KR101642232B1 - Process optimizing method using simulation of pack cementation - Google Patents

Process optimizing method using simulation of pack cementation Download PDF

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KR101642232B1
KR101642232B1 KR1020150127805A KR20150127805A KR101642232B1 KR 101642232 B1 KR101642232 B1 KR 101642232B1 KR 1020150127805 A KR1020150127805 A KR 1020150127805A KR 20150127805 A KR20150127805 A KR 20150127805A KR 101642232 B1 KR101642232 B1 KR 101642232B1
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amount
pack
weight
iron
activator
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Korean (ko)
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김상권
이재훈
여국현
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한국생산기술연구원
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    • G06F17/5009—
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/34—Embedding in a powder mixture, i.e. pack cementation
    • G06F19/702—
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06F—ELECTRIC DIGITAL DATA PROCESSING
    • G06F9/00—Arrangements for program control, e.g. control units
    • G06F9/06—Arrangements for program control, e.g. control units using stored programs, i.e. using an internal store of processing equipment to receive or retain programs
    • G06F9/44—Arrangements for executing specific programs
    • G06F9/455—Emulation; Interpretation; Software simulation, e.g. virtualisation or emulation of application or operating system execution engines

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  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The objective of the present invention is to provide a simulation method and optimized composition ratio according to the same, in order to reduce efforts and consumption of energy required to directly implement a process of obtaining a composition ratio of a reactant in a pack cementation process. The present invention provides a simulation method for calculating a range of a composition ratio of x:y having a production ratio of iron halogenide approaching to 0 by: changing a composition ratio (weight ratio) of Cr:Fe to x:y (x=0-100, y=100-0); calculating a mole ratio of a production produced depending on a mole ratio of a reactant and production from a reaction formula by setting the reaction formula for generating chromium halogenide by making Cr react with an activator; and calculating a production ratio of the iron halogenide by using the mole ratio of the production and setting a reaction formula for generating the iron halogenide, a simulation program recording medium, and an optimized pack cementation composition ratio calculated through simulation.

Description

[0001] PROCESS OPTIMIZING METHOD FOR USING SIMULATION OF PACK CEMENTATION [0002]

The present invention relates to a process for producing a product having various three-dimensional shapes by carrying out coating using packing, in which a chemical reaction occurring in a packing process is simulated in advance to obtain an optimum And a method for finding a process. Particularly, the present invention relates to a simulation technique for a process of inducing the reverse chromium coating and nickel back diffusion of stainless steel as a base material.

The pack cementation method is very advantageous for coating the base material of the three-dimensional shape or coating simultaneously with sintering. A desired coating layer can be obtained as an in-situ CVD method by supplying a carrier gas and a reactive gas necessary for the process while heating the base material to a necessary temperature by filling the coating powder, the activator and the filler necessary for the coating.

Such a packaging method is particularly advantageous for forming a coating layer on a base material composed of iron or SUS which is an inexpensive material, in particular, when physical properties requiring an expensive rare-earth metal component are desired. In Korean Patent No. 10-1361814, a cobalt boride layer is coated on the surface of an iron-based metal by pack cementation.

Particularly, when a chromium layer having a high hardness is to be coated on various products having a three-dimensional shape composed of SUS, if chromium powder is packed in a pack and hydrogen or hydrocarbon is supplied as a reaction gas to perform packementation, Ni The component is diffused into the surface layer to obtain a coating layer of excellent physical properties in which nickel and chromium carbide are alloyed.

The pack contains a mixture of expensive chromium powder and an activator (NH 4 Cl, NH 4 F, NaCl, NaF, etc.) containing a halogen group element and an inert filler so as to generate a metal halide gas. As the filler, alumina (Al 2 O 3 ) is mainly used.

However, in the pack cementation reaction, the reaction between the activator and the iron contained in the base material causes the coating layer to be roughened, the coating layer to be uneven, and the pore to be formed in the coating layer. In particular, the inventors have found that, by the chromium and the active agent contained in the pack reaction halogenated chromium in the iron-based base material surface is chrome is deposited while forming a (NH 4 Cl chloride, chromium is used) halide is, occurs when the chromium coating be made on a base material surface Hydrogen (hydrogen chloride in the case of NH 4 Cl) combines with the iron atoms of the base material to produce iron chloride, and then escapes from the base material to deposit the iron component again in the pack. This phenomenon is problematic because it makes the base material porous, damages the coating layer and contaminates the pack.

In order to solve the above problems, it is necessary to analyze the reaction mechanism analytically to find a solution to the problem.

