Hardening:
Pure iron, wrought iron, and extremely low carbon steels cannot be appreciably hardened by heat treatment, since they contain no hardening element. Cast iron can be hardened, but its heat treatment is limited. When cast iron is cooled rapidly, it forms white iron, which is hard and brittle. When cooled slowly, it forms gray iron, which is soft but brittle under impact. In plain carbon steel, the maximum hardness depends almost entirely on the carbon content of the steel. As the carbon content increases, the ability of the steel to be hardened increases. However, this increase in the ability to harden with an increase in carbon content continues only to a certain point. In practice, that point is 0.85 percent carbon content. When the carbon content is increased beyond 0.85 percent, there is no increase in wear resistance.
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For most steels, the hardening treatment consists of heating the steel to a temperature just above the upper critical point, soaking or holding for the required length of time, and then cooling it rapidly by plunging the hot steel into oil, water, or brine. Although most steels must be cooled rapidly for hardening, a few may be cooled in still air. Hardening increases the hardness and strength of the steel but makes it less ductile.
When hardening carbon steel, it must be cooled to below 1,000 °F in less than 1 second. Should the time required for the temperature to drop to 1,000 °F exceed 1 second, the austenite begins to transform into fine pearlite. This pearlite varies in hardness, but is much harder than the pearlite formed by annealing and much softer than the martensite desired. After the 1,000 °F temperature is reached, the rapid cooling must continue if the final structure is to be all martensite. When alloys are added to steel, the time limit for the temperature drop to 1,000 °F increases above the 1 second limit for carbon steels. Therefore, a slower quenching medium will produce hardness in alloy steels. Because of the high internal stresses in the “as quenched” condition, steel must be tempered just before it becomes cold. The part should be removed from the quenching bath at a temperature of approximately 200 °F, since the temperature range from 200 °F down to room temperature is the cracking range. Hardening temperatures and quenching mediums for the various types of steel are listed in Figure 5-6.
Hardening Precautions
A variety of different shapes and sizes of tongs for handling hot steels is necessary. It should be remembered that cooling of the area contacted by the tongs is retarded and that such areas may not harden, particularly if the steel being treated is very shallow hardening. Small parts may be wired together or quenched in baskets made of wire mesh.
Special quenching jigs and fixtures are frequently used to hold steels during quenching in a manner to restrain distortion.
When selective hardening is desired, portions of the steel may be protected by covering with launder cement or some other insulating material. Selective hardening may be accomplished also by the use of water or oil jets designed to direct quenching medium on the areas to be hardened. This also is accomplished by the induction and flame hardening procedures previously described, particularly on large production jobs.
Shallow hardening steels, such as plain carbon and certain varieties of alloy steels, have such a high critical cooling rate that they must be quenched in brine or water to effect hardening. In general, intricately shaped sections should not be made of shallow hardening steels because of the tendency of these steels to warp and crack during hardening. Such items should be made of deeper hardening steels capable of being hardened by quenching in oil or air.
Tempering
Tempering reduces the brittleness imparted by hardening and produces definite physical properties within the steel. Tempering always follows, never precedes, the hardening operation. In addition to reducing brittleness, tempering softens the steel.
Tempering is always conducted at temperatures below the low critical point of the steel. In this respect, tempering differs from annealing, normalizing, or hardening, all of which require temperatures above the upper critical point. When hardened steel is reheated, tempering begins at 212 °F and continues as the temperature increases toward the low critical point. By selecting a definite tempering temperature, the resulting hardness and strength can be predetermined. Approximate temperatures for various tensile strengths are listed in Figure 5-6. The minimum time at the tempering temperature should be 1 hour. If the part is over 1 inch in thickness, increase the time by 1 hour for each additional inch of thickness. Tempered steels used in aircraft work have from 125,000 to 200,000 psi ultimate tensile strength.
Generally, the rate of cooling from the tempering temperature has no effect on the resulting structure; therefore, the steel is usually cooled in still air after being removed from the furnace.
Annealing
Annealing of steel produces a fine grained, soft, ductile metal without internal stresses or strains. In the annealed state, steel has its lowest strength. In general, annealing is the opposite of hardening.
