JB/T 13023-2017 PDF in English
JB/T 13023-2017 (JB/T13023-2017, JBT 13023-2017, JBT13023-2017)
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Technical requirements of nitride carbonize and ozidize multi-treatment(QPQ)
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Standards related to (historical): JB/T 13023-2017
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JB/T 13023-2017: PDF in English (JBT 13023-2017) JB/T 13023-2017
JB
MECHANICAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 25.200
J 36
Registration number. 57803-2017
Technical requirements of nitride carbonize
and oxidize multi-treatment (QPQ)
ISSUED ON. JANUARY 09, 2017
IMPLEMENTED ON. JULY 01, 2017
Issued by. Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 4
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 6
4 Equipment requirements ... 7
4.1 General requirements... 7
4.2 Preheating furnace ... 7
4.3 Nitrocarburizing furnace ... 7
4.4 Oxidation furnace ... 8
4.5 Control system ... 9
4.6 Cleaning device ... 9
4.7 Polishing equipment ... 10
4.8 Oil tank ... 10
4.9 Ventilation system ... 10
4.10 Lifting system ... 11
5 Process material requirements ... 11
5.1 Composition of process materials ... 11
5.2 Process material properties ... 11
5.3 Use and Maintenance ... 12
5.4 Packaging, marking ... 12
6 Process requirements ... 13
6.1 Process flow ... 13
6.2 Process specifications ... 13
6.3 Process requirements ... 13
7 Quality control and inspection ... 20
7.1 Quality control ... 20
7.2 Quality requirements and inspection ... 20
8 Safety, hygiene and environmental protection requirements ... 22
Appendix A (Normative) Waste gas collection and treatment device principle
... 23
A.1 Outdoor part of ventilation system ... 23
A.2 Absorption tower internal structure ... 24
Appendix B (Normative) Cyanate chemical analysis method ... 25
B.1 Reagents ... 25
B.2 Analytical determination ... 25
B.3 Preparation of 0.1 mol/L NaOH standard solution ... 26
Appendix C (Informative) Common typical workpiece salt bath nitrocarburizing
temperature and nitrocarburizing time ... 28
Appendix D (Informative) Recommended ventilation for different mass of salt
baths ... 29
Appendix E (Informative) QPQ heat treatment production process record card
... 30
Technical requirements of nitride carbonize
and oxidize multi-treatment (QPQ)
1 Scope
This standard specifies the terms and definitions, equipment requirements,
process material requirements, process requirements, quality control and
inspection, safety, hygiene and environmental protection requirements of the
nitride carbonize and oxidize multi-treatment (QPQ) technology.
This standard applies to the nitride carbonize and oxidize multi-treatment (QPQ)
of black metal, cast iron and stainless steel.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 230.1 Metallic materials - Rockwell hardness test - Part 1. Test method
(scales A, B, C, D, E, F, G, H, K, N, T)
GB/T 443 L-AN full loss system oil
GB/T 4340.1 Metallic materials - Vickers hardness test - Part 1. Test method
GB 5959.1 Safety in electroheat installations - Part 1. General requirements
GB 5959.4 Safety in electroheat installations - Part 4. Particular
requirements for safety resistance heating installations
GB/T 6067.1 Safety regulations for lifting appliances - Part 1. General
GB/T 7232 Terminology of metal heat treatment
GB/T 8121 The terminology of technological materials for heat treatment
GB/T 9452 Testing method for working zone of heat treatment furnace
GB/T 10067.1 Basic specifications for electroheat installations Part 1.
General
GB/T 10067.4 Basic technical conditions for electroheat equipment - Part 4.