And when as a reaction gas into the chamber into an inert gas, such as argon, a hydrocarbon and a carrier gas is heated to a temperature of 700 to 1200 ℃, Cr and active gases in the metal raw material powder to react iron-chromium complex halide gas (FeCl 2, CrCl 2 ). At this time, the Ni component contained in the stainless steel itself as a raw material is reverse-diffused to the surface layer. Stainless steel inherently contains about 13% by weight of Ni, so that if the high-temperature process is continued, Ni will spread to the surface layer. As a result, a Ni-Cr alloy coating layer having a content of Ni of about 10 to 30% is produced in the surface layer. As such, the coating layer containing Ni has a very stable cryogenic resistance to thermal expansion.

That is, the following chemical reaction takes place in the pack cementation,

- The process of halogen gas evolution of the active agent in the pack

(1-a) NH 4 Cl (s) → NH 4 Cl (g) = NH 3 (g) + HCl (g)

(1-b) NH 4 F (s) → NH 4 F (g) = NH 3 (g) + HF (g)

(1-c) 2NaCl (s)? 2NaCl (g) + H 2 (g) = 2Na (g) + 2HCl (g)

(1-d) 2NaF (s)? 2NaF (g) + H 2 (g) = 2Na (g) + 2HF (g)

(2) 2NH 3 (g) - > N 2 (g) + 3H 2 (g)

(3) 2HCl (g) + Cr (s) = CrCl 2 (g) + H 2 (g)

(3-a) 2HF (g ) + Cr (s) = CrF 2 (g) + H 2 (g)

(4-a) CrCl x (g) + 1/2 x H 2 (g) = Cr (s) + x HCl (g)

(4-b) CrF x ( g) + 1/2 xH 2 (g) = Cr (s) + xHF (g)

The reactions taking place at the surface of the product also occur as in (5) and (6).

(5-a) CrCl 2 ( g) + H 2 (g) = Cr (s) + 2HCl (g)

(5-b) CrF 2 ( g) + H 2 (g) = Cr (s) + 2HF (g)

(6-a) 2HCl (g ) + x (Cr, Fe) (s) = (Cr, Fe) x Cl 2 (g) + H 2 (g)

(6-b) 2HF (g ) + x (Cr, Fe) (s) = (Cr, Fe) x F 2 (g) + H 2 (g)

(6-a), HCl (g) remaining in the decomposition reaction as shown in Equation (5-a) reaches the halide species on the surface of the active agent in the pack, , The amount of reaction is increased, and they react with hydrogen to become hydrogen chloride, and to produce iron chloride continuously. In the F system, the reaction is basically the same as that of the Cl system, and the reaction takes place in the coating as in (1-b) to (6-b).

However, in the case of halogenation of a Group 1 element such as Na, a gas species that generates a salt unrelated to the reaction as in (1-c) and (1-d) And hydrogen gas or the like should be added to the reaction gas to induce the reaction of the halogen gas. On the other hand, NH 4 Cl is most widely used because it can generate carrier gas without additional gas due to hydrogen decomposition by ammonia gas as in (2-a) after the reaction.

The above-mentioned chemical reaction is performed by reacting the iron or the coating layer of the base material with the activator which is reduced on the surface of the coating layer by moving to the base material while reacting the chromium and iron-based raw materials etc. with the activator in the pack, (Fig. 1) of the active agent which is expressed by the following formula (1).

If the amount of (Cr, Fe) x Cl (g) produced increases as shown in Equation (6), the reverse reaction due to the circulation of the activator occurs on the surface of the material or on the surface of the coating layer and the thickness of the chromium carbide coating layer becomes very thin, The surface is made or the surface of the sintered product is melted, and such surface melting phenomenon is intensified unless it is a uniform material, and a non-uniform coating layer is formed. Therefore, in order to suppress the reverse reaction generated on the surface of the product through the Cr and Fe composition as a coating material, it is necessary to produce FeClx in advance in the pack composition so that chromium and iron react with the coating layer at the same time, . That is, the diffusion principle or the chemical equilibrium theory is applied to suppress the reverse reaction.

As a result, It is necessary to set various composition ratios in the pack within the reaction temperature range and then test it to find the optimal or critical range. Implementing many of these sampling processes is actually very wasteful. The fact that the pack cementation process has to proceed for several hours at high temperature, that various physical properties should be measured for the obtained samples, and that the sample which is not satisfied with the properties are to be discarded, It can be very unreasonable in terms of.

