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Company Standard
Tufftride Q DO/200/026
Surface hardening 2010-08-02

Issue P ERF 8461

Preamble
This company standard specifies a surface treatment process applicable to components designed or
specified by the Glenrothes plant of Bosch Rexroth, Hydraulics division, Drives group (DCH-DR) for use in
radial piston hydraulic motors.

Section 6 specifies the method to be employed for Tufftride Q treatment. Section 7 outlines the quality
assurance criteria and measures that should be fulfilled by contractors approved for this treatment.

1. Aims
• To specify an approved process for the treatment of components formed from ferrous or nickel-based
metals containing ≥25% iron by liquid salt-bath nitrocarburising at sub-critical temperatures.
• To define an assessment framework and criteria for the approval of contractors to undertake application
of Tufftride Q on behalf of Bosch Rexroth, Glenrothes, comprising the basic Tufftride Q process (sections
5, 6) and the supporting quality management systems (sections 7, 8).

2. Scope
© Bosch Rexroth AG 2009

This standard only applies to those components where the Rexroth component drawing, specification or
standard calls for its use. This includes use as a substitute for gas nitriding per Bosch Rexroth specification
DO/200/020 – refer to Section 9 below.

3. Responsibilities
The Engineering Department at Bosch Rexroth Glenrothes (DCH-DR/ENR) is responsible for the
preparation and maintenance of this standard.

4. Commercial arrangement
The term “Tufftride” is used in this standard to cover a single proprietary process, which carries different
brand names in different geographic locations for commercial and historical reasons.

Tufftride: Brand name for a liquid salt bath nitrocarburising process in the UK, various English-
speaking countries and Asian countries.
Tenifer: Brand name for the Tufftride process in Germany and other European countries.
Melonite: Brand name for the Tufftride process in North America.

For all countries, independent of the local brand name, commercial responsibility for “Tufftride” processes
rests with the national subsidiary of Durferrit GmbH or its parent company, HEF Groupe.

The contractor must ensure that their selected process follows the principles of Tufftride Q and must
maintain the appropriate technical and commercial relationships with the HEF/Durferrit subsidiary company
holding national authority for “Tufftride” processes.

Alternative liquid salt-bath nitrocarburising technologies, which may be covered by brand names not listed
above and/or not supplied by HEF/Durferrit, are outside the scope of this standard and may not be used in
substitution for Tufftride Q without the written authorisation of the Quality Manager, Bosch Rexroth
DO/200/026_EN_2010-08-02

Glenrothes.

Bosch Rexroth Ltd prepared: DCH-DR/ENR31, Kermode

Viewfield Industrial Estate Glenrothes, KY6 2RD approved: DCH-DR/ENR2, Haddow
Tel. +44 1592 631777 • Fax +44 1592 631888 released: DCH-DR/ENR, Dobbie
Additional information Page 1/19
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5. Effects of process
5.1 Nitrocarburising operation
Hardness profile: Surface hardness is increased, primarily due to the diffusion of nitrogen into the
surface (and to a lesser extent, carbon).
Compound layer1: A solid outer layer of iron nitride is formed, predominantly with an epsilon-nitride
structure (Fe3N). Alloying elements, if present, may also form nitrides. The outer
surface of the compound layer has a porous microstructure.
Diffusion zone: A region is formed directly beneath the compound layer, in which the concentration
of dissolved nitrogen decreases continuously with increasing depth.
Residual stress profile: The compound layer and diffusion zone contain a compressive residual stress.
Dimensions: Component dimensions are changed by the growth process inherent in the
formation of the compound layer. Unless otherwise stated, Bosch Rexroth
drawings specify dimensions post-treatment.

5.2 Quenching operation

Oxide layer: An outer layer of iron oxide is formed, predominantly of magnetite form (Fe3O4) and
with a characteristic black appearance. The formation of the oxide layer partially
fills the microscopic pores of the compound layer.
Passivation: The active chemical agents of the nitrocarburising operation are neutralized.

Within the scope of this standard, the quenching operation must be regarded as an integral part of the
Tufftride process, whether or not the process is defined under its full term “Tufftride Q”. The quenching
operation must not be omitted under any circumstances.

5.3 Application benefits

The physical and chemical properties of the component surface are changed by Tufftride Q treatment as
follows:
• The hard compound layer increases resistance to wear and fatigue, which is beneficial for surfaces
subjected to cyclical contact stress. Resistance to abrasive wear is increased.
• The predominantly epsilon nitride structure of the compond layer is more ductile and can withstand
higher Hertzian contact stress than the predominantly gamma-prime nitride structure (Fe4N) that may be
formed by alternative processes, e.g. gas nitriding, giving and improved resistance to adhesive wear.
• The residual compressive stress improves wear resistance by resisting micro-level crack propagation.
• The microscopic pores on the finished surface enhance the tribological performance by functioning as
micro-reservoirs for hydraulic fluid.
• The oxide layer acts as a solid lubricant, reducing the coefficient of boundary friction and reducing the
susceptibility to adhesive wear. This is particularly beneficial during initial running-in of the surface and
in conditions where the lubrication is marginal.
• Processing is carried out at sub-critical temperatures, avoiding thermally-induced changes to the
microstructure. This minimises the volume change and dimensional stability.
• Resistance to corrosion is improved by the low reactivity of the outer oxide and nitride layers (not
generally a significant benefit).

