42
New - hot high pressure technologies for high performance MgB2 conductors in application perspectives. A. Morawski 1 , T. Cetner 1 , A. Zaleski 2 , D. Gajda 3 , M. Rindfleish 4 , M. Tomsic 4 , R. Diduszko 5 , T. Czujko 6 1. Institute of High Pressure Physics, Polish Academy of Sciences, Warsaw , Poland 2. Institute of Low Temperature and Structure Research Polish Academy of Sciences, Wroclaw, Poland 3. International Laboratory of High Magnetic Fields and Low Temperatures,Wroclaw, Poland 4. Hypertech Research, Inc., Columbus , Ohio, United States 5. Institute of Tele- and Radiotechnic, Warsaw, Poland 6. Military Technical Academy, Warsaw, Poland See also the poster presentation concerning: HIP positive influence on pure MgB 2 wires.. Presented by : - Daniel Gajda S-P-326 ( May 1st ) poster

New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

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Page 1: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

New - hot high pressure technologies for high performance MgB2 conductors in application

perspectives.

A. Morawski1, T. Cetner1, A. Zaleski2, D. Gajda3, M. Rindfleish4, M. Tomsic4, R. Diduszko5, T. Czujko6

1. Institute of High Pressure Physics, Polish Academy of Sciences, Warsaw , Poland 2. Institute of Low Temperature and Structure Research Polish Academy of Sciences, Wroclaw, Poland 3. International Laboratory of High Magnetic Fields and Low Temperatures,Wroclaw, Poland 4. Hypertech Research, Inc., Columbus , Ohio, United States 5. Institute of Tele- and Radiotechnic, Warsaw, Poland 6. Military Technical Academy, Warsaw, Poland

See also the poster presentation concerning: HIP – positive influence on pure MgB2 wires.. Presented by :

- Daniel Gajda S-P-326 ( May 1st ) poster

Page 2: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Content of the presentation

Principal attributes of high pressure HIP applicated for MgB2 wires sintering

Surprisingly high Jc of MgB2 in/ex-situ wires obtained by HIP in 2005

The stress effect & rapid degradation of Jc in wires over certain strain (1,3 GPa)

Solid state reaction and the pressure dependence of Mg melting by DTA

The kinds of PIT technology for high Jc classic and new (ex/in) wires technology

Morphology of the HIP-ed wires from both techniques ( in/ex and HyperTech)

The Jc and Fp ( pining force ) for HIP-ed in solid state and liquid phase wires

Proposal of the next investigations and conclusions

Page 3: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Mains attributes of HIP (Hot Isostatic Pressing) applied to MgB2 structure

HIP is high densification process enabled to obtain the best grains connectivity during sintering by simultaneous pressure and temperature action at isostatic conditions. Typically for the grains dimensions as low as tens nano meters a few GPa pressure is required, to get highest ceramic density without cracks. High pressure can substantially modify the liquid – solid line of the Mg melt temperature (Tm), which change the phase diagram. Due to the higher melting temperature of Mg under high pressure the solid state reaction of the substrates is occurred and the grains growth is strongly restricted and limited. The plasticity of the wire core obtained by the solid state reaction of the nano grains, is

much better than that obtained with liquid Mg or other liquid phases as : Mg2Si, Mg-Cu etc. The stress applied to the sheath material by HIP can be transmitted directly to the in situ core

and is constant during all HIP process! Contrary to the CIP all other cold deformation processes, which act only on the beginning of the sintering/ synthesis, due to the high shrinkage of the Mg+2B sintering and softening of any of the sheaths metal at high temperatures - so CP process is much less effective than HIP in densification of nano grains structure.

The HIP easily avoid the grains growth and effectively block the growth of grain at the last part of sintering process especially (where the applied temperature is usually made higher) due to the high nano dispersion of the final MgB2 hard grains- self reinforcement.

