1. Heat Treatment of Steel

2. Heat-Treatment
Heat treatment is a method used to alter the physical, and sometimes chemical properties of a material. The most common application is metallurgical
It involves the use of heating or cooling, normally to extreme temperatures, to achieve a desired result such as hardening or softening of a material
It applies only to processes where the heating and cooling are done for the specific purpose of altering properties intentionally
3. … heating and cooling often occur incidentally during other manufacturing processes such as hot forming or welding

3. Types of Heat-Treatment (Steel)
Annealing / Normalizing,
Case hardening,
Precipitation hardening,
Tempering, and Quenching

4. Figure - Phase diagramam for iron‑carbon system, up to about

6. Iron has Several Phases, depending on Temperature
The phase at room temperature is alpha (), called ferrite (BCC)
At 912C (1674F), ferrite transforms to gamma (), called austenite (FCC)
This transforms at 1394C (2541F) to delta () (BCC)
Pure iron melts at 1539C (2802F)

7. Iron as a Commercial Product
Electrolytic iron - the most pure, at about 99.99%, for research and other purposes where the pure metal is required
Ingot iron - contains about 0.1% impurities (including about 0.01% carbon), used in applications where high ductility or corrosion resistance are needed
Wrought iron - contains about 3% slag but very little carbon, and is easily shaped in hot forming operations such as forging

8. Solubility Limits of Carbon in Iron
Ferrite phase can dissolve only about 0.022% carbon at 723C (1333F)
Austenite can dissolve up to about 2.1% carbon at 1130C (2066F)
The difference in solubility between alpha and gamma provides opportunities for strengthening by heat treatment

9. Time-Temperature-Transformation (TTT)Curve
TTT diagram is a plot of temperature versus the logarithm of time for a steel alloy of definite composition.
It is used to determine when transformations begin and end for an isothermal heat treatment of a previously austenitized alloy
TTT diagram indicates when a specific transformation starts and ends and it also shows what percentage of transformation of austenite at a particular temperature is achieved.
There is also Continuous Cooling Transformation (CCT) Diagram
Austenite -> a solid solution of ferric carbide or carbon in iron; cools to form pearlite or martensite. In plain-carbon steel, austenite exists above the critical eutectoid temperature

10. Time-Temperature-Transformation (TTT)Curve
If austenite is cooled slowly to a temperature below LCT (Lower Critical Temperature), the structure that is formed is Pearlite
The TTT diagram for AISI 1080 steel (0.79%C, 0.76%Mn) austenitised at 900°C

11. Decarburization during Heat Treatment
Decrease in content of carbon in metals is called Decarburization
It is based on the oxidation at the surface of carbon that is dissolved in the metal lattice
In heat treatment processes iron and carbon usually oxidize simultaneously
During the oxidation of carbon, gaseous products (CO and CO2) develop
In the case of a scale layer, substantial decarburization is possible only when the gaseous products can escape
4. … i.e., when the equilibrium pressures of the carbon oxides are high enough to break the scale layer or when the scale is porous.

12. Decarburization Effects
The strength of a steel depends on the presence of carbides in its structure
In such a case the wear resistance is obviously decreased
In many circumstances, there can be a serious drop in fatigue resistance
To avoid the real risk of failure of engineering components, it is essential to minimize decarburization at all stages in the processing of steel
… therefore, loss of carbon from the surface softens and weakens the surface layers .
High %age of carbon in the surface imparts compressive residual stresses that retard initiation of crack
Apply special high-temperature paint on the surface

13. Annealing
It is a heat treatment wherein a material is altered, causing changes in its properties such as strength and hardness
It the process of heating solid metal to high temperatures and cooling it slowly so that its particles arrange into a defined lattice

14. Types of Annealing Full Annealing
Stress-Relief Annealing (or Stress-relieving)
Normalizing
Isothermal Annealing
Spheroidizing Annealing (or Spheroidizing )

15. 
 +Fe3C

16. Full Annealing
raising the temperature about 50 ºC (90 ºF) above the Austenitic temperature line A3 or line ACM in the case of Hypoeutectoid steels (steels with < 0.77% Carbon) and 50 ºC (90 ºF) into the Austenite-Cementite region in the case of Hypereutectoid steels (steels with > 0.77% Carbon).
cooled at the rate of about 20 ºC/hr (36 ºF/hr) in a furnace to about 50 ºC (90 ºF) into the Ferrite-Cementite range.
The grain structure has coarse Pearlite with ferrite or Cementite (depending on whether hypo or hyper eutectoid). The steel becomes soft and ductile.

