National University of Engineering

FACULTY OF ENGINEERING GEOLOGICAL, MINING AND

METALLURGICAL-FIGMM

STRUCTURE AND PROPERTIES OF MATERIALS

I-524R

Report: RECRYSTALLIZATION

Name: Tinoco Falero Junior Anderson

Code: 20132220B

Professor: Ing. Manuel Cruz Torres

LIMA - PERU
2017
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Index

Objectives .... Pg. 2

Theoretical basis ....... Pg 3-6

Equipment and Materials . Pg 7

Experimental procedure ...... Pg 7-9

Results ........ Pg 10-18

Conclusions .... Pg 19

Recommendations Pg 19

Bibliography .... Pg 20

Questionnaire . Pg 21-29

Annexs . Pg 30-31

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Objectives

I. To study the effect of annealing time on the crystallization to

specimens of ASTM A36 steel worked in cold (wires).
II. Determine the average grain size, according to the ASTM E112, for
specimens of ASTM A36 steel annealed at different times and to
determine the effect of annealing time on the average grain size.
III. Determine the effect of the degree of crystallization on the hardness
of the steel ASTM A36.

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Theoretical basis

Annealing of the materials deformed

Metallic materials harden when deformed (phenomenon of acrimony and soften

when they are annealed. This behavior has been known to man since the
beginning of our civilization, and today it is exploited in the industrial production
of metals and alloys using the thermo mechanical treatment.

During thermomechanical treatment, the metal is exposed to a force of plastic

deformation, that hardens and at a high temperature, which leads to a softening
either during or after deformation . A thermomechanical pulping process can, for
example, be in hot, cold rolling or cold-rolled followed by an annealing, that is to
say, a thermal treatment at elevated temperatures.

The exposure to the strength and temperature gives rise to the dynamic
processes of recovery and recrystallization dynamics. In the case in which the
heat (annealing) is applied after the deformation, the processes that are given
are the recovery, the recrystallization and grain growth. These processes directly
affect the properties of the metal (Figure 1 and 2). This is because there are
substantial and important relationships between the structure of metallic
materials and their properties.

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Figure N1: Change of hardness, electrical resistivity and stored energy (represented
by a differential of power) for the treatment of pure copper deformed.

Figure N2: elastic limit (YS) and the ultimate tensile strength (UTS) at room
temperature after warming up a sheet of aluminum foil in cold weather.

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2.2. Determination of the average grain size

The determination of the size of grain is a measurement is very important for the
characterization and development of materials, as well as for quality control in the
manufacturing process. The grains are crystals of irregular shapes whose spatial
dimensions are very difficult to measure. The STEREOLOGY allows to infer
properties of three-dimensional bodies from their projections in a plane; that is,
flat obtained from cross sections of the bodies. There are several methodologies
to measure the size of grain on a surface properly prepared and then convert
them mathematically in space estimators of grain size. The measurements are
usually performed on microstructural features zero, uni-dimensional and the grain
size is expressed in units of Linear or two-dimensional (lengths and areas).

The ASTM E112, standard method to determine the size of grain, covers four
methods, which are the following:

Planimetric Method or Jeffries

Method of Abrams

Method of Heyn

Method of Hilliard

For this job is going to perform the measurement of the size of grain by the
method of Jeffries, detailing this procedure.

2.2.1. Method planimeter of Jeffries

In the planimetric procedure is part of a circle or rectangle of area known (usually

5000 mm2 to simplify the calculation) in an electron micrograph or glass on the
screen, you must select an extension to give you at least 50 grains in the field to
be counted (this to give more accurate results).

Then when the image is centered correctly, count the number of grains within that
area, the sum of all the grains included completely within the area known more
than half of the number of kernels cut by the circumference of the area gives the
number of grains equivalent, as measured by the extension used, within the area.
If this number is multiplied by the multiplier of Jeffries, f, the product will be the
number of grains per square millimeter NA. The number of grains per square
millimeter at 1X, NA, is calculated from:

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= ( + ) . . 1
2

Where:
2
: Jeffries ( = )

M: Magnification used

To: Area in square millimeters.

After taking this value you can go to tables (see annex 2), or by using the following
equation to calculate the value of G (number of grain size according to ASTM).

