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Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25 Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review. Journal of Mechanical Engineering Research & Developments, 42(1): 17-25. ISSN: 1024-1752 (Print) CODEN: JERDFO REVIEW ARTICLE ARTICLE DETAILS Article History: Received 20 November 2018 Accepted 26 December 2018 Available online 22 January 2019 ABSTRACT The detailed surface is the boundary between the machine part and the working environment or with other machine parts in the structure of the machine. The surface is directly affected by the mechanical, physical and chemical effects of the environment. It is also the first place to receive loads, often subject to friction, abrasion The surface of the machine is where the hardest working conditions are, so it is also vulnerable to abrasion. There are many methods to the durable surface; But the most common method is diffusion. In diffusion method, there are many methods, but the chapter only focuses on the gas nitriding method and control of the gas nitriding process. Nitriding process can only be best achieved by control of the gas nitriding process, in particular by controlling the amount of incoming air at each stage. The specifications of the gas nitriding process will determine the quality of the nitriding layer. One of the very difficult parameters to control this process is the concentration of NH3 and N2 into the air. In order to control this air which will use the air control equiments but to control the permeability components in the equipment need special control processes with modern equipment. In this paper, we present a technique for control of the gas nitriding process by sensor hydro. KEYWORDS gas nitriding process, sensor hydro, abrasion, friction 1. INTRODUCTION The detail surface is the boundary between the machine part and the work environment as well as with other machine parts. The surface of the machine is often directly affected by the mechanization as well as the first place to receive the load; frequently subjected to abrasion and abrasion; This is also the most distorted and destructive [1-3]. In order to increase the life expectancy, the durability of the first workpiece must be carried out in the surface finishing process for details. The detail need to treated by surface heat treatment. These are the details required for the mechanical heterogeneity between the surface and the substrate (often called the core) of the detail. These are the details required for the hardness and abrasion resistance at the surface while the requirements of the base are tough, resistant to bending, twisting, impact ... [4-10]. There are many the strength surface methods: Increasing the hardness and abrasion resistance of the surface by the surface quenching (in the core – non quenching), mechanical surface hardening (spraying ball) ... but common Particularly strength surface methods by diffusion or thermal treatment. This method is done by placing the detail in a rich elements that needs to be diffused into the surface (carbon, nitrogen, elemental types such as chromium, titanium, etc.), at a certain temperature and time. The above elements diffuse into the detail surface over certain distances [3,11- 15]. The nitriding gas process is a common method of heat treatment that changes the chemical composition of the surface, increasing the nitrogen content of the surface, making the surface more detailed, with a higher hardness, abrasion resistance, fatigue resistance than the inside detail. In many cases these methods also have the effect of increasing the resistance to erosion [16,17]. The purpose of the methods is: - Increased hardness and wear resistance, fatigue strength of components. This purpose of heat treatment is similar to the surface quenching method but is more effective. - Enhanced anti-corrosion and chemical resistance (high temperature antioxidant), acid resistance of the steel surface. Tools such as dies, diecast molds, extruded molds, high durability requirements, high impact toughness, hardness requirements at high temperatures. Some gears, shafts ... bearing heavy loads are also impregnated with nitriding gas process. These parts are made from medium carbon steel, usually alloyed with various elements depending on work requirements, are high strength and hardness, hardness (core) is about 35-55HRC before nitriding gas process. Some of the parts are made of tool steel with high carbon content such as stamping dies, parts made from wind and steel ... which are impregnated with nitrogen. Nitriding process is also used to impregnate stainless steel to increase the abrasive ability of medical knives. However, in this case it may have to sacrifice some anti-corrosion [17-23]. In the nitriding gas process, it is important to control the parameters of Journal of Mechanical Engineering Research & Developments (JMERD) DOI : http://doi.org/10.26480/jmerd.01.2019.17.25 CONTROL GAS NITRIDING PROCESS: A REVIEW Nguyen Duong Nam 1* , Nguyen Anh Xuan 1 , Nguyen Van Bach 1 , Le Thi Nhung 1 , Le Thi Chieu 2 1 Vietnam Maritime University, Haiphong city, Vietnam 2 Ha Noi University of Science and Technology *Corresponding Author Email: [email protected] This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited

