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Publication numberUS3895894 A
Publication typeGrant
Publication dateJul 22, 1975
Filing dateApr 23, 1973
Priority dateApr 26, 1972
Also published asDE2220349A1, DE2220349B2, DE2220349C3
Publication numberUS 3895894 A, US 3895894A, US-A-3895894, US3895894 A, US3895894A
InventorsBiermann Klaus, Burbach Jurgen, Gimpel Horst, Zirpins Burckhard
Original AssigneeKrupp Gmbh
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Device for generating high pressures and temperatures
US 3895894 A
Abstract
A device for generating high pressures and temperatures, in which in the pressure chamber of a high strength metallic pressure container, a charge of material laterally surrounded by electrically insulating material by means of two piston rams movable in opposite direction with regard to each other and sealed relative to the pressure container is subjected to pressure while being electrically heated. The pressure container comprises at least two axially aligned metallic ring members of high strength hard metal which define a pressure chamber, while between the rings and between the rings and a matrix surrounding the rings, pressure resistant electrically insulating material is provided. Outside the pressure chamber, sealing means of plastically deformable strong metallic material are provided between the piston rams and the rings.
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Description  (OCR text may contain errors)

[451 July 22,1975

United States Patent [1 1 Biermann et al.

3,727,028 4/1973 Kuratomi.............................. 425/77 DEVICE FOR GENERATING HIGH PRESSURES AND TEMPERATURES [75] Inventors: Klaus Biermann; .liirgen Burbach; Primar Examinerfijames Jones Horst Gimpel; Burckhard zirpins, Attorney, Agent, or Fzrm-Walter Becker all of Essen, Germany Assignee: Fried. Krupp Gesellschaft mit [57] ABSTRACT A device for generating high pressures and temperatures, in which in the pressure chamber of a high strength metallic pressure container, a charge of matebeschrankter Haftung, Essen, Germ any [22] Filed: 1973 rial laterally surrounded by electrically insulating ma- 21 Appl. No.: 353,738

terial by means of two piston rams movable in opposite direction with regard to each other and sealed rel- A ative to the pressure container is subjected to pressure [30] A gg l g n piglcauon Pnonty Data while being electrically heated. The pressure container pr. ermany............................

2220349 comprises at least two axially aligned metallic ring members of high strength hard metal which define a pressure chamber, while between the rings and between the rings and a matrix surrounding the rings, ressure resistant electrically insulating material is rovided. Outside the pressure chamber, sealing means of plastically deformable strong metallic matep 404 5N5 W References Cited UNITED STATES PATENTS rial are provided between the piston rams and the rings.

425/77 425 77 Ishizuka................................ 425/77 10 Claims, 3 Drawing Figures 2,94l,247 6/1960 2,995,776 8/196] Giardini et al...... 3,543,347 12/1970 PATENTED JUL 2 2 ms FIG. 1b

SHEET PATENTEDJUL 22 ms Q $35 a m m b Q m Q m N QZEQS o mzimzwm 2 cm on 3 mm Q as E 2. ON om QM mm g cm om E. om cm A a: L O Q N at 3. g 3 (cm) X W07 HNIHJVN DEVICE FOR GENERATING HIGH PRESSURES AND TEMPERATURES The present invention relates to a device for generating high pressures and temperatures, in which in the pressure chamber of a high-strength metallic pressure container a charge or filling of different materials laterally surrounded by electric insulating material is adapted to be subjected to pressure by means of two counter acting conical piston rams which are sealed relative to the pressure container, the respective charge or filling being adapted by electric current passing through the piston rams to be heated up directly or indirectly.

A device of this type has become known in which the conically designed pressure container is lined with bricks which have to meet two requirements, namely on the one hand to electrically insulate the two piston rams relative to the pressure container and on the other hand to seal the high pressure chamber. Embedded in the brick lining is a reaction vessel which receives the respective filling and which is made of insulating material. This known device has the drawback that for each test or experiment the brick lining has to be applied anew. This, however, involves considerable work and costs in view of the complicated design of the high pressure chamber. Furthermore it is disadvantageous that the limited deformability of the brick material does permit only a limited change of the high pressure volume under pressure.

It is, therefore, an object of the present invention to provide a device for generating high pressures and temperatures which will overcome the above mentioned drawbacks.

These and other objects and advantages of the inven tion will appear more clearly from the following specification in connection with the accompanying drawings, in which:

FIG. la illustrates a maximum pressure device according to the invention in non-loaded condition.

FIG. 1b shows the device of FIG. Ia under load.

FIG. 2 represents a prepared diagram for measuring and controlling the pressure, in which a test curve has been entered as an example.

