AEROSPACE AMS 2759/8A

MATERIAL Issued JAN 1992

SPECIFICATION Revised JUN 2007

Superseding AMS 2759/8

(R) Ion Nitriding

RATIONALE

AMS 2759/8A changes thermal management, testing, and process requirements.

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 ion nitriding process is typically applied to increase surface hardness, increase wear resistance, and reduce
coefficient of friction of alloy steels, tool steels, nitriding steels, corrosion resistant steels (CRES), carbon steels, ferrous
powder metal products, and other ferrous alloys but usage is not limited to such applications. See 8.2.6 for other materials
that can be ion nitrided.

2. APPLICABLE DOCUMENTS

The issue of the following documents in effect on the date of the purchase order forms a part of this specification to the
extent specified herein. The supplier may work to a subsequent revision of a document unless a specific document issue
is specified. When the referenced document has been cancelled and no superseding document has been specified, the
last published issue of that document shall apply.

2.1 SAE Publications

Available from SAE International, 400 Commonwealth Drive, Warrendale, PA 15096-0001, Tel: 877-606-7323 (inside
USA and Canada) or 724-776-4970 (outside USA), www.sae.org.

AMS 2429 Bronze Plating

AMS 2418 Copper Plating
AMS 2759 Heat Treatment of Steel Parts, General Requirements

ARP1820 Chord Method of Evaluating Surface Microstructural Characteristics

ARP 1962 Training and Approval of Heat Treating Personnel

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 infringement arising therefrom, is the sole responsibility of 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 2007 SAE International
All rights reserved. No part of this publication may be reproduced, stored in a retrieval system or transmitted, in any form or by any means, electronic, mechanical, photocopying, recording,
or otherwise, without the prior written permission of SAE.
TO PLACE A DOCUMENT ORDER: Tel: 877-606-7323 (inside USA and Canada)
Tel: 724-776-4970 (outside USA)
Fax: 724-776-0790
Email: custsvc@sae.org
SAE WEB ADDRESS: http://www.sae.org
SAE AMS 2759/8A -2-

2.2 ASTM Publications

Available from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959,
Tel: 610-832-9585, www.astm.org.

ASTM A 370 Standard Test Methods and Definitions for Mechanical Testing of Steel Products
ASTM E 3 Preparation of Metallographic Specimens
ASTM E 18 Rockwell Hardness and Rockwell Superficial Hardness of Metallic Materials
ASTM E 92 Vickers Hardness of Metallic Materials
ASTM E 140 Standard Hardness Conversion Tables for Metals
ASTM E 384 Microindentation Hardness of Materials

2.3 ASM Publications

Available from ASM International, 9639 Kinsman Road, Materials Park, OH 44073-0002, Tel: 800-336-5152 (inside U.S.
and Canada), 440-338-5151 (outside USA), www.asm-intl.org.

ASM Metals Handbook, Metallography and Microstructure, Volume 9, 9th Edition.

3. TECHNICAL REQUIREMENTS

3.1 Heat Treatment Prior to Nitriding

Prior heat treatment shall conform to AMS 2759 or document approved by cognizant engineering organization 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 Pyrometry

3.2.1 Pyrometric equipment shall conform to AMS 2759 except that temperature uniformity survey (TUS) and system
accuracy test (SAT) requirements do not apply. The temperature range shall be 50 F (28C) or less at nitriding
temperatures determined by four thermocouples during processing of each production load. The maximum
temperature shall not exceed the limits of 3.4.2 and 3.4.3 or as otherwise established during preproduction testing.

3.2.1.1 Thermocouples shall be placed in parts or representative specimens distributed in the load and near test
samples in accordance with 4.2 and 4.3 and represent the extreme and mid-range temperatures of the load. A
control thermocouple and/or over-temp thermocouple may be used as one of the four thermocouples required
by 3.2.1.

3.2.1.2 Alternatively, infrared pyrometry may be used when acceptable to the cognizant engineering organization.
Unless specified otherwise, the calibration shall be quarterly and shall be in accordance with the vessel system
manufacturer instructions.