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Page 1: Journal of Mechanical Engineering Research & Developments ...No.1(2019)/17-25.pdf · Highly activated atomic nitrogen produces adsorption and diffusion into the steel surface. Nitrogen

Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

ISSN: 1024-1752 (Print)

CODEN: JERDFO

REVIEW ARTICLE

ARTICLE DETAILS

Article History:

Received 20 November 2018 Accepted 26 December 2018 Available online 22 January 2019

ABSTRACT

The detailed surface is the boundary between the machine part and the working environment or with other machine

parts in the structure of the machine. The surface is directly affected by the mechanical, physical and chemical effects

of the environment. It is also the first place to receive loads, often subject to friction, abrasion The surface of the

machine is where the hardest working conditions are, so it is also vulnerable to abrasion. There are many methods to

the durable surface; But the most common method is diffusion. In diffusion method, there are many methods, but the

chapter only focuses on the gas nitriding method and control of the gas nitriding process. Nitriding process can only

be best achieved by control of the gas nitriding process, in particular by controlling the amount of incoming air at each

stage. The specifications of the gas nitriding process will determine the quality of the nitriding layer. One of the very

difficult parameters to control this process is the concentration of NH3 and N2 into the air. In order to control this air

which will use the air control equiments but to control the permeability components in the equipment need special

control processes with modern equipment. In this paper, we present a technique for control of the gas nitriding

process by sensor hydro.

KEYWORDS

gas nitriding process, sensor hydro, abrasion, friction

1. INTRODUCTION

The detail surface is the boundary between the machine part and the work

environment as well as with other machine parts. The surface of the

machine is often directly affected by the mechanization as well as the first

place to receive the load; frequently subjected to abrasion and abrasion;

This is also the most distorted and destructive [1-3].

In order to increase the life expectancy, the durability of the first

workpiece must be carried out in the surface finishing process for details.

The detail need to treated by surface heat treatment. These are the details

required for the mechanical heterogeneity between the surface and the

substrate (often called the core) of the detail. These are the details

required for the hardness and abrasion resistance at the surface while the

requirements of the base are tough, resistant to bending, twisting, impact

... [4-10].

There are many the strength surface methods: Increasing the hardness

and abrasion resistance of the surface by the surface quenching (in the

core – non quenching), mechanical surface hardening (spraying ball) ... but

common Particularly strength surface methods by diffusion or thermal

treatment. This method is done by placing the detail in a rich elements that

needs to be diffused into the surface (carbon, nitrogen, elemental types

such as chromium, titanium, etc.), at a certain temperature and time. The

above elements diffuse into the detail surface over certain distances [3,11-

15].

The nitriding gas process is a common method of heat treatment that

changes the chemical composition of the surface, increasing the nitrogen

content of the surface, making the surface more detailed, with a higher

hardness, abrasion resistance, fatigue resistance than the inside detail. In

many cases these methods also have the effect of increasing the resistance

to erosion [16,17].

The purpose of the methods is:

- Increased hardness and wear resistance, fatigue strength of components.

This purpose of heat treatment is similar to the surface quenching method

but is more effective.

- Enhanced anti-corrosion and chemical resistance (high temperature

antioxidant), acid resistance of the steel surface.

Tools such as dies, diecast molds, extruded molds, high durability

requirements, high impact toughness, hardness requirements at high

temperatures. Some gears, shafts ... bearing heavy loads are also

impregnated with nitriding gas process. These parts are made from

medium carbon steel, usually alloyed with various elements depending on

work requirements, are high strength and hardness, hardness (core) is

about 35-55HRC before nitriding gas process. Some of the parts are made

of tool steel with high carbon content such as stamping dies, parts made

from wind and steel ... which are impregnated with nitrogen. Nitriding

process is also used to impregnate stainless steel to increase the abrasive

ability of medical knives. However, in this case it may have to sacrifice

some anti-corrosion [17-23].