6. Method
6.1 Process specification (general)
The contractor’s method must be fully compliant with the latest process specification for the Tufftride Q
process, which is available from the following sources:

Durferrit UK Ltd Durferrit GmbH HEF USA

Wood Lane, Erdington Industriestrasse 3 2015, Progress Drive
Birmingham B24 9QL D-68169 Mannheim Springfield, OH 45505
United Kingdom Germany USA

Tel. +44 (0)121 382 6839 Tel. +49 (0)621 / 32 22 40 Tel. +1 937 323 2556
Email: enquiries@durferrit.co.uk Email: info@durferrit.com Email: sales@hefusa.net
Changes to the contractor’s method, including changes related to any of the points in Section 6, must be
approved by Bosch Rexroth prior to implementation. Refer to Section 8.4 for more details.

1
Compound layer may also be known as nitride layer, white layer or connection layer.
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6.2 Quality grades

In order to meet technical and commercial requirements, two distinct quality levels are defined for the
Tufftride Q process and effect. The Default quality grade is applicable unless otherwise stated on the
component drawing. A summary of the specific requirements for components requiring the ENHANCED
QUALITY grade is presented in Table 6.1.

Table 6.1 – Summary of Tufftride Q quality grades

Requirements (para) Default quality grade ENHANCED QUALITY grade
Handling of components (6.3) No specific requirement Pistons to be individually picked and placed
Compound layer sampling
Low sampling frequency Higher sampling frequency
frequency (7.2.3)
Compound layer specification Higher min. compound layer thickness
Compound layer thickness
(7.2.3) Incorporation of porosity spec.
TF1 bath composition (7.3.1) No specific requirement Compliant with Durferrit specification
Drawing specification (9) No specific requirement Drawing states “ENHANCED QUALITY”

6.3 Handling of components

It is essential to prevent damage to the finely toleranced and critical surfaces. Components are particularly
vulnerable at all stages up to and including the nitrocarburising process, during which the surface hardness
increases, reducing the risk of damage. Components must be handled with care during all stages of
treatment.

It is the responsibility of the contractor to identify any components showing unacceptable damage on
receipt, to segregate these components without further processing, and to make a report promptly to the
Quality Department at Bosch Rexroth Glenrothes. In the absence of such a report, Bosch Rexroth may
reject any components showing unacceptable damage post-Tufftride at the contractor’s liability.

It is the responsibility of the contractor to implement consistently the necessary measures for damage-free
handling, storing and transport of components, including loading into the Tufftride nitrocarburising bath, and
to make evidence of these measures available to Bosch Rexroth on request.

ENHANCED QUALITY PISTONS: Pistons must be individually picked and placed into the carrier by hand.
It is unacceptable to tip pistons in bulk into the carrier. Pistons must be
protected from impact damage to the outermost cylindrical surface.

6.4 Component preparation

6.4.1 Post-machining washing
It is essential to remove traces of cutting fluid and swarf and to add a corrosion-preventative surface film
prior to despatch for Tufftride Q treatment. Components must be washed according to standard process
work instructions as follows:
Pistons: WI-MAN-009
Cylinder blocks: WI-MAN-043 or WI-MAN-044 (as applicable)
Supplied components*: Supplier is responsible for controlling cleanliness of components
* Components for which a supplier to Bosch Rexroth is responsible for procuring the Tufftride Q treatment.

6.4.2 Pre-Tufftride washing

Components must be washed immediately prior to Tufftride Q treatment to minimise the possibility for
further contamination. Cleanliness criteria:
• Free of swarf, scale, oxide or any material picked up during storage and transit
• Dry i.e. free of oil, grease, water or other residue. Note: detergent residue is water-soluble.

Pre-washing must be carried out by complete immersion in an agitated bath containing an aqueous
solution at the manufacturer’s recommended concentration and temperature. The agitation of the cleaning
liquid and/or the components must be sufficient to cause turbulent flow of liquid over the entire surface of
the components. Critical process parameters for pre-Tufftride washing must be clearly indicated on a work
instruction.

Note: It is essential that the detergent separates oily residue to form a creamed emulsion (“skin”) on the
surface of the bath. This skin must be removed, e.g. by a weir arrangement, prior to the components being
raised out of the bath. Alternative detergents that form a dispersed emulsion may not be used.
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6.4.3 Loading into carrier

Components must be arranged and secured within an appropriately-designed carrier during treatment.

Depending on the contractor’s preferred method, the carrier may be loaded before or after the pre-washing
process (6.3.2 above). If the carrier is loaded after the components have been washed, it must have been
previously washed immediately prior to loading.

The design of the carrier, positioning of components and loading/handling method must be established by
trial and then standardised by means of a work instruction, in order to ensure:
• Adequate circulation of pre-heat air and salts around and through the treated components
• Minimal impact of treated components to each other, and to the carrier
• Specified maximum density of components (e.g. fill level per shelf) is not exceeded
• Components are not laid one on top of the other, and especially not with full contact of flat surfaces

The contractor’s work instruction must contain specific instruction for each design of component, as
required to ensure consistent process quality. This may include:
• Total number of parts per carrier tray/bracket
• Number of carrier trays/brackets in bath
• Arrangement of carrier trays/brackets in bath (stacking)

The contractor is responsible for carrying out process-development trials to ensure that all critical locations
on all components throughout the bath receive treatment uniformly within specification. Any necessary
countermeasures e.g. special settings to the agitation of the bath, or raising/lowering the carrier during
treatment, must be stated in the contractor’s quality control documentation.