The high pressure powder technology can be used for powder mixing ,cleaning and pulverize of the agglomerates e.g. US-HP

Page 4: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Why such high Jc at high magnetic field after the HIP treatment at 1 GPa made on Cu/MgB2 sheathed wires was found by us at 2005? ; presented at MT-20

High Jc ( a) and Fp (pining) ( b) was found to be the effect of the solid state reaction performed by the HIP for an infiltration process in in situ composite wires with Cu stabilizer (without any expensive Nb barrier) due to the solid state process and further high pressure infiltration in the obtained MgB2 nano grains . The high densification, and the best possible connectivity with limited grains growth was performed at 1 GPa isostatic pressure see; (A.Morawski B. Głowacki, - MT20 & Hipermag EU project reports).

Page 5: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Where is a limit of the stress apllied to the MgB2 ceramic at ambient temperature?

Stress in the steel matrix of a multifilamentary conductor during manufacture. The critical current drops rapidly above the marked strain, corresponding to a wire diameter of around 0.9 mm. – the core break effect (B.Głowacki)

Page 6: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The High Pressure (HIP) and (HP) Processes adapted for MgB2 wires and tapes preparation in these investigations:

HIP up to 1.6 GPa in argon gas medium, Temp up to 1200 oC

HIP up to 1 GPa in liquid medium KCl+ NaCl, silicon oil ( 450 -700 oC) HP up to 0.3 GPa in solid - plastic medium 0.3 GPa ( BN, graphite)

Page 7: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

High Pressure HIP — (Hot Isostatic Pressing) chamber up to 1.6 GPa used for MgB2

Pressure – up to 1.6 GPa (argon, nitrogen, helium & oxygen up to 0.2 GPa), Temperature ( max 2100 deg C) – here from 550 to 1200 oC, typically 700 oC

Duration of the process ( longest 120 hours) – here 5...1600 min

Hot Isostatic Pressing – HIP- laboratory gas medium equipment

Page 8: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The components of the furnace set for HIP & DTA crucible construction

Furnace for HIP or DTA experiment

or Mg+2B

Graphite

High pressure plug

Fit trough and reference thermocoupletype T

Outside and inside thermocouples type K

Cu tube like conteiner

Alumina oxide tube & ampules

Page 9: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

4050 4100 4150 4200

560

570

580

590

600

610

620

630

640

650

660

670

680

Tm = Tref+ Tt =48deg C + Tt

Tt in

de

g C

time in [s]

furnace control thermocouple line

independent thermocouple

immersed thermocouple

pressure = 0.39 GPa= 3900 bar

9910 9920 9930 9940 9950 9960 9970 9980

580

590

600

610

620

630

furnace control thermocouple line

independent thermocouple

immersed thermocouple

Tt in

de

g C

time in [s]

p= atmospheric pressure

Tm = Tref+ Tt =48deg C + Tt

1000 1500 2000 2500

500

550

600

650

700

750

800

850

furnace control thermocouple line

independent thermocouple

immersed thermocouple

Te

mp

era

ture

de

gC

time in [s]

8200 8210 8220 8230 8240 8250 8260 8270 8280 8290

530

540

550

560

570

580

590

600

610

620

630

640

650

660

670

680

690

furnace control thermocouple line

independent thermocouple

immersed thermocouple

Tm = Tref+ Tt =48deg C + Tt

Tt in

d

eg

C

time in [s]

p=0.147GPa= 1470 bar

DTA profiles taken at various argon pressures for Mg melting experiment

Page 10: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Melting temperature of pure Mg +2B at various Ar pressure (plot and fit)

0,0 0,5 1,0600

650

700

750

800

850

Tm

(d

eg

. C

)

Pressure (GPa)

Equation y = a + b*x

Adj. R-Square 0,98865

Value Standard Error

Tm Intercept 645,26277 2,41871

Tm Slope 146,36345 5,92147

Melting temperature of Mg+ 2B system at high pressure of argon

Page 11: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

4 6 8 10 12 14 16 18 20

1E-13

1E-12

1E-11

1E-10

1E-9

1E-8

1E-7

1E-6

1E-5

1E-4

1E-3

0,01

0,1

1649,8800

Gas + B(s)

