Chapter V

Apply Heat Treatment and Metallurgical Processes

Red Seal Practice study guide with diagrams.

Applying Heat Treatments and Metallurgical Processes

Introduction to Heat Treatment of Steels

Heat treatment is the set of controlled heating and cooling operations applied to a metal in its solid state, with the goal of modifying its mechanical, physical, or chemical properties. For the tool and die maker, mastery of these processes is essential: dies, punches, cutting tools, and gauges must exhibit precise hardness, toughness, and wear resistance depending on their function.

The iron-carbon (Fe-C) diagram is the fundamental basis for understanding all heat treatments. It illustrates phase transformations as a function of temperature and carbon content (0 to 6.67% C). The important critical points are:

A₁ (723 °C): eutectoid temperature where the pearlite ↔ austenite transformation occurs.
A₃: solubility limit of ferrite in austenite for hypoeutectoid steels (< 0.8% C).
Acm: solubility limit of cementite in austenite for hypereutectoid steels (> 0.8% C).

The notations Ac₁, Ac₃, Acm designate the critical temperatures on heating, while Ar₁, Ar₃, Arm designate those on cooling. This distinction is crucial: thermal hysteresis means that transformations on cooling occur at lower temperatures than those on heating.

The Four Basic Operations

Educational Diagram — Heat Treatment of Steels Heat Treatment of Steels Educational Diagram — Annealing, Quenching, Tempering ANNEALING Initial microstructure Pearlite + Ferrite Slow heating ~723 °C (A1) Slow cooling in the furnace Result: Softened steel Lamellar pearlite Easy machining QUENCHING Initial microstructure Pearlite + Ferrite Heating for austenitizing 800–950 °C Rapid cooling Water / oil / brine Result: Martensite (very hard) Brittle, internal stresses Requires tempering TEMPERING Initial microstructure Martensite (quenched) Moderate heating 150–650 °C Air cooling or water cooling Result: Tempered martensite (troostite / sorbite) Balanced hardness + toughness KEY NOTES Objectives of treatment: • Soften (annealing) • Harden (quenching) • Stabilize (tempering) Temperatures: Annealing: ~723 °C Quenching: 800–950 °C Tempering: 150–650 °C Microstructures: Annealing → Pearlite Quenching → Martensite Tempering → Tempered martensite ⚠ Important: Quenching creates internal stresses — always temper afterwards. Red Seal — Interprovincial Standards • Heat Treatment of Steels

1. Annealing

Annealing consists of heating the steel to a temperature above its critical point (generally 30 to 50 °C above A₃ or A₁), holding it at that temperature (soaking time), then cooling it very slowly (in the turned-off furnace or in an insulating medium such as lime, vermiculite, or ash).

Objectives:

Reduce hardness and improve machinability.
Eliminate residual internal stresses.
Refine the grain.
Prepare the structure for a subsequent heat treatment (e.g., quenching).

Types of annealing:

TypeTemperatureCoolingApplication
Full annealingA₃ + 30–50 °C (hypoeutectoid) or A₁ + 30–50 °C (hypereutectoid)Very slow in furnaceFree-cutting steels, forged parts
NormalizingA₃ + 50–60 °CCooling in still airGrain refinement, homogenization
Stress-relief annealing (subcritical)550–650 °C (below A₁)Slow, then airStress relief after machining
Soft annealing (spheroidizing)Just below A₁ (700–720 °C)Very slowHypereutectoid tool steels

Soaking time calculation: approximate rule of 1 hour per 25 mm (1 inch) of maximum part thickness, plus 1 additional hour. For alloy steels, this time must be increased by 25 to 50%.

2. Quenching

Quenching consists of heating the steel to the austenitizing temperature (generally A₃ + 30 to 50 °C), holding it at that temperature, then cooling it rapidly in an appropriate medium (water, oil, forced air, salt bath) to obtain a hard martensitic structure.

Typical austenitizing temperatures:

0.45% C steel: 820–850 °C.
0.80% C steel (eutectoid): 760–790 °C.
1.20% C steel (tool steel): 770–800 °C.
Alloy steel (e.g., AISI O1): 790–815 °C.

Quenching media and their severity:

MediumCooling power (H factor)Applications
Brine (10% NaCl)2.0 – 5.0Plain carbon steels
Water1.0 – 1.5Carbon steels, simple shapes
Oil (quenching)0.3 – 0.6Alloy steels, complex shapes
Forced air0.1 – 0.2Highly alloyed steels (H13, D2)
Salt bath0.5 – 1.0Martempering

Risks of quenching:

Distortion: due to thermal and transformation stresses.
Cracking: caused by too-severe cooling, sharp corners, varying cross-sections.
Decarburization: loss of surface carbon at high temperature in an oxidizing atmosphere.

Precautions: preheating at 500–650 °C for alloy steels, protection with a controlled atmosphere or stainless steel wrap, immersion with agitation, correct part orientation (thin sections enter first).

3. Tempering

Tempering is a mandatory heat treatment after quenching. It consists of reheating the quenched steel to a temperature below A₁ (150–650 °C), holding it at that temperature, then cooling it in still air.

