SAE AMS*2759/B 92 m 7943325 0527133 833 W

The E n g i m h g Society
=For Advancing Mobility
Land Sea Air and Space@ AEROSPACE J)T AMS 275918
INTERNATIONAL
400 Commonwealth Drive, Warrendale, PA 15096-0001 MATERIAL
SPECIFICATION Issued JAN lgg2

Submitted for recognition as an American National Standard I

ION NITRIDING
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1. SCOPE:
1.1 Purpose:
This specification establishes the requirements and procedures for producing
a hard, wear resistant ion nitrided surface on steel parts.
1.2 Application:
The nitriding process, described herein, is applicable to alloy steels, tool
steels, nitriding steels, corrosion resistant steels, and other ferrous
al 1 oys.
2. APPLICABLE DOCUMENTS:
The following publications form a part of this specification to the extent
specified herein. The latest issue of SAE publications shall apply. The
applicable issue o f other publications shall be the issue in effect on the
date of the purchase order.
2.1 SAE Publications:
Available from SAE, 400 Commonwealth Drive, Warrendale, PA 15096-0001.
AMS 2418 Copper Plating
AMS 2759 Heat Treatment of Steel Parts, General Requirements
AMS 2759/6 Gas Nitriding and Heat Treatment o f Low-Alloy Steel Parts
ARP1820 Chord Method of Evaluating Surface Characteristics

SAE Technical Standards Board Rules provide that: "This report is published by SAE to advance the state of technical and engineering
sciences. The use of this report is entirely voluntary, and its applicability and suitability for any particular use, including any patent
infringementarising therefrom, is the sole responsibilityof the user."

SAE reviews each technical report at least every five years at which time it may be reaffirmed, revised, or cancelled. SAE invites your
written comments and suggestions.

Copyright 1992 Society of Automotive Engineers, Inc.

All rights reserved. Printed in U.S.A.
91-094îi EG

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I ANS 275918 SAE ANS 275918

2.2 ASTM Publications:

Available from ASTM, 1916 Race Street, Philadelphia, PA 19103-1187.
ASTM E 18 Rockwell Hardness and Rockwell Superficial Hardness of Metallic
Materi al s
ASTM E 92 Vickers Hardness o f Metallic Materials
ASTM E 384 Microhardness of Materials
3. TECHNICAL REQUIREMENTS:
3.1 Heat Treatment Prior to Nitriding:
Shall conform to AMS 2759 and its applicable detail specification and to the
requirements specified herein for the particular grade of material treated.
For steels not covered by AMS 2759, heat treatment shall be in accordance
with steel supplier recommendations and process controls shall be in
accordance with AMS 2759.
3.2 Pyrometric equipment shall conform to AMS 2759 except that temperature
uniformity shall be 115 O F (M OC) with the glow discharge power on.
3.2.1 Thermocouples: Shall be protected to prevent deterioration due to
contamination by furnace atmospheres. Thermocouples shall be isolated
electrically from both the anode and cathode to prevent heating of the
I thermocouple by the glow discharge.
3.2.2 Vacuum (Pressure) Controls: Equipment shall be available for measuring,
control 1 i ng , and recording vacuum (pressure) 1 eve1 s i n the vessel during
heating and at any time the power is on for glow discharge. The control
equipment shall be capable o f maintaining the vacuum (pressure) level at
any setpoint within the equipment operating range with sufficient accuracy
to meet the processing requirements of the parts being treated.
3.2.3 Nitriding Atmosphere: The type of surface layer is influenced by gas
composition. The nitriding gas composition shall be selected to produce a
monophase compound layer or a pure diffusion zone as specified by the
cognizant engineering organization. Guidelines on gas composition effects
on compound layer formation are as follows:
3.2.3.1 Effects of Nitriding Atmosphere on Type of Compound Layer Produced: The
type of nitride layer produced is mainly influenced by the composition
and substrate material. Steels with high carbon content, greater than 1%
by weight, readily form the epsilon iron nitride phase as carbon is
soluble in and stabilizes this phase. Carbon in the form of methane or
CO2 reacts to stabilize the epsilon phase. This phase is desired only
for plain carbon steels and cast irons. Presence of oxygen may also lead
to an epsilon phase. Treatments to produce an epsilon phase compound
layer are referred to as nitrocarburizing treatments and are not covered
by this specification. Nitrogen is necessary for compound layer
formation. The following minimum levels of nitrogen in the ingoing gas
are given as a guideline:

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ANS 2759f8 SAE ANS 275918

3.2.3.2 Low-alloy steels (containing up to 5% nominal alloying elements by

weight) - 5% nitrogen by volume, to ensure at least a diffusion zone.
3.2.3.3 High alloy, corrosion resistant, and tool steels (steels with more than
5% nominal alloying elements by weight) - 15% nitrogen by volume.
3.2.3.4 When a compound layer is required, a minimum of 25% nitrogen by volume is
suggested, unless otherwise determined by preproduction tests.
3.2.4 Atmosphere Control : Equipment shall be available for mixing the nitrogen
and hydrogen gases in variable ratios so that the process gas may be varied
from 0% nitrogen (pure hydrogen) to 100% nitrogen, and for introducing the
mixture o f these into the vacuum chamber at a controlled rate.
Alternatively, a premixed gas o f certified composition can be used. The
atmosphere equipment shall be capable of providing a measured value of the
components o f the mixed gas within 11% by volume of the selected value.
For example, if the gas contains 25% nitrogen, the concentration can range
from 24 to 26%.
3.2.5 Leak Rate: The furnace leak rate, expressed as microns per hour shall be
measured before each treatment cycle. The leak rate shall not exceed
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10 microns per hour. Leak rate shall be determined, before starting the
heat cycle, after loading and closing the vessel, and evacuating to
75 microns (10 Pa) or lower, closing all valves to the vessel chamber. The
initial pressure is recorded and a second reading taken at least
15 minutes after the first reading. Leak rate shall be calculated by
subtracting the first reading from the second, dividing the result by the
time interval, and multiplying the resultant number by 60.
3.2.6 Initial Evacuation of Vessel: At the start of each cycle, before admitting
nitriding gas and before turning on power for heating, the vessel shall be
evacuated to a pressure of 75 microns (10 Pa) or lower.
3.3 Nitriding Requirements:
3.3.1 Surfaces to be nitrided shall be free from decarburization.
3.3.2 All heat treatable steels to be nitrided shall be hardened and tempered
prior to nitriding. The nitriding temperatures shall be no higher than
25 OF (14 O C ) below the part tempering temperature.
3.3.3 Parts which have been ground, straightened, etc before nitriding may be
stress relieved prior to nitriding. The stress relieving temperature shall
be in accordance with AMS 2759 and its applicable detail specification.
For materials, such as tool steels, which are not covered by AMS 2759,
stress relieving temperature shall be not less than 20 O F (11 OC) above the
nitriding temperature. Surfaces to be nitrided shall be mechanically or
chemically cleaned subsequent to stress relieving and prior to nitriding.
3.3.4 Parts to be nitrided shall be free o f grease, oil, and other contaminants.
Equipment shall be available to suitably degrease and otherwise clean areas
of the part to be nitrided. (Cleaning agents shall be free of water or
compounds which would inhibit nitriding).