Gas+MgB7

Gas + MgB4

Gas + MgB2

Solid Mg + MgB2

Liq Mg + MgB2

Temperature [o C]

2000 1500 1000 500

Ar

ga

s p

res

su

re o

ve

r M

g+

2B

in

[ G

Pa

]

1/T (10-4/K)

new solid - liq. line of Mg

up to now known line

1 bar Ar pressure; down limit of melt experiment

New solid Mg region

Experimentally modified Mg-B phase diagram after high gas pressure investigations

4 6 8 10 12 14 16 18 20

1E-13

1E-12

1E-11

1E-10

1E-9

1E-8

1E-7

1E-6

1E-5

1E-4

1E-3

0,01

0,1

1649,8800

Gas + B(s)

Gas+MgB7

Gas + MgB4

Gas + MgB2

Solid Mg + MgB2

Liq Mg + MgB2

Temperature [o C]

2000 1500 1000 500

Ar

ga

s p

res

su

re o

ve

r M

g+

2B

in

[ G

Pa

]

1/T (10-4/K)

new solid - liq. line of Mg

up to now known line

1 bar Ar pressure; down limit of melt experiment

New solid Mg region

Page 12: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

(a)Traditional PIT concept; (b) PIT with metal Nb barrier; (c) The new concept of PIT

typical for e.g. HyperTech The in/ex situ/ Cu-stabilizer; patent

PIT concept technology

Title: Composite Electrical Conductors and Method for Their Manufacture Inventors: Dr Bartek Glowacki and Dr Andrzej Morawski Filing Date: 10 April 2007 Filing No: GB 0706919.8 Country: Great Britain Title: Composite Electrical Conductors and Method for Their Manufacture Inventors: Dr Bartek Glowacki and Dr Andrzej Morawski Filing Date: 10 April 2007 Filing No: 60/907590 Country: USA

FF~0.15 FF~0.50

Page 13: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Sheathed composite superconducting MgB2 wires

Sheathed MgB2 superconducting wires — Cu- and Fe-

Easy to produce long tape or wire

Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic stability. High thermal

conductivity of Cu. Minimum quantity of stabilizer is required. Chemical stability. Mechanical stability, good mechanical properties. Low material

cost. Length of composite wires over few km

«Know how» - ex situ barrier in Fe or Cu /MgB

2 superconducting

wires

Ex situ as a barrier between inner in situ and outer Fe/Cu layers

Problems of Cu-sheathed wires developemnt Reaction between inner in situ and outer Fe or Cu

sheath or expensive Nb barrier uses.

Cu or Fe sheath

In situ core

In situ core Cu or Fe sheath

Ex situ barrier

Page 14: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

CIP-ed powder

2. Billet for drawing:

3. After drawing:

1. Powder compacting by CIP-in argon gas pressure medium from 0.8...1.0 GPa in rubber mould

Length 120-620 mm OD diameter – up to 38 mm ID diameter – up to 24 mm

Length up to 500 m Diameters 0.5...1.4 mm

Preparation of the Cu-sheathed ex/in wires

Page 15: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

SEM crossection micrograph of the composite ( ex/in) superconducting MgB2

wire in the Cu sheath – before HIP

The superconducting wire with Ø ca 1, mm diameter was made with the SCIP (Sequential Cold Isostatic

Pressing) method, the own technological

achievement of the group.

