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IS 7739-8 (1975): Code of Practice for Preparation ofMetallographic Specimens, Part 8: Nickel and its alloys andtheir examination [MTD 22: Metallography and HeatTreatment]

IS : 7739 ( Part VIII ) - 1975 ( Reattirmed 1996 )

Indian Standard

CODE OF PRACTICE FOR PREPARATION OF METALLOGRAPHIC SPECIMENS

PART VIII NICKEL AND ITS ALLOYS AND THEIR EXAMINATION

( First Reprint FEBRUARY 1998 )

UDC 620.182.2 : 669.24

(6 Copyrighf 1976

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Gt 2 June 1976

IS : 7739 ( Part VIII ) - 1975

Indian Standard

CODE OF PRACTICE FOR PREPARATION OF METALLOGRAPHIC SPECIMENS

PART VIII NICKEL AND ITS ALLOYS AND THEIR EXAMINATION

Metallography and Heat-Treatment Sectional Committee, SMDC 27

Chairman Representing

SHRI K. V. CHINNAPPA International Nickel ( India ) Pvt Ltd, Bombay

Members

SHRI M. ANJANEYULU Mining & Allied Machinery Corporation Limited, Durgapur

SHRI N. V. RAGHWAN ( Alternate ) SHRI N. C. BAGCHI National Test House, Calcutta SHRI S. N. BANERJEE Indian Institute of Metals, Calcutta SHRI S. S. BHATNAGAR National Metallurgical Laboratory ( CSIR ),

Jamshedpur DR S. K. CHATTERJEE Guest, Keen, Williams, Ltd, Howrah

SHRI S. K. BASU ( Alternate ) SHRI DASARATHA The Mysore Iron & Steel Ltd, Bhadravati

SHRI B. HARIDASACAAR ( Alternate ) SHRI D. M. DAVAR Premier Automobiles Ltd, Bombay

SHRI A. T. BORATE ( Alternate ) D;;;g Y DIRECTOR ( MET)-% Ministry of Railways

CHEMIST & METALLURGIST (, Alternate ) SHRI A. K. GUI-IA Directorate General of Supplies & Disposals

( Inspection Wing ), New Delhi SHRI P. C. MUSTAFI ( Alternate 1

SHRI H. A. JAISINGHANI Mahindra & Mahindra Ltd, Bombay SHRI A. R. RANADIVE ( Alternate )

SHRI M. L. KATYAL Bajaj Auto Ltd, Pune DR D. M. LAKHIANI Indian Iron & Steel Co Ltd, Burnpur

SHRI D. R. DASGUPTA ( Alternate ) SHRI N. MAJUMDAR Indian Aluminium Co Ltd, Calcutta

SHRI S. N. BOSE ( Alternate ) DR G. MUKHERJEE Hindustan Steel Ltd, Ranchi

SHRI D. K. BAGCHI ( Alternate ) SHRI A. PADMANABAN Ashok Leyland Ltd, Madras

(Continued on page 2)

@ Copyright 1976 BUREAU OF INDIAN STANDARDS

This publication is protected under the Indian Copyright Act ( XIV of’1957 ) and reproduction in whole or in part by any means except with written permission of the publisher shall be deemed to be an infringement of copyright under the said Act.

IS : 7739 ( Part VIII ) - 1975

( Continued from page 1 )

Members

SHRI %. M. PAI

Representing

The Alloy Steel Producers’ Association of India, Bombay

SHRI S. A. MALWADE ( Alternate ) DR P. S. PATXHAL Tata Engineering & Locomotive Co Ltd, Jamshedpur

SHRI J. C. KAPOOR ( Alternate ) SHRI N. M. RAJU Hindustan Motors Ltd, Uttarpara SHRI B. RAMA KRISHNA Indian Telephone Industries Ltd, Bangalore

SHRI J. NAGESH BHAT ( Alternate ) SHRI V. RAMA SWAMY Ministry of Defence (DGI ), Department of

Defence Production SHRI R. H. G. RAU Mukand Iron & Steel, Bombay SHRI G. G. SAHA Ministry of Defence ( R & D ) SHRI H. N. SINGH Textile Machinery Corporation Ltd, Belgharia DR L. R. VAIDYANATH Indian Copper Information Centre, Calcutta SHRI V. V. VIRBHADRAYYA Directorate General of Technical Development

SHRI K. L. CHATTERJEE ( Alternate ) SHRI SUBHASH WADHAVAN Murarka Engineering Works, New Delhi SHRI C. R. RAMA RAO, Director General, ISI ( Ex-officio Member )

Director ( Strut & Met )

Secretary

SHRI B. MUKHERJI Deputy Director ( Met ), ISI

2

IS : 7739 ( Part VIII ) -

Indian Standard

CODE OF PRACTICE FOR PREPARATION OF METALLOGRAPHIC SPECIMENS

PART VIII NICKEL AND ITS ALLOYS AND THEIR EXAMINATION

0. FOREWORD

1975

0.1 This Indian Standard ( Part VIII ) was adopted by the Indian Standards Institution on 31 December 1975, after the draft finalized by the Metallography and Heat-Treatment Sectional Committee had been approved by the Structural and Metals Division Council.