17. Process Annealing
heating it to about 700 ºC (1292 ºF) should suffice. This is held long enough to allow recrystallization of the ferrite phase, and then cooled in still air.
the only change that occurs is the size, shape and distribution of the grain structure.

18. Causes of Residual Stresses
Stress-Relief Annealing
Causes of Residual Stresses
1. Thermal factors (e.g., thermal stresses caused by temperature gradients within the workpiece during heating or cooling) 2. Mechanical factors (e.g., cold-working) 3. Metallurgical factors (e.g., transformation of the microstructure)

19. Stress-Relief Annealing
It is an annealing process below the transformation temperature A1 ( ºC), with subsequent slow cooling, the aim of which is to reduce the internal residual stresses in a workpiece without intentionally changing its structure and mechanical properties
Critical Temperature of Steel is 724°C

20. How to Remove Residual Stresses?
R.S. can be reduced only by a plastic deformation in the microstructure.
This requires that the yield strength of the material be lowered below the value of the residual stresses.
The more the yield strength is lowered, the greater the plastic deformation and correspondingly the greater the possibility or reducing the residual stresses
The yield strength and the ultimate tensile strength of the steel both decrease with increasing temperature
Last -> Because of this, stress-relief annealing means a through-heating process at a correspondingly high temperature

21. Stress-Relief Annealing Process
For plain carbon and low-alloy steels the temperature to which the specimen is heated is usually between 450 to 650˚C, whereas for hot-working tool steels and high-speed steels it is between 600 to 750˚C
This treatment will not cause any phase changes, but recrystallization may take place.
Machining allowance sufficient to compensate for any warping resulting from stress relieving should be provided

22. Stress-Relief Annealing – R.S.
In the heat treatment of metals, quenching or rapid cooling is the cause of the greatest residual stresses
To activate plastic deformations, the local residual stresses must be above the yield strength of the material.
Because of this fact, steels that have a high yield strength at elevated temperatures can withstand higher levels of residual stress than those that have a low yield strength at elevated temperatures
Soaking time also has an influence on the effect of stress-relief annealing
… A high level of residual stress is generally to be expected with workpieces that have a large cross section, are quenched at a high cooling rate, and are made of a steel of low hardenability .
… i.e., on the reduction of residual stresses
Soaking time -> The hold time at maximum temperature for a heat-treatment process

23. Relation between heating temperature and Reduction in Residual Stresses
Higher temperatures and longer times of annealing may reduce residual stresses to lower levels

24. Stress Relief Annealing - Cooling
The residual stress level after stress-relief annealing will be maintained only if the cool down from the annealing temperature is controlled and slow enough that no new internal stresses arise.
New stresses that may be induced during cooling depend on the (1) cooling rate, (2) on the cross-sectional size of the workpiece, and (3)on the composition of the steel
2. Composition of steel has complicated effect on residual stresses during cooling phase

25. 2. Normalizing
A heat treatment process consisting of austenitizing at temperatures of 30–80˚C above the AC3 transformation temperature followed by slow cooling (usually in air)
The aim of which is to obtain a fine-grained, uniformly distributed, ferrite–pearlite structure
Normalizing is applied mainly to unalloyed and low-alloy hypoeutectoid steels
For hypereutectoid steels the austenitizing temperature is 30–80˚C above the AC1 or ACm transformation temperature
Hypoeutectoid -> At L.H.S of Eutectoid point
For hypereutectoid steels, normalizing is a special process

26. Normalizing – Heating and Cooling
a, Heating; b, holding at austenitizing temperature; c, air cooling; d, air or furnace cooling

27. Normalizing – Austenitizing Temperature Range
For hypereutectoid steels, whether to heat above ES line or SK line depends upon alloying materials and content. Heating above SE line is ONLY required for the alloy steels whose alloying elements form secondary carbides (e.g. Vanadium Carbide, WC, etc). For unalloyed hyper steels, heating above Ac1 (SK) line is enough