3.2.1.3 If a thermocouple fails or has a suspect reading during processing, suppliers engineering and quality
departments shall review the run to determine if product conforms to specified requirements. Results of the
analysis and any additional evaluation shall be documented, including assessment of corrective actions or
improvement to prevent recurrence.

3.3 Equipment

Vessels, associated equipment, and controls shall be maintained in accordance with the manufacturers recommendations
or the processors internal procedures.

3.3.1 Vessels may additionally be equipped with radiation shields and/or auxiliary resistance heating.
SAE AMS 2759/8A -3-

3.3.2 Vacuum (Low Pressure) Controls

Equipment shall have calibrated recording instruments for sensing, measuring, controlling, and recording pressure during
the entire cycle. The control equipment shall be capable of maintaining the operating pressure level at any setpoint within
the equipment operating range with sufficient accuracy to meet the processing requirements of the parts being treated.

3.3.3 Nitriding Atmosphere

The nitriding gas composition shall be selected to produce a compound layer or a pure diffusion zone as specified by the
cognizant engineering organization. Guidelines on gas composition effects on compound layer formation are found in
8.2.5.

3.3.4 Atmosphere Control

Equipment for mixing gases shall be calibrated and capable of providing a measured ratio of the components of the mixed
gas within 3% by volume of the selected value or as approved by the cognizant engineering organization. For example, if
the gas contains 25% nitrogen, the concentration can range from 22 to 28%. Alternatively, a premixed gas of certified
composition may be used.

3.3.5 Leak Rate (Rise in Pressure)

The vessel leak rate, expressed as microns per hour shall be measured before each treatment cycle. The leak rate shall
not exceed 90 microns per hour or other leak rate acceptable to the cognizant engineering organization. Leak rate shall be
determined, before starting the heat cycle, after loading and closing the vessel, evacuating to 75 microns (10 Pa) or lower,
and closing all valves to the vessel chamber to isolate the pumps. 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. Alternatively, another method
approved by the cognizant engineering organization may be used.

3.3.6 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.

3.4 Nitriding Requirements

3.4.1 Surfaces to be nitrided shall be free from decarburization.

3.4.2 Heat treatable steels shall be hardened and tempered prior to nitriding. The nitriding temperatures shall be no
higher than 50 F (28 C) below the tempering or aging temperature. When approved by the cognizant engineering
organization, higher temperatures may be used if core hardness is maintained and all metallurgical and
dimensional requirements are met as demonstrated by testing and sectioning of specimens.

3.4.3 Parts that have been ground or straightened before ion nitriding may be stress relieved prior to nitriding. Based on
material, tolerance, and processing, parts that have been straightened, rough machined, rough ground or
otherwise mechanically worked after heat treatment may be stress relieved in accordance with AMS 2759 or
customer requirement prior to machining or grinding and ion nitriding.

3.4.3.1 When stress relieving has been performed, the nitriding temperature shall be 50 F (28 C) or more below the
stress relieving temperature. When approved by the cognizant engineering organization, higher temperatures
may be used if core hardness is maintained and all metallurgical and dimensional requirements are met as
demonstrated by testing and sectioning of specimens. Surfaces to be nitrided shall be mechanically or
chemically cleaned subsequent to stress relieving and prior to nitriding.

3.4.4 Parts to be nitrided shall be free of grease, oil, and other contaminants.
SAE AMS 2759/8A -4-

3.4.5 When selective nitriding is required, mechanical masking shall be used to prevent nitriding of selected surfaces.
When acceptable to the cognizant engineering organization, pastes, paints, or plating may be used. When used,
copper plating shall be in accordance with AMS 2418, or bronze plating in accordance with AMS 2429. Tin-bearing
masking material shall not be used. Alternatively, when acceptable to the cognizant engineering organization,
parts may be nitrided all over and the case machined off surfaces not to be nitrided. See 8.11.

3.5 Procedure

3.5.1 Establishment of Processing Procedure

For each part number, the following shall be established and documented: the minimum and maximum number of parts
allowed per load, the loading layout (a sketch, diagram, or photograph of part locations and thermocouple locations),
masking/fixturing, processing parameters, specimen type and locations, and testing practice.