High Pressures Methods for cleaning and mixing of the

nano and micro metric powders, ultrasonic high

pressure US-HP and ultrasonic activated vacuum sublimation US-VS, have

been worked-out and checked in practice in the specially made devices

The Cu/ex/in-situ technology and other high pressure powder processing designed and manufactured in IHPP-UNIPRESS since 2005

Page 16: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The high pressure infiltration process, presented by Unipress in HIPERMAG project meeting at 2005 & at MT-20 conference in Philadelphia 2006,

followed by HIP-ing of the ex/in situ wires or tapes at high argon pressure

The highly stressed ( over 1.3 GPa) nano-grains of dense MgB2 net is produced by solid state reaction of in situ core ,below Tm temp. of (Mg +2B) mixture The self densification & infiltration is provided by migration / diffusion process which take place ( belowe, but close to Tm;e.g. 570 -680 0C

of (Mg +2B), under high pressure) The effective diffusion barrier for Mg and Cu by ex situ hard micro grains & dense material is produced

(the apropiate quantity of nano blocker to the grains boundary is supplied) Simultanously the effective self-reinforcement by ex situ hard composite ceramic sheath is applied at elevated temp. at the second step of

short HIP process ( at temperature over 780oC) Final HIP results in:

high densification of highly sterssed , well connected nano part of grains and aglomerates (of primary in situ- actually ex situ) core and the final high densifications and sintering of both unificated ex situ cores.

Page 17: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The cross section of the Cu / ex / in situ wire with nano additives

Cu/EX+nano SiC+nano Nb/In+nanoSiC

Before HP annealing

After HP annealing

HP

Page 18: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

What is the difference after HIP annealing?

The traditional PIT in Cu The Cu/ex/in concept of PIT

(a) The SEM micrograph of the coaxial in situ / ex situ wire after final HIP process: the in situ - ex situ interface can not be

resolved, and there is any of a Cu-Mg layer at the copper-MgB2 border

(b) The SEM micrograph of a conventional copper-matrix in situ MgB2 wire for comparison: a large thick layer

of MgCu2 and Mg2Cu exists at the copper MgB2 border

Page 19: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The critical current density vs. magnetic fields at 4.2 K - comparison

0 2 4 6 8 10 12 14

1

10

100

1000

Schlachter (0.9Mg+2B+10 wt% SiC)

/Nb/Cu/SS =164 µm

Improved precursors

Nano-Mg:

Yamada et al., MgB2/Fe

Mechanical alloying:

Fischer et al., MgB2/Fe

In-Situ wires with commercial Mg and B powders

Goldacker et al.: MgB2/Fe/SS =310 m

Sumption et al.: 19-fil. Mg1.1

B2/Nb/Cu/Monel

Improved Precursors and SiC-doping:

Mg + n SiC-doping:

Morawski et al:: HIP/MA/MgB2/in-ex/

Cu+10% nSiC

Dou et al.: MgB2/Fe + 10% SiC

Sumption et al.: MgB2/Fe + 10% SiC

Jc [

kA

/cm

2]

B [T]

Schlachter (0.9Mg+2B)/Nb/Cu/SS

=164 µm

Cu-comp. /ex/in situ +10%nSiC-MA/HIP1GPa /680-780/30 min.

MA-W. Haesler, Dresden. rolled tapes

Page 20: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Strand #

#

Mon

o Barrier

Mono

sheath

Multi

sheath

B

source Mg:B Additive dia (mm) % powder

961-03 6 Nb Cu Monel SMI 1:2 C 0.83 17.7

961-18 6 Nb Cu Cu 99B 1.10:2 SiC 0.83 14.9

961-22 18 Fe Cu Glidcop Ts 1:2 C4H6O3 0.83 13.9

1019-30 6 Nb Cu Monel 99B 1.10:2 SiC 0.83/0.63 15

1019-43 18 Nb Cu Monel 99B 1.10:2 0.83/0.63 15

961-70 1 Fe Cu Ts 1:2 C4H6O3 0.83 28.7

961-76 6 Nb Cu Glidcop 99B 1.10:2 SiC 0.83 16.6

961-92 6 Nb Cu Cu 99B 1.10:2 0.83 19.4

The Hypertech Inc. Columbus , Ohio, USA wires samples used for HIP investigation

Stand 1019-30 Stand 1019-43

OD of 0.63 and OD of 0.83 mm multicore wires were investigated

Page 21: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The standard ambient argon pressure annealing was performed at 700 oC/15 min.

and the highest HIP applied pressure was the 1.4 GPa at 700 oC / 30 min.

