Nitriding Nitrocarburizing Complying To Automotive Aerospace Specs

Nitriding / Nitrocarburizing complying to automotive & aerospace specs.
Nitriding / Nitrocarburizing
Measurement and control complying

to automotive and aerospace
specifications
Jens Baumann
PROCESS-ELECTRONIC GmbH
About United Process Controls Group
Process-Electronic is a member of United Process Controls Group

combining the expertise in heat treatment controls and automation of
Furnace Control Corp. Sensors & Analyzers
Marathon Monitors Inc. Sensors & Controls
Process-Electronic Sensors, Controls &

Management Systems
Waukee Engineering Flow Controls,
Compressors,
Endogas & Direct Injection
Page 2
Agenda
1. Nitriding / Nitrocarburizing
2. AMS 2750 Pyrometry
3. AMS 2759/6
4. AMS 2759/10
5. AMS 2759/12
6. AIAG CQI-9 specifications
Graph: UPC Nitriding Solution Package

Page 3
Scope of Nitriding and Nitrocarburizing is to enhance work properties of treated parts by

introducing Nitrogen (when Nitriding) and Nitrogen and Carbon (when Nitrocarburizing) in
the surface layer of iron and its alloys.
Nitriding / Nitrocarburizing is
typically performed at a process
temperature between 490C and
590C, below AC1 in the
Fe-N-Phase Diagram of the
material to be treated.
At low temperature solubility

of Nitrogen is only little,
resulting in formation
of iron (carbo)nitrides.
Diagram: H.A. Wriedt, N.A. Gocken and R.H. Nafziger, 1987
Page 4
While Nitriding is typically aiming for a comparably deep

hardened case caused by Nitrogen diffusing into the iron
lattice and forming nitrides with nitride forming alloying
elements, such as Chromium, Titanium, Aluminum etc.
Nitrocarburizing is typically aiming for a compound layer of

Fe2-3N or Fe4N iron nitrides of high hardness, increasing
corrosion resistance and lowering the coefficient of friction.
Micrographs: IWT Bremen, Germany

Page 5
A typical equipment used for Nitriding comprises of a retort furnace, a process gas supply
offering Ammonia, dissociated Ammonia and Nitrogen.
For Nitrocarburizing there has to be at least one additional gas line providing a Carbon
bearing gas such as Carbon Dioxide.
Both processes require perfectly cleaned but also chemically activated (better to say
depassivated )parts, which is often achieved by a pre-oxidation stage.
In order to enhance chemical resistance of the

compound layer even further, Nitrocarburized
parts are often additionally oxidized. So-called
post-oxidation applies a Magnetite layer on top
of the compound layer.
Graph: IWT Bremen, Germany

Page 6
A Nitriding installation comprises of:
1) Gas tight furnace

2) Power, control and gas cabinet
3) Gas supply system
4) Ammonia dissociator
5) Exhaust gas burner
6) Racking
7) Closed-loop water cooling systems
Schema: Nitrex Metal Inc., Canada

Page 7
Controlling a Nitriding Installation requires:
1) Furnace temperature control

2) Nitriding atmosphere control
3) Gas flow control
4) Safety Loops
5) Local capability of performing recipes
Graph: Main Control Screen UPC Nitriding Solution Package

Page 8
Specifications applying to Nitriding and Nitrocarburizing
AMS 2750 Pyrometry

AMS 2759-6 Gas Nitriding and Heat Treatment
of Low-Alloy Steel Parts
AMS 2759-10 Automated Gaseous Nitriding Controlled
by Nitriding Potential
AMS 2759-12 Gaseous Nitrocarburizing, Automatically
Controlled by Potentials
CQI-9 Heat Treatment Assessment Forms
Page 9
AMS 2750 issued 1980, actual version E since July 2012
Photograph: Heating elements of two zone pit type furnace

Page 10
AMS 2750 specifies

furnace temperature uniformity best
achieved by cascaded temperature
control but also
sensors and instrumentation

accuracy
Graph: Temperature Control Screen UPC Nitriding Solution Package
Page 11
AMS 2750 E requires