The device according to he present invention is characterized primarily in that the pressure container comprises at least two axially successively arranged rings which surround the cylindrical pressure chamber with a metallic wall and which consist of hightensile hard metal, while between the rings and also between the rings and the surrounding fitting of high-tensile steel there is arranged pressure-resistant electric insulating material. The device according to the invention is furthermore characterized in that the seals provided outside the pressure chamber between the piston rams and the rings consist of a plastically deformable strong metallic material.

According to an advantageous feature of the invention, the electric insulating material may consist of thin layers of mica or similar pressure-resistant substances.

Referring now to the drawings in detail, the cylindrical high pressure chamber 12, in which the not illustrated filling material is surrounded by a tube 11 of a plastically deformable electric and, if desired, heat insulating material, preferably Whetstone, is enclosed by a metallic wall formed of three rings l-3 of high-tensile hard metal. While various types of filling material may be used, merely by way of example such filling material may consist of a mixture of percent by weight of carbon to 30 percent by weight of nickel. Between the rings 1-3 of high-tensile hard metal consisting e.g. of 88 percent by weight of tungsten carbide and 12 percent by weight of cobalt, on the one hand and between the rings and a fitting ring 4 which surrounds the rings 1-3 and consists of high-tensile steel on the other hand, there is provided a pressure-resistant electric insulating material in the form of thin mica layers 7. The installa tion of the mica layers 7 is carried out with high precision. During the assembly of the high pressure device, damage to the mica layers must be avoided. The fitting ring consists in a non-illustrated manner of a plurality of segments which together with the hard metal rings 1-3 and the mica layers 7 are simultaneously inserted into a steel ring 5. This whole assembly is subsequently without any change inserted into the main fitting ring 6 or matrix in such a way that a maximum pressure preload will be obtained in the hard metal rings l3.

According to a further feature of the invention, between the conical piston rams 8, 8a and the rings 1 and 3 surrounding the rams 8, 8a and provided with a corresponding conical chamber there are arranged cap-like seals 9, 9a which are located outside the pressure chamber 12 and which consist of plastically deformable strong metallic material. As an example for such material there may be mentioned steel containing 0.40 percent by weight of carbon, 0.050 percent of phosphorus and 0.050 percent by weight of sulfur, and having a tensile strength of from 6070 Kp/mm The device according to the invention will, in view of the metallic seal, permit a long ram stroke. Furthermore, the device can easily be made ready for a new test or experiment. To this end, the old sample is in a simple manner pressed out of the cylindrical pressure chamber and new filling material is introduced. Also new sealing caps are in a simple manner placed upon the piston rams 8, 8a. These two steps require little work and little time.

Inserted into the cap-like seals 9, 9a are conical intermediate punches 10, 10a of hard metal by means of which the piston rams 8, 8a act upon the charge or filling material. It is a well-known fact that the front ends of the piston rams which act upon the charge or filling material are, due to the combined stresses caused by the high pressures and temperatures, subjected to considerable wear. The intermediate punches 10, 10a can in a simple manner together with the seals be exchanged. In this way it is not necessary after the front ends of the piston rams are worn down to exchange the entire piston rams, which means a considerable saving in material.

Between the caps 9, 9a and the tube 11 there is provided a lead ring 13 which is simple to produce. This arrangement will assure that during the pressure buildup during which the distance between the rams 8, 8a is reduced, no material can escape from the high pressure chamber 12 because the gap between the intermediate punches 10, 10a and the hard metal rings 1 and 3 becomes smaller and smaller. Inversely, the lead ring will prevent that a portion of the material of the sealing caps 9, 90 will, during the building up of the pressure, be squeezed into the high pressure chamber. In this way it will be prevented that high frictional forces are generated between the punches 10, 10a on the one hand and the hard metal rings 1, 3 on the other hand whereby they might be destroyed or damaged. Furthermore it will be assured that the pressure will build up in the high pressure chamber 12 to the desired extent.

The piston rams 8, 8a are so designed that during the change in the shape of the caps, in other words during the building up of pressure in the high pressure chambet, the contacting surfaces between the rams and the caps will remain constant to a major extent. In this way it will be assured that not too great a portion of the outer forces exerted upon the rams 8, 8a will be consumed for changing the shape of the caps. According to an advantageous feature of the invention, the caps 9, 9a will during the building up of pressure exert an increasing lateral pressure upon the intermediate punches 10, 10a. In this way the extent to which these punches can be subjected to a load will be greatly increased in the direction in which they are subjected to their main load.