= (3.321928 ) 2.954 . 2

It should be noted that the equation N1 is valid for circles, but for this job will
work with square, due to reasons that will be explained below, whose formula is
also covered in the standard and is the following:

2
= ( + + 1) . . 3
2

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Equipment and Materials

The equipment used in the experimental procedure were:

1. Pieces of wire drawing steel ASTM A36.

Figure N3: Measuring cylinder of steel ASTM A36.

2. Sandpaper Number # 150, 200, 300, 400, 600, 800.1000, alumina 0.5um
2um and nital metallographic preparation and chemical attack
respectively.

Figure N4: Equipment for the metallographic

preparation.

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3. Oven for heat treatment.

Figure N5: oven for heat treatment of metals (relays).

4. Metallographic microscope.

Figure N6: metallographic microscope (Zeiss).

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EXPERIMENTAL PROCEDURE
1. In the first place, is the metallographic preparation of the specimens of
steel (ASTM A36), for this case are six test pieces.

2. Once the metallographic preparation (up to the alumina) proceeds with the
heat treatment in the oven, 6 recociendo The pieces to 450C and 600C,
but with different times of annealing and previously the six
specimens without treatment are the development of microstructure (to
be used as a standard), as detailed in the table below.

Table N1: annealing times for each test piece at 450C.

Annealing Temperature: 450C Time of annealing

0C 0 minutes
51C 5 minutes
450C 47 minutes
450C 167 minutes

Table N2: annealing times for each test piece at 600C.

Annealing Temperature: 600C Time of annealing

0 C 0 minutes
51 C 5 minutes
600 C 67 minutes
600 C 162 minutes

3. Once the heat treatment is applicable to the development of the

microstructure (but not before giving a polished thin the test tubes) using
chemical reagents suitable for this case is use the nital to 2.5%.

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RESULTS
1. Metalografias of the cylinders :

LAS SEIS PROBETAS STANDARD TRACCIONADAS

Probeta 1:

Figura N7: Probeta 1 estndar (sin tratamiento trmico)

donde se observan los granos deformados, 500x.

Probeta 2

Figura N8: Probeta 2 estndar (sin tratamiento trmico) donde se

observan los granos deformados, 500x

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Probeta 3:

Figura N9: Probeta 3 estndar (sin tratamiento trmico)

donde se observan los granos deformados, 500x

Probeta 4:

Figura N10: Probeta 4 estndar (sin tratamiento

trmico) donde se observan los granos deformados, 500x

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Probeta 5:

Figura N11: Probeta 5 estndar (sin tratamiento

trmico) donde se observan los granos deformados, 500x

Probeta 6:

Figura N12: Probeta 4 estndar (sin tratamiento

trmico) donde se observan los granos deformados, 500x

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LAS SEIS PROBETAS TRATAMIENTO TRMICO 450C

Probeta 1:

Figura N13: Probeta 1 con tratamiento trmico 450 C donde

se observan casi todos los granos ya cristalizados,500x.

Probeta 2

Figura N14: Probeta 2 con tratamiento trmico donde se

observan casi todos los granos ya cristalizados, 500x.

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Probeta 3:

Figura N15: Probeta con tratamiento trmico donde se

observa dos zonas con diferentes tamaos de grano, 500x.

Probeta 4:

Figura N16: Probeta con tratamiento trmico donde se

observan todos los granos ya cristalizados,500x.

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Probeta 5:

Figura N17: Probeta con tratamiento trmico donde se

observan todos los granos ya cristalizados,500x.

Probeta 6:

Figura N18: Probeta con tratamiento trmico donde se

observan todos los granos ya cristalizados,500x.

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LAS SEIS PROBETAS TRATAMIENTO TRMICO 600C

Probeta 1:

Figura N19: Probeta 1 con tratamiento trmico a 600 C

donde se observan los granos deformados, 500x.

Probeta 2

Figura N20: Probeta con tratamiento trmico donde se

observan casi todos los granos ya cristalizados, 500x.

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Probeta 3:

Figura N21: Probeta con tratamiento trmico donde se

observa dos zonas con diferentes tamaos de grano, 500x.

Probeta 4:

Figura N22: Probeta con tratamiento trmico donde se

observan todos los granos ya cristalizados,500x.

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Probeta 5:

Figura N23: Probeta 5 con tratamiento trmico donde

se observan todos los granos ya cristalizados,500x.