The pressure influences on the microstructure and density of the cross section and longitudinal views is shown.

The microstructural SEM comparison of the pressure effect on the standard ambiante pressure annealing and high pressure HIP of pure MgB2 samples

Results for thicker 1019-43 wires: of 0.83 mm in diameter

Page 22: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The 1 GPa constant pressure HIP- annealing time dependence on the Jc, Fp and microstructure of the core

Results for thicker 1019-43 wires: of 0.83 mm diameter

Page 23: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The high pressure HIP effect on Jc and Fp rises at high magnetic fields, especially in comparison to the standard ambient pressure annealing parameters at 700oC.

Results for thicker 1019-43 wires: of 0.83 mm in diameter

Page 24: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Temp

The critical transport parameters and n value of wires HIP-ed at equal 1GPa pressure and equal time of annealing but at various temperatures.

The Jc and Fp did not changed substantially but the n-value parameter increase efficiently, for the wires of 0. 83 mm diameter with rising temperature.

Results for thicker 1019-43 wires: of 0.83 mm in diameter

Page 25: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The Jc and Fp comparison of two different dimension of the wires obtained at exactly the same HIP experiment ( e.g. pressure. temperature, and time of annealing). See the evolution of the Jc & Fp properties of thin 0.63 mm and thick 0.83 mm wires, with increasing temperature of each HIP experiment.

Page 26: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The Kramer’s plots, reduced Fp and n- value dependence on the wires diameters and specific high pressure and temperature conditions.

Page 27: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

HU-1019-43 after 1 GPa / 710 oC ramp to 780 oC / 22 min. HIP in Ar Pure MgB2- any additives, amorphous boron, Nb barrier in Cu and Monel

0 20 40 60 80 100 120 140-10

0

10

20

30

40

50

60

U

[V 1

0-6

]

I [A]

8 T

10 T

12 T

6 T

7,5 T

0 2 4 6 8 10 12 14-10

-5

0

5

10

15

20

25

30

35

40

45

50

U [

V 1

0-6

]

B [T]

15 A

30 A

4,5 A

10,5 A

45 A

60 A

75 A

The transition from superconducting to the normal state measured by resistive method at Bitter type magnet in current rise and magnetic field rise mode

HyperTech Inc.- Unipress HIP-ed wires

Constant magnetic field ( clasic)

Constant current measurements

Page 28: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

HU-1019-43 after 1 bar (upper line) & 1 GPa (lower line) / 710 oC ramp to 780 oC /in t=22 min Pure MgB2- any additives, amorphous boron, Nb barrier in Cu and Monel

1 bar Ar

1 GPa Ar

HyperTech Inc.- Unipress HIP-ed wires

Page 29: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

HU # 1019- 43 after 1 GPa / 710 oC ramp to 780 oC / 22 min. HIP in Ar Pure MgB2- any additives, amorphous boron, Nb barrier in Cu and Monel

Pining force vs. magnetic I_ field Critical current density at 4,2 K , I_ field

0 1 2 3 4 5 6 7 8 9 10 11 12 13 1410

2

103

104

105

106

107

Jc

[A

/cm

2]

B [T]

1GPa

1 bar

10 000 A/cm2

Our current sorce limit

HyperTech Inc.- Unipress HIP-ed wires

0 2 4 6 8 10 12 140

5

10

15

Fp [G

N/m

3]

B=[T]

1GPa)

(1 bar = 100 kPa)

Page 30: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

HU-1019-30 after 1 bar (upper line) & 1 GPa (down line) / 710 oC ramp to 780 oC/30 min Nano SiC additives, amorphous boron, Nb barrier in Cu and Monel

