US2941241A - High temperature high pressure apparatus - Google Patents

Description

June 21, 1960 H. M. STRONG 2,941,241

HIGH TEMPERATURE HIGH PRESSURE APPARATUS Filed Feb. 14, 1955 11 ;;l inventor.- l Henber-L'MSt-rcng His Attorney.

United States Patent HIGH TEWERATURE HIGH PRESSURE APPARATUS Herbert M. Strong, Schenectady, N.Y., assignor to General Electric Company, a corporation of New York Filed Feb. 14, 1955, Ser. No. 488,027

7 Claims. (Cl. 18-165) My invention relates to high temperature high pressure apparatus and specifically to such apparatus in which high temperatures and high pressures are maintained for prolonged periods of time.

An apparatus which is capable of producing temperatures of the order of several thousand degrees Centigrade and pressures of the order of 40,000 to 90,000 atmospheres for long time intervals is desirable to effect and control reactions occurring under such conditions. It is necessary to carefully design a vessel which is subjected to pressures of the above order to prevent explosive rupture of the device. The application of temperatures of the order mentioned greatly increases such design and construction problems. The invention of the present application provides an apparatus which produces concurrent high temperatures and high pressures of such orders for sustained periods of time without rupturing of the device.

Accordingly, it is an object of my invention to provide a new and improved high temperature high pressure apparatus.

It is another object of the invention to provide an improved apparatus which produces concurrent high temperature high pressure conditions for long time intervals.

It is a further object of the invention to provide an improved high temperature high pressure apparatus which effects and controls reactions at temperatures of the order of several thousand degrees Centigrade and pressures of the order of 40,000 to 90,000 atmospheres.

In carrying out my invention in one form, a reaction vessel is positioned within a member which is opposed by a die to provide a specimen chamber to be subjected to high temperature and high pressure conditions.

These and various otherobjects, features and advantages of the invention will be better understood from the following description taken in connection with the accompanying drawing in which:

Fig. 1 is a front elevational view of a hydraulic press with a high temperature high pressure apparatus which embodies my invention;

Fig. 2 is an enlarged sectional view of the high temperature high pressure apparatus which is shown in Fig. l; and

Fig. 3 is a modified high temperature high pressure apparatus.

In Fig. l of the drawing, a hydraulic press comprises a base with a press bed 11 on which is mounted a plurality of vertical shafts 12 to support a carriage 13 with a hydraulic shaft 14. A pair of opposed pistons 15 and 16 on bed 11 and carriage 13 are recessed to partially position members 17 therein. A layer of electrical insulation 18 is provided between at least one member 17 and its associated piston 15 to prevent conduction of electric current through the press. Upper member 17 comprises a central die 19 with one or more surrounding binding rings 20 which is opposed to a lower member 17 having a central block 21, an annular ring 22 thereon, and a plurality of binding rings 23. An electrical connection to each member 17 is provided by a conducting ring 24 with 2,941,241 Patented June 21, 1960 connector 25, which ring is positioned around the periphery of each outer binding ring to supply electric current from a source of power (not shown) through members 17 to the high temperature high pressure reaction vessel which is described below.

As is best shown in Fig. 2, die 19 of upper member 17 is tapered outwardly toward its center to provide a flat face. The upper face of block 21 of lower member 17 is tapered towards its center to support an annular ring 22 which tapers inwardly towards its center to provide a tapered outer surface adjacent a central aperture 26 in axial alignment with die 19. A reaction vessel 27 which is located within aperture 26 comprises a pair of spaced conductive discs 28 with a hollow conductive cylinder 29 therebetween adapted to contain a specimen 30 to be subjected to high temperatue high pressure conditions. A disc assembly 31 is located between block 21 and its associated disc 28 to provide a heat insulating core 32 with a surrounding outer conductive ring 33 in electrical contact with the block. A cylinder 34 of electrically insulating material surrounds discs 28, conductive cylinder 29 and disc assembly 31 to complete the assembly of reaction vessel 27. If it is desired, vessel 27 may be in the form of a hollow casing which is in electrical contact with block 21 but which is thermally insulated from annular ring 22.

Cylinder 34 is provided with a peripheral recess 35 adjacent the'open end of aperture 26 to support a hollow insulating sleeve 36 thereon. A pressure transmitting member 37, which is positioned within sleeve 36 between the face of die 19 and upper disc 28 of vessel 27, is tapered toward the center of its lower surface. A laminated conical gasket assembly 38 surrounds sleeve 36 and is mounted on the outer face of annular ring 22. Gasket assembly 38 is shown as comprising a plurality of thermal and electrical insulating and pressure resistant washers 39 with a metallic washer 40 between adjacent washers 39 to increase the pressure surrounding member 37 during operation of the apparatus. Sleeve 36 aligns member 37 with the face of die 19 and upper disc 28 while it prevents short-circuiting the flow of current through annular ring 22 of the press. Examples of suitable materials from which core 32, cylinder 34 and washers 39 may be made are pyrophyllite and catlinite.