Probeta 6:

Figura N24: Probeta 6 con tratamiento trmico donde

se observan todos los granos ya cristalizados,500x.

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Conclusions
1. The annealing time significantly influences the degree of crystallization
and about the size of grain crystallized and this influences the mechanical
properties of the material, that is to say, more time of annealing decreases
the temperature of recrystallization.

2. Once you reach the complete crystallization and recociendo annealing

(longer) increases the size of grain influencing negatively on the
mechanical properties of the material.

3. The main objective of the annealing is to reduce the excessive hardness

of the material product of the phenomenon of "sourness" and this is with
the recrystallization as shown in TABLE N 1 and N 2.

4. When an excessive amount of time of annealing occurs the process known

as "Grain" that is the growth of grain, so that the hardness decreases to
values lower than his cold worked and this is a negative aspect in the
material by what must be avoided.

5. Another important factor to point out for the crystallization is the degree of
deformation of the material that translates into elastic energy stored and
this is the cause of the existence of the recrystallization of the material.
The greater the degree of deformation it is said that decreases the
temperature of recrystallization of the material.

Recommendations
1. It is recommended to work carefully in the metallographic preparation and
especially in the chemical attack to avoid burning the specimen is tested
with different times and different concentrations of reagent Nital, for this
case used the reagent with a concentration of 2.5%.

2. For the measurement of the size of grain before everything must be

calibrated by means of the microscope micrometers in order to have a real
scale of the image and be able to work properly as you said the ASTM E
112.

3. The method of Jeffries tells us that we can work with circles or rectangles,
but for this case is going to work with rectangles since the error is less than
working with circles as will be explained below.

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Bibliography
1. SYDNEY H.AVNER (1988). Introduction to the Physical Metallurgy. Mc
Graw Hill.

2. ASTM International - E112 - 10. Current edition approved Nov. 1, 2010.

Published December 2010.Originally approved in 1955. Last previous
edition approved 2004 as E112 - 96(2004). United States.

3. TASM INTERNATIONAL (1987). Metal's Handbook Volume 09

METALLOGRAPHY and Structure.

4. "Evaluation of the estimation methods for the measurement of grain size,

and effects the size of grain in the microhardness", University Thesis,
Lima-peru, 2013.

5. "Theory of the recrystallization", Ing. July Uzzah Teruya, class notes,

Lima-peru, 2016.

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Questionnaire
1. Mechanisms that occur in the recovery phase, recrystallization and
grain size.
Plastically deforms when a metal at temperatures well below its melting
point, it is said that the metal has been cold worked. Most of the energy
used in this deformation is dissipated as heat, storing a small fraction as
deformation energy. The latter is accumulated in the form of dislocations
and point defects, for example: broken links and vacancies. How
increasing the density of dislocation is not smooth, there are areas of
higher density, which leads to the generation of cells.
When heated this material occur two processes that decrease the internal
energy stored, recovery and recrystallization.
In addition to the above-mentioned processes and depending on the time
and the temperature at which heat the material, there may be a third
process called grain growth, this occurs when annealing is continued
after the completion of the recrystallization.

Recovery mechanisms:

The recovery is the first stage of the annealing process. The relief of
internal efforts caused by cold working, ( residual stresses), on the other
hand, microstructural changes and modification of some properties,
among which we can highlight: the annihilation of point defects, the poly
and the decrease in electrical resistance.

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Temperature Mechanism
Low Migration of point defects
toward sinks (grain boundaries,
dislocations, etc.)
Combination of point defects
Media New array of dislocations
Annihilation of dislocations
Growth of subgranos
High Climbed dislocations
Agglutination of dislocations
Poly
Of recrystallization mechanisms:

The recrystallization occurs due to the nucleation and growth of new grains
that contain few dislocations.
The growth of these new grains occurs at the edges of the cell structure
pollinated, eliminating most of the dislocations.
The new recristalizados grains taken at more or less regular forms, due
to the anisotropies their rate of growth.
When beans come in contact with each other, it is just the phase knock
recrystallization and enters the phase called grain growth.
How has significantly reduced the number of dislocations, the metal
recrystallized has low resistance, but a high ductility.

Grain growth mechanisms:

In a metal completely crystallized, the driving force for the growth of the
grains corresponds to the decrease in the energy associated with the
edges of grain.
The growth of the new grain is produced by movement of the
recrystallized grain-grain interface deformed.
The edges of grain tend to move toward the center of the curve.
The angle between three edges of grain is of about 120.