3.5.1.1 Previously Approved Procedure

It is permissible, for specific parts, to use equipment, practices and test methods which conformed to the original
publication of AMS 2759/8 and were previously acceptable to the purchaser.

3.5.2 For parts expected to be nonrecurring (8.12.1) the processing procedure may be limited to vessel log/recorder
entries (4.5) and records (4.6).

3.5.3 Test specimens as in 4.3 shall be placed in each load at locations representing the extremes and mid-range of
work temperature established in 3.2.1 or by other analysis or test data.

3.5.4 Processing parameters shall be documented and shall result in the meeting of all specified requirements.

3.5.5 Nitrided parts shall not be removed from the vessel at temperatures above 300 F (140 C).

3.5.6 Unless otherwise required by the cognizant engineering organization, nonrecurring loads (8.12.1) of different parts
that require the same process parameters may be combined and processed together in the same load, if testing in
accordance with 4.3.1 verifies that the requirements of 3.7 are attained.

3.6 Post Nitriding Operations

3.6.1 Compound Layer Removal

When removal of compound layer generated by 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 3.6.2 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 minimized and shall
be no greater than 0.0005 inch (0.0127 mm), unless otherwise required by the cognizant engineering organization.

3.6.2 Stress Relief

Parts ground after nitriding shall be stress relieved by heating to a temperature within the range 325 to 650 F (163 to 343
C) holding at the selected temperature within 15 F (8 C) for not less than two hours and cooling in air.

3.6.3 Copper plating when used for masking shall be chemically stripped. The stripping process shall not roughen, pit,
or embrittle the base metal or adversely affect part dimensions.

3.6.4 Paint or paste masking materials shall be removed without affecting the surface roughness.
SAE AMS 2759/8A -5-

3.7 Properties

Nitrided surfaces shall conform to the following requirements.

3.7.1 Type of Compound Layer

When the phase composition of the compound layer is specified, verification shall be performed by using metallurgical
evaluation. If required by the cognizant engineering organization, X-ray diffraction shall be used. See 8.8 and 8.9.

3.7.1.1 Compound zone layer depth (thickness), when specified, shall be measured metallographically at 400X
magnification or greater.

3.7.1.2 Uniformity of Nitride Case

There shall be no continuous nitride network or grains fully encircled by nitrides along boundaries when examined at 400X
magnification or greater.

3.7.2 Case depth shall be as specified by the cognizant engineering organization. The effective and total case depths
shall be determined by microhardness traverse in accordance with ASTM E 384, on metallographically prepared
specimens or parts, or in accordance with ARP1820. Unless specified otherwise case depth shall be defined as in
3.7.2.1 and 3.7.2.2.

3.7.2.1 Total Case Depth

Unless otherwise specified, total case depth is the depth below the surface at which microhardness is 50 HV or 50 HK
units, higher than that of core, as determined by microhardness traverse in accordance with ASTM E 384.

3.7.2.2 Effective Case Depth

Unless otherwise specified, is the maximum depth below the surface at which a specified hardness is achieved as
measured by microhardness traverse in accordance with ASTM E 384.

3.7.2.2.1 Low Alloy Steels such as 4140 and 4130

Unless otherwise specified, effective case depth is the maximum depth below the surface at which a hardness of 40 HRC
equivalent is achieved.

3.7.2.2.2 Tool Steels such as A, D, H, M, and CPM

Unless otherwise specified, effective case depth is the maximum depth below the surface at which a hardness of 60 HRC
equivalent is achieved.

3.7.2.2.3 All Other Steels, Including Nitralloy

Unless otherwise specified, effective case depth is the maximum depth below the surface at which a hardness of 50 HRC
equivalent is achieved.

3.7.3 Surface hardness shall be as specified by the cognizant engineering organization and in accordance with Table 1
using Vickers or Knoop with specified load or HR15N and reported using original scale/load used in accordance
with ASTM E 18 or ASTM E 92 as applicable or other method acceptable to the cognizant engineering
organization.