Indirect resistance furnace
GB/T 11354-2005 Steel-iron parts - Determination of nitrided case depth and
metallographic examination of nitriding structure
GB 14554 Emission standards for odor pollutants
GB 15735 Requirements for the safety and health in production process of
metal heat treatment
GB/T 22560 Gas nitrocarburizing of iron and steel parts
GB/T 27945.1 The management of hazardous solid wastes from heat
treatment salt - Part 1. General management
GB/T 27945.2 The management of hazardous solid wastes from heat
treatment salts - Part 2. Test method of extractives
GB/T 27945.3 The management of hazardous solid wastes from heat
treatment salts - Part 3. Method of innocent treatment
GB/T 27946 Limited value of hazardous substance in the air of heat
treatment working place
GB/T 30822 Environmental protection technical requirements for heat
treatment industry
GB/T 32529 Technical requirement of cleaning liquid waste recycling and
emissions for heat treatment
GB/T 32541 Quality control system for heat treatment
JB/T 6050 Generalization of hardness test for heat treated iron and steel
parts
JB/T 6090 Polishers
3 Terms and definitions
The definitions of GB/T 7232, GB/T 8121, GB/T 11354-2005 and the following
terms and definitions apply to this document.
3.1
Nitride carbonize and oxidize multi-treatment (Quench-Polish-Quench,
QPQ)
4.4.5 Oxidation furnace shall have salt leakage alarm device and corresponding
safety protection device.
4.4.6 Oxidation furnaces shall have air extraction devices and shall comply with
the requirements of 4.9.
4.4.7 Oxidation furnace can choose electric lifting furnace lid or pneumatic lifting
furnace lid, and set up the salt addition port on the furnace lid.
4.5 Control system
4.5.1 The external heat crucible resistance furnace shall meet the requirements
of GB/T 32541 for equipment and instruments.
4.5.2 Each heating zone shall have two thermocouples, one is connected to
temperature control instruments and installed between the crucible and the
resistance wire, the other is connected to the temperature recording instrument
and installed in the crucible, the instrument shall have the alarm function; the
thermocouples shall be checked regularly to ensure normal use.
4.5.3 The control system shall be able to display, control and record the
temperature, as well as record and store the whole process. It has the functions
of automatic temperature timekeeping, automatic timing alarm and salt leakage
alarm, it has the functions of overcurrent, overload and phase failure protection.
4.6 Cleaning device
4.6.1 Cleaning device is divided into pre-cleaning and post-cleaning device, it
may use cleaning tank or cleaning machine.
4.6.2 The cleaning tank shall be made of glass steel or stainless steel, with
stirring function, and its effective size is determined in accordance with the size
of the nitriding furnace crucible.
4.6.3 The temperature control device of the hot water cleaning tank is subject
to temperature measurement by a thermocouple or a thermal resister, and
temperature control by temperature control instrument, with the operating
temperature ≥ 80 °C.
4.6.4 The pre-cleaning device shall be provided with a waste water recovery
device.
4.6.5 The post-cleaning device shall be provided with a waste salt recovery
device.
4.6.6 If cleaning the workpiece with a washing machine, the washing machine
4.10 Lifting system
4.10.1 Lifting machinery shall meet the operational requirements of the QPQ
production line and use the electric hoist with the corresponding load in
accordance with the QPQ equipment specifications.
4.10.2 The design, manufacture and installation of the lifting system shall
comply with the provisions of GB/T 6067.1.
5 Process material requirements
5.1 Composition of process materials
Process materials consist of base salts, regenerated salts, and oxidized salts.
5.2 Process material properties
5.2.1 Base salt
5.2.1.1 Base salts are mixtures of carbonate, sodium, lithium carbonates and
cyanates. The base salt is added into the nitrocarburizing furnace, mainly
providing active nitrogen carbon atoms to the salt bath nitrocarburizing of the
workpiece, when the liquid level in the nitrocarburizing furnace falls, the base
salt shall be added to raise the liquid surface.
5.2.1.2 The base salt is in the form of a white block, powder, or other shape and
shall not contain heavy metals; it shall not produce gas when the base salt is
added and supplemented.
5.2.1.3 The base salt can be used in the range of 480 °C ~ 650 °C. The cyanide
content (mass fraction) in the salt bath at the time of exit-factory is 37% or
negotiated between the supplier and the purchaser, the deviation does not
exceed ±1%.