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2. Describe and substantiate the acrimony and annealing.

The acrimony:

It is a mechanical property that acquire the metals as a result of the cold

deformation, also known as hardening process by acrimony, that increases its
hardness, brittleness and resistance, although the loss, at the same time, its
ductility and malleability. In fact, the materials with a high pungency are also
referred to as citrus fruits.

The annealing:

It is one tratamiento trmico of whose purpose is the softening, the recovery of

the structure or the elimination of internal tensions generally in metals.Any metal
that has been treated has resulted in an alteration of the physical properties of
the same. The annealing consists in heating the metal to a certain temperature
to then leave it to cool slowly, usually, by turning off the oven and leaving the
metal in its interior to its temperature decreases gradually. The process ends
when the metal has reached room temperature. Through the combination of
several jobs in cold and several soft annealed coils are able to obtain large
deformations in metals that, otherwise, we would not be able to achieve.

Annealing against acrimony

The acrimony against annealing is a heat treatment of metals whose goal is to

return to the metal, that has gone through a cold deformation, features such as
the plasticity, ductility, toughness, in addition to eliminating internal tensions, all
of which results in that the metal retrieves conditions to be worked again. It is a
process that has three phases: heat the material up to the annealing temperature,
keep it at that temperature for a period of time, and, finally, let it cool down slowly
and gradually.

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3. The photomicrographs of the measuring standard and

recristalizadas to 450 C and 600 C. Find the speed of global
warming oven yes ( 600 C= 27 minutes and 450 C).

T 450C :
Time (min) T C
Note: Due to the fact that they took a
0 0 few points cannot be taken as a
5 51 heating profile, since according to
47 450 criterion was due to take temperature
167 450 every 30 minutes

Rate of heating The Oven 450 C

500
450
400
350
Temperature C

300
250 Speed global 9.54552276
200
warming
150
100
50
0
0 50 100 150 200
Time (minutes)

T 600C :

Time (min) T C Note: Due to the fact that they took a

0 0 few points cannot be taken as a
5 51 heating profile, since according to
67 600 criterion was due to take temperature
162 600 every 30 minutes

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Rate of heating of the Oven 600 C

700

600

500
Temperature C

400

300
Pending= speed
200

100

0
0 50 100 150 200
Time (minutes)

Speed 8.91277818
global
warming
4. Find the grain size of the measuring standards ASTM A36 of
recrystallization temperature to 450 C and 600 C by the planimetric
method of JEFFRIES. and method of Hillary.

As we mentioned before is going to perform this method by using

rectangles, as this avoids the error produced by the count of grains in the
circumference using the equation N3.

2
= ( + + 1) . . 3
2

1-piece: "Standard"

Steps:
1) Using the Image program "J" we opened the image and to put my
scale of work:

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Where:

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2) By using the tools then selects the first rectangle in the first quadrant
in the following way:

3) Then we proceed to improve the image to count the grains inside and
the queestan that intersect the rectangle:

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4) The data found are the following:

= 500

= 16

= 12

= 520.576 2

Replacing in the equation N3:

5002 12
= ( 16 + + 1)
520.576 2

= 11045.46 , 1
2

Replacing in the equation N2:

= (3.321928 ) 2.954 . 2

= 10.4771

Approaching this value to your nearest integer:

= 10

In the same way you work for the following rectangles, way to have grain sizes
since metalografias for each test piece

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5. Define Ostwald ripening in recrystallization for both liquids and

solids.

The molecular diffusion or Ostwald ripening is an observed phenomenon in

solid or liquid solutions soles that describes the change of a homogeneous
structure with time. With time, the small crystals or particles of sun dissolved,
and become deposited in large crystals or particles of sun.[]

The dissolution of small crystals or particles of sun and soil redeposition of the
species dissolved in the surfaces of the larger crystals or particles of sun was
described for the first time Wilhelm Ostwald in 1896.[] Ostwald ripening is
usually found in water-in-oil emulsiones, while the floculacin is in oil-in-water
emulsions

Figure N25: outline of the process of ripening Ostwald

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X. Annexs
1. Digital Archive.

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2. ASTM, table to find the ASTM grain size (G).

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