28. Effect of Normalizing on Grain Size
Normalizing refines the grain of a steel that has become coarse-grained as a result of heating to a high temperature, e.g., for forging or welding
Fig. - Carbon steel of 0.5% C. (a) As-rolled or forged; (b) normalized. Magnification 500
Normalizing generally gives slightly harder substrate as compared to annealing because of fine grained pearlite in normalizing as compared to coarse-grained in annealing

29. Need for Normalizing
Grain refinement or homogenization of the structure by normalizing is usually performed either to improve the mechanical properties of the workpiece or (previous to hardening) to obtain better and more uniform results after hardening
Normalizing is also applied for better machinability of low-carbon steels

30. Normalizing after Rolling
After hot rolling, the structure of steel is usually oriented in the rolling direction
To remove the oriented structure and obtain the same mechanical properties in all directions, a normalizing has to be performed
1. … mechanical properties differ between the rolling direction and the direction perpendicular to it

31. Normalizing after Forging
After forging at high temperatures, especially with workpieces that vary widely in crosssectional size, because of the different rates of cooling from the forging temperature, a heterogeneous structure is obtained that can be made uniform by normalizing

32. Normalizing – Holding Time
Holding time at austenitizing temperature may be calculated using the empirical formula:
t = 60 + D
where t is the holding time (min) and D is the maximum diameter of the workpiece (mm).

33. Normalizing - Cooling
Care should be taken to ensure that the cooling rate within the workpiece is in a range corresponding to the transformation behavior of the steel-in-question that results in a pure ferrite–pearlite structure
If, for round bars of different diameters cooled in air, the cooling curves in the core have been experimentally measured and recorded, then by using the appropriate CCT diagram for the steel grade in question, it is possible to predict the structure and hardness after normalizing

34. 3. Isothermal Annealing
Hypoeutectoid low-carbon steels as well as medium-carbon structural steels are often isothermally annealed, for best machinability
An isothermally annealed structure should have the following characteristics:
1. High proportion of ferrite
2. Uniformly distributed pearlite grains
3. Fine lamellar pearlite grains
1. … because a well-differentiated, nontextured (non-directional) ferrite–pearlite structure is the optimum structure for machinability of these steels. If low-carbon steels are soft (Spheroidizing) annealed, they give long shavings when turned and a bad surface appearance because of the accumulation of the material on the tool’s cutting edge. On the other hand, nonannealed workpieces, having harder structural constituents like bainite, result in heavy wear of the cutting edge when machined.

35. Principle of Isothermal Annealing
Bainite formation can be avoided only by very slow continuous cooling, but with such a slow cooling a textured (elongated ferrite) structure results (hatched area)
M-> Martensite; B-> Bainite; F-> Ferrite
There is only one way to avoid both the formation of bainite and the formation of a textured structure and this is the isothermal annealing process,

36. Process - Isothermal Annealing
Austenitizing followed by a fast cooling to the temperature range of pearlite formation (usually about 650˚C.)
Holding at this temperature until the complete transformation of pearlite
and cooling to room temperature at an arbitrary cooling rate
M-> Martensite; B-> Bainite; F-> Ferrite

37. 4. Spheroidizing Annealing
It is also called as Soft Annealing
Any process of heating and cooling steel that produces a rounded or globular form of carbide
It is an annealing process at temperatures close below or close above the AC1 temperature, with subsequent slow cooling

38. Spheroidizing - Purpose
The aim is to produce a soft structure by changing all hard constituents like pearlite, bainite, and martensite (especially in steels with carbon contents above 0.5% and in tool steels) into a structure of spheroidized carbides in a ferritic matrix
a medium-carbon low-alloy steel after soft annealing at 720C;
h-speed steel annealed at 820C.
0. The microstructure of steel before soft annealing is either ferrite–pearlite (hypoeutectoid steels), pearlite (eutectoid steels), or cementite–pearlite (hypereutectoid steels)
For hypoeutectiod steels, there is no need to do Spheroidizing annealing

39. Spheroidizing - Uses
Such a soft structure is required for good machinability of steels having more than 0.6%C and for all cold-working processes that include plastic deformation.
Spheroidite steel is the softest and most ductile form of steel
… Whereas for cold-working processes the strength and hardness of the material should be as low as possible, for good machinability medium strength or hardness values are required.
Spheroidite can form at lower temperatures but the time needed drastically increases, as this is a diffusion-controlled process.