5.2.2 Regenerated salt
5.2.2.1 The salt bath decomposes naturally during workpiece salt bath
nitrocarburizing reaction and heating, the content of cyanide in the salt bath will
continuously decrease. The regenerated salt is an organic substance used to
adjust the content of the active ingredient cyanate in the salt bath.
5.2.2.2 The regenerated salt is white and shall not contain heavy metals; only
traces of gas can be produced when regenerated salt is added.
6.3.2.2 The maximum loading amount per furnace is less than 50% of the salt
bath mass.
6.3.2.3 Workpieces shall avoid direct contact with the workpiece and fixtures,
to prevent degradation of the nitriding quality of the contact layer.
6.3.2.4 For the workpieces with blind holes or grooves, blind holes or grooves
shall be downwards to avoid accumulation of salt.
6.3.2.5 Rod shape and plate shape workpieces shall be clamped vertically to
reduce distortion.
6.3.2.6 When the workpiece is processed, the fixture for mounting the
workpiece shall be suspended in the crucible; the distance between the bottom
end of the fixture and the bottom of the crucible shall be ≥ 50 mm, the distance
between the top of the fixture and the salt bath surface in crucible shall be ≥ 50
mm.
6.3.3 Pre-cleaning
6.3.3.1 The cleaning tank shall meet the requirements of 4.6.
6.3.3.2 The clamped workpiece shall be cleaned with a metal cleaner solution,
cold water and hot water, to remove the oil and dirt from the workpiece.
6.3.3.3 Wash the workpiece with a washing machine, remove the oil and dirt
from the workpiece, blow (bake) dry, then clamp it.
6.3.3.4 Metal cleaner shall meet the requirements for use.
6.3.3.5 The cleaning process must not have a detrimental effect on the surface
of the workpiece.
6.3.4 Preheating
6.3.4.1 The preheating furnace shall meet the requirements of 4.2.
6.3.4.2 The role of the preheating process is to remove the moisture from the
surface of the workpiece and blind holes, to prevent the salt solution from
splashing and injuring people as water enters the nitrocarburizing furnace,
ensure that the temperature of the nitrocarburizing furnace does not decrease
too much, and improve the workpiece surface quality.
6.3.4.3 The preheating temperature and the preheating time are properly
selected in accordance with the workpiece material, the loading amount per
furnace, and the like.
6.3.4.4 The preheating temperature is generally 350 °C ~ 400 °C. The
6.3.5.5 The nitrocarburizing temperature in the salt bath and the
nitrocarburizing time in the salt bath for commonly used materials are given in
Appendix C.
6.3.5.6 Through the inspection of preliminary heat treatment specimens,
reasonably determine the salt bath nitrocarburizing processing parameters.
6.3.5.7 Correct the salt bath nitrocarburizing process parameters by checking
the test specimens.
6.3.5.8 After the workpiece enters the nitrocarburizing furnace, if the furnace
temperature does not drop by more than 20 °C, the nitrocarburizing time starts
from the point when the workpiece enters the furnace. If the furnace
temperature drops by more than 20 °C, the nitrocarburizing time shall starts
from the point when the furnace temperature rises to the setting temperature.
6.3.5.9 The content of cyanate in the nitrocarburizing salt bath shall be strictly
controlled. The content of cyanate in the salt bath at the beginning of production
shall be measured every day. The cyanate can be measured once or twice a
week after the production enters into normal conditions.
6.3.5.10 After the nitrocarburizing salt bath treatment for a certain period of time,
the regenerated salt shall be added at a suitable time in accordance with the
change of the cyanate content.
6.3.5.11 When adding regenerated salt, the salt bath temperature shall be
controlled at 540 °C ± 10 °C, so that the regenerated salt reaction is more fully,
reducing the evaporation of the regenerated salt and increasing the yield.
6.3.5.12 The salt bath shall react for 1 h after adding the regenerated salt before
it can continue production; when a large amount of regenerated salt is needed
to substantially increase the content of cyanate, it shall follow the principles of
more number of additions but less amount of additions.
6.3.5.13 When the liquid level of the nitrocarburizing salt bath drops, the base
salt shall be added. The amount of base salt added shall be determined by the
liquid level of the nitrocarburizing salt bath.