6.4.4 Preheating
The function of preheating is to remove any water from the components, reduce thermal shock on loading
in the TF1 bath, and reduce the initial temperature dip of the TF1 bath.

Preheat the components in air after loading into the carrier. Parameters:
Air temperature: 350-400°C
Duration of preheat: To be fixed by process-development trial and stated in the contractor’s quality
control documentation.

Maximum preheat duration must be defined and controlled to ensure that no scaling occurs on the
component surface prior to TF1 treatment. It is acceptable for component surfaces to turn slightly blue
during the preheating but scaling is not permitted.

6.5 Nitrocarburising operation (TF1 bath)

Temperature of the TF1 bath must be controlled to 580 ±10°C.

After loading, the bath temperature dips then recovers due to the heating of the components and carrier as
shown by Figure 6.1. The controlled treatment time starts when temperature has recovered to the specified
level (soaking time). The initial dip in temperature must not exceed 40°C and the soaking time must not
exceed 30 minutes. If these requirements are not met, the contractor must notify Bosch Rexroth Glenrothes
Quality Department and quarantine all affected parts until disposition is authorised by Bosch Rexroth.

The controlled treatment time is specified as follows:

Material Nitrocarburising treatment time (TF1 bath)

Alloy and carbon steels 90 ±5 minutes
Spheroidal graphite iron and grey cast iron 165 ±5 minutes

At the end of the controlled treatment time, the carrier is transferred to the AB1 bath. It is acceptable to hold
the carrier over the TF1 bath to permit salt to flow back into the bath, but the total transfer time should not
exceed 30 seconds to prevent excessive cooling or incorrect oxidation.
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Bath
temperature Loading
Soaking time Controlled treatment time
≤30 minutes
580 ±10°C
Dip ≤40°C

Time
Figure 6.1

6.6 Quenching operation (AB1 bath)

Temperature of the AB1 bath must be controlled to 380 ±10°C.

The controlled treatment time is specified as follows:

Material Quenching treatment time (AB1 bath)

All materials 10 ±1 minutes

It is the responsibility of the contractor to ensure that the quenching operation is never omitted.

6.7 Cooling and washing

Air-cooling is essential to prevent formation of quench stresses, which may cause component failure. Air
cooling must not continue to room temperature because components cannot be washed effectively when
the salt solution has fully solidified.

Method:
1. Cool the components in air until the surface temperature is in the range 80-150°C.
2. Clean the components by immersion in agitated water using a multi-stage cascade arrangement with a
counter-flow arrangement i.e. the components are immersed in a series of baths containing
progressively cleaner water. Water temperature of the baths must be in the range 60-80°C.

6.8 Post-processing
6.8.1 De-watering fluid
De-watering fluid must not be applied.

6.8.2 Cleanliness standard

Cleanliness/contamination level on arrival at Glenrothes must meet the requirements of Bosch Rexroth
Glenrothes standard DO/200/30.

6.8.3 Packaging for shipment to Glenrothes

The contractor is responsible for the secure and damage-free condition of the treated components returned
to Bosch Rexroth Glenrothes.

In most cases it will be possible to reuse the packaging in which the components were delivered from
Bosch Rexroth Glenrothes. Components are generally packaged in robust plastic trays with formed
features matching the component geometry to locate, support and separate the components.

Original packaging should be checked prior to reuse and remedial action taken as follows:
• Damaged packaging should not be reused.
• Contaminated packaging may be reused following a suitable washing and drying process.

Damage and contamination to packaging can be prevented by making suitable arrangements for fully-
enclosed storage of the packaging while the components are being treated.

Damaged or contaminated packaging should be reported to the Quality Manager, Bosch Rexroth
Glenrothes. Packaging and shipment of parts should be postponed until suitable packaging is available.
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6.9 Extended process specifications

This basic Tufftride Q process specified by section 6 of this standard may be called by reference from other
Bosch Rexroth Glenrothes standards.

Note: the second “Q” (quench) process included within an extended QPQ treatment may have different
duration from the initial Q process specified in 6.6 above.

7. Quality assurance
7.1 General
The requirements of Section 7 do not preclude the contractor from carrying out their own quality-assurance
activities.

Appearance of treated components can indicate whether acceptable processing has occurred. Treated
surfaces shall have a continuous, uniform and non-blotchy appearance with a glossy, deep, black finish.
Appearance of the components should be assessed in clean condition i.e. before the application of de-
watering fluid per 6.8.1 above or after removal of de-watering fluid residue using Action Can TF-90 (or
equivalent).

7.2 Batch-level
7.2.1 Compound layer integrity check (“drop test“)
Purpose: The Drop Test verifies the presence of a homegeneous compound layer of iron nitride. It
can be used to determine broadly that a component has been through the TF1
nitrocarburising process.
Frequency: One component or one sample per batch

Method:
1. Identify a test location from Appendix 1.
2. Polish the test location using 800-grade lapping paper until the black oxide colour has just been
removed.
3. Degrease the test location using Action Can TF-90 aerosol solvent (or equivalent).
4. Apply a few drops of test liquid to the test location. Test liquid: aqueous solution of 4.2% NH4Cl +
5.4% CuCl. The test liquid has a distinctive blue-green appearance when new and should be
exchanged as soon as it degrades.
5. Wait for 2 minutes. Diagnosis:
If the solution turns BROWN-RED  FAIL
If the solution does not change colour  PASS
6. In the event of a PASS, immediately remove the test liquid from the surface of the component
using Action Can TF-90 aerosol solvent (or equivalent).