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 AMS 275918 SAE AMS 275918

3.3.5 Ion nitriding may cause sputtering o f commonly used masking materials. As
a result, the preferred method of masking is by mechanical means such as
plates or other covers which act as barriers between the glow discharge and
the part surfaces. Other masking materials, such as copper plate masks o r
copper paste, may be used if approved by the cognizant engineering
organization. When copper plating is used, it shall be applied in
accordance with AMS 2418. Tin-bearing masking material shall not be used.
When copper plate or paint is used for masking, ion power voltage shall be
limited to 600 volts. As an alternative to masking, parts may be nitrided
all over and the case ground from the surface where a nitride case is not
des i red.
3.4 Procedure:
3.4.1 Test specimens as in 4.3 shall be placed at locations representing the
extremes of work temperature established in preproduction testing.
3.4.2 Nitriding: Parts shall be processed in ion nitriding equipment in the
selected gas environment at a temperature and for a time sufficient to
produce the specified depth of case and compound layer. After completion
of the nitriding cycle and prior to removal from the furnace, parts and
test specimens shall be cooled to 300 O F (149 O C ) or below in either the
nitriding atmosphere, a non-reactive atmosphere, or vacuum. Removal of
parts at higher temperatures shall be approved by the cognizant engineering
organization.
3.5 Post Nitriding Operations:
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3.5.1 Compound Layer Removal: When removal o f compound layer generated during
nitriding is required, it should be accomplished by lapping or honing with
maximum stock removal of 0.001 inch (0.025 mm). If grinding is used, the
parts shall be stress relieved as in 3.5.2, after grinding. Alternatively,
compound layer may be removed by chemical means if approved by the
cognizant engineering organization. When remaining compound layer is
permitted, the depth of the compound layer shall be no greater than
0.0005 inch (0.0127 mm), unless otherwise permitted by the cognizant
engineering organization.
3.5.2 Stress Relief: Parts ground after nitriding shall be stress relieved by
heating to a temperature within the range 325 - 650 O F
(163 - 343 OC), holding at the selected temperature within +15 O F (+8 OC)
for not less than 2 hours, and cooling in air.
3.5.3 Stripping of Masking Materials: Shall be accomplished by use of a non-
embrittling stripper.
3.6 Properties:
Shall be as follows, determined on parts or on test specimens.
3.6.1 Compound Layer and Nitride Distribution: The compound layer, when
permitted, shall be single phase.

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AMS 2759/8 SAE AMS 275918

3.6.1.1 Compound Layer Identification: After qualification of the procedures in

preproduction testing, one or both of the etching techniques described in
8.9 and 8.10 may be used to detect and identify compound layer.
Alternatively, the type of compound layer may be identified by x-ray
di ffraction.
3.6.1.2 Nitride Distribution: The finished case shall show a uniform
distribution of nitrides, diminishing gradually from the surface to the
core. There shall be no evidence of continuous nitride-networks.
Examination shall be made on specimens polished, etched, and examined at
not lower than 400X magnification.
3.6.2 Case Depth: Shall be as specified by the cognizant engineering
organization. The effective and total case depths shall be determined by
microhardness surveys in accordance with ASTM E 384, on metallographically
prepared specimens or parts, or in accordance with ARP1820. Case depth
shall be defined as in 8.3 and 8.4.
3.6.3 Surface Hardness: Shall be as specified by the cognizant engineering
organization or as follows:
3.6.3.1 For nitriding grade steels, the surface hardness shall be as specified in
AMS 2759/6, determined in accordance with ASTM E 18 or ASTM E 92, as

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appl i cab1 e.
3.6.4 Evidence o f arcing on the part surfaces shall be cause for rejection.
4. QUALITY ASSURANCE PROVISIONS:
Shall be as follows:
4.1 Responsibility for Inspection:
Shall be as specified in AMS 2759.
4.2 Classification of Tests:
Shall be as specified in AMS 2759 and as follows:
4.2.1 Acceptance Tests: In addition to the tests specified in AMS 2759, the
tests in 3.6 shall be performed on each furnace load.
4.2.2 Preproduction Tests: In addition to the tests specified in MS 2759, t,,e
following shall be performed prior t o any production nitriding for each
piece of equipment to be used.
4.2.2.1 Certification of leak rate and accuracy of vacuum measuring and
controlling instrumentation acceptable to the cognizant quality assurance
organization.
4.2.2.2 Certification of gas m i x accuracy acceptable to the cognizant quality
assurance organization.