6.3.5.14 The slag removal shall be performed after the nitrocarburizing salt bath
treatment for 10 h.
6.3.5.15 The slag extracted from the nitrocarburizing salt bath is broken after
cooling and placed in an oxidization salt bath.
6.3.5.16 The addition of base salts is usually performed in conjunction with the
regenerated salt addition and the slag removal process.
6.3.5.17 In case of salt bath nitrocarburizing, if it requires leading compressed
6.3.7.5 The water in the first cold water tank shall be periodically treated and
drained after reaching to the environmental protection requirements.
6.3.7.6 The second cold water tank is cleaned with running water and the
wastewater can be discharged normally.
6.3.7.7 The cleaning process shall not have a detrimental effect on the surface
of the workpiece.
6.3.8 Polishing
6.3.8.1 The purposes of polishing is to remove the loose layer from the surface
of the workpiece and reduce the roughness of the surface of the workpiece, in
order to greatly improve the corrosion resistance of the workpiece after
secondary oxidation.
6.3.8.2 Reasonably select the polishing method and polishing equipment in
accordance with the workpiece shape, technical requirements, etc.
6.3.8.3 The polishing equipment shall meet the requirements of 4.7.
6.3.8.4 Helical vibration polishers and centrifugal vibratory polishers are
suitable for shallow polishing of small parts and irregular parts.
6.3.8.5 Rod-shaped centerless grinding and polishing machine is suitable for
the polishing of rod and rod-shaped parts such as piston rod and pin shaft.
6.3.8.6 Ordinary wheel-type polisher is suitable for the polishing of parts with
large size and relatively regular shape. Select different types of polishing
wheels to achieve different polishing results.
6.3.8.7 Reasonable control the polishing degree in accordance with the
appearance of the workpiece and performance requirements.
6.3.8.8 Polishing process shall not adversely affect the surface of the workpiece.
6.3.9 Secondary salt bath oxidation
6.3.9.1 The secondary salt bath oxidation temperature is generally 400 °C ~
450 °C, salt bath oxidation time is generally 10 min ~ 60 min.
6.3.9.2 Others shall meet the requirements of 6.3.6.
6.3.10 Re-cleaning
Re-cleaning shall be performed in accordance with the requirements of 6.3.7.
6.3.11 Oil immersion
compound layer is measured, the depth of the diffusion layer is measured only
when required.
7.2.5 Metallographic organization
Metallographic organizations shall meet the technical requirements of the
normal organization, it shall not be less than the requirements of GB/T 11354.
7.2.6 Distortion
Distortion shall meet the technical requirements of the workpiece.
7.2.7 Others
In accordance with the technical requirements of the workpiece, the relevant
standards can be followed to perform test of such items of the corresponding
specimens as mechanical properties, wear resistance, corrosion resistance and
so on.
8 Safety, hygiene and environmental protection
requirements
8.1 Safety and hygiene requirements shall comply with the provisions of GB
15735, GB 5959.1, GB 5959.4 and GB/T 30822.
8.2 The waste water, waste liquid, waste gas, and waste residue generated
from the process material production process and process implementation shall
be collected and treated in a manner that does not adversely affect the
environment.
8.3 Waste gas and wastewater discharge during the production process and
process implementation of process materials shall meet the requirements of GB
14554, GB 15735, GB/T 27946, GB/T 30822 and GB/T 32529.
8.4 The discharge of solid waste generated during the production process and
process implementation of process materials shall be performed in accordance
with GB/T 27945.1 and GB/T 27945.2.
8.5 In the event of sudden power failure or water stoppage during production,
the equipment shall have corresponding protective measures to protect the
safety of personnel, equipment and parts.
8.6 Warning signs shall be set up in all places that may cause personal injury.
Appendix B
(Normative)
Cyanate chemical analysis method
B.1 Reagents
B.1.1 Mixed indicator. WEIGH 0.03 g of methyl red, DISSOLVE it in 50 ml of
absolute ethanol, USE distilled water to dilute it to 100 mL; WEIGH 0.015 g of
methylene blue, DISSOLVE it in 15 mL of water. After the two are completely
dissolved, MIX them and CONTAIN it into the dropping bottle.