3.7.4 Evidence of arcing on the part surfaces requires customer notification and identification of parts for customer
disposition.
SAE AMS 2759/8A -6-

4. QUALITY ASSURANCE PROVISIONS

4.1 Responsibility for Inspection

The processor shall be responsible for the performance of all required tests. When parts or representative specimens are
to be tested, the parts shall be supplied by purchaser. The cognizant engineering organization reserves the right to sample
and to perform any confirmatory testing deemed necessary to ensure that nitrided parts conform to specified requirements.

4.2 Classification of Tests

4.2.1 Acceptance Tests

When the following characteristics are specified, they are acceptance tests and shall be performed on each vessel load in
accordance with section 4.3.1: total case depth (3.7.2.1), effective case depth (3.7.2.2), surface hardness (3.7.3),
compound layer depth (thickness) (3.7.1), and uniformity of nitride case (3.7.2).

4.2.1.1 Hardness shall be in accordance with ASTM A 370, ASTM E 92, ASTM E 18, ASTM E 140, or ASTM E 384.
The appropriate conversion of tensile strength requirements from hardness shall be in accordance with ASTM A
370 and the hardness conversion table for metals shall be in accordance with ASTM E 140.

4.2.1.1.1 Verification of hardness testing machines shall be performed daily when used and the results documented.

4.2.1.1.2 Servicing and calibration of hardness testing machines shall be annually unless otherwise specified by the
cognizant quality assurance organization.

4.2.1.2 Metallographic examination, including mounting and polishing shall be performed in accordance with ASTM E 3
and ASM Metals Handbook Vol. 9 or equivalent.

4.2.2 Periodic Test

When compound layer type (phase composition) is specified (3.7.1), verification shall be a periodic and shall be performed
at a frequency determined by the processor, unless a specific frequency is required by the cognizant engineering
organization.

4.3 Sampling and Testing

A lot shall be all parts of the same alloy and configuration, heat treated to the same requirements and nitrided in the same
vessel at the same time. For nonrecurring loads (See 8.12.1) a lot shall be different parts that require the same process
parameters that are processed together in the same vessel load, in accordance with 3.5.6.

4.3.1 Acceptance tests

Each vessel load shall have at least four specimens in accordance with 4.3.1.1 or 4.3.1.2 tested for compliance with the
specified requirements. When more than one layer of parts is processed in a load, a minimum of one specimen shall be
positioned in each layer of the vessel to represent the low, mid-range, and high temperatures of the load and where
possible placed near thermocouples. The top and the bottom layers shall have a minimum of two specimens unless
otherwise permitted in accordance with 4.3.1.5.

4.3.1.1 When the working volumes of vessels exceed 150 cubic feet one additional specimen shall be tested for each
additional 50 cubic feet.

4.3.1.2 Actual parts are the preferred test specimen and shall be used when practical and approved by the purchaser.
SAE AMS 2759/8A -7-

4.3.1.3 Representative specimens provided by the purchaser, i.e., 3-4 gear teeth, sharp profiles or inside configurations
may be used in lieu of actual parts. The representative specimen shall be fabricated from the same steel alloy,
shall be similar in configuration, surface condition (roughness) and geometry, and shall have the same
processing history (including hardening, tempering, masking) as the parts to be represented. They shall be
placed in an area that represents the surface that requires ion nitriding. Tests as in 4.2.1 shall be performed to
establish that these specimen characteristics are representative of the parts.

4.3.1.3.1 When established by testing in accordance with 4.2.1, at least two parts or representative parts located in the
high and low temperature areas may be used with round specimens approximately one inch diameter and
made of the same steel alloy and processing history to comprise the required number of specimens.

4.3.1.3.2 In nonrecurring loads (8.12.1) the representative specimens material may differ from the part material,
provided a correlation between the two materials has been established, and demonstrated.