In addition, the advantage of the above reaction is limited to thin chromium diffusion coating of stainless steel which can not be achieved by packementation using only conventional chromium or pack chroming, and does not apply to a hard coating. Accordingly, it is necessary to search for additional activator components in the combination of the chromium coating and the despread material.

Accordingly, an object of the present invention is to provide a coating material in which chromium and iron are mixed with SUS as a base material, an activator (NH 4 Cl, NH 4 F, NaCl, NaF, etc.) containing a halogen group element and an inert filler in a pack, In the pack cementation process, the composition of the chromium and iron is varied, and the actual implementation of the pack cementation process is imitated to observe the change in the amount of FeCl 2 produced during the chemical reaction. From this, the pack cementation process simulation And to provide an optimum composition ratio thereof.

(X = 0 to 100, y = 100 to 0) in a composition ratio (weight ratio) of Cr: Fe,

A reaction formula of Cr with the activator to produce chromium halide is set up to calculate the molar ratio of the product to the reaction product based on the molar ratio of the reaction product to the product,

A simulation method for calculating a composition ratio range of x: y in which the formation ratio of iron halide is close to 0 by calculating a reaction formula for generating iron halide by using the molar ratio of the product to calculate the formation ratio of iron halide; Lt; RTI ID = 0.0 > compositional < / RTI >

In the above simulation method, NH 4 Cl is substituted as an activator to obtain a composition ratio of Cr: Fe x: y (x = 40 to 60, y = 60 to 40) in which the FeCl 2 generation ratio starts to approach zero Therefore, the composition ratio of Cr can be set to 60 or more, and packing can be performed.

On the other hand, when the base material is made of stainless steel, it is preferable to add rare earths to enhance the coating of Cr and to improve the hardness. Accordingly, the present invention is characterized in that Y 2 O 3 is added to the pack composition, and the composition ratio of Cr: Fe is set to one of the optimum ranges as described above. The optimum weight ratio of Y 2 O 3 and activator is calculated by computer simulation Respectively.

According to the present invention, an active agent (NH 4 Cl, NH 4 F, NaCl, NaF, etc.) containing a halogen-group element and a coating material in which chromium and iron are mixed with SUS as a base material and an inert filler are packed and heated to a high temperature The optimum composition ratio of chromium and iron which can prevent the thickness of the chromium carbide coating layer from being thinned in the pack cementation process can be prevented by simulation rather than experimentation, and waste of effort and material can be prevented. As a result, SUS A chromium carbide coating layer excellent in physical properties can be manufactured at a relatively low cost. That is, the quality of the coating layer can still be improved by mixing the expensive chrome powder with the iron powder to control the composition ratio while lowering the cost.

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a schematic diagram showing an active agent depletion model for the generation of active gas in the pack and on the surface of the coating layer by the active agent.
FIG. 2 is a graph showing the simulation results of different packing ratios of Cr: Fe in pack cementation according to the present invention.
FIG. 3 is a graph collecting the molar concentration of the products produced during the reaction in terms of the composition ratio of Cr: Fe from the simulation results of FIG.
FIG. 4 is a graph showing simulation results showing the molar concentration of the products produced during the packing process by adding Y 2 O 3 to the pack composition and varying the weight ratio thereof and the activator composition ratio.
FIG. 5 is a graph showing the molar concentration change of the products depending on the reactants, Y 2 O 3, and activator composition ratio as a result of the simulation of FIG.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

In this embodiment, an active agent (NH 4 Cl, NaCl, NaF, etc.) and an inert filler (Al 2 O 3 ) containing a halogen group element and a coating material obtained by mixing chromium and iron with an iron- In a packed cementation process in which the mixture is heated at a high temperature, and the quantitative transition of the product is obtained by computer simulation while increasing the temperature.

In other words, the real implementation of the pack cementation process is performed by computer simulation, and the transition of the FeCl 2 production amount during the chemical reaction is examined. From this, the critical chromium and iron composition ratios are found. Actually, And the chemical reaction equation and the reaction temperature are derived, and the quantitative transition of the product is calculated.

Therefore, we input the chemical formula of the reactant into the computer, input the chemical reaction formula caused by the reactants, enter the reaction temperature range, and input the quantitative ratio in the desired range for those that need to find the optimal composition ratio among the reactants. The amount of the reactant is calculated by computer using the chemical equilibrium principle according to the chemical reaction formula in consideration of the reaction temperature range, and the amount of the product is calculated by a table or a graph. From this, to be.

