US3416977A - Cryogenic cooling - Google Patents

Cryogenic cooling Download PDF

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Publication number
US3416977A
US3416977A US539429A US53942966A US3416977A US 3416977 A US3416977 A US 3416977A US 539429 A US539429 A US 539429A US 53942966 A US53942966 A US 53942966A US 3416977 A US3416977 A US 3416977A
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United States
Prior art keywords
quenching
liquid nitrogen
cooling
heat
temperature
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Expired - Lifetime
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US539429A
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English (en)
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Richard H Rein
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Union Carbide Corp
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Union Carbide Corp
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Priority to US539429A priority Critical patent/US3416977A/en
Priority to GB14510/67A priority patent/GB1157296A/en
Priority to CH458167A priority patent/CH480427A/fr
Priority to DE19671551391 priority patent/DE1551391A1/de
Priority to BE696473D priority patent/BE696473A/xx
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/62—Quenching devices
    • C21D1/63—Quenching devices for bath quenching
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/613—Gases; Liquefied or solidified normally gaseous material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/62—Quenching devices
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor

Definitions

  • ABSTRACT OF THE DISCLOSURE A method for controllably extracting heat from a ma terial over a predetermined temperature range by contacting said material with a fluid dispersion comprising at least one cryogenic fluid which is at its boiling point, and at least one finely divided solid additive, charac- Patented Dec. 17, 1968 It is known that in heat treating various metal and alloys rapid cooling is critical within a particular temperature range, depending on the particular metallic.
  • Thisapplication relatesto a method for improving the heat transfer characteristics of cryogenic fluids, to the fluids thus improved. and to a method for utilizing such fluids toextract heat rapidly and controllably from materials.
  • Dullberg in US. Patent No. 3,185,600 discloses a process for quenching hot sheet metal parts, at their solution heat treatment temperature, directly into a cryogenic fluid, such as liquid nitrogen, so as to reduce the temperature of the part as rapidly as possible below -50 F.
  • a cryogenic fluid such as liquid nitrogen
  • quenching medium having a controllable cooling rate over a predetermined temperature range.
  • Anotherv object of this invention to provide 7 a method for extracting heat rapidly andcontrollably from a material in such manner that the material will not be distorted, nor substantially reduced in strength.
  • One aspect of this invention comprises a method for improving the heat transfer characteristics of a cryogenic 1 fluid at its boiling point, particularly its ability to extract heat from a material or surface. This method consists of adding a finely divided solid to such cryogenic fluid.
  • the finely divided solid must have its melting point, and at least a portion of its stable liquid phase, within the temperature range formed by the boiling point'of the cryogenic fluid and the temperature of the material from which heat is to be extracted.
  • a second aspect of the present invention consists of the'cryogenic fluid mixture itself which is a dispersion of theabove defined solid in the cryogenic fluid, said mixture having a greater ability to extract heat from a material than the pure cryogenic fluid.
  • a third aspect of the present invention consists of a method't'or controllably extracting heat from a material over a predetremined temperature range comprising contacting said material with a fluid dispersion comprising: (i) a cryogenic fluid, which is at its boiling point and (2) a finely divided solid additive characterized by having its melting point, and at least a portion of its stable liquid phase, within the temperature range formed by the boiling point of the cryogenic fluid and the temperature of the material from which heat is to be extracted,
  • FIGURE 1 is a graphshowing the cooling curves obtained on quenching copper test specimens into respectively: pure liquid nitrogen, finely divided ice particles in liquid nitrogen (dispersions varying in solids content from to 65%) and water.
  • FIGURE 2 is a graph showing the cooling curves obtained on quenching copper test specimens into respectively: pure liquid nitrogen, and mixtures of various finely divided solid additives dispersed in a liquid notrogen.
  • FIGURE 3 is a graph showing the cooling curves obtained on quenching test specimens, initially at a temperature of 330 F., into. respectively: pure liquid nitrogen, and a 50% solids dispersion of finely divided ice in liquid nitrogen.
  • FIGURE 4 is a graph showing the cooling curves obtained on quenching test specimens, initially at a temperature of 225' F., into respectively: pure liquid nitrogen, and a 50% solids dispersion of finely divided ice in liquid nitrogen.
  • FIGURE 5 is a graph showing the cooling curves obtained on quenching test specimens, initially at a temperature of 145' F., into respectively: pure nitrogen, and a 50% solids dispersion of finely divided ice in liquid nitrogen.