In the nitriding gas process, it is important to control the parameters of

Journal of Mechanical Engineering Research & Developments (JMERD)

DOI : http://doi.org/10.26480/jmerd.01.2019.17.25

CONTROL GAS NITRIDING PROCESS: A REVIEW

Nguyen Duong Nam1*, Nguyen Anh Xuan1, Nguyen Van Bach1, Le Thi Nhung1, Le Thi Chieu2

1Vietnam Maritime University, Haiphong city, Vietnam 2Ha Noi University of Science and Technology *Corresponding Author Email: [email protected]

This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited

Page 2: Journal of Mechanical Engineering Research & Developments ...No.1(2019)/17-25.pdf · Highly activated atomic nitrogen produces adsorption and diffusion into the steel surface. Nitrogen

Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

the infiltration process as it determines the quality of the permeability and

the life of the detail. The parameters of the permeation process include

two groups of parameters that need to be controlled [24-26]:

- Parameters of process temperature

- Parameters of air flow or gas decomposition. This parameter is especially

important and difficult to control. Infiltration flow will determine the

quality of the permeability.

Thus, in this chapter the authors focus on controlling the flow of air

permeable through nitrogen gas adsorption by hydrogen sensor. The main

contents of the lecture are: theory of nitrogen gas adsorption; Parameters

influencing nitrogen gas adsorption and methods of automatic control of

nitrogen gas adsorption process.

2. THEORY ABOUT GAS NITRIDING PROCESS

Nitrogen gas is a surface-hardening process in which nitrogen is

introduced into the steel surface by keeping the metal at an appropriate

temperature and exposure to permeable air, typically ammonia or

ammonia and nitrogen mixtures, ammonia mixtures with nitrogen or

hydrogen. Permeable temperature for all types of steel in the range of 495

÷ 565°C. When heated in the ammonia gas stream, within this temperature

range, the ammonia is decomposed rapidly by the reaction [27,28]:

2 3 23 2

NH H N→ + (1)

Figure1: Simulation of nitriding gas process

Factor required by reaction:

3/2

24

3

a PN HK

PNH

= (2)

Highly activated atomic nitrogen produces adsorption and diffusion into

the steel surface.

Nitrogen can dissolve into iron α with very small solubility resulting in an

intermittent solid α. The maximum dissolved concentration of 0.1% was

reached at 590°C. The solubility of nitrogen in Feγ is greater, the largest is

2.8% at 6500C.

Nitrogen combined with iron makes up different substances depending on

the content. In the wage range of 5.7 to 6,1%, nitrogen together with iron

produces the γ' phase - solid solution on the basis of phase alternating Fe-

4N with austenite network. When the nitrogen content is greater, it will

produce a phase ε - phase alternating with Fe2-3N.

Figure 2: Phase diagram Fe-N [29]

Table 1: Content of Nitrogen in phases [29]

Phase Nature Content N Properties

δFe Solid solution of N in

phase δFe

0 to ~ 0,9

γFe Solid solution of N in

phase γFe

0 to 2,8

αFe Solid solution of N in

phase αFe

0 to 0,1 Hard

γ’Fe4N alternating phase Fe4N 5,7 to 5,9

ε alternating phase Fe2-3N ~ 4 to ~

11

Very hard

Fe2N alternating phase ~11,1

FeN6 alternating phase ~ 61

FeN9 alternating phase ~ 69

Mactenxit solid solution too

saturated of N in αFe

0 to 0,6

Fe16N2 ~ 3,0

Page 3: Journal of Mechanical Engineering Research & Developments ...No.1(2019)/17-25.pdf · Highly activated atomic nitrogen produces adsorption and diffusion into the steel surface. Nitrogen

Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

Figure 3: Microstructure of phase

The higher the carbon content and the higher the alloying component, the

more likely it is to make ε phase

-The ε hardness is very high, higher than the γ' phase, which is less susceptible to cracking. -Up temperature 480oC, the phase area γ is narrowed.