In this embodiment, Cr and Fe are set as input materials, NH 4 Cl as an activator is set as an input, the amount of NH 4 Cl is kept constant, and the composition ratio (weight% ratio) of Cr: Fe, (x = 0 to 100, y = 100 to 0).

As a chemical reaction formula,

(1) NH 4 Cl (s ) → NH 4 Cl (g) = NH 3 (g) + HCl (g)

(2) 2NH 3 (g) - > N 2 (g) + 3H 2 (g)

(3) 2HCl (g) + Cr (s) = CrCl 2 (g) + H 2 (g)

(4) CrClx (g) + 1/2 xH 2 (g) = Cr (s) + xHCl (g)

(5) CrCl 2 (g) + H 2 (g) = Cr (s) + 2HCl (g)

(6) 2HCl (g) + x (Cr, Fe) (s) = (Cr, Fe) x Cl 2 (g) + H 2 (g)

, And the molar amount of Cr, NH 4 Cl, Fe, and Y 2 O 3 added was calculated in terms of the addition amount.

The reaction temperature range was 800 to 1200 占 폚.

The mole balance of FeCl 2 , CrCl 2 , CrCl 3 , CrCl 6 , CrN, Cr 2 N, HCl, N 2 and H 2 is traced by temperature by applying chemical equilibrium theory.

Here, the composition ratio range of x: y in which the formation ratio of iron halide (FeCl 2 ) is close to zero is obtained.

FIG. 2 shows eight graphs showing changes in the product every time the composition ratio of Cr: Fe is changed by 10 units by weight. (FeCl 2 , CrCl 2 , CrN, Cr 2 N, and the like) as a molar ratio of Cr: Fe in the abscissa and a ratio of the product in the ordinate as shown in FIG. 3, , ≪ / RTI > HCl) products. It can be seen that starting from when the composition ratio of Cr: Fe is 40:60 (wt.%), As the Cr composition is increased, almost no iron halide (FeCl 2 ) is produced. More safely is from when the composition ratio of Cr: Fe is 60:40 (wt%). Therefore, it is preferable to mix at least Cr (60 wt%) with respect to Fe in actual packing.

In addition, as described above, the same simulation work can be performed using the chemical reaction formula described in the technical item of the background of the invention for active agents such as NH 4 F, NaCl, and NaF. That is, the change of the amount of FeCl 2 produced can be examined by substituting the activator.

On the other hand, when the base material is made of stainless steel, it is preferable to add rare earths to enhance the coating of Cr and to improve the hardness. That is, when the pack composition for the stainless steel base material is composed of only Cr and Fe, the proportion of Cr contained in the coating film is too low. Therefore, rare earths are added to improve the coating film properties. Accordingly, the present invention adds Y 2 O 3 to the pack composition.

The composition ratio of Cr: Fe (weight% ratio) was set to 70:30, and the amount of Y 2 O 3 added to the total amount of the pack composition was changed to 0.1 part by weight to 1 part by weight based on the total amount of the pack composition. 4 Cl was changed to 0.1 part by weight to 2 parts by weight.

The reaction temperature is from 0 to 1200 ° C, and the equations for obtaining the chemical reaction formulas and products are as in the above (1) to (6).

The simulation results are shown in FIG. 4, and FIG. 5 summarizes the partial pressure calculation results of the products according to the composition changes in two graphs.

0.1 to 1 part by weight of Y 2 O 3 and 0.1 to 0.4 part by weight of the activator are preferable because iron halide (FeCl 2 ) is not produced.

Ultimately, when a chromium coating is formed on a base material such as stainless steel by pack cementation, the Cr: Fe composition ratio is 60 to 100: 40 to 0 by weight, Y 2 O 3 is 0.1 to 10 parts by weight, 1 part by weight, and the activating agent is preferably about 0.1 to 0.4 part by weight.

In developing the simulation program, HSC Chemistry 7.1 Outotec is used as a development tool capable of developing various chemical reaction simulation software by incorporating a chemical DB, but the present invention is not limited thereto.

It is to be understood that the invention is not limited to the disclosed embodiment, but is capable of many modifications and variations within the scope of the appended claims. It is self-evident.

No reference symbol.