Perpendicular and longitudinal cross section

1 bar Ar =>

1 GPa Ar =>

HyperTech - Unipress HIP-ed wires

Page 31: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

HU-1019-30 after 1 bar (upper line) & 1 GPa (down line) / 710 oC ramp to 770 oC /30 min

Nano SiC additives, amorphous boron, Nb barrier in Cu and Monel

Longitudinal cross section Broken wire, powder morfology

1 bar Ar =>

1 GPa Ar =>

Page 32: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The coils of 24 mm diam. of # 30 & # 43 wires after HIP and further neutron flux investigations in Wiena.

The inox-steel spools with Cu connectors of 12, 14 and 24 mm diameters for winding the HyperTech „green body” wires, destined later for HIP process and ITER regarding the neutrons flux examinations of Jc.

The MgB2 coils for neutron flux experiment destinated for HIP

Page 33: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

0 2 4 6 8 10 12 14

100

1000

cB cI

30 fi=0.63 ||

30 fi=0.83

Jc (

A/m

m2)

B (T)

10000 A/cm2

P= 1GPa; T=7000C; 15 min - const. annealing temperature

10.8 T

0 2 4 6 8 10 12-0,5

0,0

0,5

1,0

1,5

2,0

2,5

3,0

3,5

4,0

4,5

P= 1GPa; T=7000C; 15 min- const. annealing temperature

cB cI

30 fi=0.63 ||

30 fi=0.83

Fp

(G

N/m

3)

B (T)

Hypertech - Unipress HIP-ed wires and 14 mm diam. coils Nano SiC additives, amorphous boron, Nb barrier in Cu and Monel; HU # 1019- 30 after HIP at various p,T, t , const. Temp. conditions

3 4 5 6 7 8 9 10 11 12 13

100

1000

P= 1GPa; T=7100C; 15 min- const. annealing temperature

30 fi=0.63 coil 14 pom.07.10 (cB cI)

30 fi=0.63 coil 14 pom.27.10 (cB cI)

Jc (

A/m

m2)

B (T)

10 000 A/cm2

10.1 T0 2 4 6 8 10 12

-0,5

0,0

0,5

1,0

1,5

2,0

2,5

3,0

3,5

4,0

4,5

P= 1GPa; T=7100C; 15 min.- const. annealing temperature

30 fi=0.63 coil 14 pom.07.10 (cB cI)

30 fi=0.63 coil 14 pom.27.10 (cB cI)

Fp

(G

N/m

3)

B (T)

Coils for neutrons flux examination

Wires from similar HIP process

Page 34: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Hypertech - Unipress HIP-ed wires; Nano SiC additives, amorphous boron, Nb barrier in Cu and Monel; HU # 1019- 30 after HIP at various p,T, t , ramp conditions

0 2 4 6 8 10 12 14 16-1

0

1

2

3

4

5

6

7

P= 1.0GPa; T=660-7050C; 15 min- ramping annealing temperature

cB cI

30 fi=0.63 wire

30 fi=0.83 wire

Fp

(G

N/m

3)

B (T)

2 4 6 8 10 12 1410

100

1000

10000

P= 1.0GPa; T=700-7450C; 15 min.- ramping annealing temperature

cB cI

30 fi=0.63 _|_ wire

30 fi=0.83 wire

Jc (

A/m

m2)

B (T)12.7T

10 000 A/cm2

0 2 4 6 8 10 12 14 16

0

2

4

6

8

P= 1.0GPa; T=700-7450C; 15 min.- ramping annealing temperature

cB cI

30 fi=0.63 _|_ wire

30 fi=0.83 wire

Fp

(G

N/m

3)

B (T)

2 4 6 8 10 12 14 16

100

1000

P= 1.0GPa; T=660-7050C; 15 min. - ramping annealing temperature

cB cI

30 fi=0.63 wire

30 fi=0.83 wire

Jc (

A/m

m2)

B (T) 12T

11.2T

10 000A/cm2

Ramping type of annealing can protect a little leaking of the Nb barrier!