  • the process of this invention is useful for cooling any material which requires rapid and controlled cooling from a relatively high temperature.
  • a material is most frequently a metal, particularly an alloy requiring heat treatment, but it may be a nonmetallic material as for example, a cermet, a ceramic, a cementitious material, or a natural or synthetic rubbery or resinous material.
  • the material may be in any physical formtthus, it may be particulate or be an object such as'a sheet, a rod, a slab. a fiber, or a complex fabricated part.
  • cryogenic fluid as used throughout this disclosure, is intended to mean a substance having its normal boiling point below the freezing point of water, i.e., 32' F.
  • Illustrative cryogcnic fluidsin include liquid air, as well as, the fluids listed in Table i.
  • the finely divided solid useful as an additive'in the present invention to aiterthe heat transfer characteristics of cryogenic fluid must have at least a portiono! its stable liquid phase within the temperature range formed by the boiling point of the cryogenic fluid and the temperature of the material from which heat is to be extracted. All materials which fall within this generie'deiinltion are suitable forcarrying out the processes of this invention.
  • a preferred class of flnely divided solids is character- 1 the boiling point of the cyrogenic fluid and the temperature of the material from which heat is to be extracted.
  • FIGURE 1 shows cooling curves, i.e., a plot of time versus temperature, for a 5%, Va a a a and a mixtureof ice in liquid nitrogen.
  • cooling curves i.e., a plot of time versus temperature
  • Va a a a and a mixtureof ice in liquid nitrogen For purposes of comparison curves for liquid water and pure liquid nitrogen are also shown. All percentages are by weight.
  • FIGURE 1 demonstrates that the cooling ability of liquid nitrog'enice mixtures are far greater than that of pure liquid nitrogen. As the percentage of solids decreases, it tends to approach that of the pure cryogenic fluid. However, it can, be seen that as little as 10 percent ice has a great effect upon the cooling rate of the liquid nitrogen.
  • the useful upper limit of the solids content is dependent upon the fluidity of the mixture. In order to be useful in the process of this invention the mixture must be fluid.
  • the solids concentration at which fluidity ceases depends upon several factors, including the relative densities of the cryogenic fluid and the finely divided solids, the average permitting adequate fluidity.
  • Cryogenic fluids are generally regarded as poor media'- for heat transfer.
  • the reason for this is believed to be that heat transfer by the slow film-boiling mechanism takes place on smooth surfaces having temperatures more than about 40' F. higher than thenormal boiling point of the fluid.
  • the addition of finely divided solids having the'specified characteristics improves heat transfer to cryogenic fluids by causing the heat transfer, in part at least. to occur by melting of the solid and by nucleate-boiling of the resulting liquid on the surface of the material from which heat is being extractedrlt is visualized that this process takes place in three distinct zones.
  • the first zone consists of the material being cooled.
  • the second zone consists of a gas space adjacent to the surface of the material being cooled. and contains solid as well as melted additive particles.
  • the third zone consists of the main body of the cryogenic fluid containing the solid additive particles. In other words'. zone two is located in between zone one 'andzonethree. This arrangement is thought to be representative of the situation during the film-boiling regime of the cryogenic fluid. As cryogenic fluid boils away, the additive particles in zone three are 6 without having reachedtheheat source. This theory is consistent with the data in Table 3 showing that very fine particles (below mesh) and very large particles (above 6 mesh) have little or no effect upon the cooling rate of the cryogenic mixture, and that optimum cooling depends on having an optimum particlev size.
  • the quenching mixtures were prepared as follows. Where the additive was a liquid at room temperature and pressure, the cryogenic quenching mixtures were prepared by atomizing the liquid and spraying the atomized droplets 1 into cryogenic fluid which was contained in a dewar. Atomization was caused-by forcing the liquid through an atomizing nozzle at a pressure of about 5 p.s.i.g. The dispersion was prepared by holding the top of the atomizer about one inch above the level of the cryogenic fluid. The atomized droplets f-roze upon contacting the cryogenic fluid. The mixture was continuously stirred with a conventional two blade laboratory mixer to avoid formation of a frozen crust on the surface of the mixture. The dispersions were prepared in a dewar which held about five pounds of mixture.
  • thermocouple was fused in the center of each specimen for recording its temperature.
  • the thermocouple cold junction was maintained at -320 F... and temperatures were recorded with an automatic fast response millivolt recorder having a chart travel speed of one inch per 10 seconds.
  • the experimental procedure consisted of heating the test specimen in a salt bath un il the entire specimen reached thermal equilibrium. .900 F. in case of the data plotted in FIGURES l and 2. and 330 F.. 225' F., and F. respectively in case of FIGURES 3. 4 and 5.
