfa

ce re

sist

ance

Rs (O

hm)

10-4

10- 3

10- 2

10-1 Temperature (K)

10-2 100

Freq

uenc

y sh

ift (M

Hz)

from

9.9

36 G

Hz

0.8

0.9

1

1.05

(a)

(b)

FIG. 4. (a) Surface resistance of a 3D printed cavity withpolished internal surfaces and extremely low coupling as mea-sured through the TE1,1,1 mode at 9.9 GHz, and (b) frequencyshift of the same mode as a function of temperature. Becausethe coupling must necessarily be set extremely low to allowan intrinsic measure of quality factor, the mode cannot beobserved above the superconducting transition temperatureof 1.2 K.

twelve lowest order modes in COMSOL Multiphysics (seeTable ) showed a large variation in geometric factor of themodes, indicating that cavity Q-factor is not an accuratecomparison between different modes. Thus, we computethe surface resistance RS using the geometric factor andmeasured quality factor. Based on the choice of probe lo-

Frequency (GHz) Mode Geometric Factor

10.0 TE(1,1,1) 300.411.2 TM(0,1,0) 334.512.35 TM(0,1,1) 29213.4 TE(1,1,2) 432.515.2 TE(2,1,1) 353.815.2 TM(0,1,2) 358.517.6 TE(2,1,2) 426.517.6 TE(1,1,3) 592.417.9 TM(1,1,0) 528.918.6 TE(0,1,1) 755.919.0 TM(0,1,3) 44720.6 TE(0,1,2) 885.3

TABLE I. Summary of lowest order modes and their geomet-ric factors as modelled using COMSOL Multiphysics

cation and the aforementioned difficulties in setting thecoupling to an appropriately small value at room tem-perature, the modes TE1,1,1 at 9.9 GHz, TE0,1,0 at 11.2GHz and TE1,1,2 at 13.4 GHz were selected, as these werefound to be the easiest to couple to. Somewhat surpris-ingly, it was found that leaving the cavity walls rough,i.e. as-printed by the SLM machine, had no disadvan-tage compared to machining the internal surfaces of thecavity smooth and polishing with diamond paste. Anydifference observed resulted in an improvement of ∼10%,which is within the error of the Q-factor measurement.

Following these measurements, annealing of the cavityat 770 K for 4 hours was performed. This was foundto have a larger effect, resulting in an improvement inquality factor for the highly polished cavity, but hav-ing no effect for the rough ‘as-printed’ cavity. We an-ticipate that the losses here are dominated by the sur-face roughness and thus no improvement in Q-factor isseen after annealing. In the best case, the Q-factor of amode was improved from 1.6 million to 3.8 million. After3D printing, the silicon content of the cavity is approx-imately 6-7%, however the solubility of Si in Al is only∼1.5%, and nearly zero at room temperature. Annealingat high temperature followed by slowly letting the cavitycool to room temperature was found to drive off mostof the silicon, leaving a pure aluminium matrix behind.The brightness of the cavity finish was also noticeablychanged from dark to light grey after annealing.

Fig. 3 shows the S21 transmission coefficient of theTE1,1,2 mode, which is well modelled by a Fano reso-nance fit14,15 - a pure Lorentzian lineshape profile withan asymmetry factor. The Q-factor of each mode wascomputed by fitting a Fano resonance to the transmis-sion curve, and taking the ratio of center frequency andlinewidth extracted from the Lorentzian part of the fit.

Fig. 4 shows the surface resistance (as calculated fromthe measured Q-factor and modelled geometric factor)and frequency shift of the TE1,1,1 mode as a function oftemperature for an internally polished cavity. At 20 mil-likelvin temperature a Q-factor of 1.5×106 was obtained.

In order to determine the superconducting critical

Page 4: A 3D Printed Superconducting Aluminium …A 3D Printed Superconducting Aluminium Microwave Cavity Daniel L. Creedon,1 Maxim Goryachev, 2Nikita Kostylev, Tim Sercombe,3 and Michael

4

magnetic field of the cavities, an external DC magneticfield was applied parallel to the cavity axial direction.The magnetic sensitivity of the cavities was found to bein good agreement with the known critical field for alu-minium, with the superconducting effect being destroyedand the quality factor of the mode degraded to the pointof the mode disappearing entirely after the applicationof a field greater than 10 mT . Even after ramping thefield back to zero, the mode could not be recovered untilthe cavity was heated above its superconducting criticaltemperature of 1.2K to release trapped magnetic flux.Modes that were highly overcoupled remained visiblewith the application of magnetic field, and underwentno change in quality factor. For instance, when highlyovercoupled, we found that the TE1,1,1 mode in anas-printed cavity exhibits Q∼ 1.5 × 104, a value thatremained constant up to applied external DC magneticfield values of in excess of 5 T. This may be importantfor axion detection experiments, which require verylarge cavities in high magnetic field with quality factorson the order of the axion linewidth of 106. The modemeasured here corresponds to Q∼ 7 × 104 at the axionsearch frequency of 500 MHz, given the constant ratio ofquality factor to frequency.