B.1.2 ADD 0.1 g of phenolphthalein (100% high purity) into 100 mL of ethanol
(ethanol solution concentration 90%) to obtain a 0.1% mass fraction
phenolphthalein solution.
B.1.3 PREPARE the formaldehyde (1.1) into 500 mL or 1000 mL in accordance
with the specimen requirements. MEASURE the blank value once every
preparing the solution (100mL of formaldehyde plus 100 mL of distilled water).
B.1.4 BOIL the 10% (mass fraction) NaOH in distilled water to prepare it (e.g.
WEIGH 10 g of NaOH, USE 90 mL of boiled distilled water to dissolve it).
B.1.5 1 mol/L H2SO4 [e.g. 28 mL of 95% ~ 98% (mass fraction) concentrated
sulfuric acid, distilled water 472 mL].
B.1.6 Configuration and calibration of 0.1 mol/L NaOH solution.
B.2 Analytical determination
B.2.1 Sampling
USE a stainless steel rod of about Φ30 mm to insert about 100 mm into the
nitriding salt bath, then quickly LIFT it up. After the salt flakes around the rod
fall off, COLLECT them in a container and prepare for the test. Specimens are
ground fine in a mortar, PLACE it in an oven at 80 °C ~ 90 °C, BAKE it for 1 h,
COOL it in a desiccator (a new salt sample is taken and tested immediately,
without the need of baking). WEIGH 5 g of salt sample in a small beaker, ADD
50 mL of distilled water, HEAT it on an electric furnace to make it completely
dissolve, TAKE it off and COOL it, TRANSFER it into a 250 mL volumetric flask,
USE distilled water to make its volume reach to the mark, SHAKE it uniformly,
USE rapid quantitative filter paper to filter it dry to prepare for use.
B.2.2 Determination
PIPETTE 10 mL of the above solution, ADD 20 mL of distilled water in a 250
mL flask, ADD 5 mL of H2SO4 solution (2N), COVER with a small funnel, HEAT
to boil it for 2 min, REMOVE and COOL it down. ADD 2 drops of mixing indicator,
SHAKE it uniformly, the solution is purple red [If it is green, add 2 mL of H2SO4
(1 mol/L) boil for 2 min, the solution shall still be purple], ADD 10% (mass
fraction) NaOH solution to neutralize the solution to green (add in drops and
shake it uniformly). Then ADD 1 mol/L H2SO4 dropwise until the solution turns
red. USE a small amount of distilled water to rinse the bottle wall, ADD 0.1 mol/L
NaOH dropwise until it is green, ADD 10 mL of formaldehyde (1.1) solution,
SHAKE it uniformly and LET it be standing for 1 min, ADD 4 drops of
phenolphthalein indicator, USE the 0.1mol/L NaOH standard solution to titrate
it, the solution turns bright red from purple to red, USE a steady reddish color
as the end point, RECORD the titration millimeters V1. TAKE another 10 mL of
formaldehyde (1.1) in a 250 mL conical flask, ADD 5 mL of distilled water, ADD
4 drops of phenolphthalein, USE 0.1 N NaOH standard solution to titrate it to
the slight reddish color, RECORD the number of milliliters of titration. This is
blank value V2.
B.2.3 Calculation
The cyanate ion content is calculated by the formula (B.1).
Where.
w (CNO-) - Mass fraction of cyanate ions;
N - The amount of substance concentration of sodium hydroxide standard
solution, in moles per liter (mol/L);
V1 - The volume of sodium hydroxide standard solution consumed when
titrating the sample and reagent mixture, in milliliters (mL);
V2 - The volume of sodium hydroxide standard solution consumed when
titrating the reagent, in milliliters (mL);
G - The mass of the specimen in the determined sample solution, in grams
(g).
B.3 Preparation of 0.1 mol/L NaOH standard solution
B.3.1 Weigh 40 g of NaOH (excellent grade) into a 1000 mL beaker, ADD 400
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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