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AMS 275918 SAE AMS 275918

4.2.2.3 Certification of pressure vs. temperature program for avoidance of hollow

cathodes, for each part number to be processed, by a method acceptable to
the cognizant quality assurance organization.
4.2.2.4 Establishment of Processing Procedure: For each part number, a loading,
operating, and testing practice shall be established. This shall
include, for each furnace in which the parts are to be processed, the
fol 1 owing :
4.2.2.4.1 Loading diagram showing the location and spacing o f each identical part
number.
4.2.2.4.2 Minimum and maximum number o f parts which can be run with the same
practice.
4.2.2.4.3 Other part numbers or geometries which can be run in the same load.
4.2.2.4.4 Location of work thermocouples and method of attaching to the load.
4.2.2.4.5 Procedure of masking.
4.2.2.4.6 Description of test specimens and their location in the load.
4.2.2.4.7 Specification of fixturing used including auxiliary anodes or cathodes.
4.2.2.4.8 Program for pressure vs. temperature and gas mixture to be used
throughout the nitriding cycle.
4.2.2.4.9 Verification of temperature uniformity for the load and for the range
of acceptable variations of the loading parameters.
4.2.2.4.10 Limits of gas composition to be used to produce the specified compound
1 ayer.
4.3 Sampling:
Shall be in accordance with AMS 2759 and as follows:
4.3.1 Each specific production part number or lot of parts nitrided in one
furnace charge shall be accompanied by at least two test specimens as in
4 . 3 . 1 . 3 or 4 . 3 . 3 . 1 .

4.3.1.1 In the case of furnace lots containing more than one steel, one suitable
specimen for each steel shall be used.
4.3.1.2 Test specimens shall accompany the parts through all processing
operations, including hardening, tempering, masking, nitriding, mask
removal , etc.
4.3.1.2.1 Each test specimen shall be identified for correlation of the test
specimen to furnace lot o f parts.

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ANS 275918 SAE AMS 275918

4.3.1.3 The preferred test specimen shall be a finished part of each part number
in the load.
4.3.1.3.1 As an alternative, a specimen having the same processing history as the
parts can be used if approved by the cognizant quality assurance
organization. The specimen shall be fabricated from the same steel as
the parts and shall have hardness in the same range as the parts. The
test specimen shall be similar in dimensions, tolerances, and geometry
as the part which it represents. It shall have been verified to be
representative in preproduction tests as in 4.2.2.4.
4.3.2 When a re-nitriding cycle is required, one half of all the original coupons
plus a new set of coupons shall be included in the rerun. Alternatively, a
cut face from the original specimen may be used to verify the nitriding
parameters provided that the new specimen created meets the requirements of
4 . 3 . 1 . Where the likelihood of retreatment is high, the specimens can be
partially masked during the first treatment. If a second treatment is
required, the masking is removed and the same test pieces rerun. The use
of either of these alternative procedures shall be approved in advance by
the cognizant quality assurance organization.
4.4 Approval :
4.4.1 Vendors (Subcontractors): Approval of a facility shall be in accordance
with the applicable requirements of AMS 2759 and 4.2.2.
4.4.2 Personnel: Qualification of personnel shall be in accordance with the
applicable requirements of AMS 2759.
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4.5 Furnace Log Entries and Recorder Chart Entries:

Shall be n accordance with AMS 2759, and in addition, shall include the
fol 1 owing for each furnace load:
Ion voltage at each temperature and pressure used
Ion current at each temperature and pressure used
Fur ace pressure before start of heating and at each temperature used
Gas mixture
Leak test results prior to starting of cycle
Calibration of gas mixture
Sketch, diagram or photograph of 1 oad arrangement and work thermocouple
locations, indicating location of control point
Type and description of masking used
4.6 Records:
Shall be in accordance with AMS 2759.
4.7 Reports:
Shall be in accordance with AMS 2759.