Multi-point calibration for all connected thermocouples
Graph: Furnace View & Thermocouple Calibration Screen UPC Nitriding Solution Package
Page 12
AMS 2759/6 issued 1987, actual version B since November 2011
Photograph: Pit type nitriding installation

Page 13
AMS 2759/6 specifies
Maximum allowed for compound layer thickness of nitrided parts
Class 1: 13 m
Class 2: 25 m
Independent from the aimed for case depth,

using Ammonia based only atmospheres and
controlling Dissociation.
D = 100% - residual Ammonia in exhaust

Schema: Weissohn, K.H.
Page 14
AMS 2759/6
By using Ammonia based atmospheres only

Dissociation defined as 100% - R-NH3 can be determined by
D = 4/3 * H2 percentage in exhaust

Visible indication of
- atm. Potential
- Sampling gas flow
Data and alarm interfaces

- Analog / digital
- Modbus RTU
- TCP/IP
- CAN
- Webserver
Analyzer: H2Smart, United Process Controls Group

Page 15
AMS 2759/6 requires excellent temperature uniformity
Consequently equipment used must comply to furnace class 3 and

better according to AMS 2750
Page 16
AMS 2759/6 requires use of flow controllers
Visible indication of
- Gas flow
Manual overwrite
Data and alarm interfaces

- Modbus TCP
- Webserver
Flow Controller: Waukee Engineering, a member of United Process Controls Group
Page 17
AMS 2759/6 use of Ammonia dissociator is recommended
Different types
- horizontally
- vertically
- various flows
Photograph: Ammonia dissociator

Page 18
AMS 2759/6 requires atmosphere uniformity
Converts to * 5% = 3.75% of H2
Photograph: H2 analyzer mounted close to a nitriding furnace

Page 19
AMS 2759/6 typical process setup
Process may be performed in

one or two stages, temperature
in first stage is typically lower
to temperature in second
stage (Floe-Process).
Graph: Winter, K.-M.
Page 20
AMS 2759/10 issued 1999, actual version A since June 2006
Photograph: Fully automated nitriding line

Page 21

Maximum allowed for compound layer thickness of nitrided parts
Class 0: no CL permitted
Class 1: 13 m
Class 2: 25 m
Independent from the aimed for

case depth, controlling Nitriding
Potential.
KN = pNH3 / p3/2H2
Allowing use of Ammonia Nitrogen

gas mixtures!
Graph: Lehrer Diagram Screen UPC Nitriding Solution Package
Page 22
AMS 2759/10 requires use of anhydrous Ammonia and Nitrogen
Purity grades of 3.8 and better is comparably easy to accomplish
but
Dew Point has to be below -48C !

Portable Dew Point Analyzer: Furnace Control Corp., a member of United Process Controls Group
Page 23
AMS 2759/10 Table defining nitriding potentials
has to be interpreted as:
KN setpoints depending on
temperature, process stage
and aimed for compound
layer thickness
Page 24
AMS 2759/10 Nitriding potentials for AISI 4140 at 548C
Nitriding potential has to be controlled within +/- 10% of setpoint,

Temperature throughout load has to stay within given furnace class
tolerances.
Diagram: Winter, K.-M., How do allowed for tolerances affect nitriding / nitrocarburizing results ?, Presentation at Nitriding Seminar 2013, Las Vegas, USA
Page 25
AMS 2759/10 Allowing for nitrogen diluted atmospheres
theoretically requires to measure NH3 plus H2.
As gas flows have to be monitored (and controlled) it is also possible to

measure hydrogen and take the gas flows on the inlet into account.
NH3 Dissociation
d-NH3 Nitriding Potential
N2
etc.
Photograph: Gas cabinet for nitriding and nitrocarburizing installation
Page 26
AMS 2759/12 issued 2007
Photograph: box type nitrocarburizing furnace Nitrex USA

Page 27

Percentage of allowed for porosity on nitrocarburized compound layer
Class 1: P 15 %
Class 2: 10 % P 50 %
By concurrently controlling
KN = pNH3 / p3/2H2 and
KCB = pCO / pCO2
Percentage porosity is defined as:

P = porous (D2) / total (D1) compound layer thickness * 100%
Page 28
AMS 2759/12 is using the effect that

Porosity can be influenced by compound layer composition
N = 8.0 wt% N = 7.6 wt% N = 7.2 wt%

C = 0.5 wt% C = 1.0 wt% C = 1.6 wt%
1010, 1010, Sample 1 1010, Sample 2
N = 7.0 wt% N = 6.5 wt% N = 7.0 wt%

C = 2.4 wt% C = 3.1 wt% C = 3.5 wt%
1010, Sample 3 1010, Sample 4 1010, Sample 5
Figure: Winter, K.-M., Phase Controlled Gaseous Nitriding and Nitrocarburizing, Presentation at FNA 2007, Detroit, USA
Page 29
AMS 2759/12 Table defining nitriding and carburizing potentials
has to be interpreted as:

KN / KCB setpoints depending
on temperature, process stage
and aimed for compound
layer thickness
Page 30
AMS 2759/12 Selected pairs of KN and KCB

are always aiming to achieve Epsilon Carbonitrides with defined
percentages of Nitrogen and Carbon in the compound layer.
KN and KC(Boudouard) to build iso-concentration lines in Epsilon

Preferred Ratio C/N 0.02 0.12 0.2
R 8.314410 N+C 8.60 N 8.43 6.50 7.17
Temp [C] 575 N+C 7.30 C 0.17 0.80 2.10
wt%N wt%C wt%Fe zFe zN zC Sz at%Fe at%N at%C

6.50 0.80 92.70 1.66 0.46 0.07 2.19 75.7750823 21.1843313 3.04058642
75.7750823 21.1843313 3.04058642
KN KCB AC yFe yN yC
0.76 0.12 2.63 1 0.27956857 0.04012647
Weight% to Atomic %
KCW Atomic % to Fraction
0.33
Test
KCW 0.10 %N 6.50%
AC 0.76 %C 0.80%
KCB 0.04
Graph: NICARM Diagram Screen UPC Nitriding Solution Package, calculation based on Kunze
Page 31
AMS 2759/12 controlling KN and KC concurrently
theoretically requires to measure NH3, H2, CO and CO2.
As gas flows have to be monitored (and controlled) we can derive

potentials from measuring Hydrogen and Oxygen
NH3 Dissociation
d-NH3 Nitriding Potential
CO/Endo Carburizing Potential
CO2
N2
Page 32
AIAG CQI-9 issued 2006, actual Version 3rd Edition, Oct. 2011
Page 33
AIAG CQI-9 Heat Treat System Assessment

Section 1 Management Responsibility & Quality Planning
The heat treater shall have written process

specifications for all active processes and identify
all steps of the process including relevant
operating parameters. Examples of operating
parameters include process temperatures, cycle
times, load rates, atmosphere or gas flow
settings, belt speeds, quench agitation speeds,
Is there arecipes
99 internal written process
etc. Such parameters shall not only be defined,
1.6 specification for all active
32 stages per recipe
processes?
they shall have operating tolerances as defined
by the organization in order to maintain process
control.
All active processes should have a written
process specification.
These process specifications may take the form
of work instructions, job card, computer-based
recipes, or other similar documents.
Graph: Recipe Screen UPC Nitriding Solution Package

Page 34

The heat treater shall have written process

specifications for all active processes and identify
all steps of the process including relevant
operating parameters. Examples of operating
parameters include process temperatures, cycle
times, load rates, atmosphere or gas flow
settings, belt speeds, quench agitation speeds,
Is there a written process
etc. Such parameters shall not only be defined,
1.6 specification for all active
they shall have operating tolerances as defined
defined tolerances for processes? by the organization in order to maintain process
all process parameters control.
All active processes should have a written
process specification.
These process specifications may take the form
of work instructions, job card, computer-based
recipes, or other similar documents.
Graph: Recipe Stage Screen UPC Nitriding Solution Package