  • the specimen was then removed from the molten salt bath and immediately plunged into the bath of stirred quenching mixture.
  • the specimen was allowed to remain in the cryogenic dispersion until it came to thermal equilibrium with the bath.
  • the hot'obiect may be contacted with the quenching propelled toward the heat source (zone one) and their traiectory within zone two is determined by ,the balance of forces acting upon the particles. These particles are accelerated towards the heat sources because of the large valume changes that occur when the cryogenic fluid evaporates. After a particle has entered zone two, itis acted upon by at least four separate forces. Vetrically downwardis a gravational force and in the opposite direction there is a viscous drag force due to the gases rushingup through.
  • FIGURE 1 which compares the effect of the solids content of a dispersion of ice in liquid nitrogen has already been discussed.
  • FIGURE 2 shows the cooling curves obtained using a copper test specimen quenched in the followin media: pure liquid nitrogen. 10 and 50 percent bv weight dispersions, respectively. of finely divided crystals of methanol and kerosene. 10 percent brine crystalstcontnining 10% NaCl in water). 10 percent sulfur. and 10 ercent ferric chloride. all dispersed in liquid nitrogen These curves demonstrate how the cooling rate of an immersed object can be varied by the quantity and ltind of the solid additive. t
  • FIGURES 3. 4 ands demonstrate the effect of varying the initial temperature of the material being cooled. It can be seen that'in each case the use ofa dispersion of 50% ice in liquid nitrogen results in a shorter cooling time than the use of pure liquid nitrogen. However. as the temperature of the hot material is lowered, .the differences between the cooling curves become less. 'Thus, while the improvements resulting from the practice of this invention are properties for the specimen as when quenched in pure liquid nitrogen. Comparison of the cooling curves for achieved even when the temperature of the material, being. I
  • cryogenic mixtures for quenching aluminum alloy 7075 was also investigated.
  • This alloy which has a nominal composition of 1.5 percent copper, 2.5 percent magnesium, 2.5 percent zinc and minor amounts of silicon, iron and manganese was selectedfor testing because it is one of the most difiieult to heat. treat since its physical properties show a high sensitivity to the quenching rate.
  • Aluminum alloy 7075 is one of the strongest of the aluminum alloys and capable of achieving a tensile strength as high as 83,000 p.s.i. in the wrought condition. Maximum strength is obtained by heat treating it to the T-6 condition.
  • test specimens of aluminum alloy 7075 were measured after being quenched in various media from the solution testtreating temperature (9i0-930' F.) and temperature to the T-6 condition as described above. Tensile specimens having a one inch gage length were cut from Ms inch thick sheets in the transverse direction. Two tensile specimens were prepared for each quenching condition. Table 4 below contains a tabulation of the mechanical properties obtained.
  • Aluminum parts are frequently highly complex, fabricated pieces which have been machined to close mechanical tolerances. These parts must not only be strong but must be substantially free of distortion. in the past, it has frequently been neces-. sary to go through costly straightening operations to cure the warpage caused by heat treating and quenching operations.
  • the tendency of various quenching media to causewarpage or distortion wasexperimentally determined with a modified NavyC test'specimen fabricated from it inch thick aluminum sheet. This test is described-more fully.
  • Table 5 shows the distortion that occurred using water, liquid nitrogen, and a dispersion of 50% ice in liquid nitrogen. Each of theresults reported is the averages of five testspecimens. it can be seen that by far thegreatest warpage occurred on quenching in water. it can also be seen that the distortion is minimal with liquid nitrogen .material over" a predetermined temperature range, comprising contacting said material with a fluid dispersion comprising: (i) at least one cryogenic fluid which is at its boiling point, and (2) at least onefinely divided solid additive characterized byhaving its melting point and at least a portion of its stable liquid phase within the temperature range formed by the boiling point of the cryogenic fluid and the temperature of said material, and
  • a method'for controllably extracting heat from a fabricated metallic article over a predetermined temperature range comprising: quenching said article in a fluid dispersion of ice in liquid nitrogen which is at its boiling point, said dispersion containing 10 to 70 percent by weight ice having a particle size of from'about 3 to 250 mesh.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
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US539429A 1966-04-01 1966-04-01 Cryogenic cooling Expired - Lifetime US3416977A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US539429A US3416977A (en) 1966-04-01 1966-04-01 Cryogenic cooling
GB14510/67A GB1157296A (en) 1966-04-01 1967-03-30 Improvements in and relating to Cryogenic Fluid Cooling Agents
CH458167A CH480427A (fr) 1966-04-01 1967-03-31 Procédé d'extraction de chaleur d'une matière et composition pour sa mise en oeuvre
DE19671551391 DE1551391A1 (de) 1966-04-01 1967-03-31 Kuehlfluessigkeit und Verfahren zu ihrer Verwendung
BE696473D BE696473A (OSRAM) 1966-04-01 1967-03-31