If the caps 9, 9a are subjected to a major deformation, there exists the danger that, in view of the nonhomogeneity of the material, the device will, when the pressure build-up starts, act eccentrically. This can be avoided in a simple manner by respectively inserting electrically insulating rings 15, a of synthetic material, e.g. the material sold under the trademark Adipren, between the holding means 14, 14a of the piston rams 8, 8a and the outer fitting members 4, 5, 6 of the high pressure chamber. These rings are during the pressure build-up uniformly elastically deformed with relatively small forces. In view of the large effective lever arms, a centering of the main fitting 6 toward the piston rams 8, 8a is forced. At the same time these rings serve as safety rings which are adapted to catch any material which might escape under pressure from the high pressure chamber.

Inasmuch as during the pressure generation there will neither material of the caps 9, 9a to any material extent escape into the high pressure chamber nor material escape from the high pressure chamber, a pressure gauging and pressure measuring can be effected in the following manner:

The total force required for deforming the caps is, independent of the respective pressure build-up in the high pressure chamber, a definite easily measurable monotonic decreasing function of the stroke performed by the rams 8, 8a. It may be assumed that the stroke is A h, the total force generated by the press is K and the force absorbed by the caps is K K (A 11). There is then obtained for the medium pressure p in the high pressure chamber the equation:

P K n in which F designates the cross sectional surface of the high pressure chamber.

Thus, if during the high pressure tests, by means of an x,y-coordinate recorder the total force K, which is adapted to be measured by means of a load cell, is recorded as a function of the stroke A h, which stroke is adapted to be directly measured by means of a motion pick-up, and if this function is entered or plotted in prepared diagrams, for instance a diagram according to FIG. 2, which are placed on the x,y-recorder, it is possible during the test at any time to read the pressure and, if necessary, to adjust or control the same. In the preprepared diagrams (see the stroke load diagram of the pressure measurement of FIG. 2), a family of curves is plotted for discrete values ofp constant which values where obtained on the basis of the above equation. The

family of curves can by means of electric resistance measurements on known metals be checked at certain pressures. The family of cures is as to the illustrated extent only valid for load condition; for no load or expansion another family of curves would have to be ascertained.

The heating of the high pressure chamber may be effected by suitable tubes of metal or graphite which are fitted into the insulating Whetstone tubes 11 and are electrically conductively connected to the rams 8, 8a. The rams are electrically insulated relative to the press generating the force. If desired, it is also possible to operate the device with centrally inserted heated conductors or with direct heating of the probes. The supply means for the current may in a non-illustrated manner be simply connected to the holding means 14, 14a of the rams 8, 8a.

As will be evident from the above, the device according to the present invention has several advantages over heretofore known devices of the type involved. Thus, the device according to the invention makes it possible with large starting volume of the filling material to produce high pressures also with substances of high compressibility. The metallic seals will, in view of their good deformability, permit a long stroke of the piston rams. During the high pressure tests, no electric contact is established between the two piston rams through the hard metal rings or the fittings therefor. Thus, the device according to the invention is suited for carrying out maximum pressure syntheses within a pressure range of from 30 to kbar. The device according to the invention may, for instance, be employed for producing diamonds, in which instance the starting materials may be highly compressible.

Another advantage of the device according to the invention is seen in the fact that the resetting of the device for a new test requires only little time and work. It is merely necessary that new sealing caps are inserted. Still another advantage of the invention consists in that the conditions for a structurally simple lining of the high pressure chamber for good thermal and electric insulation are given and also for simple and reliable pressure measuring methods in the high pressure chamber.

The actual construction of the device according to the invention with respect to the selection of the material and the geometry of the high pressure volume depends on the respective goal (pressure and temperature range, properties of the respective substance, as for instance compressibility). Accordingly, the principle of the invention embraces numerous possibilities of application and of design.

It is, of course, to be understood that the present invention is, by no means, limited to the particular showing in the drawings but also comprises any modifications within the scope of the appended claims.

What we claim is:

1. A device for generating high pressures and temperatures, which includes in combination: a high-strength metallic pressure container comprising a pressure chamber adapted to receive a tubular member of plastically deformable and electrically insulating material with a charge of material to be compressed therein, two oppositely located conical piston ram means arranged in axial alignment with each other and with said pressure chamber and movable toward and away from each other and said pressure chamber for respectively compressing a charge of material in a tubular member received in said pressure chamber and relieving the thus compressed charge, electric current conveying means electrically connected to said piston ram means for heating a charge to be compressed received in said pressure chamber, said pressure chamber being defined by at least two axially aligned annular members of high strength hard metal, pressure resistant insulating material interposed between and electrically insulating said annular members from each other, annular fitting means surrounding said annular members, additional pressure resistant mica insulating means permanently interposed durably between the outer periphery of said annular members and the inner peripheral surface of said fitting means and electrically insulating the same from each other, and strong metallic sealing means arranged between said piston ram means and at least the respective adjacent one of said annular members.