Page 35: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Hypertech - Unipress HIP-ed wires; Nano SiC additives, amorphous boron, Nb barrier in Cu and Monel; HU # 1019- 30 after HIP at various p,T, t , ramp conditions

0 2 4 6 8 10 12 14 1610

100

1000

Jc

[A

/mm

2]

B [T]

1 GPa //

1 bar = amb. press. //

1 GPa I_

1 bar = amb. press. I_

10 000 A/cm2

B I_ over 14.4 T

B // over 15.2 T

0 2 4 6 8 10 12 14 160

1

2

3

4

5

6

7

8

9

Fp [G

N/m

3]

B [T]

1 GPa //

1 bar= amb. press. //

1GPa I_

1 bar= amb. press. I_

6.6 T 9.2 T

Pining force vs. magnetic field Critical current density at 4,2 K

Hypertech - Unipress HIP-ed wires - The best results for ramping type annealing ! Nano SiC additives, amorphous boron, Nb barrier in Cu and Monel; HU # 1019- 30 after clasic 1 bar 700oC & 1 GPa / 710-ramp to 770oC/ in t= 34 min. HIP

2 4 6 8 10 12 14

100

1000

P= 1.0GPa; T=735-7800C; 15 min. -ramping annealing temperature

30 fi=0.83 wire _|_Jc (

A/m

m2)

B (T)11.8T

10 000A/cm2

0 2 4 6 8 10 12 14

0

1

2

3

4

5

6P= 1.0GPa; T=735-780

0C; 15 min. -ramping annealing temperature

30 fi=0.83 wire _|_

Fp

(G

N/m

3)

B (T)

Page 36: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The scheme of the liquid medium HIP apparatus for examination of short wires samples at pressure up to 1.0 GPa and temperature up to 700 oC

The pistons of the 250 ton press

Heater with the kanthal furnace

The washers pressboard

Piston of alumina oxide :ZrO2

The eutectic of NaCl-KCl liquid or silicon oil

High resistant of the stress at eleveted temperatures and salts, alumina oxide :ZrO2 - high pressure cell.

The wires or tapes samples

Page 37: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

2 4 6 8 10 12

500

1000

1500

2000

2500

3000

3500

4000

OD 0.63 mm

OD 0.83 mm

Fp[M

N/m

3]

B[T]

2 4 6 8 10 1210

100

1000

Jc[A

/mm

2]

B[T]

OD 0.63 mm

OD 0.83 mm

10 000 A/cm2

0,0 0,2 0,4 0,6 0,8 1,00,0

0,2

0,4

0,6

0,8

1,0

Volume pinning

Fp=h

0(1-h)

2

Surface pinning

Fp=h

0.5(1-h)

2

Point pinning

Fp=h

1(1-h)

2

OD 0.63 mm

Fp/F

pm

ax

B/Birr

2 4 6 8 10 1210

100

1000

Jc[A

/mm

2]

B[T]

OD 0.83 mm

OD 0.63 mm

10 000 A/cm2

2 4 6 8 10 120

2000

4000

6000

8000

10000

Fp[M

N/m

3]

B[T]

OD 0.83mm

OD 0.63 mm

0,0 0,2 0,4 0,6 0,8 1,00,0

0,2

0,4

0,6

0,8

1,0

Volume pinning

Fp=h

0(1-h)

2

Surface pinning

Fp=h

0.5(1-h)

2

Point pinning

Fp=h

1(1-h)

2

OD 0.83mm

OD 0.63mm

Fp/F

pm

ax

B/Birr

0 2 4 6 8 10 12 140,1

1

10

100

Ic[A

]

B[T]