4.3.1.3.2.1 Round specimens shall be approximately one inch (25 mm) diameter and 0.25 to 0.31 inch (6 to 8 mm)
thick. The specimen shall be round and approximately one inch diameter and 0.25 to 0.31 inch (6 to 8 mm)
thick, the lot of material shall have a certification of chemistry and the surfaces shall be free of visual
oxidation and contamination.

4.3.1.4 Vessel loads containing multiple lots of parts shall have at least one representative specimen for each lot but not
less than four specimens per vessel load.

4.3.1.5 After nitriding all specimens are to be tested for compliance with the requirement and identified to the vessel
load and product lot. If a significant procedural change has not occurred in accordance with 4.4.3 after three
runs that meet the requirements, one less sample (in accordance with 4.3.1 and 4.3.1.1) may be run and tested.
The remaining specimens shall be placed in locations shown to represent the high, mid-range, and low
temperature areas.

4.3.2 Periodic testing

When a renitriding (rework) cycle is required, segments of all the original specimens shall be included in the rerun After
renitriding, segments shall meet the requirements of 4.3.1.

4.4 Approval

4.4.1 Processors (Subcontractors)

Approval of a processing facility shall be in accordance with the requirements of this specification. The heat treating
processor shall have a copy of his shop procedures available for the cognizant engineering organizations. It shall include a
full description of all equipment and procedures that are used to process parts to this specification.

4.4.2 Personnel

Qualification of personnel performing heat treating and associated operations shall be trained and approved in accordance
with a procedure such as ARP1962.

4.4.3 If the processor makes a significant change to any material, process, or control factor from that which was used
for process approval, all preproduction tests shall be performed and the results submitted to the purchaser for
process reapproval unless the change is approved by the cognizant engineering organization. A significant change
is one in which, in the judgment of the cognizant engineering organization, could affect the properties or
performance of the parts.
SAE AMS 2759/8A -8-

4.5 Log

A record that is written or electronic storage media shall be traceable to and retained for each vessel load. The information
on the combination of documents shall contain the following: Part number, number of parts, type of material, equipment
number, temperatures used and actual processing times, required hardness, vessel pressure, gas mixture, pump down
and leak up obtained and date.

4.6 Records shall include vessel logs, recorder charts, all other shop records, and all test and inspection records. They
shall be kept available to the cognizant quality assurance organization for five years after the heat treament unless
otherwise required by the cognizant engineering organization.

4.7 Reports/Certification

A certified quality assurance report shall be furnished with each shipment of parts, shall be traceable to the heat treat
control number(s), and state the parts were processed in accordance with AMS 2759/8. The report shall include purchase
order number, part number, alloy, quantity of parts in shipment, identification of vessel used, actual test results, the
requirement, and a statement of conformance or nonconformance to requirements. The data shall be reported in
accordance with the heat treaters documented procedures.

5. PREPARATION FOR DELIVERY

Identification, protective treatment, and packaging shall be in accordance with AMS 2759 or as acceptable to the cognizant
engineering organization.

5.1 Identification

Identification shall be maintained on parts during shipping.

5.2 Packaging

5.2.1 When specified by the procuring activity, parts shall be protected with corrosion preventative compound during
shipping.

5.2.2 Parts shall be packaged in accordance with commercial practices and in compliance with applicable rules and
regulations pertaining to the handling, packaging and transportation of parts to ensure carrier acceptance and safe
delivery.

6. ACKNOWLEDGMENT

The processor shall mention AMS 2759/8A in all quotations and when acknowledging purchase orders.

7. REJECTIONS

Parts not meeting requirements of this specification or modifications authorized by the cognizant engineering organization
will be subject to rejection.

8. NOTES

8.1 A change bar (|) located in the left margin is for the convenience of the user in locating areas where technical
revisions, not editorial changes, have been made to the previous issue of a specification. An (R) symbol to the left of
the document title indicates a complete revision of the specification, including technical revision. Change bars and
(R) are not used in original publications, nor in specifications that contain editorial changes only.
SAE AMS 2759/8A -9-

8.2 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 ion nitriding.