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3656826A (en) * 1970-07-17 1972-04-18 Westinghouse Electric Corp Method for the preparation and handling of highly oxygen reactant materials
US3906742A (en) * 1972-12-04 1975-09-23 Borg Warner Air conditioning system utilizing ice slurries
US4093553A (en) * 1974-07-05 1978-06-06 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Treating molten metal with a mixture of a cryogenic fluid and solid carbon black
US4181522A (en) * 1974-07-05 1980-01-01 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method of retarding the cooling of molten metal
US5964100A (en) * 1998-01-06 1999-10-12 Integrated Biosystems, Inc. System for freeze granulation
US6003300A (en) * 1997-01-21 1999-12-21 Stephen C. Bates Technique for high mixing rate, low loss supersonic combustion with solid hydrogen and liquid helium fuel
US6079215A (en) * 1998-01-06 2000-06-27 Integrated Biosystems, Inc. Method for freeze granulation
US20030003034A1 (en) * 2000-11-09 2003-01-02 Khan Mohamed H. Apparatus for producing nano-particles of molybdenum oxide
US20090169437A1 (en) * 2000-11-09 2009-07-02 Cyprus Amax Minerals Company Apparatus for Producing Nano-Particles of Molybdenum Oxide

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2772540A (en) * 1952-01-23 1956-12-04 Vierkotter Paul Cooling process and device for the performance of same
US2919862A (en) * 1953-08-31 1960-01-05 Knapsack Ag Process and apparatus for comminuting solid viscous substances, with a liquefied gas as a precooling agent
US2949392A (en) * 1958-12-18 1960-08-16 Aluminum Co Of America Method of relieving residual stresses in light metal articles
US3228838A (en) * 1959-04-23 1966-01-11 Union Carbide Corp Preservation of biological substances

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2772540A (en) * 1952-01-23 1956-12-04 Vierkotter Paul Cooling process and device for the performance of same
US2919862A (en) * 1953-08-31 1960-01-05 Knapsack Ag Process and apparatus for comminuting solid viscous substances, with a liquefied gas as a precooling agent
US2949392A (en) * 1958-12-18 1960-08-16 Aluminum Co Of America Method of relieving residual stresses in light metal articles
US3228838A (en) * 1959-04-23 1966-01-11 Union Carbide Corp Preservation of biological substances

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3656826A (en) * 1970-07-17 1972-04-18 Westinghouse Electric Corp Method for the preparation and handling of highly oxygen reactant materials
US3906742A (en) * 1972-12-04 1975-09-23 Borg Warner Air conditioning system utilizing ice slurries
US4093553A (en) * 1974-07-05 1978-06-06 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Treating molten metal with a mixture of a cryogenic fluid and solid carbon black
US4181522A (en) * 1974-07-05 1980-01-01 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method of retarding the cooling of molten metal
US6003300A (en) * 1997-01-21 1999-12-21 Stephen C. Bates Technique for high mixing rate, low loss supersonic combustion with solid hydrogen and liquid helium fuel
US5964100A (en) * 1998-01-06 1999-10-12 Integrated Biosystems, Inc. System for freeze granulation
US6079215A (en) * 1998-01-06 2000-06-27 Integrated Biosystems, Inc. Method for freeze granulation
US6170269B1 (en) 1998-01-06 2001-01-09 Integrated Biosystems, Inc. System for freeze granulation
US20030003034A1 (en) * 2000-11-09 2003-01-02 Khan Mohamed H. Apparatus for producing nano-particles of molybdenum oxide
US20060120950A1 (en) * 2000-11-09 2006-06-08 Khan Mohamed H Molybdenum oxide nano-particles
US7438888B2 (en) 2000-11-09 2008-10-21 Cyprus Amax Minerals Company Molybdenum oxide nano-particles
US20090142597A1 (en) * 2000-11-09 2009-06-04 Cyprus Amax Minerals Company Nano-Particles of Molybdenum Oxide
US20090169437A1 (en) * 2000-11-09 2009-07-02 Cyprus Amax Minerals Company Apparatus for Producing Nano-Particles of Molybdenum Oxide
US7622098B2 (en) 2000-11-09 2009-11-24 Cyprus Amax Minerals Company Method for producing nano-particles of metal oxide
US7749463B2 (en) * 2000-11-09 2010-07-06 Cyprus Amax Minerals Company Apparatus for producing nano-particles of molybdenum oxide
US7829060B2 (en) 2000-11-09 2010-11-09 Cyprus Amax Minerals Company Nano-particles of molybdenum oxide
US7883673B2 (en) 2000-11-09 2011-02-08 Cyprus Amax Minerals Company Apparatus for producing nano-particles of molybdenum oxide

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DE1551391A1 (de) 1971-03-04
BE696473A (OSRAM) 1967-10-02
GB1157296A (en) 1969-07-02
CH480427A (fr) 1969-10-31

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