Pengaruh Temperatur Pemanasan pada Superkonduktor Magnesium Diboride (MgB2)

LAMPIRAN 1
GAMBAR BAHAN DAN ALAT PENELITIAN

1.

Bahan Penelitian

Serbuk MgB2 Komersil

Sampel dalam Tube

Sampel siap untuk diuji

Preparasi sampel uji Cryogenic

Preparasi sampel uji SEM

Preparasi sampel uji XRD

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60

2.

Alat Penelitian

Neraca Digital Kern EW 220-

Spatula

3NM

SS304 Tube

Jangka Sorong

Alat pemotong SS304 Tube

Mesin Grenda Konvensional


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Mesin Press Hidrolik

Muffle Furnace

Alat uji DTA/TGA

Auto Fine Coater

Alat uji SEM-EDS

Alat uji XRD

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Cryogenic Magnet

Circulatiom Pump

Compressor gas Helium

Temperature and Magnet Controller

Kertas Timbang

Alkohol

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Masker

Tissue


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LAMPIRAN 2
HASIL DIFFERENTIAL THERMAL ANALYSIS

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Coefficient
Temperatur 0C)

Rel. mass change (%)


Heat flow (Mw)

40

1.4770

-1.6895

50

1.8393

-0.5566

60

2.1077

0.5667


70

2.2806

1.4860

80

2.3614

2.5153

90

2.2805

3.6522

100


1.6317

5.0779

110

1.9218

6.3887

120

1.9044

7.4662

130

1.7752


8.8301

140

1.8608

10.0585

150

1.7095

11.0338

160

1.7809

12.2108


170

1.8939

13.1219

180

2.0385

13.8059

190

1.9805

14.3299

200


2.1959

14.7144

210

2.0548

14.8797

220

2.2430

15.4169

230

2.3178


16.1119

240

2.2784

16.5881

250

2.4240

16.9586

260

2.5986

17.6185

270

2.5807

17.9631

280

2.6452

18.8508

290

2.6787

19.5533

300

2.9619

21.0117

310

2.7525

21.8036

320

3.0309

23.1975

330

3.0588

24.6968

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340

3.0209

26.0184

350

3.0786

27.2933

360

3.0283

28.8938

370

3.0831

30.2873

380

3.0071

31.8247

390

3.1327

33.3545

400

3.2092

34.8348

410

3.1398

36.2978

420

3.3989

37.5204

430

3.2024

38.5090

440

3.4897

39.7111

450

3.3208

40.4935

460

3.4941

41.0530

470

3.5312

41.8646

480

3.8039

42.6736

490

3.7600

43.1559

500

3.7313

43.2322

510

3.8353

42.9747

520

3.7573

42.8942

530

3.9604

43.0470

540

4.1583

42.7631

550

3.9751

42.1667

560

4.3172

42.0288

570

4.4968

41.4787

580

4.3763

41.2319

590

4.6096

40.2213

600

4.6227

39.4112

610

4.8626

38.8176

620

4.9512

37.7002

630

5.0216

36.7547

640

5.1939

35.3661

650

5.3296

34.5894

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660

5.6535

33.4306

670

5.8574

32.8004

680

6.0579

32.3899

690

6.4175

31.7342

700

6.6705

30.6334

710

6.8740

29.3946

720

7.3315

28.6399

730

7.8647

27.9309

740

8.1848

27.1170

750

9.0063

26.8579

760

9.6467

26.8443

770

10.3384

27.3428

780

11.2869

27.7066

790

12.1212

27.8825

800

12.9602

28.0397

810

14.2119

27.8019

820

15.2567

27.2207

830

16.4746

25.8721

840

17.7224

24.2014

850

18.8497

22.0245

860

19.8812