8.2.1 The workpieces to be ion nitrided are suspended or placed in a vacuum vessel in such a way that there is an
effective isolation from the anode. Together with the vacuum pump, the gas distribution system enables the vessel
to be evacuated, filled with the appropriate treatment gas, and maintained at the required vacuum level while
retaining a constant gas flow, usually between 13.3 to 1333 Pa (0.1 to 10 Torr).

8.2.2 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 vessel , the former being connected as the cathode and the latter
as the anode. Under this potential, the molecules and atoms of the treatment gas are excited and ionized,
producing the typical luminous phenomenon known as glow discharge around the exposed surfaces of the
workpieces.

8.2.2.1 When copper plating, paste, or paint is used for masking, glow discharge voltage, current, and pressure should
be limited and monitored during the entire cycle.

8.2.3 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.

8.2.4 The temperature of the workpiece is measured with the aid of thermocouples and/or infrared instruments and
regulated by means of a controller varying the power output of the electric unit. The treatment temperature is, in
most cases, set between 750 and 1110 F (399 and 599 C), depending on the composition and structure of the
steel to be treated, as well as the stress which the workpiece will have to resist.

8.2.5 Effects of Nitriding Atmosphere on Type of Compound Layer Produced

The type of nitride layer produced is mainly influenced by the gas composition as well as the composition of the 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.
Presence of oxygen may also lead to an epsilon phase. The following are suggested minimum levels of nitrogen in the
input gas:

8.2.5.1 Low-alloy steels containing up to 5% nominal alloying elements by weight should have 5% nitrogen by volume,
to ensure at least a diffusion zone.

8.2.5.2 High alloy, corrosion resistant, and tool steels (steels with more than 5% nominal alloying elements by weight)
should have 15% nitrogen by volume.

8.2.5.3 When a compound layer is required, a 25% nitrogen by volume is suggested, unless otherwise determined by
preproduction tests.

8.2.6 Titanium alloys, and nickel alloys are ion nitrided. Ion nitriding of these alloys is typically performed in accordance
with instructions from the cognizant engineering organization.

8.3 Types of Surface Layers

Ion nitriding, unlike the other nitriding processes, may produce ion nitrided layers or zones with a compound layer or
without a compound layer.
SAE AMS 2759/8A - 10 -

8.3.1 Diffusion Zone

In the steel itself, nitrogen diffuses according to classical principles, producing a hardened zone by precipitation and solid
solution hardening. This is known as the diffusion zone and may be detected as an etched 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.

8.3.2 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 also called white layer.

8.4 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.

8.5 Ion nitriding can be used to process a wide variety of steels. Table 1 shows typical results that can be achieved for
various steels.

8.6 Hollow 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.

8.7 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 to
chip.

8.8 To differentiate between the types of nitrides produced in the white layer, the following metallographic procedure
may be used to make evident the phases of a compound layer:

8.8.1 To make an etching reagent (Marble's Solution) it is recommended that the following should be added to the
mixing vessel in the following order while being continuously stirred.

50 mL Water
50 mL Ethyl Alcohol (Ethanol)
50 mL Hydrochloric Acid
2 grams Copper Sulfate

8.8.2 Application

After normal metallographic preparation and etching in nital (3% nitric acid in ethyl alcohol), the compound layer, if present,
does not etch and stays white at this stage. It is useful to take a photomicrograph of the nital etched surface for
comparison with the Marble's etched surface produced next. Repolish and then hold for a second in the Marble's Solution
(by immersion, not swabbing).

8.8.3 Interpretation of Results

There may be three phases present:

8.8.3.1 If the compound layer remains white, an epsilon phase is present.

8.8.3.2 A black compound layer means a gamma prime phase is present.

8.8.3.3 A black-white layer means a mixture of epsilon phase and gamma prime phase is present.
SAE AMS 2759/8A - 11 -

8.8.3.3.1 With mixed phase, one can occasionally observe that the portion of one or the other phase is more strongly
represented. There can also be two layers present, one over the other.