-Phase formation depends on steel composition, temperature, NH3 decomposition, and nitriding gas time

-When nitrogen is applied to the steel, it generates phases, as shown in the Fe-N phase diagram. The permeable structure of nitrogen-permeable steel, including the diffusion and composite regions, is shown in Fig 5. The

mixture area may or may not depend on the type and content of the alloy elements as well as the temperature-time absorbed in a specific nitrogen uptake.

-Nitrogen fertilizers grow by diffusion, increasing with temperature and time

-The surface hardness of the permeable layer is obtained by the nitrite phase. CrN is Fe3N, Fe4N.

Figure 4: Hardness test on microstructure (X500)

Figure 5: Microstructure of 410 steel quenched at 845oC, tempered in 2 hours at 620oC, after: nitriding gas process in 24 hours at 525oC, decomposed from 20 to 30% [29].

3. MAIN PARAMETERS IN NITRIDING GAS PROCESS

3.1 Decomposition

Atomic nitrogen is produced in the decomposition furnace by ammonia

decomposition. During infiltration, the decomposition may vary

depending on the flow of NH3.

The decomposition of the permeate is determined as follows:

3

3

NH decomposition

NH begin = (3)

NH3 decomposition is the volume of NH3 decomposed by equation (1). At

a fixed temperature and pressure, the NH3 doesn’t constant. When low β

means that NH3 is introduced more and more nitrogen is produced, the

amount of active nitrogen is greater. When β is high, the NH3 content is

less and the active nitrogen is less. Nitriding is carried out at low

temperatures so that the nitrogen diffusion coefficient is small, so the

penetration time is usually long and the thickness of the thin layer is low.

The permeability class depends on the degradation of NH3 in the

permeation medium. If the flow of NH3 is constant, the decay increases

with time. When decomposition is too great, there may not be enough

nitrogen atoms for the permeation process. Although seepage occurs with

varying degrees of decomposition, it only starts when the decomposition

rate reaches 15-30%. The process lasts about 4-10 hours depending on the

permeation cycle. With a 15-30% decomposition will produce white

Page 4: Journal of Mechanical Engineering Research & Developments ...No.1(2019)/17-25.pdf · Highly activated atomic nitrogen produces adsorption and diffusion into the steel surface. Nitrogen

Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

nitriding layer on the steel surface. This microstructure is highly hardness

and crispy. When the amount of NH3 decomposes is large, ie the number

of Natom generated much, the amount of Natom created on the surface of the

large permeability, the phase ε - phase alternating between Fe2-3N large,

making the white layer high hardness and brittle, easy cracking. On the

other hand, Fe2-3N phase prevents the osmosis of the next nitrogen atoms

as thin layer. Permeability at higher temperatures, ammonia

decomposition strongly, atomic nitrogen form many as thinly permeable

layers and reduce the quality of the permeability. The nitrogen is worked

at the temperature from 495 to 530oC [29].

4. NITRIDING GAS PROCESS: ONE STAGE AND TWO STAGE

Nitrification with ammonia can be carried out in one or two stages. One-

stage nitrogen fertilization is a nitrogen uptake in which the amount of

NH3 is supplied constant throughout the infiltration process. Two-stage

nitrogen permeation is the impregnation process consisting of two stages

of gas supply. Phase one NH3 is provided with high flow, low

decomposition, second stage the amount of NH3 is reduced for greater

decomposition. Two-stage penetration increases the diffusion and hence

shortens the penetration time,

The two-stage impregnation process has the advantage of reducing the

thickness of the white nitriding layer because, in the later stage, the

nitrogen content decreases, the atomic nitrogen condenses deep into the

core, reducing nitrogen in the substrate. In the one-stage impregnation

process, the permeation temperature is in the range of 495 ÷ 525°C and

the decomposition is in the range of 15 ÷ 30%. This process produces a

white layer rich in nitrogen on the surface is white, mainly nitrite high

hardness and crunchiness. Then to the two-phase mixture and into the

deep layer of solid solution.