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AMS 2759/8 SAE AMS 2759/8

5. PREPARATION FOR DELIVERY:

Identification, protective treatment, and packaging shall be in accordance
with AMS 2759.
6. ACKNOWLEDGMENT:
A vendor shall mention this specification number in all quotations and when
acknowledging purchase orders.
7. REJECTIONS:
Parts on which the ion nitr ding does not conform to this specificat on, or to
modif i cations authorized by purchaser, will be subject to rejection.
8. NOTES:
8.1 Definition of Ion Nitriding:
Ion nitriding is a vacuum process for producing a nitrided case on ferrous
materials using a glow discharge, Various terms have been used to describe
the process, including plasma, plasma/ion nitriding, and ionitriding.
8.1.1 The workpieces to be ion nitrided are suspended or placed in a vacuum
furnace in such a way that effective electrical isolation is provided.
Together with the vacuum pump, the gas distribution system enables the
furnace to be evacuated, filled with the appropriate treatment gas, and
maintained at the required vacuum, usually between 133 to 1333 Pa
(1 to 10 Torr).

8.1.2 Voltage, which can be set to any value from 300 volts to approximately
1000 volts, is applied between the workpiece to be ion nitrided and the
wall of the furnace, the former being connected as the cathode and the
latter as the anode. Under this potential, the molecules and atoms o f the
treatment gas are excited and ionized, producing the typical luminous
phenomenon known as glow discharge around the exposed surfaces of the
workpi eces.
8.1.3 Ion nitriding can be carried out using either pure nitrogen or mixtures of
nitrogen with hydrogen or suitable hydrocarbons. Gas composition
determines the type of surface layer to be produced for the particular
steel processed. Treatments using hydrocarbons are considered to be
nitrocarburizing.
8.1.4 The temperature o f the workpiece is measured w th the aid of thermocouples
and regulated by means of a controller varying the power output of the
electric unit. The treatment temperature is, n most cases, set between
750 and 1110 O F (399 and 599 OC), depending on the composition and
structure o f the steel to be treated, as well as the stress which the
workpiece will have to resist.

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AMS 2759/8 SAE AMS 2759/8

8.2 Types of Surface Layers:

In ion nitriding, as in other nitriding processes, two types of surfaces may
be produced.
8.2.1 Diffusion Zone: In the steel itself, nitrogen diffuses according to
classical principles, producing a hardened zone by precipitation and sol id
solution hardening. This is known as the diffusion zone and is detected as
a dark etching region below the surface varying in hardness from the
surface to the core. This is the region measured as the case in nitrided
steels and may be as deep as 0.035 inch (0.89 mm) depending upon the steel,
time, and temperature.
8.2.2 Compound Layer: The surface of the steel may be converted to one or more
compounds of essentially pure nitrides of metal, primarily iron. The layer
formed, usually less than 0.001 inch (0.025 mm) in thickness, remains
unetched when a metallographic sample is etched with nital etchant and
appears white in the microscope. For this reason, the layer is commonly
called white layer in gas nitriding. When the layer i s very thick or
contains a mixture of the two dominant nitride phases predicted by the
iron-nitrogen phase diagram, this layer is very brittle and shall be
removed.
8.3 Total case depth is defined as the maximum depth below the surface at which a
Rockwell C hardness, or equivalent, of five HRC units above core hardness is
achi w e d ,
8.4 Effective case depth is defined as the maximum depth below the surface at
which a hardness o f 50 HRC, or equivalent, i s achieved.
8.5 Allowance should be made for dimensional growth during nitriding. Growth
varies with steel and specific treatment and should be determined by
preproduction testing. In the absence of data, a growth of 0.0001 inch per
0.005 inch (0.0025 mm per 0.127 mm) diffusion depth may be considered
typical.
8.6 Ion nitriding can be used to process a wide variety of steels. Table 1 shows
typical results which can be achieved for various steels.
8.7 Hol 1 ow Cathode:
An effect created by gaps, holes, or cavities in parts resulting in an
intense localized glow discharge. The intensity of the localized glow
discharge is a function of temperature, pressure, gas composition, and length
(depth) of the cavity divided by its width (or diameter in case of holes).
Hollow cathode may result in localized overheating which can be detected by
hardness tests as soft areas near susceptible areas.
8.8 Sharp corners or edges on parts should be avoided wherever possible. Growth
takes place on all surfaces and combines at the corners to form projections
containing a high nitrogen content which are very brittle and likely t o chip.