8.9 Test for Compound Layer Presence

To detect the presence of compound layer on steel parts, a copper sulfate solution may be used, as follows:

8.9.1 Composition

40 grams copper sulfate (CuS045H20)

1000 mL water
5 mL wetting agent
3.9 to 4.1 pH

8.9.2 Application

Areas to be tested shall be cleaned and then swabbed with the solution of 8.9.1. The solution should be left on the surface
for at least 30 seconds.

8.9.3 Interpretation

Copper will not plate on surfaces containing a continuous compound layer. If a copper color occurs in 30 seconds or less,
no compound layer is present.

8.10 Representative treatments and results of ion nitriding for various materials are listed in Table 1.

8.11 Copper (AMS 2418), bronze (AMS 2429), nickel or other plates that require chemical stripping are the least
desirable methods.

8.12 Terms used in AMS are clarified in ARP1917 and as follows:

8.12.1 Nonrecurring Load

Customer has not notified processor that future lots of these parts are expected to be nitrided.

8.13 Dimensions and properties in inch/pound units and the Fahrenheit temperatures are primary; dimensions and
properties in SI units and the Celsius temperatures are shown as the approximate equivalents of the primary units
and are presented only for information.

8.14 Purchase documents should specify not less than the following:

AMS 2759/8A
Size of parts
Quantity of parts
Part number or product identification
Steel alloy designations
Heat treating operations required
Hardness, case depth, compound layer type and thickness.

PREPARED BY AMS COMMITTEE "B" AND AMEC

SAE AMS 2759/8A - 12 -

TABLE 1 - TYPICAL RESULTS OF ION NITRIDING FOR STEELS

Surface
Hardness Thickness of
Core Tensile Temperature HRC Compound Layer
Strength Nitriding (equivalent HV) Total Case Depth Inch x10
4
Most Common
Range Treatment After inch (mm) After (Micron) After Compound Layer After
Steel Group ksi (MPa) F (C) Ion Nitriding Ion Nitriding Ion Nitriding Ion Nitriding
LOW ALLOY
STEELS
AISI 9310 or 9315 80 - 102 970 - 1020 49 - 58 0.012 - 0.028 0.160 - 3.15 Fe4N or Fe4N+Fe2-3 N
(552 - 703) (521 - 549) (500 - 653) (0.30 - 0.71) (4 - 8)
AISI 4140 or 4340 138 - 160 950 - 1020 52 - 58 0.008 - 0.024 1.60 - 3.15 Fe4N or Fe4N+ Fe2-3N
(951 - 1103) (510 - 549) (550 - 653) (0.20 - 0.61) (4 - 8)

NITRIDING STEELS
Nitralloy 135M 125 - 150 950 - 1020 67 0.008 - 0.020 0.8 - 3.95 Fe4N or Fe4N+Fe2-3N
(862 - 1034) (510 - 549) (900 - 1150) (0.20 - 0.51) (2 - 10)

STAINLESS &
HEAT
RESISTANT STEEL
AISI 436 116 - 138 1020 - 1060 68.5 0.004 - 0.008 1 Fe4N or Fe4N+Fe2-3N
(800 - 951) (549 - 571) (950 - 1100) (0.10 - 0.20) ( 25)
AISI 304 73 - 102 1020 - 1075 62 - 66 0.002 - 0.004 1 None, Fe4N +
austenite, or
(503 - 703) (549 - 579) (745 - 865) (0.10 - 0.10) ( 25) Fe4N+Fe2-3N

TOOL STEELS
AISI H-13 -- 840 - 1060 67 0.004 - 0.012 0.8 - 2.35 None or Fe4N
(449 - 571) (900 - 1150) (0.10 - 0.30) (2 - 6)
AISI M-2 -- 900 - 975 69 0.001 - 0.002 1 NONE or Fe4N

(482 - 524) (1000 - 1250) (0.03 - 0.05) ( 25)

PRECIPITATION
HARDENING
ALLOY
17-4 PH 140 - 155 900 - 975 62 - 66 0.004 - 0.008 1 NONE or Fe4N
(965 - 1069) (482 - 524) (745 - 865) (0.10 - 0.20) ( 25)