Độ C

540

100

40 30 20 180 150

phútN2

NH3

CO24 l/h

10 l/h

7 m3/h 10 l/h

5 m3/h

Không khí

Phân huỷ β =35%

a) One stage b) Two stage

Figure 6: Nitriding process

In the two-stage process, the first process is similar to the one-stage but

shorter process, which is carried out as follows: Stage one gas supply with

decomposition of 15 ÷ 30% in the 495 ÷ 525°C. In the second process, the

temperature is increased to about 550-565°C, the amount of gas is reduced

to decompose up to 65-80%. In the second process, the decay increases,

the amount of Nnt produced decreases, the temperature is increased, so

the nitrogen is diffused into the interior, the amount of nitrogen on the

surface decreases, not enough to form the phase ε - alternating phase Fe2-

3N reduces the hardness, crispy, cracked. The permeable layer consists of

a better solids-permeable mechanical layer. Parallel to that, nitrogen

diffuses deep into the thickening layer.

Figure 7: Influence of one-stage and two-stage impregnation of ASM 6470.

Prior to infiltration, the steel was at 900°C, cooled in oil, tempering at 605°C for 2 hours, a) Nitrogen gas nitrification at 525°C for 30 hours, the

organization includes: the background is ramenite oxide, Fe2N coating 0.01-0.013mm, b) Conditions such as (a) but infiltration for 36 hours, riveted nitric layer 0.023-0.025mm.

c) The above conditions are two-stage, stage 1; infiltrated for 5 hours at

525°C, phase 2 permeated for 20 hours at 565°C. The coating decreases

due to the diffusion of nitrogen in the second stage to form a solid solution

d) Condition as c) but the surface is burnt [29].

Page 5: Journal of Mechanical Engineering Research & Developments ...No.1(2019)/17-25.pdf · Highly activated atomic nitrogen produces adsorption and diffusion into the steel surface. Nitrogen

Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

5. CONTROL GAS NITRIDING PROCESS BY HYDROGEN SENSOR

The gas nitriding control system consists of two basic systems: hardware

and software (see Figure 4). Hardware is designed with unique

parameters with the standard system of infiltration as the temperature

and composition of the infiltration during gas nitriding processes. This

system includes sensors; these sensors will record the parameters of the

gas nitriding process and thus determine the formation of atomic Nitrogen

(decomposition of the permeability); These results will determine the

formation of permeable layers on steel. For the programming module, this

section uses the most up-to-date system equipment in the world; These

devices allow to calculate the parameters of this process; These results

provide the technologist with parameters to control the process or the

formation of nitrites. Therefore, the technology can provide the

appropriate solutions [30-36].

Figure 8: System’s general concept [37]

5.1 Designing Block of Process Parameters

5.1.1 Guidelines

When calculating and designing the gas nitriding process, according to

Kansei's method, there are some things to pay attention to as follows:

- Principle of Exception: While calculating the gas nitriding process, it is

necessary to use different values of input matrix parameters.

- Principle of target concentration: Determine the specific target of the

infiltration process (hardness, distribution of permeability, composition of

permeability layer ...); These values control the smallest parameters of the

process such as temperature changes, the composition of the permeate in

the process, and the control of the decomposition of NH3.

- Preliminary Information limit rule: Use limited information to control

the infiltration process.

- The rules for using a knowledge database means that databases

related to the parameters of the gas nitriding process will be collected and

processed to create a common database for later this process.

The using of the Kansei method to assist in the design of the gas nitriding

process has been demonstrated by increasing the number of mandatory

attributes associated with permeable layers as well as other elements.