Annealing of steel is accomplished by heating the metal to just above the upper critical point, soaking at that temperature, and cooling very slowly in the furnace. (Refer to Figure 5-6 for recommended temperatures.) Soaking time is approximately 1 hour per inch of thickness of the material. To produce maximum softness in steel, the metal must be cooled very slowly. Slow cooling is obtained by shutting off the heat and allowing the furnace and metal to cool together to 900 °F or lower, then removing the metal from the furnace and cooling in still air. Another method is to bury the heated steel in ashes, sand, or other substance that does not conduct heat readily.
Normalizing
The normalizing of steel removes the internal stresses set up by heat treating, welding, casting, forming, or machining. Stress, if not controlled, will lead to failure. Because of the better physical properties, aircraft steels are often used in the normalized state, but seldom, if ever, in the annealed state.
One of the most important uses of normalizing in aircraft work is in welded parts. Welding causes strains to be set up in the adjacent material. In addition, the weld itself is a cast structure as opposed to the wrought structure of the rest of the material. These two types of structures have different grain sizes, and to refine the grain as well as to relieve the internal stresses, all welded parts should be normalized after fabrication.
Normalizing is accomplished by heating the steel above the upper critical point and cooling in still air. The more rapid quenching obtained by air cooling, as compared to furnace cooling, results in a harder and stronger material than that obtained by annealing. Recommended normalizing temperatures for the various types of aircraft steels are listed in Figure 5-6.
Casehardening
Casehardening produces a hard wear-resistant surface or case over a strong, tough core. Casehardening is ideal for parts which require a wear-resistant surface and, at the same time, must be tough enough internally to withstand the applied loads. The steels best suited to casehardening are the low carbon and low alloy steels. If high carbon steel is casehardened, the hardness penetrates the core and causes brittleness. In casehardening, the surface of the metal is changed chemically by introducing a high carbide or nitride content. The core is unaffected chemically.
When heat treated, the surface responds to hardening while the core toughens. The common forms of casehardening are carburizing, cyaniding, and nitriding. Since cyaniding is not used in aircraft work, only carburizing and nitriding are discussed in this section.
Carburizing
Carburizing is a casehardening process in which carbon is added to the surface of low carbon steel. Thus, a carburized steel has a high carbon surface and a low carbon interior. When the carburized steel is heat treated, the case is hardened while the core remains soft and tough.
A common method of carburizing is called “pack carburizing.” When carburizing is to be done by this method, the steel parts are packed in a container with charcoal or some other material rich in carbon. The container is then sealed with fire clay, placed in a furnace, heated to approximately 1,700 °F, and soaked at that temperature for several hours. As the temperature increases, carbon monoxide gas forms inside the container and, being unable to escape, combines with the gamma iron in the surface of the steel. The depth to which the carbon penetrates depends on the length of the soaking period. For example, when carbon steel is soaked for 8 hours, the carbon penetrates to a depth of about 0.062 inch.
In another method of carburizing, called “gas carburizing,” a material rich in carbon is introduced into the furnace atmosphere. The carburizing atmosphere is produced by the use of various gases or by the burning of oil, wood, or other materials. When the steel parts are heated in this atmosphere, carbon monoxide combines with the gamma iron to produce practically the same results as those described under the pack carburizing process.
A third method of carburizing is that of “liquid carburizing.” In this method, the steel is placed in a molten salt bath that contains the chemicals required to produce a case comparable with one resulting from pack or gas carburizing.
Alloy steels with low carbon content as well as low carbon steels may be carburized by any of the three processes. However, some alloys, such as nickel, tend to retard the absorption of carbon. As a result, the time required to produce a given thickness of case varies with the composition of the metal.
Nitriding
Nitriding is unlike other casehardening processes in that, before nitriding, the part is heat treated to produce definite physical properties. Thus, parts are hardened and tempered before being nitrided. Most steels can be nitrided, but special alloys are required for best results. These special alloys contain aluminum as one of the alloying elements and are called “nitralloys.”
In nitriding, the part is placed in a special nitriding furnace and heated to a temperature of approximately 1,000 °F. With the part at this temperature, ammonia gas is circulated within the specially constructed furnace chamber. The high temperature cracks the ammonia gas into nitrogen and hydrogen. The ammonia which does not break down is caught in a water trap below the regions of the other two gases. The nitrogen reacts with the iron to form nitride. The iron nitride is dispersed in minute particles at the surface and works inward. The depth of penetration depends on the length of the treatment. In nitriding, soaking periods as long as 72 hours are frequently required to produce the desired thickness of case.