Response: Where one component from a batch fails the Drop Test, the entire batch must be
quarantined, and the Quality Manager at Bosch Rexroth Glenrothes must be notified as
soon as possible. Components passing the Drop Test may be returned to production stock.

7.2.2 Hardness test

Purpose: The Hardness Test verifies that the nitrocarburising process has been carried out and that
a basic quality level has been achieved.
Frequency: One component or one sample per batch.
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Method:
1. Identify a test location from Appendix 1.
2. Polish the test location lightly using 6µm diamond paste (or similar). Note: the purpose of polishing
is to remove the oxide layer around the test point to improve the contrast of the apparently darker
indentation mark.
3. Make three hardness test indentations using a Vickers indenter.
4. Calculate the arithmetic mean of the three measurements and record the result.

Key quality criteria are defined in Table 7.1.

Table 7.1 – Acceptance criteria for hardness tests

Mean hardness
Typical components Material Core condition
HV1 HV0.1
Cylinder blocks, all HD pistons,
Alloy steels Q+T to T 530-730 580-790
MCR15/20 LD pistons
Carbon steel BS970
Brake washers Q+T to S 450-650 500-700
070M55
Steel Distributors & MCR3/5
Other carbon steels Normalised
LD pistons 300-500 450-700
Cast Distributors SG Iron As cast

Response: All components failing the Hardness Test must be quarantined, and the Quality Manager at
Bosch Rexroth Glenrothes must be notified as soon as possible.
Components passing the Hardness Test may be returned to production stock.

7.2.3 Compound layer examination

Purpose: The photomicrograph examination provides essential characteristic data on the quality of
the heat treatment process.
Frequency: As specified in Table 7.2.

Table 7.2 – Minimum sampling frequency for compound layer examination

Component ENHANCED QUALITY DEFAULT QUALITY
Cylinder One cylinder bore, from One cylinder bore from one block every 2 weeks and a
blocks one block per batch. different size of block to be used each time. All block bore
sizes processed must be checked at least every 2 months.
Pistons One piston per batch. One sample component per week processed with a production
All other N/A batch, to be checked within 1 day of treatment. Over any 4-
component week period, the samples chosen must cover the full range of
types material grades processed.

Method:
1. Prepare a microsection at the standard location defined in Appendix 1.
2. Produce a photomicrograph of the microsection with a magnification of 500x, over a minimum
visible surface length of 100µm.
3. Assess the compound layer thickness and depth of porosity according to the following guidelines:

• Microsection and micrograph must meet the requirements of Bosch Rexroth Glenrothes DO/200/40.
• Measurements are preferably made automatically by the microscope control system to remove the
possibility for human error e.g. by incorrect selection of magnification.
• Measurement symbols should be distinctive i.e. with suitable size, thickness and colour to be easily
readable on the image whether viewed in isolation or embedded in a report document.
• Layer thickness and depth of porosity may vary locally. A minimum of two measurements each of layer
thickness and porosity, comprising the maximum and minimum measurements, should be indicated in
“balloons” on the micrograph.
• If available, the microscope system should insert a measurement reference graticule on to the image
with a suitable scale, e.g. 5 or 10 µm (not shown by Figure 7.1). The procedure for adding this graticule
should be mistake-proofed as far as possible.

Figure 7.1 below provides a worked example of compound layer quality assessment, compliant with most
of the above criteria. Refer to Appendix 3 for an additional go/no-go guideline.
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Key quality criteria are defined in Table 7.3. Materials may be identified using DO/400.

Table 7.3 – Quality specification – compound layer

Alloy steels
DEFAULT ENHANCED Carbon steels SG iron
Key parameters
QUALITY QUALITY
Compound layer thickness 10-20 µm 12-20µm 10-20µm 10-20µm (Note 1)
Depth of porosity (% of
N/A ≤40% N/A N/A
compound layer thickness)

Notes 1: Compound layer thickness for SG iron is measured remote to any graphite nodules that may be
present in the compound layer.

Step 1: Raw micrograph image Measurement balloons

(minimum number shown)
14 µm

Porous zone

Compound layer

Diffusion zone
Step 2: Identify boundaries
14 µm

Outer surface of part

Base of porosity

Base of compound
layer
Step 3: Read off representative measurements
14 µm

Cmin Pmax Pmin Cmax

Read off maximum and

minimum measurements for
both Compound layer thickness
and depth of Porosity

Figure 7.1
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Step 4: Calculation of key parameters

Cmax  Cmin Pmax  Pmin
Compound layer thickness = Depth of porosity =
2 2

In the event of a rejection per the requirements of Table 7.3, the contractor must:
• Halt all further Tufftride processing for Bosch Rexroth Glenrothes.
• Notify Bosch Rexroth Glenrothes Quality Department.
• Quarantine all affected parts until disposition is authorised by Bosch Rexroth Quality Department.
• Following adjustments to the process, all process parameters must be confirmed prior to restart.

7.2.4 Management of Quality Assurance data and results

Microsection specimens must be dated and stored on site for a minimum of 1 year. Micrograph images and
quality assurance reports should be stored in electronic form for a minimum of 5 years.

