Technology 25

San Jose State University

LabNotes

Cold Working, Recrystallization, and Grain Growth of Brass

1.0 Learning Objectives
After successfully completing this laboratory workshop, including the assigned reading, the lab bluesheets, the lab quizzes, and any required reports, the student will be able to: Explain the influence of cold working on mechanical properties. Determine recovery, recrystallization, and grain growth for microstructure data and mechanical properties.

2.0 Resources
1. Callister, Materials Science and Engineering: An Introduction, Chapters 7.8-7.13 2. Recrystallization, Grain Growth & Textures, American Society for Metals. Cleveland, 1964 3. Himmel, L., Recovery and Recrystallization of Metals, Gordon & Breach, N.Y., 1963 4. Reed-Hill, R. E., Physical Metallurgy Principles, D. Van Nostrand, Princeton, 1964. 5. Barrett, Nix and Tetelman, The Principles of Engineering Materials, Prentice-Hall, N.Y., 1972.

3.0 Materials Applications

The two primary reasons for plastically deforming engineering metals and alloys are to change their shape for some particular purpose or to change their properties. Often times the deformation process alters the mechanical strength of the material. Cold worked material is harder and stronger than material deformed at other temperatures. These harder materials are advantageous for applications such as machine parts and mechanical supports.

4.0 Background on Cold Working

The temperature at which the deformation takes place is an important determinant of the final properties. If the temperature is relatively low with respect to the melting point of the material (less than 0.3 of the melting point), the deformation process is termed "cold working". A material that is plastically deformed at temperatures above 0.6 of the melting point is said to be hot worked. There are significant differences between the effects of cold and hot working on the properties and structure of materials. While cold-working a metal will tend to increase its strength, other properties such as ductility or corrosion resistance may be negatively affected. Therefore, to remove internal stresses of cold work, it is sometimes desirable to heat treat the metal after cold working. If this heat treatment, or annealing, is conducted at a sufficiently high temperature, a reduction of the stress necessary to
Cold Working of Brass LN 6-1

Technology 25

San Jose State University

LabNotes

further deform the material may be achieved as recrystallization occurs. This experiment introduces us to the relationship between cold work and recrystallization processes and their associated properties. During cold-working, it may take a considerable amount of energy to affect the change in size and shape. Some of the energy expended will appear in the form of heat. A considerable amount of the energy will also be stored in the material. This stored energy is associated with the defects created during the deformation. The free energy of the worked metal will be increased by approximately the amount represented by the stored energy. The most important result of cold working, which accompanies this increase in the number of defects, is strain hardening. Strain hardening is the increase in the yield stress of the metal after it has been deformed. This makes it more difficult to further deform the material. The increase in yield stress comes from the fact that deformation results in a higher density of dislocations. The strain fields around the dislocations most often repel one another, limiting dislocation movement.

4.1 Background on Recrystallization and Grain Growth

To release the stored energy and restore the metal to an energy level closer to its original state, the cold worked metal can be heated, either continuously from a lower to a higher temperature, or isothermally, i.e., at a constant temperature. Energy will be released in three identifiable stages: recovery, recrystallization, and grain growth. The process of releasing stored energy is called annealing. When a cold worked metal is heated, there are some rather gradual property changes that occur without appreciable microstructural alterations and other property changes that are more pronounced and accompany marked alterations in the microstructure. See Callister Fig. 7.22. Recovery is a phenomenon of the first kind that occurs at relatively lower temperatures than are required to produce major grain restructuring. During recovery there may be a slight hardening which accompanies a rearrangement of dislocations into a more stable configuration than existed in the cold-worked state. However, the density of dislocations is only slightly affected, and the basic grain structure is not at all affected. Rearrangement of point defects (such as vacancies) into multi-defect clusters may actually result in a strengthening during recovery. Recrystallization is a phenomenon of the second kind. In contrast to recovery, major structural changes occur. These involve nucleation of strain free grains from the cold-worked metal matrix. When all of the cold-worked metal structure has been replaced by strain free grains, there is a marked decrease in strength and hardness and a corresponding increase in ductility. The main variables that affect recrystallization are 1) time; 2) temperature; 3) amount of prior deformation; 4) composition; 5) initial grain size; and 6) amount of recovery prior to recrystallization.
Cold Working of Brass LN 6-2