Nitriding can be accomplished with a minimum of distortion, because of the low temperature at which parts are casehardened and because no quenching is required after exposure to the ammonia gas.
Heat Treatment of Nonferrous Metals
Aluminum Alloys
In the wrought form, commercially pure aluminum is known as 1100. It has a high degree of resistance to corrosion and is easily formed into intricate shapes. It is relatively low in strength and does not have the properties required for structural aircraft parts. High strengths are generally obtained by the process of alloying. The resulting alloys are less easily formed and, with some exceptions, have lower resistance to corrosion than 1100 aluminum.
Alloying is not the only method of increasing the strength of aluminum. Like other materials, aluminum becomes stronger and harder as it is rolled, formed, or otherwise cold worked. Since the hardness depends on the amount of cold working done, 1100 and some wrought aluminum alloys are available in several strain hardened tempers. The soft or annealed condition is designated O. If the material is strain hardened, it is said to be in the H condition.
The most widely used alloys in aircraft construction are hardened by heat treatment rather than by cold work. These alloys are designated by a somewhat different set of symbols: T4 and W indicate solution heat treated and quenched but not aged, and T6 indicates an alloy in the heat treated hardened condition.
W – Solution heat treated, unstable temper
T – Treated to produce stable tempers other than F, O, or H
T2 – Annealed (cast products only)
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T3 -Solution heat treated and then cold worked
T4 -Solution heat treated
T5 -Artificially aged only
T6 – Solution heat treated and then artificially aged
T7 – Solution heat treated and then stabilized
T8 – Solution heat treated, cold worked, and then artificially aged
T9 – Solution heat treated artificially aged, and then cold worked
T10- Artificially aged and then cold worked
Additional digits may be added to T1 through T10 to indicate a variation in treatment which significantly alters the characteristics of the product.
Aluminum alloy sheets are marked with the specification number on approximately every square foot of material. If for any reason this identification is not on the material, it is possible to separate the heat treatable alloys from the non-heat-treatable alloys by immersing a sample of the material in a 10 percent solution of caustic soda (sodium hydroxide). The heat-treatable alloys will turn black due to the copper content, whereas the others will remain bright. In the case of clad material, the surface will remain bright, but there will be a dark area in the middle when viewed from the edge.
Alclad Aluminum
The terms “Alclad and Pureclad” are used to designate sheets that consist of an aluminum alloy core coated with a layer of pure aluminum to a depth of approximately 5 1/2 percent on each side. The pure aluminum coating affords a dual protection for the core, preventing contact with any corrosive agents, and protecting the core electrolytically by preventing any attack caused by scratching or from other abrasions.
There are two types of heat treatments applicable to aluminum alloys. One is called solution heat treatment, and the other is known as precipitation heat treatment. Some alloys, such as 2017 and 2024, develop their full properties as a result of solution heat treatment followed by about 4 days of aging at room temperature. Other alloys, such as 2014 and 7075, require both heat treatments.
The alloys that require precipitation heat treatment (artificial aging) to develop their full strength also age to a limited extent at room temperature; the rate and amount of strengthening depends upon the alloy. Some reach their maximum natural or room temperature aging strength in a few days, and are designated as -T4 or -T3 temper. Others continue to age appreciably over a long period of time.
Because of this natural aging, the -W designation is specified only when the period of aging is indicated, for example, 7075-W (1/2 hour). Thus, there is considerable difference in the mechanical and physical properties of freshly quenched (-W) material and material that is in the -T3 or -T4 temper.
The hardening of an aluminum alloy by heat treatment consists of four distinct steps:
1. Heating to a predetermined temperature.
2. Soaking at temperature for a specified length of time.
3. Rapidly quenching to a relatively low temperature.
4. Aging or precipitation hardening either spontaneously at room temperature, or as a result of a low temperature thermal treatment.
The first three steps above are known as solution heat treatment, although it has become common practice to use the shorter term, “heat treatment.” Room temperature hardening is known as natural aging, while hardening done at moderate temperatures is called artificial aging, or precipitation heat treatment.