Periodic quality assurance reports must be produced no later than the despatch of the components to
Bosch Rexroth Glenrothes. Where such reports are specified to be communicated to Bosch Rexroth
Glenrothes, this should be accomplished by email to the Quality Manager no later that 3 working days
following the treatment of the components.

7.3 Monitoring and control of TF1 bath composition

7.3.1 Process specification
The bath composition must be maintained within the limits specified by Table 7.4. Limits specified for
ENHANCED QUALITY are consistent with the Tufftride Q operating instructions by Durferrit GmbH.

Table 7.4 – TF1 bath composition specification

Composition DEFAULT ENHANCED Significance for the Tufftride process
parameter QUALITY QUALITY
Cyanate (CNO-) No record 35-38% (with Active component of TF1 bath. Converted to CN- through
required evidence) the release of Nitrogen into the treated components.
Cyanide (CN-) No record ≤5% (with By-product of the nitrocarburising reaction. Converted
required evidence) back to CNO- by the addition of a “regenerator” (REG1).
Iron (Fe+) No record ≤0.02% (with Contaminant element, which causes harmful effects
required evidence) including excessive porosity of the compound layer.

The contractor is responsible for maintaining the composition parameters of all TF1 baths used for
treatment of components for Bosch Rexroth Glenrothes. For components treated to the Enhanced Quality
specifiction, evidence must be available to confirm the bath chemistry at the time of processing. Accuracy
(uncertainty) of the bath composition measurement system must be within the limits shown in Table 7.5.

Table 7.5 – Measurement accuracy for bath composition

CNO- ±0.5%
CN- ±0.3%
Fe+ ±0.005%

The temperature of the TF1 and AB1 baths should be recorded automatically by a datalogger system.
Minimum recording frequency: 1 sample per minute (mandatory while components are being treated).

Temperature and composition parameters must be recorded in an appropriate database system. The
contractor should be able to demonstrate competence in the entering and retrieval of data, the analysis of
trends, and the rapid identification of errors within the process control and quality control systems.

7.3.2 General compliance requirements

The quality of the compound layer is strongly influenced by the composition of the TF1 bath. Composition
control operations should therefore be treated as a real-time, preventative activity. The goal of controlling
the bath composition should be to prevent deviations outside the Tufftride process specification, not to
react to deviations.

Consistent procedures should be employed for sampling and analysing the bath composition. These
procedures should be standardised on appropriate work instructions.
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It is the responsibility of the contractor to control the bath composition within the limits stated in
Table 7.4 at all times when components are being treated for Bosch Rexroth Glenrothes.

It is strongly recommended that the contractor defines and applies “control limits” on critical parameters
and actively monitors the trends of these parameter values using an “original data chart” or similar 2.

In the event that a batch of components for Bosch Rexroth Glenrothes is treated with a TF1 bath that is
found to be outside specification in terms of the key composition variables (CNO- and Fe+) the following
actions must be undertaken:
• The entire batch of components must be kept at the contractor’s site and quarantined.
• A specimen component from the affected batch must be tested per 7.2 above.
• Composition data for the TF1 bath, temperature profile for the AB1 bath, micrograph and hardness data
must be reported to the Quality Manager at Bosch Rexroth Glenrothes who will decide on the necessary
actions, which may include initiating the Concession Request procedure.

7.3.3 Regeneration of Cyanate content

Cyanate content generally reduces over time. The rate of reduction is a function of several parameters:
Time: For a TF1 bath idling at 580°C with no components being treated, a reduction of 1-
2% per 24 hours may be expected.
Bath temperature: Bath temperature elevated above 580°C causes an accelerated decay of CNO-.
Loading/throughput: CNO- is consumed by the normal treatment process, so a lower cyanate
composition may be expected after the end of a standard treatment cycle.
Additionally, the quantity of the loading (number or total surface area of
components) may influence the rate of consumption.
Iron/sludge content: Loose iron particles consume cyanate parasitically. The rate of consumption can
be high because of the surface area to volume ratio of the small particles.

Cyanate content must be controlled within specification. Considerations:

CNO- above spec: Excessive porosity within compound layer, increasing component wear rate.
CNO- below spec: Compound layer too thin, and contains a greater proportion of detrimental gamma-
prime iron nitride.

Principles of CNO- bath composition control are illustrated by the following exemplary control charts:

Example 1: CNO- composition not adequately controlled

CNO- %
1b. Excessive TF1/REG1 addition
38

37
1a. Inadequate
control frequency 1c. Inadequate TF1/REG1 addition
35
Correction

Time
Figure 7.2

Explanation of Figure 7.2:

1a. Composition measurements are too infrequent, relative to the actual rate of change of
CNO- composition. The CNO- composition has already drifted out of specification before
the TF1/TF1/REG1 correction is applied.
1b. Due to an error in either the calculation or measurement of the TF1/REG1 regenerator
compound, the CNO- composition exceeds specification.
1c. Due to an error in either the calculation or measurement of the TF1/REG1 regenerator
compound, or due to the TF1/REG1 addition being omitted, the CNO- composition
continues to fall and soon becomes below the minimum specified level.