40. Spheroidizing - Mechanism
The physical mechanism of soft annealing is based on the coagulation of cementite particles within the ferrite matrix, for which the diffusion of carbon is decisive
Globular cementite within the ferritic matrix is the structure having the lowest energy content of all structures in the iron–carbon system
The carbon diffusion depends on temperature and time
Coagulate -> to change from a fluid into a thickened mass
2. i.e. Spheroidite

41. Spheroidizing - Mechanism
The solubility of carbon in ferrite, which is very low at room temperature (0.02% C), increases considerably up to the Ac1 temperature
At temperatures close to Ac1, the diffusion of carbon, iron, and alloying atoms is so great that it is possible to change the structure in the direction of minimizing its energy content

42. Spheroidizing - Process
Prolonged  heating  at  a  temperature  just  below the  lower  critical  temperature,  usually  followed  by  relatively  slow cooling
In  the  case  of  small  objects  of  high  C steels,
spheroidizing  result  is  achieved  more  rapidly by  prolonged heating to temperatures alternately within and slightly below the critical temperature range
Tool steel is generally spheroidized by heating to a temperature of 749°-804°C and higher for many alloy tool steels, holding at heat from 1 to 4 hours, and cooling slowly in the furnace
1. 25 – 35 hours heating

43. CASE HARDENING
Case hardening or surface hardening is the process of hardening the surface of a metal, often a low carbon steel, by infusing elements into the material's surface, forming a thin layer of a harder alloy.
Case hardening is usually done after the part in question has been formed into its final shape

44. Case-Hardening - Processes
Flame/Induction Hardening
Carburizing
Nitriding
Cyaniding
Carbonitriding

45. Flame and induction hardening
Flame or induction hardening are processes in which the surface of the steel is heated to high temperatures (by direct application of a flame, or by induction heating) then cooled rapidly, generally using water
This creates a case of martensite on the surface.
A carbon content of 0.4–0.6 wt% C is needed for this type of hardening
Application Examples -> Lock shackle and Gears
Lock -> where the outer layer is hardened to be file resistant; Gears -> where hard gear mesh surfaces are needed to maintain a long service life while toughness is required to maintain durability and resistance to catastrophic failure

46. Carburizing
Carburizing is a process used to case harden steel with a carbon content between 0.1 and 0.3 wt% C.
Steel is introduced to a carbon rich environment and elevated temperatures for a certain amount of time, and then quenched so that the carbon is locked in the structure
Example -> Heat a part with an acetylene torch set with a fuel-rich flame and quench it in a carbon-rich fluid such as oil

47. Carburizing Contd.
Carburization is a diffusion-controlled process, so the longer the steel is held in the carbon-rich environment the greater the carbon penetration will be and the higher the carbon content.
The carburized section will have a carbon content high enough that it can be hardened again through flame or induction hardening

48. Carburizing Contd.
The carbon can come from a solid, liquid or gaseous source
Solid source -> pack carburizing. Packing low carbon steel parts with a carbonaceous material and heating for some time diffuses carbon into the outer layers.
A heating period of a few hours might form a high-carbon layer about one millimeter thick
Liquid Source -> involves placing parts in a bath of a molten carbon-containing material, often a metal cyanide
Gaseous Source -> involves placing the parts in a furnace maintained with a methane-rich interior

49. Nitriding
Nitriding heats the steel part to 482–621°C in an atmosphere of NH3 gas and broken NH3.
The time the part spends in this environment dictates the depth of the case.
The hardness is achieved by the formation of nitrides.
Nitride forming elements must be present in the workpiece for this method to work.
Advantage -> it causes little distortion, so the part can be case hardened after being quenched, tempered and machined
4. … these elements include chromium, molybdenum, and aluminium

50. Cyaniding Cyaniding is mainly used on low carbon steels.
The part is heated to °C in a bath of sodium cyanide (NaCN)and then is quenched and rinsed, in water or oil, to remove any residual cyanide.
The process produces a thin, hard shell ( mm) that is harder than the one produced by carburizing, and can be completed in 20 to 30 minutes compared to several hours.
It is typically used on small parts.
The major drawback of cyaniding is that cyanide salts are poisonous
0. Cyaniding is a case hardening process that is fast and efficient
3. … so the parts have less opportunity to become distorted
4. … such as bolts, nuts, screws and small gears