2. A device for generating high pressures and temperatures, which includes: a high-strength metallic pressure container comprising a pressure chamber adapted to receive a tubular member of plastically deformable and electrically insulating material with a charge of material to be compressed therein, two oppositely located conical piston ram means arranged in axial alignment with each other and with said pressure chamber and movable toward and away from each other and said pressure chamber for respectively compressing a charge of material in a tubular member received in said pressure chamber and relieving the thus compressed charge, electric current conveying means electrically connected to said piston ram means for heating a charge to be compressed received in said pressure chamber, said pressure chamber being defined by at least two axially aligned annular members of high strength hard metal, pressure resistant insulating material interposed between and electrically insulating said annular members from each other, annular fitting means surrounding said annular members, additional pressure resistant insulating means interposed between the outer periphery of said annular members and the inner peripheral surface of said fitting means and electrically insulating the same from each other, strong metallic sealing means arranged between said piston ram means and at least the respective adjacent one of said annular members, each of said piston rarn means comprising an outer piston and an inner piston smaller than said outer piston and inserted into the respective adjacent metallic sealing means for acting upon a charge in said pressure chamber, each of said outer pistons being operable to act upon the pertaining inner piston, holding means respectively connected to said outer pistons for holding the same, matrix means with a substantially cylindrical inner wall surrounding said pressure chamber, and elastically deformable electrically insulating ring means arranged between said holding means and said matrix means for centering said holding means relative to said matrix means.

3. A device according to claim 1, in which said first mentioned and said additional pressure resistant electrically insulating material includes layers of mica.

4. A device according to claim 2, in which said piston ram means and said metallic sealing means are so designed that during the deformation of said sealing means during the build up of pressure, the contacting surface of the piston ram means with said sealing means remains substantially the same.

5. A device in combination according to claim 1, in which each of said piston ram means comprises an outer piston and an inner piston smaller than said outer piston and inserted into the respective adjacent metallic sealing means for acting upon a charge in said pressure chamber, each of said outer pistons being operable to act upon the pertaining inner piston.

6. A device according to claim 2, in which said inner pistons are of hard metal.

7. A device according to claim 2, in which said metallic sealing means are cap shaped so as to exert an increasing lateral pressure upon the respective adjacent inner piston in response to increasing pressure exerted by said piston ram means upon a charge in said pressure chamber.

8. A device according to claim 2, which includes two intermediate rings of a plastically deformable material respectively interposed between said metallic sealing means adjacent each of said piston ram means and the respective adjacent end of a tubular member with a charge of material to be compressed within said pressure chamber.

9. A device according to claim 8, in which said intermediate ring is of lead.

10. A device according to claim 2, which includes matrix means with a substantially cylindrical inner wall surrounding said pressure chamber.

Patent Citations
Cited PatentFiling datePublication dateApplicantTitle
US2941247 *Apr 29, 1957Jun 21, 1960Gen ElectricTwo-stage high pressure high temperature apparatus
US2995776 *Mar 31, 1960Aug 15, 1961Giardini Armando AHigh pressure, high temperature apparatus and method
US3543347 *Aug 15, 1968Dec 1, 1970Ishizuka HiroshiUltrahigh pressure apparatus
US3727028 *Dec 3, 1971Apr 10, 1973T KuratomiUltra high pressure-temperature apparatus
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US4118161 *May 20, 1977Oct 3, 1978Kennametal Inc.High temperature, high pressure apparatus having a ductile driver element
US4140448 *Mar 27, 1978Feb 20, 1979Scandiamant AktiebolagHigh pressure apparatus
US4225300 *Aug 27, 1979Sep 30, 1980High Pressure Technology, Inc.Reliable high pressure apparatus
US4302168 *Jul 29, 1980Nov 24, 1981Khvostantsev Lev GHigh pressure producing apparatus
US4927345 *Feb 27, 1989May 22, 1990Ohwada Carbon Industrial Co., Ltd.Press cylinder for high-temperature, high-pressure pressing machine
US6022206 *Mar 24, 1998Feb 8, 2000Mcnutt; Peter D.Cubic multi anvil device
Classifications
U.S. Classification425/77, 425/354
International ClassificationB01J3/06
Cooperative ClassificationB01J3/065
European ClassificationB01J3/06D