2
For further information, refer to Bosch Booklet 1, section 7.1.2.
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Example 2: CNO- composition adequately controlled:

CNO- %
2b. Appropriate TF1/REG1 addition
38

37
2a. Adequate
control frequency
Correction Correction
Correction
35

Time
Figure 7.3

Explanation of Figure 7.3:

2a. Composition sampling frequency is appropriate to the actual rate of change of CNO-
composition. In this example the rate of decay varies due to to variation in the size of the
component batches being processed, but prior experience is applied in the setting of a
cost-effective minimum sampling frequency.
2b. Calculation of the requisite TF1/REG1 addition, and the subsequent measurement of the
addition, are sufficiently accurate to prevent “overshoot” of the CNO- above 38%.

Calculation of the TF1/REG1 quantity is performed according to the Tufftride operating instructions by
Durferrit GmbH. The calculated quantity of TF1/REG1 should be measured and added to the TF1 bath with
a maximum error of ±0.1% of bath capacity.

7.3.4 Control of Fe+ content (desludging)

Iron content generally increases over time. The rate of increase is a function of several parameters:
Surface contamination: Loose particulate iron particles may be introduced to the TF1 bath on the surface
of the treated components. This may be controlled by an effective washing
procedure – refer to section 6.4 above.
Release of iron: Iron molecules may be released from the component surface during the treatment.

Iron content must be controlled within specification. Considerations:

Fe+ above spec: Excessive porosity and surface roughness of the compound layer.
Possibility that the finish of the parts will be “rusty red”.
Increased parasitic consumption of the CNO- content of the bath, requiring more
frequent additions of TF1/REG1, which increases the running cost.

Principles of Fe+ composition control are illustrated by the following exemplary control charts:

Example 3: Fe+ composition not adequately controlled:

Fe+ % Correction
Correction
Correction

0.02
Corrections

UPWARD TREND 3b. Inadequate desludging frequency

3a. Ineffective desludging

0
Time
Figure 7.4
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Explanation of Figure 7.4:

3a. Composition measurements and/or desludging operations are too infrequent, relative to the
rate of increase of Fe+ composition. Despite periodic desludging operations the Fe+
composition exceeds specification.
3b. In this example the frequency of the desludging operation is too low. The amount of Fe+
removed by the operations is high, but the Fe+ concentration has already exceeded the
specification limit.

Example 4: Fe+ composition adequately controlled

Fe+ %
4b. Effective control feedback
Sample
0.02
4a. Effective desludging Sample

UPWARD TREND
0
Time
Figure 7.5

Explanation of Figure 7.5:

4a. Desludging operations are carried out with appropriate frequency and effectiveness. The
Fe+ content of the TF1 bath remains well within specification as confirmed from a
composition sample.
4b. The Fe+ content begins to drift upwards, perhaps due to increasing level of contamination
remaining after the pre-wash (section 6.4 above). This is identified by appropriately-timed
sampling of the bath composition. A more thorough desludging operation is carried out and
action is taken to restore the effectiveness of the pre-wash.

7.3.5 Definition of effective bath control

The contractor must provide evidence of effective control of TF1 bath composition on an ongoing basis.
Effective control is defined as follows:

First control loop: Key composition parameters remain within specification throughout the treatment,
i.e. the bath composition can be maintained within specification over a day-to-day
timeframe.
Second control loop: Effectiveness of control actions (TF1/REG1 addition, and Fe+ removal/desludging)
is monitored through comparison of composition measurements before and after
control actions are carried out. Control errors are identified quickly enabling the
root causes to be addressed on a preventative basis. The bath composition is
guaranteed to remain within specification over a longer timeframe, weeks - months,
which in turn guarantees a consistent performance from batch to batch.

The contractor is responsible for setting the initial frequency of bath composition measurements based on a
Process Control study. Changes to the measurement frequency must be based on subsequent Process
Control studies. All Process Control studies must be recorded and made available for quality auditing
purposes.

The ability of the contractor to maintain Process Control over the Tufftride bath composition is a
key criterion for gaining approval by Bosch Rexroth, Glenrothes.

7.4 Treatment times

It is the responsibility of the contractor to install sufficient control measures to ensure that the specified
treatment time is consistently achieved for all stages of the Tufftride Q operation.
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7.5 Quality system

The complexity of the Tufftride Q process requires the contractor to maintain in-house an adequate level of
knowledge and competence with the processes, process control functions and the underlying technical
basis. Assessment of these competences, as embodied by the contractor’s quality systems, forms part of
the Bosch Rexroth Glenrothes approval process for Tufftride Q.

7.5.1 Essential elements of the contractor’s quality system

Contractor assessment should cover the following minimum areas:
• Standardised fixtures and arrangements
• Operating instructions for process equipment
• Work instructions and job-specific requirements
• Instrumentation and control systems, including calibration
• Bath composition analysis, including “Gauge R&R” (Repeatability and Reproducibility)
• Trend analysis
• Selection and condition of tools and portable equipment essential for running the Tufftride Q process

The contractor is responsible for maintaining practical understanding and implementation of the above
elements, supported by documentary evidence as appropriate. Evidence of this should be sought during
the contractor assessment.

7.5.2 Plant maintenance

A proactive, systematic regime of Total Productive Maintenance (TPM) is required. A preventative
approach should cost-effectively guarantee the ongoing functionality of the infrastructure, equipment and
instrumentation critical to achieving the quality requirements outlined herein. Properly organised
preventative maintenance should improve the commercial efficiency and responsiveness of the Tufftride Q
process. Contractor assessment should seek evidence of appropriate practice in this area.