5.2 Modeling of the process

5.2.1 Analysis process

Experimental data analysis involves phase formation in the nitride layer

(Figure 1) as well as the development of regions and phases in the

diffusion process. This process is described in the following equation:

*k tx ii = (4)

where:

Δxi – thickness of ith phase in n-phase layer after process time t (for the

nitrided layer, the maximum value n=3),

ki – kinetic parameter of the growth of ith phase, the so-called constant of

the parabolic growth of ith phase,

t – process time.

Equation 4 describes the development of the region and the formation of

phases in this process. In the equation above the ki constant is used to

describe the kinetic energy of the phase transformation in the

temperature. For practical reasons, this value is a full reflection of the

parameters of the case. According to Equation 4, the change in thickness

Δxi over a given period of time. However, the dynamic description of the

development of nitrite layers as well as the calculation of the diffusion

coefficient of N atom in individual layers or the calculation of N content in

phases. In addition, with this equation, it doesn’t effect of the remaining

stages which is created which results in the next phase of the development.

Therefore, it is necessary to construct a more general equation that

controls the coefficients of each development process ki and other

coefficients of the diffusion process. The construction of a general

equation for the parameters of this process helps to determine the

diffusion coefficients of the single-phase as well as to determine the

development of the phase over time. Equation 5 below describes a direct

connection of the dynamic parameters of a phase (ki) with the difference

in phase boundary and the diffusion coefficient of the phase [30,38].

2( ),1

ca k k D ci j i j i ij ef

= = i = 1,2,3 (5)

where:

,

1(3 ),, , 1

4

,

c i ji

a c c i ji j i i j

c i jj

= + =+

ki –kinetic parameters of the growth of ith and jth phase,

Δci –difference of concentrations of the diffusing element on the border of

ith phase.

Equation 5 is a nonlinear equation that can be solved by the approximation

(iteration):

2( ),

; 1, 2, 3,1 , 2 , 3

1

cD ci ief

k ii na kij jj

= = − − − =

(6)

In the method of successive approximations, e.g., for zone ε, the following

dependencies are obtained:

2( ) 2( )(1) (2)

,(0) (1)3 3

1 1

c cD c D ci ief ef

k k

a k a kij j ij jj j

= = = =

(7)

From the above equations, the larger the development of parameters, the

greater the difference in concentration at the boundaries Δci, in the phase

equilibrium diagram, as well as the greater the effective diffusion

coefficient is in a given phase– (Dci)ef. This model can also be applied for

Page 6: Journal of Mechanical Engineering Research & Developments ...No.1(2019)/17-25.pdf · Highly activated atomic nitrogen produces adsorption and diffusion into the steel surface. Nitrogen

Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

the calculations of the thickness growth of the whole zone of (carbo)

nitrides on steels, in particular on those stages of the process when phase

dominates [12].

5.3 Visualization and Control of the Process

Methods used to control the gas nitriding process which are being used

now for control purposes to determine precisely the composition of the

nitrogen environment. Sensors are used for the purpose of determining

the parameters that represent this process; permeability formation, ie, the

ability to apply algorithm in nitriding process as well as changing the

parameters of time and temperature. This is determined based on a

hydrogen temperature sensor or an ammonia component sensor and

work principle based on the absorption spectrum. However, choosing an

algorithm that is consistent with changes in the nitrogen composition as

well as the use of better and better sensors does not always produce the

expected results. In such cases, it is necessary to understand the class

structure as opposed to the expected class structure after the completion

of the process.

Hence, in the light of the growing demands for nitrided elements,

concerning above all an increase of their life, or growing demands

concerning a precise repeatability of the process results, it is

indispensable to construct a system which works on the basis of the

indications of the process result sensor. This sensor makes it possible

either to directly monitor the process course and a correction of the

changes of the process parameters in the case of its improper course, or to

control the process on the basis of the indications of the layer growth

sensor. Therefore, it becomes justifiable to add a block which represents

directly in the process a growth of the nitride layer (Figure 9) to the

process control and the adjustment system.

Figure 9: Schematic diagram of the automatic system of the nitriding process with thevisualization system for the course of the layer growth [37].