0.2 The primary object of metallographic examination is to reveal the constituents and the structure of metals and their alloys by means of a microscope. Because of diversity in available equipment, wide variety of problems encountered, and the personal element, this standard gives for the guidance of the metallographer only those practices which experience has shown are generally satisfactory.

0.3 This standard is being issued in parts. This part covers polishing, etching and examination of nickel and its alloys. The other parts of this code are as follows:

Part I General features Part II Electrolytic polishing Part III Aluminium and its alloys and their examination Part IV Copper and its alloys and their examination Part V Iron and steel Part VI Lead and its alloys and their examination Part VII Magnesium and its alloys and their examination Part IX Gold, silver, platinum, palladium and their alloys and their

examination Part X Tin and its alloys and their examination Part XI Zinc and its alloys and their examination

1. SCOPE

1.1 This standard ( Part VIII ) covers the polishing, etching and examina- tion of nickel and its alloys.

3

IS : 7739 ( Part VIII ) - 1975

2. PREPARATION OF SPECIMENS 2.0 Recommended methods of selection, size, cutting, cleaning and mount- ing of metallographic specimens are outlined in Part I of this standard.

2.1 The specimen is first ground on a series of metallographic emery papers of increasing fineness, such as No. lG, 1, 0, .OO and 000, or silicon carbide No. 240, 320, 400, 600 or 800 wet or dry ( preferably wet) mounted on wheels revolving at 400 to 600 rpm, or backed by a flat surface using hand grinding. A final grinding on a paper made by graphiting a sheet of No. 000 emery paper, or silicon carbide No. 400, may be inserted prior to wet polishing, and, if done, eliminates one wet polishing operation. When this fine paper is omitted, wet polishing is begun with a thick water suspension of No. 600 Alundum on a wheel covered with shirt broadcloth rotating at 500 to 800 rpm. The final wet polishing is done with a water suspension of magnesium oxide or levigated alumina ( settled at 6 mm/h ) on a wheel covered with velveteen, broad- cloth, or flat silk crepe. For fine work and study of nonmetallic impurities, the use of magnesium oxide on a velveteen covering or the procedure employing the graphited paper and a crepe-covered final wheel is recom- mended. The magnesium oxide shall be kept dry, and the suspension shall be made up fresh before using to prevent absorption of carbon dioxide (CO, ) and the formation of a gritty carbonate, ( For details of grit numbers of abrasive papers, see IS : 715-1966* and IS :2832-19667. ) A comparative chart of grit numbers of abrasive grains is given at Appendix A.

2.2 The specimen may also be polished on a series of rotating wheels dressed with diamond compounds using appropriate lubricants. To mini- mize waste of diamond compound a maximum speed of about 400 rpm is desirable on wheels of 200 mm diameter, that is, 3m/sec. An efficient series uses successive wheels with 14 pm, 6 pm and lprn nominal diamond particle size. The first two grades are best used with woven nylon cloth pad, the last on short pile cloth ( cotton velveteen ). For very high quality finish a further wheel with & pm diamond on cotton velveteen may be used. These are satisfactory for nickel-base alloys but for soft pure nickel and cupro-nickel finishing by hand on soft cloth using magnesium oxide paste with a few spots of wetting agent is desirable. For the preservation of some reactive inclusions polishing without water using appropriate diamond compound lubricated with ligroin, filtered paraffin, etc, of proprietary lubricant is recommended.

3. ETCHING REAGENTS 3.2 In Table 1 are given the etching reagents commonly recommended for nickel and its principal alloys. 3.2 Etched specimens shall be washed thoroughly with water and alcohol and dried in an air blast. Stains can be removed by wiping with a clean soft cloth or cotton. The specimen shouid be preserved, if required, in a desiccator.

*Specification for coated abrasives, glue bond ( second revision ). tspecification for waterproof silicon carbide paper.

4

SL No.

(1)

i)

ii)

iii)

WI

iv)

v)

vi)

vii)

TABLE 1 ETCHING REAGENTS FOR NICKEL AND ITS ALLOYS

( Clause 3.1 )

ETCHING REAGENT COMPOSITION*

(2) (3)

Flat solution HNO, 50 ml Glacial acetic acid 50 ml

CONDITIONS OF USE REMARKS

(4)

Make up fresh daily; use colourless HNO, to avoid staining. Etch by immer- sion at room temperature for 5 to 20 seconds

For nickel; Monel, and other nickel-copper alloys. Dilute with 25 to 50 percent ace- tone for alloys of less than 25 percent nickel

Electrolytic-contrast Glacial acetic acid 3 ml H,O 85 ml HNO, 10 ml

Electrolytic-sulphuric H,SO, 5 ml acid H,O 25 ml

Aquaregia HNO, 5 ml HCl 25 ml H,O 20 ml

Nit;thydrofluoric HNO, 20 ml HF (48 percent ) 15 drops

Nitric acid HNO, 3U ml H,O 70 ml

Potassium cyanide KCN

?I::, 9%

Few drops

Electrolytic etch for 20 to 60 seconds using 1.5 V dry cell and platinum wires

Electrolytic etch for 5 to 15 seconds using two or three 1.5 V dry cells and platinum wires

Etch by immersion for 4 to 2 minutes

Warm specimen in bunsen flame or boiling water and etch by immersion for 15 to 45 seconds

Etch by immersion

Etch by immersion

(5)

Very satisfactory for grain size studies. Stains less than flat solutions

For nickel end Inconel ( nickel-chromium-iron )

Inconel

Inconel

Macro-etch for nickel silver

For low-zinc nickel silver

*The use of concentrated reagents is intended, unless otherwise specified. ( Continued )

SL No.