51. Carbonitriding
Carbonitriding is similar to cyaniding except a gaseous atmosphere of ammonia and hydrocarbons (e.g. CH4)is used instead of sodium cyanide.
If the part is to be quenched then the part is heated to 775–885°C; if not then the part is heated to 649–788°C

52. PRECIPITATION HARDENING
Precipitation hardening (or age hardening), is a heat treatment technique used to increase the yield strength of malleable materials
Malleable materials are those, which are capable of deforming under compressive stress
It relies on changes in solid solubility with temperature to produce fine particles of an impurity phase, which blocks the movement of dislocations in a crystal's lattice
… include aluminum, magnesium, nickel and titanium, and some stainless steels
this is often characterized by the material's ability to form a thin sheet by hammering or rolling. Ductility and malleability do not always correlate with each other; for instance, gold is both ductile and malleable, but lead is only malleable
Precipitate -> Separate as a fine suspension of solid particles

53. Precipitation Hardening
Since dislocations are often the dominant carriers of plasticity, this serves to harden the material
The impurities play the same role as the particle substances in particle-reinforced composite materials.
Alloys must be kept at elevated temperature for hours to allow precipitation to take place. This time delay is called aging
2. e.g. secondary carbides of Tungsten in high-speed steel. Just as the formation of ice in air can produce clouds, snow, or hail, depending upon the thermal history of a given portion of the atmosphere, precipitation in solids can produce many different sizes of particles, which have radically different properties

54. Precipitation Hardening
Two different heat treatments involving precipitates can change the strength of a material:
solution heat treating
precipitation heat treating
Solution treatment involves formation of a single-phase solid solution via quenching and leaves a material softer
Precipitation treating involves the addition of impurity particles to increase a material's strength

55. Precipitation Mechanism – Aluminum Alloy

56. Effect of Aging Time on Precipitates

57. QUENCHING and TEMPERING
In quench hardening, fast cooling rates, depending on the chemical composition of the steel and its section size, are applied to prevent diffusion-controlled trans formations in the pearlite range and to obtain a structure consisting mainly of martensite and bainite
However, the reduction of undesirable thermal and transformational stresses usually requires slower cooling rates
0. the cooling rate and the shape of the cooling curve influence the course of phase transformations, residual stresses and distortion
2. Quenching processes therefore require the selection of cooling rates that are fast enough to permit the desired microstructure to form but slow enough to minimize residual stresses and distortion.

58. Quenching
To harden by quenching, a metal must be heated into the austenitic crystal phase and then quickly cooled
Cooling may be done with forced air, oil, polymer dissolved in water, or brine
Upon being rapidly cooled, a portion of austenite (dependent on alloy composition) will transform to martensite
2. Depending on the alloy and other considerations (such as concern for maximum hardness vs. cracking and distortion), …
Water soluble polymers -> Polylactic Acid and Polyethylene Glycol
3. … The quenched hardness of a metal depends on its chemical composition and quenching method

59. Quenching
Cooling speeds, from fastest to slowest, go from polymer, brine, fresh water, oil, and forced air
However, quenching a certain steel too fast can result in cracking, which is why high-tensile steels such as AISI 4140 should be quenched in oil, tool steels such as H13 should be quenched in forced air, and low alloy such as AISI 1040 should be quenched in brine
Metals such as austenitic stainless steel (304, 316), and copper, produce an opposite effect when these are quenched: they anneal

60. Tempering
Untempered martensite, while very hard, is too brittle to be useful for most applications.
In tempering, it is required that quenched parts be tempered (heat treated at a low temperature, often 150˚C) to impart some toughness.
Higher tempering temperatures (may be up to 700˚C, depending on alloy and application) are sometimes used to impart further ductility, although some yield strength is lost
2. A method for alleviating this problem is called tempering

61. Tempering
Tempering is done to toughen the metal by transforming brittle martensite or bainite into a combination of ferrite and cementite or sometimes Tempered martensite
Tempered martensite is much finer-grained than just-quenched martensite
The brittle martensite becomes tough and ductile after it is tempered.
Carbon atoms were trapped in the austenite when it was rapidly cooled, typically by oil or water quenching, forming the martensite

62. Tempering
The martensite becomes tough after being tempered because when reheated, the microstructure can rearrange and the carbon atoms can diffuse out of the distorted body-centred-tetragonal (BCT) structure.
After the carbon diffuses out, the result is nearly pure ferrite with body-centred structure.