Solution Heat Treatment
Temperature
The temperatures used for solution heat treating vary with different alloys and range from 825 °F to 980 °F. As a rule, they must be controlled within a very narrow range (±10 °F) to obtain specified properties. If the temperature is too low, maximum strength will not be obtained. When excessive temperatures are used, there is danger of melting the low melting constituents of some alloys with consequent lowering of the physical properties of the alloy. Even if melting does not occur, the use of higher than recommended temperatures promotes discoloration and increases quenching strains.
Time at Temperature
The time at temperature, referred to as soaking time, is measured from the time the coldest metal reaches the minimum limit of the desired temperature range. The soaking time varies, depending upon the alloy and thickness, from 10 minutes for thin sheets to approximately 12 hours for heavy forgings. For the heavy sections, the nominal soaking time is approximately 1 hour for each inch of cross-sectional thickness. [Figure 5-7]
Choose the minimum soaking time necessary to develop the required physical properties. The effect of an abbreviated soaking time is obvious. An excessive soaking period aggravates high temperature oxidation. With clad material, prolonged heating results in excessive diffusion of copper and other soluble constituents into the protective cladding and may defeat the purpose of cladding.
Quenching
After the soluble constituents are in solid solution, the material is quenched to prevent or retard immediate reprecipitation. Three distinct quenching methods are employed. The one to be used in any particular instance depends upon the part, the alloy, and the properties desired.
Cold Water Quenching
Parts produced from sheet, extrusions, tubing, small forgings, and similar type material are generally quenched in a cold water bath. The temperature of the water before quenching should not exceed 85 °F. Using a sufficient quantity of water keeps the temperature rise under 20 °F. Such a drastic quench ensures maximum resistance to corrosion. This is particularly important when working with such alloys as 2017, 2024, and 7075. This is the reason a drastic quench is preferred, even though a slower quench may produce the required mechanical properties.
Hot Water Quenching
Large forgings and heavy sections can be quenched in hot or boiling water. This type of quench minimizes distortion and alleviates cracking which may be produced by the unequal temperatures obtained during the quench. The use of a hot water quench is permitted with these parts because the temperature of the quench water does not critically affect the resistance to corrosion of the forging alloys. In addition, the resistance to corrosion of heavy sections is not as critical a factor as for thin sections.
Spray Quenching
High velocity water sprays are useful for parts formed from clad sheet and for large sections of almost all alloys. This type of quench also minimizes distortion and alleviates quench cracking. However, many specifications forbid the use of spray quenching for bare 2017 and 2024 sheet materials because of the effect on their resistance to corrosion.
Lag Between Soaking and Quenching
The time interval between the removal of the material from the furnace and quenching is critical for some alloys and should be held to a minimum. When solution heat treating 2017 or 2024 sheet material, the elapsed time must not exceed 10 seconds. The allowable time for heavy sections may be slightly greater.
Allowing the metal to cool slightly before quenching promotes reprecipitation from the solid solution. The precipitation occurs along grain boundaries and in certain slip planes causing poorer formability. In the case of 2017, 2024, and 7075 alloys, their resistance to intergranular corrosion is adversely affected.
Reheat Treatment
The treatment of material which has been previously heat treated is considered a reheat treatment. The unclad heat-treatable alloys can be solution heat treated repeatedly without harmful effects.
The number of solution heat treatments allowed for clad sheet is limited due to increased diffusion of core and cladding with each reheating. Existing specifications allow one to three reheat treatments of clad sheet depending upon cladding thickness.
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Straightening After Solution Heat Treatment
Some warping occurs during solution heat treatment, producing kinks, buckles, waves, and twists. These imperfections are generally removed by straightening and flattening operations.
Where the straightening operations produce an appreciable increase in the tensile and yield strengths and a slight decrease in the percent of elongation, the material is designated -T3 temper. When the above values are not materially affected, the material is designated -T4 temper.
Precipitation Heat Treating
As previously stated, the aluminum alloys are in a comparatively soft state immediately after quenching from a solution heat-treating temperature. To obtain their maximum strengths, they must be either naturally aged or precipitation hardened.