In summary, we show that 3D printing of an aluminiummicrowave cavity using commonly sourced ‘dirty’ alu-minium powder allows the observation of superconduc-tivity in the resultant metal. The results are comparableto cavities machined in the conventional way from com-mon Al-6061 alloy13, and are unaffected by the surfaceroughness of the cavity walls due to the 3D printing pro-cess. A combination of machining and polishing smooththe cavity interior, followed by annealing at 770 K for 4hours to drive off residual silicon impurities was found toimprove the Q-factor by approximately a factor of two.We anticipate that the use of highly pure metallic pow-ders, rather than the Al-12Si powder used in the presentwork, will result in further improvements comparable tostate of the art aluminium cavities manufactured in theconventional way. Such cavities have been shown to reachquality factors on the order of 0.5 ×109 for similar modefrequencies when highly pure 5N5 aluminium is used13.Indeed, we note that recently published results16 haveshown that using highly pure Niobium powder and ana different 3D printing process known as Electron BeamMelting, when combined with advanced surface prepa-ration techniques such as buffered chemical polishing,

can result in quality factors on the order of 109 for cav-ity frequencies of 3.8 GHz. For applications where suchhigh quality factors are not required, the process of SLMwith the relatively much more inexpensive Al-12Si pow-der may prove a useful and rapid way to fabricate exper-imental apparatus. Little experimental data exists in theliterature for 3D printed superconducting cavities of anydescription, and thus further work will be required to de-termine the optimum material and technique for additivemanufacturing of such devices.ACKNOWLEDGMENTS

This work was supported by the Australian ResearchCouncil grant number CE110001013.

1J. P. Turneaure and I. Weissman, Journal of Applied Physics 39,4417 (1968).

2T. L. Grimm, A. Aizaz, M. Johnson, W. Hartung, F. Marti,D. Meidlinger, M. Meidlinger, J. Popielarski, and R. C.York, IEEE Transactions on Applied Superconductivity 15, 2393(2005).

3D. G. Blair, E. N. Ivanov, M. E. Tobar, P. J. Turner, F. vanKann, and I. S. Heng, Phys. Rev. Lett. 74, 1908 (1995).

4J. P. Turneaure, C. M. Will, B. F. Farrell, E. M. Mattison, andR. F. C. Vessot, Phys. Rev. D 27, 1705 (1983).

5J. A. Lipa, J. A. Nissen, S. Wang, D. A. Stricker, and D. Avaloff,Phys. Rev. Lett. 90, 060403 (2003).

6M. Nagel, S. R. Parker, E. V. Kovalchuk, P. L. Stanwix, J. G.Hartnett, E. N. Ivanov, A. Peters, and M. E. Tobar, Nat Com-mun 6, 10.1038/ncomms9174 (2015).

7S. R. Parker, J. G. Hartnett, R. G. Povey, and M. E. Tobar,Phys. Rev. D 88, 112004 (2013).

8S. R. Parker, G. Rybka, and M. E. Tobar, Phys. Rev. D 87,115008 (2013).

9R. G. Povey, J. G. Hartnett, and M. E. Tobar, Phys. Rev. D 84,055023 (2011).

10J. Jaeckel and A. Ringwald, Annual Review of Nuclear and Par-ticle Science 60, 405 (2010).

11H. Paik, D. I. Schuster, L. S. Bishop, G. Kirchmair, G. Catelani,A. P. Sears, B. R. Johnson, M. J. Reagor, L. Frunzio, L. I. Glaz-man, S. M. Girvin, M. H. Devoret, and R. J. Schoelkopf, Phys.Rev. Lett. 107, 240501 (2011).

12A. Morse, W. O. Hamilton, W. W. Johnson, E. Mauceli, andM. P. McHugh, Phys. Rev. D 59, 062002 (1999).

13M. Reagor, H. Paik, G. Catelani, L. Sun, C. Axline, E. Holland,I. M. Pop, N. A. Masluk, T. Brecht, L. Frunzio, M. H. Devoret,L. Glazman, and R. J. Schoelkopf, Applied Physics Letters 102(2013).

14A. E. Miroshnichenko, S. Flach, and Y. S. Kivshar, Reviews ofModern Physics 82, 2257 (2010).

15T. Lepetit, E. Akmansoy, J.-P. Ganne, and J.-M. Lourtioz, Phys-ical Review B 82, 195307 (2010).

16P. Frigola, R. Agustsson, L. Faillace, M. A., G. Ciovati,W. Clemens, P. Dhakal, F. Marhauser, R. Rimmer, J. Spradlin,and W. S., in Proceedings of SRF2015, Whistler, BC, Canada(2015).