Claims (9)

A method for obtaining a composition ratio of a reactant and an activator contained in a pack by computer simulation in order to form a coating film containing chromium by pack cementation on a base material made of stainless steel or an iron base material,
As the input variables, the reactants, the amount of reactants, the reaction temperature, and the chemical reaction equations are set,
Setting the amount of products and products as output variables,
A product calculation module for calculating a product according to the amount of the reactant and a chemical reaction formula is set to obtain an amount of product,
Cr and Fe are input as reactants, a halogen compound is input as an activator,
The composition ratio of Cr: Fe is changed to x: y (x = 0 to 100% by weight, y = 100 to 0% by weight)
As the chemical reaction formula, the activator reacts with Cr to form chromium halide, the halogen chromium reacts with hydrogen to form hydrogen peroxide, and the hydrogen halide reacts with iron to form iron halide,
Wherein a composition ratio range of x: y in which the formation ratio of iron halide is close to 0 is obtained as a product. The simulation method according to claim 1, wherein the reaction temperature is set to 700 to 1200 ° C. A method for obtaining a composition ratio of a reactant and an activator contained in a pack by computer simulation in order to form a coating film containing chromium by pack cementation on a base material made of stainless steel or an iron base material,
As the input variables, the reactants, the amount of reactants, the reaction temperature, and the chemical reaction equations are set,
Setting the amount of products and products as output variables,
A product calculation module for calculating a product according to the amount of the reactant and a chemical reaction formula is set to obtain an amount of product,
Cr and Fe are input as reactants, a halogen compound is input as an activator,
The composition ratio of Cr: Fe is changed to x: y (x = 0 to 100% by weight, y = 100 to 0% by weight)
As the chemical reaction formula, the activator reacts with Cr to form chromium halide, the halogen chromium reacts with hydrogen to form hydrogen peroxide, and the hydrogen halide reacts with iron to form iron halide,
The composition ratio range of x: y in which the formation ratio of iron halide as the product is close to 0 is determined,
The obtained composition ratio of x: y is fixedly input with a reaction amount of Cr: Fe, a rare earth oxide is further added to the reaction product,
The amount of the rare earth oxide is changed from 0.1 part by weight to 1 part by weight based on the total amount of the pack composition,
Wherein the amount of the rare earth oxide and the amount of activator are calculated by changing the activator from 0.1 part by weight to 2 parts by weight as a product, the production ratio of which is close to zero. The method of claim 3 wherein the rare earth oxide is the simulation method, characterized in that Y 2 O 3. A computer-readable recording medium recording the simulation program of any one of claims 1 to 4. In order to form a coating film containing chromium by pack cementation in a base material made of stainless steel or an iron base material, the pack contains Cr and Fe as reactants,
An activator and an inert filler,
Wherein the pack is heated to form a coating film containing chromium in the base material. 7. The packementation coating method according to claim 6, wherein the Cr: Fe composition ratio is 60 to 100: 40 to 0 in weight%. The packaged coating method according to claim 7, further comprising 0.1 to 1 part by weight of Y 2 O 3 based on the total amount of the pack composition, and 0.1 to 0.4 parts by weight of the active agent. 7. The packmentation coating method according to claim 6, wherein the heating temperature of the pack is 700 to 1200 占 폚.





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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101730023B1 (en) 2016-08-03 2017-04-26 한국생산기술연구원 Method of manufacturing tungsten composite diffusion coating film using pack cementation

Citations (3)

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Publication number Priority date Publication date Assignee Title
KR920012507A (en) * 1990-12-31 1992-07-27 정명식 Method of forming a diffusion coating layer containing rare earth elements
KR20130101840A (en) * 2012-03-06 2013-09-16 한국생산기술연구원 A method of coating of sintered metal parts by pack cementation and sintered metal parts coating of pack cemetation
KR101499396B1 (en) * 2014-07-10 2015-03-06 한국생산기술연구원 Manufacturing method for member by sintering and coating simultaneously

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Publication number Priority date Publication date Assignee Title
KR920012507A (en) * 1990-12-31 1992-07-27 정명식 Method of forming a diffusion coating layer containing rare earth elements
KR20130101840A (en) * 2012-03-06 2013-09-16 한국생산기술연구원 A method of coating of sintered metal parts by pack cementation and sintered metal parts coating of pack cemetation
KR101499396B1 (en) * 2014-07-10 2015-03-06 한국생산기술연구원 Manufacturing method for member by sintering and coating simultaneously

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"팩 세멘테이션에 의한 알루미나이드 코팅의 컴퓨터 시뮬레이션", 열처리공학회지 8권 1호(페이지 3-11), 1995년 03월 *

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Publication number Priority date Publication date Assignee Title
KR101730023B1 (en) 2016-08-03 2017-04-26 한국생산기술연구원 Method of manufacturing tungsten composite diffusion coating film using pack cementation

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