7.5.3 Personnel training

Process operators undertaking Tufftride treatment operations should achieve a practical level of
understanding of the process and the significance of their actions towards reaching the quality specification
defined herein. It is the responsibility of the contractor to maintain the necessary systems to ensure that
process operators remain fully equipped with the following knowledge:
• Fundamental understanding of the Tufftride process including an awareness of the criticality of
controlling the “invisible” aspects of the process such as bath composition and treatment time.
• Criticality of specific process control activites, for example cleaning and loading arrangements and
treatment times, which may vary from one component design to the next
• Ability and motivation to raise concerns about quality issues that may be observed through the course of
routine work, e.g. accuracy of the process control or contamination of the components or baths.

Contractor assessment should emphasise operator competence, particularly if production activities are
continuous (24/7) and therefore potentially unsupervised. Documented training records should be sought
as the basis for this assessment, but not relied upon exclusively.

7.5.4 Periodic auditing by Durferrit GmbH (“health check”)

In addition to the contractor’s in-house process controls, calibration practices and quality assurance
systems, the “health check” service offered at no cost by Durferrit GmbH may be beneficial. A contractor
using this service will be in possession of a history of audit reports received from Durferrit together with the
contemporary in-house quality data and records and a record of any identified corrective actions. This
service is strongly recommended because it provides evidence of the contractor’s level competence with
Tufftride Q over the long term.

The “health check” method is generally as follows:

• Treat a standard test specimen (provided by Durferrit) under the standard Tufftride Q process (90
minutes TF1 + 10 minutes AB1).
• Simultaneous with the treatment, take two sets of salt samples from the TF1 and AB1 baths.
• Store one set of samples in resealable polythene bags with all air removed.
• Carry out a standard composition analysis on the other set of samples.
• Despatch the bagged salt samples and the treated test specimen to Durferrit, Mannheim together with
the contractor’s own composition measurements.

The contractor should send the “health check” report to the Quality Manager at Bosch Rexroth Glenrothes.
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The “health check” should be carried out at 3-month intervals.

8. Approvals
8.1 Approval by Bosch Rexroth
The contractor’s Tufftride Q process shall be approved prior to use in series production by the Purchasing
and Quality departments at Bosch Rexroth, Glenrothes, by reference to the criteria herein. Additional
general requirements are presented in specification F6-11.

8.2 Approval by process owner

The contractor is responsible for obtaining approval of their Tufftride Q process by the local subsidiary of
the HEF/Durferrit group. Refer to sections 4 and 6.1 for guidance.

The contractor is responsible for implementing in full the specifications and guidelines (formal or informal)
that may be issued by the local subsidiary of the HEF/Durferrit group.

8.3 Health, safety and environment (HSE) requirements

Tufftride Q contractors must be approved by the HSE Manager at Bosch Rexroth, Glenrothes. The
following requirements should be regarded as a basic minimum guideline for HSE compliance. Further
details are available from the HSE Manager.

1. The contractor must be able to demonstrate compliance with the relevant environmental legislation.
2. Contractors operating in the UK who do not have IPC Part A and Part B permits in place for their
operational process must have written confirmation of exemption from their local environmental
authority.
3. An adequate Consent to Discharge must be in place and available for inspection by Bosch auditor.
4. The contractor is preferably certified to ISO 14001 or is working towards certification.
5. MSDS must be available for inspection for all materials used in processes, including transit rust
inhibitors.
6. Hazardous waste consignment notes must be available for inspection by Bosch auditor.
7. A formal fire risk assessment, conducted by a competent person, must be available for inspection by
Bosch auditor.

8.4 Changes to the approved process

Following approval of the contractor’s Tufftride Q process by Bosch Rexroth, any subsequent changes or
developments to the process must be notified to Bosch Rexroth via a formal Process Change Request and
approved by Bosch Rexroth prior to introduction in series production, according to the requirements of F6-
11 (section Q8) and ZA 08946 AN1 (section 4) (as applicable).

8.5 Approved Contractors

Only approved contractors may carry out Tufftride Q treatment of components on behalf of Bosch Rexroth,
Glenrothes. Refer to DO/210/01 for the master list of approved contractors.

Suppliers of finished components to Bosch Rexroth, Glenrothes, who may engage a contractor to perform
Tufftride Q treatment on these components, are responsible for approving their contractor against this
standard and undertaking the quality management activities necessary to ensure continuing compliance.

9. Drawing specification
Drawings of components for which Tufftride Q treatment at default quality is required must indicate the
requirement as follows within the “treatment” box:

TUFFTRIDE Q PER DO/200/026

Tufftride Q treatment at ENHANCED QUALITY should be applied only to alloy steel components where the
higher cost can be justified. Drawings of components for which Tufftride Q treatment at ENHANCED
QUALITY grade is required must indicate the requirement as follows within the “treatment” box:

TUFFTRIDE Q PER DO/200/026

ENHANCED QUALITY
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Note: Tufftride Q treatment at default quality grade may be used in substitution for the alternative gas
nitriding treatment per Bosch Rexroth Glenrothes specification DO/200/020. In this case the treatment box
on relevant component drawings will indicate:

SPECIAL NITRIDE PER DO/200/020

10. References
Documents identified * are particularly relevant to the contractor assessment process.

10.1 Normative references

The following documents are referenced directly from this standard.