Technology 25

San Jose State University

LabNotes

The recrystallization temperature is usually defined as the temperature at which the highly coldworked alloy completely recrystallizes in about 1 hour. After a metal has completely recrystallized, if the high temperature is maintained (or especially if it is increased), the grains will grow in size. This is the third identifiable stage of energy release during annealing: namely, grain growth. The driving force for this growth is in the surface energy of the grain boundaries. The process will measurably decrease the yield strength of the material as the yield stress is inversely proportional to the mean grain diameter. Ductility, on the other hand, increases. Hot working allows recrystallization to occur simultaneously with plastic strain because of the higher temperature. The advantage of hot working over cold-working is that much larger deformations may be made without the danger of over-hardening or cracking the material.

5.0 Cold Working Experiment 5.1 Equipment and Materials

Stanat Rolling Mill Rockwell hardness tester Electrical resistance furnaces Vernier caliper or micrometer 0.25" thick bar of Free-Cutting Brass (260 Brass: 70 Cu - 30 Zn in the dead-soft condition)
NOTE: The sample that you will be rolling is to be left for the class that follows yours. The sample that you will be using for heat treating will be the sample that was cold rolled by the class before yours

5.2 Safety Precautions

5.3.A. Stanat Rolling Mill

SAFETY PRECAUTIONS

1. The Stanat Rolling Mill is to be operated by four students at each time: one to feed, one to receive, one to pass the sample back to the feeder, and the fourth to start and stop the rolling mill. The rolling mill is to be turned off every time the students stop to take hardness and thickness measurements. 2. Use the wooden implement provided to push the specimen through the rolling mill. Do not use fingers or hands. 5.3.C. Rockwell Hardness Tester Do not use Rockwell hardness tester until you have received the necessary instructions. Do not test a specimen when it is warm. Make sure that the bottom of the specimen directly under the indenter is firmly seated on the anvil before applying the major load.

Cold Working of Brass

LN 6-3

Technology 25

San Jose State University

LabNotes

5.3 Cold Working Procedure

1. Read the safety precautions in Section 5.3. 2. Measure the thickness and width of the metal specimen with a micrometer. 3. Carefully read the Rockwell Hardness directions provided by your instructor. Take Rockwell hardness readings on the as-received (annealed) specimen. 4. Roll the specimen in stages using the Stanat Rolling Mill. Reduce the thickness by rolling from approximately 0.25" to 0.125". Use the sequence indicated in the Rolling Schedule instructions provided in Section 5.4. 5. The thickness and hardness of the cold-rolled sample is to be measured at the beginning, and after, each stage. Please remember that each stage consists of four passes. (If you measure the thickness after each pass, you might be there for four hours!) 6. When the thickness has reached approximately 0.125", test for final hardness and measure the width of the sample. 7. Place the pieces from the previous lab section in the respective annealing furnaces per the annealing schedule in Section 5.5. 8. After the prescribed time remove the samples and place them on an aluminum block for rapid cooling to room temperature. 9. Take Rockwell hardness measurements. Use the B Scale.

5.4 Rolling Schedule

Roll in stages from 0.25" to 0.125". Take initial hardness, thickness, and width. Each stage consists of 4 passes as follows: ("zero" rolls to let sample just slip through; then begin rolling in the following manner) One complete revolution equals a pass Reduction per pass = 0.005" Reduction per stage = 0.020" 6-7 stages should be involved to reach 0.125" REMEMBER: - One direction through mill - Record final width

5.5 Annealing Instructions

1. Upon completion of the cold-rolling, the following annealing schedule should be performed. Five post heating temperatures will be used, with a heat treat time of 45 minutes. CAUTION: Always use tongs to place and remove specimens from the furnace. Hot Plate Furnace #4 Furnace #2 Furnace #1 Furnace #3 100C 260C 350C 450C 565C

Cold Working of Brass

LN 6-4

Technology 25

San Jose State University

LabNotes

2. Specimens at temperatures less than 300oC can be directly water quenched to terminate exposure. For higher temperatures (T>300oC), specimens are to be set on aluminum metal blocks to cool for 3 minutes before water quenching. 3. Take the average of three independent readings (RB) for each exposure and record your results on the table provided.