Objectives:

Reduce the brittleness of martensite.
Relax internal stresses.
Adjust hardness and toughness according to the application.

Effect of tempering temperature on hardness (quenched 0.80% C steel):

Tempering temperature (°C)Approximate Rockwell C hardness (HRC)
150 – 20060 – 63
300 – 35050 – 55
450 – 50040 – 45
550 – 60030 – 35
65025 – 30

Temper embrittlement: certain alloy steels (Cr-Ni, Cr-Mn) exhibit increased brittleness when cooled slowly through the 375–575 °C zone after tempering. The solution is to cool rapidly (in oil or water) after tempering in this range.

Practical rule: tempering soak time is 1 hour per 25 mm of thickness, with a minimum of 1 hour.

4. Normalizing

Normalizing consists of heating the steel to A₃ + 50–60 °C, holding it, then cooling it in still air. It refines the grain and homogenizes the structure. It is often applied before machining or before quenching for forged or rolled parts.

Thermochemical Treatments

Carburizing

Carburizing is a process that introduces carbon into the surface layer of a part made of mild or low-alloy steel (0.10–0.20% C), in order to obtain a hard surface (58–62 HRC) and a tough, strong core.

Methods:

Pack carburizing: parts buried in a carbonaceous compound (charcoal + carbonates) at 900–950 °C for 4 to 8 hours.
Gas carburizing: atmosphere rich in methane (CH₄) or propane (C₃H₈) at 900–950 °C.
Liquid carburizing: cyanide salt bath at 850–950 °C.

Case depth: depends on time and temperature. Approximate rule: depth (mm) ≈ 0.025 × √(time in hours) at 925 °C. For example, 4 hours gives approximately 0.5 mm.

After carburizing: the part is quenched (directly or after cooling and reheating) then tempered at low temperature (150–200 °C).

Nitriding

Nitriding introduces nitrogen into the steel surface at a temperature of 500–580 °C, without austenitic transformation. It produces a very hard layer (68–72 HRC) with excellent wear and fatigue resistance, but a shallow depth (0.1–0.5 mm).

Suitable steels: special steels containing aluminum, chromium, molybdenum, or vanadium (e.g., Nitralloy 135M, H13).

Advantages: no distortion (low temperature), no subsequent treatment required, improved corrosion resistance.

Carbonitriding and Nitrocarburizing

Carbonitriding combines carbon and nitrogen at 750–900 °C, producing a hard case with increased hardenability. Nitrocarburizing (or ferritic carbonitriding) is done at 570–590 °C and produces a thin layer (10–20 μm) with very high wear resistance.

Surface Treatments

Cryogenic Treatment

Cryogenic treatment (cooling to -80 °C or -196 °C in liquid nitrogen) is applied after quenching and before tempering to convert retained austenite into martensite. It improves dimensional stability and tool life for cutting tools.

Ion Nitriding (Plasma)

Performed under vacuum with a nitrogen plasma at 350–550 °C, it allows precise control of case thickness and avoids the brittle white layer. Used for extrusion dies and injection molds.

Hardness Testing

Hardness verification is essential after any heat treatment. The most common scales:

ScaleIndenterLoad (kgf)Application
Brinell (HB)10 mm ball3000Rough parts, cast iron, mild steel
Rockwell C (HRC)120° diamond cone150Hardened and tempered steels
Rockwell B (HRB)1/16 in ball100Mild steels, brass
Vickers (HV)Diamond pyramid1–120Thin layers, carburized surfaces
Shore (HS)ReboundMassive parts, rollers

Approximate conversion rule: HRC ≈ (HB/10) – 15 for steels in the 200–400 HB range. These conversions are approximate and must not replace a direct test.

Precautions during Rockwell testing: clean and flat surface, minimum thickness of 10 times the penetration depth, distance between indentations of at least 3 indentation diameters, rigid and clean support.

Tool Steels: Classification and Treatment

Tool steels are classified according to the AISI/SAE system:

GroupDesignationCharacteristicsQuenchingTypical tempering
Water-hardeningW1, W2Carbon 0.60–1.40%Water or brine150–200 °C
Oil-hardeningO1, O2, O6Carbon + Mn, Cr, WOil150–250 °C
Shock-resistantS1, S5, S7Carbon + Si, Cr, MoOil or air200–400 °C
Cold work (medium)A2, A6, A8Carbon + Cr, Mo, VAir200–300 °C
Cold work (high)D2, D3, D6Carbon 1.5–2.3% + Cr 12%Air or oil200–500 °C
Hot workH10–H19, H21–H26Cr, W, Mo, VForced air550–650 °C
High-speedT1, M2, M42W, Mo, Cr, V, CoAir, oil, salt bath540–580 °C (double temper)

Example of a complete cycle for O1 steel (oil-hardening):

76.Preheat at 650 °C (1 hour).
77.Austenitize at 790–815 °C (30 minutes after reaching temperature).
78.Quench in oil until 50–70 °C (remove before complete cooling).
79.Temper immediately at 150–250 °C depending on desired hardness (1 hour minimum).
80.Cool in still air.