19.1937

870

21.0250

17.1923

880

22.2482

16.9149

890

23.3280

18.2395

900

24.4826

22.4316

910

25.7979

27.3652

920

27.0660

30.8920

930

28.4397

34.2750

940

29.8792

37.8309

950

31.0229

43.0673

960

32.5844

48.7970

970

33.9044

54.8659

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980

35.3592

60.8807

990

36.7630

67.6390

1000

38.3097

74.0435

1010

39.7312

77.5121

1020

41.3296

78.0544

1030

42.8376

77.2370

1040

44.3071

76.4849

1050

45.9954

76.0177

1060

47.3504

74.9828

1070

48.9722

73.9994

1080

50.4446

73.4988

1090

52.1065

72.5987

1100

53.7226

72.1208

1110

55.0668

70.7375

1120

56.8689

69.7677

1130

58.5210

68.7437

1140

60.0677

67.0920

1150

61.7661

66.1807

1160

63.4522

65.1780

1170

65.0653

64.2197

1180

66.5990

62.9771

1190

68.2836

61.7278

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LAMPIRAN 3
HASIL XRD MATCH DAN PERHITUNGAN KRISTALIN

1. Hasil XRD Sampel MgB2 Komersil Tanpa Pemanasan

Puncak-puncak difraksi sinar-X
Pos.
[°2Th.]

Height
[cts]

FWHM Left
[°2Th.]

d-spacing
[Å]

Rel. Int.
[%]

Phase
Name

25.4866

798.27

0.1535

3.49499

3.38

33.7178

7523.79

0.1791

2.65826

31.85

MgB2

35.7504

641.83

0.1279

2.51165

2.72

MgB4

38.9227

255.11

0.1791

2.31394

1.08

39.9934

81.72

0.3070

2.25443

0.35

41.0004

120.27

0.5117

2.20135

0.51

42.6215

23619.91

0.2558

2.12130

100.00

MgB2

43.1098

1578.45

0.1791

2.09840

6.68

MgO

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46.2954

185.32

0.2047

1.96116

0.78

48.0868

57.65

0.3070

1.89220

0.24

48.9839

95.99

0.2558

1.85963

0.41

52.0839

2647.43

0.1791

1.75600

11.21

56.3140

70.57

0.3070

1.63372

0.30

60.0676

4513.92

0.1560

1.53902

19.11

60.2574

2462.71

0.1248

1.53844

10.43

62.4500

475.09

0.2184

1.48592

2.01

63.3925

1406.49

0.2496

1.46607

5.95

66.2126

588.28

0.1872

1.41030

2.49

70.5719

510.12

0.2496

1.33349

2.16

76.2797

1919.57

0.2184

1.24728

8.13

76.5509

1021.53

0.1248

1.24662

4.32

78.7371

113.75

0.1872

1.21440

0.48

MgB2

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2. Hasil XRD Sampel MgB2 Komersil Pemanasan 4000C

Puncak-puncak difraksi sinar-X
Pos.
[°2Th.]

Height
[cts]

FWHM Left
[°2Th.]

d-spacing [Å]

Rel. Int.
[%]

25.2310

32.43

0.1574

3.52982

3.66

33.4895

290.41

0.0886

2.67585

32.75

MgB2

35.5281

34.81

0.1574

2.52685

3.93

MgB4

38.7698

14.14

0.2362

2.32271

1.59

42.4181

886.80

0.0689

2.13101

100.00

MgB2

42.8937

81.55

0.1968

2.10847

9.20

MgO

51.8420

93.60

0.2755

1.76363

10.55

Phase
Name

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59.8789

150.29

0.1378

1.54470

16.95

62.2850

30.02

0.2362

1.49069

3.39

63.2185

44.94

0.3542

1.47091

5.07

66.0305

16.85

0.3149

1.41492

1.90

70.4418

13.26

0.3149

1.33674

1.49

76.0790

55.32

0.1574

1.25111

6.24

83.1950

50.87

0.4723

1.16124

5.74

MgB2

3. Hasil XRD Sampel MgB2 Komersil Pemanasan 7500C

Puncak-puncak difraksi sinar-X
Pos.
[°2Th.]