#43 tape 0.15x4 mm

I_ to c axis

I_ to a - b axis

// to c axis

4 6 8 10 12 1410

100

1000

#43 tape 0.15x4 mm

I_ to c axis

I_ to a - b axis

// to c axis

Jc[A

/mm

2]

B[T]

10 000 A/cm2

4 6 8 10 12 140

2500

5000

7500

10000

12500

15000

#43 tape 0.15x4 mm

I_ to c axis

I_ to a - b axis

// to c axis

Fp[M

N/m

3]

B[T]

HT-UN #43

t=5 min (up 60, down 90)

T= 700 0C

P= 0.3 GPa

OD 0.83 mm

HT-UN #43

t=5 min (up 60, down 90)

T= 700 0C

P= 0.3 GPa

OD 0.63 mm

1019 # 43 wires

HIP in liquid; 1019 # 43 tape 0.15 X 4 mm

HT- UN #30

T= 700

0C

P= 0.3 GPa

t=5min. (up 60, down 90)

OD 0.63 mm

HT- UN #30

T= 700

0C

P= 0.3 GPa

t=5min. (up 60, down 90)

OD 0.83 mm

1019 # 30 wires

Hot Isostatic Presssed samples of wires and tapes in liquid the medium

Page 38: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The pictorial design of the first prototype of liquid salt / graphite , HIP machine designated for MgB2 MRI, Ind. Heaters, ITER, etc., coils up to 1000 mm of diameters or/and for „wind and react” long wires productions by the HIP method in liquid medium at pressure up to 1.4GPa and temperatures up to 780 0C, as well as for rewinding wires from „react and wind”. Actually accepted for the new technology program at the New Technology Investment Park in Celstynów, Poland

Up to 3000 tons

Liquid salt pompe

Ceramic or WC piston

Hot plates ~ 550-780 0C

Liquid salt

High pressure sills

Coil with MgB2 winded wires

Superconducting „geen body” wires for HIP

Up to 3000 tons

Page 39: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Temporary used for testing the press machine up to 1000 tons at Unipress with new 350 mm toroidal chamber and high pressure generator designated for HIP experiments with operating annealing temperature up to 750 0C.

Page 40: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

The homo barrier, made of ex situ MgB2 is effective against the Cu and Mg inter reaction process as well as for B reaction with metals Cu, Fe, Ni alloys. It selves can conduct very high current see PhD of A. Kario - Dresden,2011 (increase FF at last 3 times) Posses very low normal state resistivity. The long wire is easy for preparation by CP or CIP, extrusion or drawing.

All HyperTech HIP-ed wires had significant increase of Jc nad Fp . The tightness /quality of Nb barrier is the most important factor of Jc increasing receiving by the HIP process

Any kind of cold deformation (CP) is „not sufficient” for high state densification of the conductor contrary to the HIP process which permit to compensate the 25 % shrinking of in situ material, continuously during all HIP process and the stress on the core is independent of the any sheaths softening at elevated temperature of sintering.

The melting temperature of the Mg or Mg + B substrates can be easily adjusted by the pressure – its permits to make the solid state reaction in relatively short time with absence of the liquid growth- it results in very dens nano grains of the final composite. It reflect directly by the high Jc increases at elevated magnetic fields especially.

The tightness of the ex situ barrier is a function of:

the nano granulates of ex situ MgB2 and nano additives added, purity of all components

thickness of the barrier,

final annealing temperature regime and outside stress pressure, applied during the wire/tape sintering preparation- e.g. HIP.

The Jc of all investigated kind of HIP-ed wires increases and gets the 104 A/cm2 at 4.2 K already at around 14 T and even for undoped core materials reach 13 T. The Nb free barrier can carry the same current at such high fields, but the costs of wire productions is much smaller.

Summary& Conclusions

Page 41: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic

Thank you for your

attention

Page 42: New - hot high pressure technologies for high performance ... · Hot Isostatic Pressing ... Advantages of Cu. Why Cu copmposite sheath? Presence of Cu as stabiliser for cryogenic