During this hardening and strengthening operation, precipitation of the soluble constituents from the supersaturated solid solution takes place. As precipitation progresses, the strength of the material increases, often by a series of peaks, until a maximum is reached. Further aging (overaging) causes the strength to steadily decline until a somewhat stable condition is obtained. The sub-microscopic particles that are precipitated provide the keys or locks within the grain structure and between the grains to resist internal slippage and distortion when a load of any type is applied. In this manner, the strength and hardness of the alloy are increased.
Precipitation hardening produces a great increase in the strength and hardness of the material with corresponding decreases in the ductile properties. The process used to obtain the desired increase in strength is therefore known as aging, or precipitation hardening
The strengthening of the heat-treatable alloys by aging is not due merely to the presence of a precipitate. The strength is due to both the uniform distribution of a finely dispersed sub-microscopic precipitate and its effects upon the crystal structure of the alloy.
The aging practices used depend upon many properties other than strength. As a rule, the artificially aged alloys are slightly overaged to increase their resistance to corrosion. This is especially true with the artificially aged high copper content alloys that are susceptible to intergranular corrosion when inadequately aged.
The heat-treatable aluminum alloys are subdivided into two classes: those that obtain their full strength at room temperature and those that require artificial aging. The alloys that obtain their full strength after 4 or 5 days at room temperature are known as natural aging alloys. Precipitation from the supersaturated solid solution starts soon after quenching, with 90 percent of the maximum strength generally being obtained in 24 hours. Alloys 2017 and 2024 are natural aging alloys.
The alloys that require precipitation thermal treatment to develop their full strength are artificially aged alloys. However, these alloys also age a limited amount at room temperature, the rate and extent of the strengthening depending upon the alloys.
Many of the artificially aged alloys reach their maximum natural or room temperature aging strengths after a few days. These can be stocked for fabrication in the -T4 or -T3 temper. High zinc content alloys such as 7075 continue to age appreciably over a long period of time, their mechanical property changes being sufficient to reduce their formability.
The advantage of -W temper formability can be utilized, however, in the same manner as with natural aging alloys; that is, by fabricating shortly after solution heat treatment, or retaining formability by the use of refrigeration.
Refrigeration retards the rate of natural aging. At 32 °F, the beginning of the aging process is delayed for several hours, while dry ice (-50 °F to -100 °F) retards aging for an extended period of time.
Precipitation Practices
The temperatures used for precipitation hardening depend upon the alloy and the properties desired, ranging from 250 °F to 375 °F. They should be controlled within a very narrow range (±5 °F) to obtain best results. [Figure 5-8]
The time at temperature is dependent upon the temperature used, the properties desired, and the alloy. It ranges from 8 to 96 hours. Increasing the aging temperature decreases the soaking period necessary for proper aging. However, a closer control of both time and temperature is necessary when using the higher temperatures.
After receiving the thermal precipitation treatment, the material should be air cooled to room temperature. Water quenching, while not necessary, produces no ill effects. Furnace cooling has a tendency to produce overaging.
Annealing of Aluminum Alloys
The annealing procedure for aluminum alloys consists of heating the alloys to an elevated temperature, holding or soaking them at this temperature for a length of time depending upon the mass of the metal, and then cooling in still air. Annealing leaves the metal in the best condition for cold working. However, when prolonged forming operations are involved, the metal will take on a condition known as “mechanical hardness” and will resist further working. It may be necessary to anneal a part several times during the forming process to avoid cracking. Aluminum alloys should not be used in the annealed state for parts or fittings.
Clad parts should be heated as quickly and carefully as possible, since long exposure to heat tends to cause some of the constituents of the core to diffuse into the cladding. This reduces the corrosion resistance of the cladding.
Heat Treatment of Aluminum Alloy Rivets
Aluminum alloy rivets are furnished in the following compositions: Alloys 1100, 5056, 2117, 2017, and 2024.
Alloy 1100 rivets are used in the “as fabricated” condition for riveting aluminum alloy sheets where a low strength rivet is suitable. Alloy 5056 rivets are used in the “as fabricated” condition for riveting magnesium alloy sheets.
Alloy 2117 rivets have moderately high strength and are suitable for riveting aluminum alloy sheets. These rivets receive only one heat treatment, which is performed by the manufacturer, and are anodized after being heat treated. They require no further heat treatment before they are used. Alloy 2117 rivets retain their characteristics indefinitely after heat treatment and can be driven anytime. Rivets made of this alloy are the most widely used in aircraft construction.