Height
[cts]

FWHM Left
[°2Th.]

d-spacing [Å]

Rel. Int.
[%]

25.2959

50.79

0.1771

3.52090

3.06

33.5129

526.96

0.1574

2.67404

31.74

MgB2

35.5313

53.26

0.1968

2.52663

3.21

MgB4

Phase
Name

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36.8866

8.55

0.4723

2.43685

0.51

38.1040

11.65

0.2362

2.36175

0.70

38.7359

20.29

0.1968

2.32467

1.22

42.4337

1660.40

0.1968

2.13025

100.00

MgB2

42.9346

140.83

0.1574

2.10656

8.48

MgO

46.0396

7.39

0.4723

1.97146

0.45

51.8668

187.67

0.1574

1.76284

11.30

59.8781

271.15

0.1181

1.54472

16.33

62.2559

56.73

0.1181

1.49132

3.42

63.1817

95.61

0.2755

1.47167

5.76

66.0485

42.13

0.1968

1.41458

2.54

70.4348

31.84

0.3936

1.33685

1.92

76.1027

111.98

0.1968

1.25078

6.74

78.7017

8.82

0.3936

1.21586

0.53

83.1608

118.26

0.1574

1.16163

7.12

MgB2

4. Hasil XRD Sampel MgB2 Komersil Pemanasan 8800C

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Puncak-puncak difraksi sinar-X
Pos.
[°2Th.]

Height [cts]

FWHM Left
[°2Th.]

d-spacing
[Å]

Rel. Int.
[%]

25.2412

52.37

0.1968

3.52841

3.38

28.8328

6.44

0.4723

3.09655

0.42

33.4823

487.53

0.1181

2.67641

31.51

MgB2

35.4849

116.46

0.1378

2.52983

7.53

MgB4

36.8883

18.92

0.3149

2.43674

1.22

38.1059

18.74

0.2362

2.36164

1.21

38.8120

53.22

0.1574

2.32028

3.44

39.7307

18.23

0.2362

2.26872

1.18

41.0092

34.61

0.5510

2.20090

2.24

42.4264

1547.38

0.0689

2.13061

100.00

MgB2

42.9100

174.67

0.1968

2.10771

11.29

MgO

44.9535

13.86

0.3936

2.01653

0.90

46.0424

27.23

0.2362

1.97134

1.76

48.6929

12.80

0.3149

1.87006

0.83

49.5019

12.40

0.2362

1.84137

0.80

51.8238

151.79

0.1378

1.76420

9.81

56.2305

10.44

0.3149

1.63595

0.67

59.8658

265.17

0.1181

1.54501

17.14

62.2628

61.26

0.2755

1.49117

3.96

63.1625

84.14

0.3149

1.47208

5.44

66.0189

34.36

0.1968

1.41514

2.22

70.4334

28.77

0.3149

1.33688

1.86

76.1328

113.31

0.1574

1.25036

7.32

Phase
Name

MgB2

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78.5692

11.62

0.4723

1.21758

0.75

83.1343

106.58

0.2755

1.16193

6.89

5. Gabungan Hasil Karakterisasi X-Ray Diffraction MgB2 Komersil Dengan
Pemanasan
MgB2 400C
Mgb2 750C
Mgb2 880C

Intensitas (arbitrary unit (a.u))

Keterangan :
MgB2
MgB4
MgO

10

20

30

40

50

60

70

80

90

Sudut 2-theta

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LAMPIRAN 4
HASIL SEM – EDS SAMPEL MgB2 KOMERSIL
1. Hasil SEM-EDS Sampel MgB2 Komersil Tanpa Pemanasan (Perbesaran
500x dan 1000x)

8000

001

Acquisition Parameter

7200

Instrument

MgKa

6400

Acc. Voltage : 15.0 kV

5600

Probe Current: 1.00000 nA

4000

PHA mode

: T3

3200

Real Time

: 37.96 sec

Live Time

: 30.00 sec

Dead Time

: 20 %

2400
1600

OKa

4800

BKa

Counts

: 6390(LA)

800

Counting Rate: 4344 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00

Energy Range :

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.3750
Element

(keV)

Mass%

Error%

Atom%

B K*

0.183

34.26

0.58

51.40

3.1942

O K

0.525

13.71

0.59

13.90

18.5034

Mg K

1.253

52.02

0.33

34.70

78.3023

Total

100.00

Compound

Mass%

Cation

K

100.00

JED-2300 AnalysisStation

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2. Hasil SEM-EDS Sampel MgB2 Komersil Pemanasan 4000C dengan 3 spot
Title