Page 35

Process control parameters shall be monitored

per frequencies specified in Process Tables.
Are process control Refer to Process Tables, Section 3.0. Computer
parameters monitored per monitoring equipment with alarms and alarm logs
2.14
frequencies specified in satisfy the verification requirement. A designated
Process Tables? floor person shall verify the process parameters,
e.g., by initialing a strip chart or data log.
Management review is required per Question 1.9.
built-in chart recorder to

display up to 64 pens in
8 charts
Graph: Chart Recorder Screen UPC Nitriding Solution Package

Page 36

The heat-treat furnaces, generators, and quench
systems shall have proper process controls and
related equipment. Examples include
Do furnaces, generators, and
temperature, carbon potential/dew point, gas
3.1 quench systems have proper
flows, quench monitoring system including
process control equipment?
agitation, temperature control and quenching oil
analysis, etc. as listed in the applicable Process
Tables, Section 1.0.
Generator control including

- Temperature
- Carbon potential
- Gas and air flows
Photograph: Lambda measuring block and control and power cabinet endo generator United Process Controls Group
Page 37

The variation between the furnace-control

Is the variation of the furnace
thermocouple and the set point temperature shall
controlled thermocouple from
be within the limits defined in the applicable
3.5 set point within the
Process Tables, Section 2.0. This does not apply
requirements in the Process
to the first zone of a multi-zone continuous
Table?
furnace.
Tolerance band violations

will automatically raise an
alarm message and initiate
visual and acoustic alarm
Graph: Alarms Screen UPC Nitriding Solution Package

Page 38

The atmosphere control system shall maintain

the atmosphere dew point/carbon potential set
point within the parameters specified in the
control plan or internal procedures. The heat
treater shall have a back-up method of checking
the carbon potential/dew point. Examples are
dew point, electrical wire resistance, gas
analysis, shim stock, carbon bar, etc. The
automatic and continuous atmosphere control
system shall consist of sensors such as oxygen
probes or on-line Infrared (IR) gas analysis. See
Process Table A, Sect. 3.0 for verification
frequencies.
Portable 3-Gas IR Analyzer and Dew Point Analyzer: Furnace Control Corp., a member of United Process Controls Group
Page 39

Modular flow meter and

flow control equipment
allows for configuration
tailored to customer needs
and easy upgrade
Flow Meter and Flow Controller: Waukee Engineering, a member of United Process Controls Group
Page 40
PROCESS TABLE B - Nitriding (Gas) and Ferritic-Nitrocarburizing (Gas or Salt)
Item # Related Category/Process Steps Batch Continuous Generators Salt Bath

HTSA Furnace Furnace*
Question #
B1.1 3.1 All furnaces, generators and quench systems shall Yes Yes Yes Yes
3.7 have temperature indicating instruments.
B1.2 3.1 Continuous strip charts and/or data loggers are Yes Yes Yes Yes -
3.7 required for temperature and carbon monitoring unit, For
e.g., dew point, oxygen probe, IR gas analyzer, etc. temperature
only
B2.1 3.2 Thermocouples and calibration of thermocouples Yes Yes Yes Yes
3.3 shall conform to AMS 2750D.
B2.2 3.2 Instrument Calibration per AMS 2750D shall be Yes Yes Yes Yes
3.3 quarterly at a minimum.
Frequency reductions per AMS 2750D are not

allowed.
B2.5 3.5 Recorded temperature(s) shall be controlled within Yes Yes - In ----- Yes
+/- 9C (or +/- 15F) of the set point as evidenced by Qualified Work
continuous recording pyrometers. Furnace Zone
temperature shall be controlled with soak times
starting at the lower tolerance limit (as defined
above).
Page 41

Question #
B3.1 1.4 Monitor primary temperature control instrument(s). Each batch Each lot or Each Shift Every 2 hours
2.14 or continuous continuous & after any
recording recording with change
with sign-off sign-off every 2
every 2 hours. Alarm
hours. Alarm systems satisfy
systems the sign-off
satisfy the requirement
sign-off
requirement
SCADA: Protherm 9800 Heat Treat Management System Process-Electronic, a member of United Process Controls Group
Page 42