Double tempering: mandatory for high-speed steels (M2, T1) and recommended for hot-work steels (H13). The first temper transforms retained austenite into martensite; the second temper tempers this new martensite.

Heat Treatment Defects and Their Prevention

DefectCausePrevention
Excessive distortionUneven heating, severe quenching, unfavorable geometryPreheating, martempering, appropriate supports
Quench cracksToo-rapid cooling, sharp corners, coarse carbidesRound the corners, oil quench, prior normalizing
DecarburizationOxidizing atmosphere, excessive temperatureControlled atmosphere, stainless steel wrap, neutral salt bath
Insufficient hardnessAustenitizing temperature too low, short soak time, inadequate quenching mediumCheck the thermocouple, increase medium severity
Coarse grainTemperature too high, soak too longStrict temperature control, normalizing
Temper embrittlementSlow cooling in the critical 375–575 °C zoneRapid cooling after tempering

Furnaces and Equipment

Furnaces used in toolmaking are classified according to their energy source and mode of operation:

Batch furnace: electric resistance or gas heating, air or controlled atmosphere.
Salt bath furnace: bath of molten salts (chlorides, nitrates) offering excellent heat transfer and protection against oxidation.
Vacuum furnace: heating under vacuum (10⁻² to 10⁻⁴ mbar) with gas cooling under pressure (nitrogen, argon). Ideal for high-alloy tool steels.
Controlled atmosphere furnace: endothermic or exothermic atmosphere to prevent decarburization and oxidation.

Temperature control: thermocouples (type K: chromel-alumel, type S: platinum-rhodium) must be calibrated regularly. The typical tolerance is ±5 °C for tooling treatments.

Practical Calculations and Golden Rules

Heating time: rule of 1 minute per millimeter of thickness for carbon steels, 2 minutes per millimeter for alloy steels, starting from the preheat temperature.

Salt bath dilution volume: to adjust a bath temperature, add cold salt in small quantities (never more than 5% of the total volume at once).

Case depth: d (mm) = K × √t, where K ≈ 0.5 at 925 °C, 0.4 at 900 °C, 0.3 at 875 °C, and t in hours.

Hardness after tempering: hardness decreases by approximately 1 HRC per 10 °C increase in tempering temperature in the 200–400 °C range for carbon steels.

Applicable Canadian Standards

Although heat treatment is primarily governed by internal specifications and ASTM/SAE standards, the tool and die maker must be familiar with the following Canadian standards:

CSA W47.1: Certification of companies for fusion welding of steel (relevant if weld repairs are performed on tooling before or after treatment).
CSA B149.1: Natural gas and propane code (applicable to gas-fired furnaces).
CSA C22.1 (Canadian Electrical Code, Part I, Chapter V): applicable to the electrical installation of resistance furnaces. Rule 8-200 concerns the calculation of electrical load for circuits.
CSA Z432: Safeguarding of machinery (relevant for safety around furnaces and handling equipment).

Compliance with occupational health and safety regulations (WHMIS for quenching salts and atmospheres) is also mandatory.

Pitfalls to Avoid

104.Confusing Ac and Ar: transformation temperatures on heating are higher than those on cooling. Steel heated to 723 °C is not fully austenitized.
105.Quenching a hypereutectoid steel at A₃ instead of A₁ + 30–50 °C: this causes grain coarsening and excessive brittleness.
106.Forgetting immediate tempering after quenching: waiting for the part to cool completely before tempering increases the risk of cracking.
107.Using water for an alloy steel: excessive severity causes cracks. Use oil or air according to hardenability.
108.Neglecting decarburization: a decarburized surface gives falsely low hardness readings on the Rockwell test.
109.Confusing carburizing and nitriding: carburizing adds carbon and requires quenching; nitriding adds nitrogen without quenching.
110.Ignoring retained austenite: in high-carbon and high-alloy steels, cryogenic treatment or double tempering is necessary.
111.Treating a hardness conversion as an exact value: conversion tables are approximate and depend on the alloy.
112.Heating a tool steel too quickly: thermal shock causes cracks. Always preheat at 500–650 °C.
113.Not accounting for part thickness: thick sections require longer soak times and more severe quenching media.

Summary

Heat treatment is based on the Fe-C diagram and the critical temperatures A₁, A₃, Acm.
The four basic operations are: annealing (slow cooling), quenching (rapid cooling), tempering (reheating below A₁), normalizing (air cooling).
Quenching produces hard but brittle martensite; tempering is always mandatory after quenching.
Thermochemical treatments (carburizing, nitriding) modify the surface composition to achieve high hardness with a tough core.
Tool steels are classified into groups (W, O, S, A, D, H, T, M) with specific treatment cycles.
Hardness tests (Rockwell, Brinell, Vickers) are the primary means of verification; conversions between scales are approximate.
Common defects (distortion, cracks, decarburization) are preventable through rigorous control of temperature, time, and medium.
CSA standards (W47.1, B149.1, C22.1) apply to related aspects (welding, gas, electricity) of heat treatment facilities.

To pass the exam: memorize the temperature ranges for each treatment, the quenching media suited to each type of steel, and the soak time rules. Practice reading a complete heat treatment cycle and identifying errors in a given sequence.

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