(1)

viii)

W

ETCEIING REAGENT

(2)

Ammonium hydro- xide - hydrogen peroxide

Frys

xl Q\

Cyanidepersulphate

xi) Acid-ferric chloride

xii) Hydrofluoric acid- glycerol

xiii) Dilute sulphuric acid

xiv) Glyceregia

TABLE 1 ETCHING REAGENTS FOR NICKEL AND ITS ALLOYS-Cm&

(hWOSTION+

(3)

NH,OH 85 ml H,G, 15 ml

CuCl, (saturated 100 ml solution in water )

HCI 20 to 50 LlJl

NaCN (100 g/l 50ml solution)

(NH,)&% 50 ml (lOOg/l solution)

HCI 50 ml FeCl, (200 g/l solu- 50 ml

tion in water)

H,G 85 ml Glycerol 10 ml HF 5 ml

H,SO, (10 percent - by volume)

Glycerol HCI HNO,

45 ml 10 ml 6 ml

CONDITIONS OF Use

(4)

Etch by immersion

Warm sections in hot water. Swab and wash. Etch off in alcohol

Freshly mixed before use. Use in fume cupboard with suitable precautions

Swab or immerse. Dilute if too vigorous or staining

Electrolytic-specimen ano- die 3 to 10 volts

Electrolytic-specimen ano- die 2 to 10 volts

Electrolytic- specimen ano- die 1 to 2 volts

REMARKS

(5)

For high-zinc nickel silver

Macro-etch. Nickel and nickel-chromium base alloys

Pure nickel. Electra-deposits on steel Monel

Pure nickel, cupro-nickels etc

Micro-structure nickel-chro- mium base alloys ( pre- ferred etch )

Micro-structure nickel-chro- mium base alloys ( pre- ferred etch )

As in Sl No. (xii)

,- 4’ ‘* .‘.

xv) Chemical polish/etch

xvi) Phosphoric acid

xvii) Murakamis

xviii) Caustic potash

W’O, HW, HNO,

60 ml At 80°C smoothens surface, at 20 ml lower temperature etches 20 ml

H,PO, (10 percent by volume)

Electrolytic preferably poten- tiostatic control at +1’2 V to calomel specimen anodic

KOH ( 100 g/l 50 ml Immersion in cold solution solution)

IWe B 50 ml (100 g/l solution)

KOH (560 g/l solution) Electrolytic-preferably po- tentiostatic c 0 n t r 0 1 at +0.2 to +0*3 V to calomel

Che$cal polish for nickel

Nickel-chromium base alloys. Detail studies. At t a c k s matrix leaving carbides, y, 7 and T. C. P. phases in relief

Nickel-chromium base alloys. Attacks carbides sigma but not y or 7j

Distinguishes carbides and D from y and 7 in nickel- chromium base alloys

*The use of concentrated reagents is intended, unless otherwise specified. 4

COMPARATIVE

ALUMINIUM Oxm, SILICON CARBIDE

AND GARN~

IS Number Grade

Number

14 14 16 16

00 24 24 30 30 36 36 40 46

50 54 60 60 80 80

100 100

120 120

150 150

180 180

220 220

APPENDIX A B .* ( Clause 2.1 ) 3

$4 h

CHART OF GRIT NUMBERS ( APPROXIMATE ) OF ABRASIVE GRAINS 3

FLINT GLASS CORUNDUM EMERY

IS Number Grade

r-YG- IS Grit Number Grade

‘BGrit Number Grade

Number Number Number

- - -

24 3 30 2) 36 2

40 14 50 1

60 # 80 -

100 0

120 00 150 - 180 -

- - -

24 3

30 24 36 - 40 s2 50 M2

60 - 80 -

100 F2

120 1) 150 1 180 0

- -

24 - 30 -

36 - 40 -

50 - 60 - 80 -

loo - 120 - 150 -

180 - - -

IS- B.S. Number Grade

Number

- -

24 - 30 - 36 3

40 2) 50 2

60 1t 80 1

100 F 120 FF 150 - 180 0 - -

TRADE c DESIGNATION E

v I

-

Extra Coarse Extra Coarse Coarse

Coarse

Medium Coarse Medium

Medium Medium Fine

Fine Fine Extra Fine

NOTE- Grits 240 and finer come under the sub-sieve range and as limits for these cannot be set on common silk test sieves, the grain sizes shall conform to general commercial grading, and it is recommended that the sedimentation process be adopted for their analysis.

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