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AMS 275918 SAE AMS 275918

8.9 To d i f f e r e n t i a t e between t h e types o f n i t r i d e s produced i n t h e w h i t e l a y e r ,

t h e f o l l o w i n g m e t a l l o g r a p h i c procedure may be used t o make e v i d e n t t h e phases
o f a compound l a y e r :

8.9.1 Composition o f E t c h i n g Reagent (Marble’s): S h a l l be mixed i n t h e f o l l o w i n g

succession:

50 mL Water
50 mL Alcohol (Ethanol)
50 mL H y d r o c h l o r i c A c i d
2 grams Copper S u l f a t e

8.9.2 A p p l i c a t i o n : A f t e r normal m e t a l l o g r a p h i c p r e p a r a t i o n and e t c h i n g i n n i t a l

(3% n i t r i c a c i d i n e t h y l a l c o h o l ) , t h e compound l a y e r , i f present, does not
e t c h and s t a y s w h i t e a t t h i s stage. I t i s u s e f u l t o t a k e a photomicrograph
o f t h e n i t a l etched s u r f a c e f o r comparison w i t h t h e Marble’s etched s u r f a c e
produced n e x t . Repolish and then h o l d f o r a second i n t h e Marble’s
s o l u t i o n (by immersion, n o t swabbing).

8.9.3 I n t e r p r e t a t i o n o f Results: There can be t h r e e phases p r e s e n t , as f o l l o w s :

8.9.3.1 I f t h e compound l a y e r remains white, an e p s i l o n phase i s p r e s e n t .

8.9.3.2 A b l a c k compound l a y e r means a gamma prime phase i s p r e s e n t .

8.9.3.3 A b l a c k - w h i t e l a y e r means a m i x t u r e o f e p s i l o n phase and gamma prime

phase.

8.9.3.3.1 With mixed phase, one can o c c a s i o n a l l y observe t h a t t h e p o r t i o n o f one

o r t h e o t h e r phase i s more s t r o n g l y represented. There can a l s o be two
l a y e r s present, one over t h e o t h e r .

8.10 Test f o r Compound Layer Presence:

To d e t e c t t h e presence o f compound l a y e r on s t e e l p a r t s , a copper s u l f a t e

s o l u t i o n may be used, as f o l l o w s :

8.10.1 Composition:

40 grams copper s u l f a t e (CuSO4 5H20)

1000 mL water
5 mL w e t t i n g agent
3.9 t o 4.1 pH

8.10.2 A p p l i c a t i o n : Areas t o be t e s t e d s h a l l be cleaned and t h e n swabbed w i t h t h e

s o l u t i o n o f 8.10.1. The s o l u t i o n should be l e f t on t h e s u r f a c e f o r a t
l e a s t 30 seconds.

8.10.3 I n t e r p r e t a t i o n : Copper w i l l n o t p l a t e on surfaces c o n t a i n i n g a continuous

compound l a y e r . If a copper c o l o r occurs i n 30 seconds o r l e s s , no
compound l a y e r i s present.

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AMS 2759/8 SAE AMS 2759f8

8.11 Representative treatments and results of ion nitriding for various materials
are listed in Table 1.
8.12 For direct U.S. Military procurement, purchase documents should specify not
less than the following:
Title, number, and date o f this specification
Size o f parts desired
Quantity of parts desired
Part number or product identity
Steel alloy designations
Heat treating operations desired
Hardness, case depth, compound layer type and thickness desired
Level A packaging, if required (See AMS 2759).

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PREPARED BY AMEC AND IS UNDER THE JURISDICTION OF AMS COMMITTEE "BI'.

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No reproduction or networking permitted without license from IHS Not for Resale, 10/11/2005 21:56:29 MDT
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- 12 -
Copyright SAE International
Provided by IHS under license with SAE Licensee=Messier Dowty/5905381001
No reproduction or networking permitted without license from IHS Not for Resale, 10/11/2005 21:56:29 MDT