Alloy 2017 and 2024 rivets are high strength rivets suitable for use with aluminum alloy structures. They are purchased from the manufacturer in the heat-treated condition. Since the aging characteristics of these alloys at room temperatures are such that the rivets are unfit for driving, they must be reheating treated just before they are to be used. Alloy 2017 rivets become too hard for driving in approximately 1 hour after quenching. Alloy 2024 rivets become hardened in 10 minutes after quenching. Both of these alloys may be reheating treated as often as required; however, they must be anodized before the first reheat treatment to prevent inter-granular oxidation of the material. If these rivets are stored in a refrigerator at a temperature lower than 32 °F immediately after quenching, they will remain soft enough to be usable for several days.
Rivets requiring heat treatment are heated either in tubular containers in a salt bath, or in small screen wire baskets in an air furnace. The heat treatment of alloy 2017 rivets consists of subjecting the rivets to a temperature between 930 °F to 950 °F for approximately 30 minutes, and immediately quenching in cold water. These rivets reach maximum strength in about 9 days after being driven. Alloy 2024 rivets should be heated to a temperature of 910 °F to 930 °F and immediately quenched in cold water. These rivets develop greater shear strength than 2017 rivets and are used in locations where extra strength is required. Alloy 2024 rivets develop their maximum shear strength in 1 day after being driven.
The 2017 rivet should be driven within approximately 1 hour and the 2024 rivet within 10 to 20 minutes after heat treating or removal from refrigeration. If not used within these times, the rivets should be re-heating treated before being refrigerated.
Heat Treatment of Magnesium Alloys
Magnesium alloy castings respond readily to heat treatment, and about 95 percent of the magnesium used in aircraft construction is in the cast form. The heat treatment of magnesium alloy castings is similar to the heat treatment of aluminum alloys in that there are two types of heat treatment:
(1) solution heat treatment
(2) precipitation (aging) heat treatment.
Magnesium, however, develops a negligible change in its properties when allowed to age naturally at room temperatures.
Solution Heat Treatment
Magnesium alloy castings are solution heat treated to improve tensile strength, ductility, and shock resistance. This heat-treatment condition is indicated by using the symbol -T4 following the alloy designation. Solution heat treatment plus artificial aging is designated -T6. Artificial aging is necessary to develop the full properties of the metal.
Solution heat-treatment temperatures for magnesium alloy castings range from 730 °F to 780 °F, the exact range depending upon the type of alloy. The temperature range for each type of alloy is listed in Specification MIL-H-6857. The upper limit of each range listed in the specification is the maximum temperature to which the alloy may be heated without danger of melting the metal.
The soaking time ranges from 10 to 18 hours, the exact time depending upon the type of alloy as well as the thickness of the part. Soaking periods longer than 18 hours may be necessary for castings over 2 inches in thickness. Never heat magnesium alloys in a salt bath as this may result in an explosion.
A serious potential fire hazard exists in the heat treatment of magnesium alloys. If through oversight or malfunctioning of equipment, the maximum temperatures are exceeded, the casting may ignite and burn freely. For this reason, the furnace used should be equipped with a safety cut-off that will turn off the power to the heating elements and blowers if the regular control equipment malfunctions or fails. Some magnesium alloys require a protective atmosphere of sulphur dioxide gas during solution heat treatment. This aids in preventing the start of a fire even if the temperature limits are slightly exceeded.
Air quenching is used after solution heat treatment of magnesium alloys since there appears to be no advantage in liquid cooling.
Precipitation Heat Treatment
After solution treatment, magnesium alloys may be given an aging treatment to increase hardness and yield strength. Generally, the aging treatments are used merely to relieve stress and stabilize the alloys in order to prevent dimensional changes later, especially during or after machining. Both yield strength and hardness are improved somewhat by this treatment at the expense of a slight amount of ductility. The corrosion resistance is also improved, making it closer to the “as cast” alloy.
Precipitation heat treatment temperatures are considerably lower than solution heat-treatment temperatures and range from 325 °F to 500 °F. Soaking time ranges from 4 to 18 hours.
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