In the operation of the high temperature high pressure apparatus, each member 17 with associated conducting ring 24 and connector 25 is positioned partially within the recess of its respective piston in the press. Specimen 30 which is to be subjected to a high temperature high pressure environment is placed in conductive cylinder 29 between discs 28 and within cylinder 34. A disc assembly 31 is located adjacent lower disc 28 after which reaction vessel 27 is positioned within aperture 26 of annular ring 22. Insulating sleeve 36 is fitted in recess 35 of cylinder 34 to extend therefrom. Gasket assembly 38 surrounds sleeve 36 and is mounted on the outer face of annular ring 22.

Pressure is applied to specimen 30 in cylinder 29 by member 37 which is positioned between die 19 and vessel 27. At the same time, electric current is supplied from an electrical connector, such as upper connector 25, to upper conducting ring 24, binding rings 20, die 19, member 37 and disc 28 to generate heat in cylinder 29 of reaction vessel 27. The current path continues from cylinder 29 through lower disc 28, ring 33, block 21, binding rings 23, conducting ring 24, and connector 25 to the electric source. Pressures in excess of 50,000 atmospheres at temperatures higher than 2000 C. have been maintained in such apparatus for periods of hours. If it is desired, reaction vessel 27 may also be subjected to high pressuresalone.

In Fig. 3 of the drawing, a modified high temperature high pressure apparatus is shown in. whichan insulating cylinder 41 is provided between conductive disc 28 and within insulating cylinder 34 of reaction vessel 27. A

wire heating coil. 42' is positioned around. the periphery: of cylinder 41 andis in electrical'icontactwith discs'123 to generate heat in this cylinder. Coilv 42 provides aobjects ofmy invention are attained by the "use of a reaction vessel which'is positionedfwithin a member that is opposed by adie to provide a specimen chamber to be subjected to hightemperature and 'high pressure conditions. I i

While other modifications of this invention and variations of apparatus have not bee described,the invention is intended to include all such as may be embraced within the following claims.

What I claim as newand desire to secure by Letters Patent of the United States is: e

1. A high pressure apparatus comprising a die, said die being tapered at one end to provide a flat outer surface, an opposed recessed member'facing said die, the recess in said member including a tapered outer surface adjacent a substantially cylindrical recess,-asubstantially cylindrical reaction vessel in the recess in said member, a pressure transmitting member, said pressure transmitting member having a substantially cylindrical base portion in contact with the outer face of said die, a face portion in contact with said reaction vessel, a gasket between the tapered outer surface of said recessed member and the tapered surface of said die, and means to move said die toward said recessed member.

2. A high pressure apparatus comprising a die, said die being tapered at one end to providea fiat outer surface, an opposed recessed member facing said die, said member comprising a block tapering at its outer end to-provide a fiat outer surface, an annular ring defining the recess in said member, one side of said ring positioned on and conforming to the shape ofthe tapered portion of said block, the other side of said ring conforming to the shape of the tapered portion of said die, a; substantially cylindrical reaction vessel in the recess in said member, a pressure transmitting member, said pressure transmitting member having a substantially cylindrical base portion in contact with the outer face of said die, a face portion in contact with said reaction vessel, said face portion having a tapered adjacent outer surface, a thermal and electrically insulating gasket assembly on said die betweenthe tapered portion thereof and the said conforming sides of said ring, and means to move said dietoward said ring; 1 a

3. A high pressure apparatus comprising a die, said die being tapered at one end-toprovide a fiat outer surface, an opposed recessed member facing said die-, said member comprising ablock tapering at-its outer end to provide a flat outer surface, an annular ring defining the recess in said member, one side of said ring positioned on and conforming to the shape of the tapered portion of said block, the other side of said'ring'conforming to the shape of the tapered portion of said die, a substantially cylindrical reaction vessel in the recess in said member, a pressure transmitting member, said pressure transmitting member haVinga substantially cylindrical base portion in contact with the outer face of said die, a face portion in contact with said reaction vessel, said face portion having an adjacenttapered outer surface, a conical gasket assembly surrounding said pressure transmitting memben and means to move said. die toward said recess.