External:
* Tufftride operating instructions, Durferrit GmbH

Bosch Rexroth:
DO/200/20: Surface hardening – Special nitriding process
DO/200/30: Component & assembly cleanliness specification
DO/200/40: Metallographic examination of Tufftrided components
DO/210/01: Master list of contractors approved for Tufftride processes
DO/400: Material specifications
F6-11: Requirements on suppliers
WI-MAN-009: Piston de-burring instruction
WI-MAN-043: Cylinder block deburr (HD)
WI-MAN-044: Cylinder block deburr (LD, ED)
ZA 08946 AN1: Quality Assurance Guideline for Suppliers QSL – Industry/Operating
Equipment/Services – Mandatory Agreement

10.2 Bibliography
The following documents provide relevant guidance and knowledge to support the implementation of this
standard.

External:
* Tufftride QPQ – Technical information, Dr. Joachim Boßlet & Michael Kreutz, Durferrit GmbH
DIN 17022-4: Heat treatment of ferrous metals – Part 4: Nitriding and Nitrocarburizing
SAE AMS 2753: Liquid Salt Bath Ferritic Nitrocarburizing, Non-Cyanide Bath
PRI AC7102: Baseline Nadcap Audit Criteria for Heat Treating

Bosch Rexroth:
N09.003-5: Heat treatment – Surface hardening, Salt bath nitriding (Tenifering)
ZN 92006: Heat treatment: Salt bath nitrocarburising of composite cylinders
AA 12091-102: Wärmebehandlung: Salzbadnitrocarburieren Verbundzylinder

Bosch Group:
Quality Management in the Bosch Group | Technical Statistics; Booklet 1: Basic Concepts of
Technical Statistics – Variable Characteristics
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Appendix 1: Standard locations for compound layer integrity check and hardness test
Compound layer integrity check = “drop test”

Table A1
Component Location
Cylinder Drop test must be made within at least one cylinder bore in the area identified by hatching.
blocks High displacement blocks (with stepped bore): drop test must be applied inboard of the location
used for the microsection (Appendix 2).
Low displacement blocks (with plain bore): drop test must be applied inboard of (below) the corner
radius cuts.
High displacement: Low displacement:

Note: For drop tests within cylinder bores it is essential to provide an adequate illumination level
within the bore, to distinguish the resulting colours clearly.

Hardness test must be applied on the

timing face as indicated by the
hatched area in the figure right:

Distributors Drop test and hardness test must be applied on the timing
face, as indicated by the hatched area in the figure right:

Pistons Drop test and hardness test to be applied to the flat faces indicated by the hatched areas below:
(a) Dumb-bell types (b) Separated types
(i) High displacement: (i) High displacement:

(ii) Low displacement: (ii) Low displacement:

All other Drop tests and hardness tests may be made in any convenient location, preferably flat and
components smoothly-finished. Once established by trial, locations should be fixed in work instructions.
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Appendix 2: Standard microsection locations

Standard microsection locations should be interpreted from the guideline below unless a specific instruction
is provided by Bosch Rexroth, Glenrothes. General notes:
• The angular orientation of the microsection cut must be controlled consistently according to the
guideline. This is essential because most components are formed using rotational cutting processes.
• For components with cylindrical profile, the microsection must be cut along a radius in order to prevent
inaccuracy of the thickness/depth assessments. Refer to Figure A2 below.
• Microsection position and orientation are indicated by a thick black mark which is not necessarily
representative of the actual cut line.

Table A2
Component type Location
Pistons

Microsection should be cut parallel to main axis of piston. Rotational position (around axis of
piston) should match the sketch drawing.
Cylinder blocks

Microsection should be cut parallel to main axis of cylinder bore at a depth of 20±2mm from
the outside face. Rotational position (around axis of bore) may be freely chosen, except for
some LD blocks (as right) in which the section must be taken from the side face to ensure
that the microsection is positioned fully within the smooth-cut cylindrical surface.
Distributors View on timing face:

Microsection must be cut on the timing face. Microsection should be oriented radially to the
distributor axis and equispaced between two adjacent ports.
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Table A2 (cont.)
Component type Location
Brake washers

Microsection should be cut across flat face of washer, oriented radially to the washer.
Shafts

Microsection should be cut perpendicular to main axis of shaft. Rotational position (around
axis of shaft) may be freely chosen. Microsection should be positioned axially along the
shaft as close as possible to the middle of the shaft length but clear of any splined or
threaded regions or any changes in section.
Timing pins

Microsection should be cut parallel to main axis of pin and positioned centrally within the
larger-diameter section of the pin.

Microsections of cylindrical components are specified in Table A1 to be cut radially. Deviation from a true radial
cut, i.e. cutting along a chord, may influence the findings of the assessment by misrepresenting the layer
thickness, porosity depth and other qualitative assessments. For this reason it is necessary to specify a
maximum allowable offset to the cutting plane.

Specification:
[Maximum permitted chordal offset] = 5% x [Diameter of cylindrical section of component]

Figure A.2
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Appendix 3: Assessment guide: compound layer quality

Micrographic images of alloy steel comopnents reproduced below may be used as a guide to
understanding acceptable and unacceptable quality of the compound layer. Note:
• These images are not included here as a guide to micrograph quality – refer to DO/200/40.
• These images are not reproduced at the same scale.

Key: L = Layer thickness; P = porosity;  = acceptable;  = unacceptable (vs. ENHANCED quality requirement).

L P L P

   

   

   

   

   

   

   