: IMG2

--------------------------Instrument

:

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

001

3600

Acquisition Parameter

3200

Instrument

MgKa

2800

: 6390(LA)

Acc. Voltage : 20.0 kV
Probe Current: 1.00000 nA

2000

PHA mode

: T3

Real Time

: 34.48 sec

800

Live Time

: 30.00 sec

400

Dead Time

: 13 %

1600
OKa

Counts

2400

1200

Counting Rate: 2255 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00

keV

Energy Range :

0 - 20 keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.4538
Element

(keV)

Mass%

Error%

Atom%

O K

0.525

29.39

0.85

38.74

35.6944

Mg K

1.253

70.61

0.54

61.26

64.3056

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

79

Title

: IMG2

---------------------------

2700

Instrument

:

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

002

Acquisition Parameter
2400

Instrument

MgKa

2100

Acc. Voltage : 20.0 kV
Probe Current: 1.00000 nA

1500

900

OKa

Counts

1800

1200

: 6390(LA)

600
300

PHA mode

: T3

Real Time

: 34.12 sec

Live Time

: 30.00 sec

Dead Time

: 12 %

Counting Rate: 2122 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00

Energy Range :

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.4594
Element

(keV)

Mass%

Error%

Atom%

O K

0.525

36.03

0.67

46.12

45.7623

Mg K

1.253

63.97

0.48

53.88

54.2377

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

80

Title

: IMG2

---------------------------

4500

:

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

003

Acquisition Parameter

4000

Instrument

MgKa

3500

: 6390(LA)

Acc. Voltage : 20.0 kV

3000

Probe Current: 1.00000 nA

2500

PHA mode

: T3

Real Time

: 35.17 sec

Live Time

: 30.00 sec

Dead Time

: 14 %

2000
OKa

Counts

Instrument

1500
1000
500

Counting Rate: 2578 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00 Energy Range :

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.3961
Element

(keV)

Mass%

Error%

Atom%

O K

0.525

31.04

0.73

40.61

38.1807

Mg K

1.253

68.96

0.47

59.39

61.8193

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

81

3. Hasil SEM-EDS Sampel MgB2 Komersil Pemanasan 7500C dengan 3 spot
Title

: IMG2

--------------------------:

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

001

10500

Acquisition Parameter
Instrument

MgKa

9000
7500

: 6390(LA)

Acc. Voltage : 20.0 kV
Probe Current: 1.00000 nA

6000

PHA mode

: T3

Real Time

: 40.65 sec

Live Time

: 30.00 sec

Dead Time

: 26 %

4500
OKa

Counts

Instrument

BKa

3000
1500

Counting Rate: 5562 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00 Energy Range :

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.3925
Element

(keV)

Mass%

Error%

Atom%

B K

0.183

66.88

0.71

80.71

14.3114

O K

0.525

5.44

0.74

4.43

8.6595

Mg K

1.253

27.69

0.20

14.86

77.0291

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

82

Title

: IMG2

---------------------------

9000

Instrument

:

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

002

Acquisition Parameter

8000

Instrument

MgKa

7000

: 6390(LA)

Acc. Voltage : 20.0 kV

Counts

6000

Probe Current: 1.00000 nA

5000
4000

2000

OKa

3000

1000

PHA mode

: T3

Real Time

: 38.57 sec

Live Time

: 30.00 sec

Dead Time

: 22 %

Counting Rate: 4629 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00

Energy Range :

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.3973
Element

(keV)

Mass%

Error%

Atom%

O K

0.525

6.02

1.65

8.87

5.4109

Mg K

1.253

93.98

0.70

91.13

94.5891

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

83

Title

: IMG2

---------------------------

9000

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

MgKa

Instrument

: 6390(LA)

Acc. Voltage : 20.0 kV

6000

Probe Current: 1.00000 nA

5000

OKa

4000

BKa

Counts

Volt

Acquisition Parameter

7000

2000

:

003

8000

3000

Instrument

1000

PHA mode

: T3

Real Time

: 39.03 sec

Live Time

: 30.00 sec

Dead Time

: 23 %

Counting Rate: 4824 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00

Energy Range :

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.4078
Element

(keV)

Mass%

Error%

Atom%

B K

0.183

73.25

0.55

85.00

20.2192

O K

0.525

4.46

0.65

3.50

8.0219

Mg K

1.253

22.29

0.17

11.50

71.7589

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

84

4. Hasil SEM-EDS Sampel MgB2 Komersil Pemanasan 8800C dengan 3 spot
Title

: IMG2

---------------------------

13500

:

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

002

Acquisition Parameter

12000

Instrument

MgKa

10500

: 6390(LA)

Acc. Voltage : 20.0 kV

9000
7500

Probe Current: 1.00000 nA

6000

PHA mode

: T3

4500

Real Time

: 41.79 sec

Live Time

: 30.00 sec

Dead Time

: 27 %

3000

OKa

Counts

Instrument

1500
0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00

keV

Counting Rate: 6274 cps
Energy Range :

0 - 20 keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.3919
Element

(keV)

Mass%

Error%

Atom%

O K

0.525

4.96

1.69

7.35

4.3808

Mg K

1.253

95.04

0.70

92.65

95.6192

Total

JED-2300

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

85

Title

: IMG2

---------------------------

002

13500

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

MgKa

Instrument

: 6390(LA)

Acc. Voltage : 20.0 kV

9000
Counts

:

Acquisition Parameter

12000
10500

Instrument

Probe Current: 1.00000 nA

7500
6000
4500
OKa

3000
1500

PHA mode

: T3

Real Time

: 41.79 sec

Live Time

: 30.00 sec

Dead Time

: 27 %

Counting Rate: 6274 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

Energy Range :

21.00

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.3919
Element

(keV)

Mass%

Error%

Atom%

O K

0.525

4.96

1.69

7.35

4.3808

Mg K

1.253

95.04

0.70

92.65

95.6192

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

86

Title

: IMG2

---------------------------

12000

:

Volt

: 20,00 kV

Mag.

: x 3,000

Date

: 2017/03/14

Pixel

: 640 x 480

003

Acquisition Parameter
Instrument

MgKa

10500
9000

: 6390(LA)

Acc. Voltage : 20.0 kV
Probe Current: 1.00000 nA

6000

PHA mode

: T3

4500

Real Time

: 41.92 sec

Live Time

: 30.00 sec

Dead Time

: 28 %

3000
1500

OKa

7500

BKa

Counts

Instrument

Counting Rate: 6379 cps

0
0.00

3.00

6.00

9.00

12.00

15.00

18.00

21.00

Energy Range :

0 - 20 keV

keV

ZAF Method Standardless Quantitative Analysis
Fitting Coefficient : 0.3853
Element

(keV)

Mass%

Error%

Atom%

B K

0.183

62.50

0.99

77.85

10.3711

O K

0.525

4.77

0.89

4.02

6.8901

Mg K

1.253

32.73

0.24

18.13

82.7388

Total

JED-2300

100.00

Compound

Mass%

Cation

K

100.00

AnalysisStation

Universitas Sumatera Utara

87

LAMPIRAN 5
HASIL CRYOGENIC MAGNET – KALEIDAGRAPH
1. Hasil Cryogenic Magnet Sampel MgB2 Komersil Tanpa Pemanasan

2. Hasil Cryogenic Magnet Sampel MgB2 Komersil Pemanasan 4000C

Universitas Sumatera Utara

88

3. Hasil Cryogenic Magnet Sampel MgB2 Komersil Pemanasan 8800C

4. Gabungan Hasil Karakterisasi Cryogenic Magnet pada Sampel MgB2
Komersil
MgB2 tanpa pemanasan
MgB2 880C
MgB2 400C
1.2

1

Resistivity

0.8

0.6

0.4

0.2

0

-0.2
10

15

20

25

30

35

40

45

Temperature (K)

Universitas Sumatera Utara