5.6 Data Analysis

1. Compare total % cold work to changes in hardness by calculating according to thickness change and also according to area change, i.e., % CW = (ti - tf)/ti and % CW = (Ai - Af)/Ai 2. Plot hardness vs % CW for the cold worked samples. 3. Plot hardness versus heat-treatment temperature for heat treated samples.

6.0 Report
Your written report should include the following sections: 1. Title Page (on short reports of less than 10 pages, the Abstract may be on the title page) 2. Abstract 3. Introduction: Explain what is going to be done, what materials and equipment will be used, and why it is going to be done (purposes). You will benefit by also indicating what possible uses such data would have in the real world. 4. Background: Explain cold working, strain hardening, recovery, recrystallization, and grain growth. Include why the phenomenon of cold working is important. 4. Procedure: Explain what you did in your own words. Include sketches. Be very careful not to plagiarize the lab notes! 5. Data, Data Analysis: Include your raw data in tables and the calculations and plots listed in Section 5.6. Think carefully about how to present the data before beginning to design your tables and graphs. Combine data into single tables wherever possible and appropriate. Be sure to clearly label all your tables and figures and refer to them in the text. 6. Discussion of Results Explain what the data mean in terms of the purposes of this experiment. Determine whether the results of your data are appropriate, i.e. whether the values make sense compared to published values and/or expectations based on readings. 7. Summary/ Conclusions Summarize what you did and the outcomes of the study. Do not include ANYTHING in this section that has not been already presented in the report. Comment on the importance and relevance of the experiment. 8. References use APA style reference formats for both in-text citations, and for your reference list. See the grading criteria on the next page.

Cold Working of Brass

LN 6-5

Technology 25

San Jose State University

LabNotes

Grading Guidelines for Laboratory Report

Cold Working of Brass

Student Name Score Writing Style & Structure Sentence structure Spelling &Neatness Paragraph structure, logical flow Clarity of writing (Gives ideas directly, does not complicate ideas) Voice (Creativity, Originality) (uses original voice, text not copied from outside source) Technical Content & Structure Abstract Introductory (& Background) Section [Overall]
Gives good overview of experiment and purposes Theory on cold working and strain hardening Theory on recrystallization and grain growth Results [Overall]: Figure Presentations (use appropriate Graphics & Labels,) Distinguishes data from results and reports results from Section 5.6 Shows how data is analyzed Makes some attempt to determine whether results are correct or sensible, links results to theory presented earlier and in texts.

this grading guideline is only a guide (6) Weak Total: /50 (7) (8) (9) (10) Effective

Total:

/100

Discussion [Overall]

Conclusion References Total Report Score = Sum of above/150

Cold Working of Brass

LN 6-6

Technology 25

San Jose State University

LabNotes

Bluesheet 1 Hardness vs Cold-Work Data

Date Group Leader Safety Expert Recorder Materials Manager

Lab Section

Other Group Members Material Original Thickness (in) Original Width (in) Final Width (in) Rockwell B Hardness Rolling Stage 0 1 2 3 4 5 6 7 8 Thickness (in) 1 2 3 AVG. % Cold Work

Cold Working of Brass

LN 6-7

Technology 25

San Jose State University

LabNotes

Bluesheet 2: Hardness vs Annealing Temperature Data Table Date Group Leader Safety Expert Recorder Materials Manager Other Group Members Material Time at temperature (minutes) Lab Section

Hardness as a function of Tempering Temperature Temp (oC) * H B A B A B A B A B A B A B A B A NOTES: *: H = Heat treatment; B = Before Tempering; A = After Tempering Normalizing Factor Average Corrected

AVG.

Cold Working of Brass

LN 6-8