4. High temperature high pressure apparatus comprising a pair of opposed, recessed pistons, means for exerting. pressure against at least one of. said pistons, a pair of members, one of said members being positioned partially within each of said recesses, a layer of insulation between one of said members and its associated piston, an electrical connection to each of said members, one of said members comprising a die, the other of said members comprising a block, the outer face of said block tapering towards its center, an annular ring positioned on said block, said ring tapering inwardly toward its center to provide a central aperture in axial alignment with said die, a reaction vessel located within the aperture of said annular ring, a pressure transmitting member positioned between said die and said vessel, an a conical gasket assembly surrounding the aperture of said annular ring, said gasket assembly comprising a plurality of insulating and pressure resisting washers, a metallic washer positioned between adjacent pressure resisting washers. 1

SJHigh temperature high pressure apparatus comprising a pair of opposed,- recessed pistons; means for exerting pressure against at least one ofsaid pistons, a pair of members, one. of said'members being positioned partially within'each of-said recessesya'layer of insulation between one of said members and itsassociated piston, an electrical connectionito each of said members,one of said members comprising a die, said die taper-ing outwardly towards its center, at'least one binding ring around said die, the other of said members comprising a block, the

outer face of said block tapering towards its center, an

annular ring positioned'on said block, said ring tapering inwardly towards itscenter to provide a central aperture in axial alignment with said die, the inner face of said ring engaging the outer face of said block, at least one binding ring surrounding said block and said ring, a reaction vessel located within the aperture'of said annular ring, said vessel comprising a pair of spaced conductive discs, a hollow conductive cylinder adapted to contain a specimen to be subjected to high temperature high pressure conditions positioned between said discs, a pressure transmitting member positioned between said die and said vessel, and a conical gasket assembly. surrounding the aperture of said annular ring, said gasket assembly comprising a plurality .of insulating and pressure resisting washers, a metallic washer positioned between adjacent pressure resisting washers.

6. High temperature .high pressure apparatus comprising a pair of opposed, recessed pistons, means for exerting pressure against at least one of said pistons, a pair of members, one of said members being positioned partially within each of said recesses, a layer of insulation between one of said members and its associated piston, an electrical connection to eachof said members, one of said members comprising a die, said .die tapering towards its center,-at least one binding ring around said die, the other of said members comprising a block, the outer face of said block taper-ing towards its center, an annular ring positioned on said block, said ring tapering inwardly towards its center to providea central aperture in axial alignment with said die, the inner face of said ring engaging the outer face of said block, at least one binding ring surrounding said block and said ring, a reactionyessel located within the aperture of said annular ring, said vessel comprising a pair-of spaced conductive. discs, a hollow conductive cylinder adapted to contain a specimen to be subjectedto high temperature high pressure conditions positioned between said-discs, aninsulating .cylinder surrounding said conductivecylinder and discs, said insulating cylinder'provided with a peripheral recess. adjacent the open end of said aperture, a hollowinsulating sleeve positioned in said recess and extending therefrom, a pressure transmitting member positioned within said sleeve between said die and said vessel, and a conical gasket assembly surrounding said sleeve and mounted on the outer face of the annular ring of said second member, said gasket assembly comprising a plurality of insulating and pressure resisting washers, a metallic washer positioned between adjacent pressure resisting washers.

7. High temperature high pressure apparatus comprising a pair of opposed, recessed pistons, means for exerting pressure against at least one of said pistons, a pair of members, one of said members being positioned partially Within each of said recesses, a layer of insulation between one of said members and its associated piston, an electrical connection to each of said members, one of said members comprising a die, said die tapering towards its center, at least one binding ring around said die, the other of said members comprising a block, the outer face of said block tapering towards its center, an annular ring positioned on said block, said ring tapering inwardly towards its center to provide a central aperture in axial alignment with said die, the inner face of said ring engaging the outer face of said block, at least one binding ring surrounding said block and said ring, a reaction vessel located within the aperture of said annular ring, said vessel comprising a pair of spaced conductive discs, a hollow insulating cylinder adapted to contain a specimen to be subjected to high temperature high pressure conditions positioned between said discs, a heating coil positioned around said cylinder, said coil being in electrical contact with said discs, a third disc assembly positioned between said block and its associated disc, said third disc assembly comprising a heat insulating core and an outer conductive ring in electrical contact with said block, a second insulating cylinder surrounding said first insulating cylinder and discs, said second insulating cylinder provided with a peripheral recess adjacent the open end of said aperture,

an insulating sleeve positioned in said recess and extending therefrom, a pressure transmitting member located within said sleeve in electrical contact with said die and said reaction vessel, and a conical gasket assembly surrounding said sleeve and mounted on the outer face of the annular ring of said second member, said gasket assembly comprising a plurality of insulating and pressure resisting washers, a metallic washer positioned between adjacent pressure resisting washers.

References Cited in the file of this patent UNITED STATES PATENTS 1,609,460 Buttles Dec. 7, 1926 2,540,457 Rice Feb. 6, 1951 2,544,414 Bridgman et a1 Mar. 6, 1951 2,554,499 Poulter May 29, 1951 2,637,203 Gehman May 5, 1953 OTHER REFERENCES

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