5.4 Selection of the Measuring Method

When a nitride layer is formed, both the electrical properties of the nitride

layers: resistivity (ρ) and magnetic properties will change. With respect to

magnetic characteristics, the magnetic field and intensity of the magnetic

field are most sensitive to the phase change and structure. One of the

important parameters determining the change in resistivity value is the

average free conduction of electronegative electrodes. During diffusion, it

decreases about development of the diffusion concentration: Nitrogen

atoms intercalate into the structure and form nitride alloys. In terms of

magnetic properties, the diffusion region is ferromagnetic, whereas the

surface area of the iron nitrites (compound regions) is far-reaching. The

ferromagnetic diffusion region, the magnetic field and the intensity of the

magnetic field are the functions of all micro and macro states of the

permeability layer. This assumes that the macro stresses are the result of

the variation in nitrogen concentration, the nitride alloys that are

responsible for the formation and growth of micro stresses. When the

nitriding process is carried out, the area covered by the change of

electromagnetic properties forms a fraction of the nitrite. This is the main

factor for controlling the change by induction. Material samples were

tested by placing them in an alternating electromagnetic field. This

process creates a vortex that controls the process of intrusion of elements

into the material [39-42]. The sensors are placed in the permeable

environment. These sensors are equipped with a dual coil. This generates

high-frequency currents that produce electromagnetic fields. As a result,

the electromagnetic field formed in the coil generates a voltage signal in

the secondary coil. As a consequence, the resultant field is formed in the

coil area, which induces a voltage signal in the secondary winding of the

coil. As a result of the testing examinations, the variant was selected with

two push-pull connected sections of the secondary coil, while the sample

tested is located in one of the sections (Figure 10). Owing to this, a change

of the voltage signal induced depends solely of the changing

electromagnetic properties of the sample [12].

Figure 10: Schematic diagram of two-winding sensor.

Finally, the voltage induced in the measuring winding of the coil is the

function of the following parameters [29,39]:

) (8)

where: – voltage induced in the measuring winding when the coil is

empty,

η – coil filling factor,

μr – relative magnetic permeability,

– effective permeability: This value makes the magnitude of the

magnetic field independent of the sample surface. The value of the current

induced in the coil depends directly on the relative permeability (μr) and

Page 7: Journal of Mechanical Engineering Research & Developments ...No.1(2019)/17-25.pdf · Highly activated atomic nitrogen produces adsorption and diffusion into the steel surface. Nitrogen

Journal of Mechanical Engineering Research & Developments (JMERD)42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

indirectly on the resistivity, which is a parameter of the permeability (

). Furthermore, by reducing the thickness of the sample, it is possible to

reduce the degree of variation in the induced voltage values due to the

resistivity. Therefore, it is possible to monitor the development of the

nitride layer by using magnetic sensors by monitoring the change in

voltage generated in the coil [16]. In the early stages of nitrided layer

formation, nitrogen diffusion induces the expansion of the surface layer of

the material. This expansion is being resisted by the rest of the material

with smaller concentrations of nitrogen. The macro stress characteristic

developed as a result of the process for those specimens, from the

diffusion point, to the finite thickness, these stresses can be described by

following equation [4]:

.( ) ( , )

( , )1

EN t N x t

x t

= −

− (9)

where: σ(x,t) – macrostresses which are parallel to the surface, in x distance

from the surface, β - Vegard constant, E - Young’s modulus, ν - Poisson

constant, [N (t)] - average nitrogen concentration in sample in t time of

process, [N(x,t)] - surface nitrogen concentration in x distance from

surface in t time of process. Due to the fact that the expansion of the lattice

caused by the diffusion of nitrogen is positive (β> 0), it follows the

equation near the surface, with the compression stress {[N (t)] <[N (x , t)],

while tensile stress exists in areas farther from the surface where {[N (t)]>

[N (x, t)]}. The above formulas show that when there is a change in the

structure and concentration of nitrogen atoms over time, the formation of

the macro stress can be simulated and calculated. Thus, the value of the

voltage change in the sensor can be compared to the change in the

magnetic stress by a function over time. At the same time, it is possible to

determine the nitrogen concentration by solving the diffusion problems

under Fick's law and form permeable layers. This means that the atomic

nitrogen concentration on the surface reaches the equilibrium value with

the nitrogen concentration inside the permeation medium.