Question #
B3.3 1.4 Monitor primary furnace atmosphere control(s). Each batch Continuous ----- Daily
2.14 (rotary recording with
3.7 furnaces sign-off every 2
only) or hours. Alarm
continuous systems satisfy
recording the sign-off
with sign-off requirement
every 2
hours. Alarm
systems
satisfy the
sign-off
requirement
B3.4 1.4 Dissociation of ammonia shall be checked in gas Each batch Every 4 hours Daily N/A
3.7 nitriding. and every 4
hours
minimum
B3.5 1.4 Gas ratios for ferritic nitrocarburizing shall be Each batch Every 2 hours
3.7 checked. minimum
Page 43

Question #
B3.8 1.4 Monitor time in furnace, cycle time or belt speed. Each batch Twice/shift & ----- Each batch
2.14 after any change
in the belt
speed.
B3.9 1.4 Monitor load size or fixturing or loading rate as Each batch Twice/shift & ----- Each batch
2.7 applicable. after any change
in loading rate.
Modular heat treatment

management system
stores all load related data
in SQL database.
Data retrievable by various

keys and tokens.
Page 44
Thank you for your attention!
Questions?
Page 45

Nitriding Nitrocarburizing Complying To Automotive Aerospace Specs

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Nitriding Nitrocarburizing Complying To Automotive Aerospace Specs

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Nitriding / Nitrocarburizing complying to automotive & aerospace specs.

Measurement and control complying

About United Process Controls Group

Process-Electronic is a member of United Process Controls Group

Furnace Control Corp. Sensors & Analyzers

Marathon Monitors Inc. Sensors & Controls

Process-Electronic Sensors, Controls &

Graph: UPC Nitriding Solution Package

Scope of Nitriding and Nitrocarburizing is to enhance work properties of treated parts by

At low temperature solubility

While Nitriding is typically aiming for a comparably deep

Nitrocarburizing is typically aiming for a compound layer of

Micrographs: IWT Bremen, Germany

In order to enhance chemical resistance of the

Graph: IWT Bremen, Germany

A Nitriding installation comprises of:

1) Gas tight furnace

Schema: Nitrex Metal Inc., Canada

Controlling a Nitriding Installation requires:

1) Furnace temperature control

Graph: Main Control Screen UPC Nitriding Solution Package

Specifications applying to Nitriding and Nitrocarburizing

AMS 2750 Pyrometry

AMS 2750 issued 1980, actual version E since July 2012

Photograph: Heating elements of two zone pit type furnace

AMS 2750 specifies

sensors and instrumentation

AMS 2750 E requires

AMS 2759/6 issued 1987, actual version B since November 2011

Photograph: Pit type nitriding installation

AMS 2759/6 specifies

Maximum allowed for compound layer thickness of nitrided parts

Independent from the aimed for case depth,

D = 100% - residual Ammonia in exhaust

By using Ammonia based atmospheres only

D = 4/3 * H2 percentage in exhaust

Data and alarm interfaces

Analyzer: H2Smart, United Process Controls Group

AMS 2759/6 requires excellent temperature uniformity

Consequently equipment used must comply to furnace class 3 and

AMS 2759/6 requires use of flow controllers

Data and alarm interfaces

AMS 2759/6 use of Ammonia dissociator is recommended

Photograph: Ammonia dissociator

AMS 2759/6 requires atmosphere uniformity

Photograph: H2 analyzer mounted close to a nitriding furnace

AMS 2759/6 typical process setup

Process may be performed in

AMS 2759/10 issued 1999, actual version A since June 2006

Photograph: Fully automated nitriding line

AMS 2759/10 specifies

Independent from the aimed for

Allowing use of Ammonia Nitrogen

AMS 2759/10 requires use of anhydrous Ammonia and Nitrogen

Purity grades of 3.8 and better is comparably easy to accomplish

Dew Point has to be below -48C !

AMS 2759/10 Table defining nitriding potentials

has to be interpreted as:

AMS 2759/10 Nitriding potentials for AISI 4140 at 548C

Nitriding potential has to be controlled within +/- 10% of setpoint,

AMS 2759/10 Allowing for nitrogen diluted atmospheres

theoretically requires to measure NH3 plus H2.

As gas flows have to be monitored (and controlled) it is also possible to