Figure 11: (a) Variation in sensor signal (magnetising current frequency f = 150 kHz) as a function of nitriding time for an iron specimen of thickness g = 1

mm. (b) Calculated changes of surface compressive macrostress in an iron specimen of thickness g = 1 mm; process parameters: T = 560oC (833 K), KN = 0.08 [37].

Figure 11a shows an example of changes in the voltage induced in a

magnetic sensor during nitrogen adsorption to a 1 mm thick steel sample.

Samples were placed in infiltration medium with KN = 0.08 permeability

at 560oC. The registered properties U = f (t) correspond to the qualitative

significance for the change of surface macro stresses (Figure 11b) as

calculated for the above parameters of the process. These macro stresses

represent the two characteristic phases of diffusion. Previously connected

with an increase in surface nitrogen concentration accompanied by an

increase in compression pressure and a decrease in the voltage signal, in

the case of the later stage there is relaxation of the stress, increasing the

voltage [43,44].

6. DESIGN AND CONTRUCTION OF MAGNETIC SENSOR

The basic part of the measuring system, i.e., the magnetic sensor, is placed

in a furnace retort, cf. Figure 12. This is a run-through sensor: the gas

nitriding atmosphere flows through it and causes the formation of a

nitride layer on the specimen placed inside the sensor.

Figure 12: Magnetic sensor placed in furnace retort

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Journal of Mechanical Engineering Research & Developments (JMERD) 42(1) (2019) 17-25

Cite The Article: Nguyen Duong Nam, Nguyen Anh Xuan, Nguyen Van Bach, Le Thi Nhung, Le Thi Chieu (2019). Control Gas Nitriding Process: A Review.

Journal of Mechanical Engineering Research & Developments, 42(1): 17-25.

Structure and principle of operation of the hydrogen sensor is shown in

Figure 13 and Figure 14.

Figure 13: Hydrogen sensor Figure 14: Diagram of hydrogen sensor

The hydrogen sensor consists of a Wheatstone bridge of four temperature

dependent resistors. Two parallel resistors placed in the gas need to be

analyzed, the other two resistors in a stable gas environment that know

exactly the thermal conductivity. During the measurement, all four

resistors were heated to above 500oC. The thermal conductivity of gases

in the environment depends primarily on the hydrogen content.

Therefore, the resistance in the test chamber will change linearly with

temperature. The more hydrogen-rich the environment, the smaller the

metal resistance, so the more electrical current it needs to get to zero. This

current is proportional to the measured hydrogen concentration. The

device measures from 0% H2 with 4mA to 75% H2 with 20mA. Based on

the change of the current signal, the H2 concentration of the medium is

determined. The hydrogen sensor is used to measure the gas outside the

furnace with the following specifications:

+ H2 concentration measurement: 0 - 75%.

+ Supply voltage: 24 V, using DC source.

+ Output current: 4- 20 mA.

+ Retention time: Output delay 6 ... 20s

This sensor operates in all temperature ranges with high reliability. The

electronic evaluation and current system integrated in the sensor. Bring a

compact design and simple connectivity. The interference effects of other

gases such as O2, N2, CO, H2O and CO2 are automatically compensated.

Thus, only one type of sensor for all gas mixtures may be required. The

hydrogen sensor can be measured in nitrogen.

7. CONCLUSION

This paper introduces the nitriding technology as well as some knowledge

of sensor permeability, particularly the hydrogen sensor. The authors

studied about nitriding technology and methods for controlling the

permeability process as well as the use of hydrogen sensors in controlling

the nitriding process.

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