Patent Grant
7985059
This invention relates to the production of superhard products such as diamond, polycrystalline diamond, and cubic boron nitride produced by the high pressure and high temperature (HPHT) method. More particularly this invention relates to the HPHT containers or can assemblies in which superhard materials are processed. Superhard materials produced by the HPHT method are generally formed by encapsulating raw ingredients into a container, variously known in the art as a container, a can, an enclosure, a cup, a shield, or a tube.
A meltable sealant may be melted to seal the can. An area of ongoing research within the field of meltable sealant sealing is into methods to prevent the meltable sealant from flowing into the mixture of raw ingredients and causing contamination. One method that may prevent the contamination of the mixture is the use of an anti-wetting material such as stop-off. An anti-wetting material performs the function of arresting the wetting of a liquid onto a solid. With respect to a meltable sealant, an anti-wetting agent may hinder the spread of the melted meltable sealant. Anti-wetting materials have taken the form of a solid plate or disc. However, anti-wetting plates or discs must be precisely cut and shaped to fit into the can to allow for impurities to leave the diamond and to prevent meltable sealant from contaminating the diamond. Additionally, the process of manufacturing and using stop-off discs may be costly and due to improperly fitted discs may lead to low yields.
U.S. Pat. No. 4,333,902 to Hara which is herein incorporated by reference for all that it contains, discloses a process of producing a sintered compact comprising filling a cup with a powdered material to be sintered, putting on an opening of the cup a covering member consisting of a lid and solder so as to permit ventilation between the interior and exterior of the cup to form a cup assembly, applying heat as well as vacuum to the cup assembly to degas the powdered material, melting the solder by the continuation of heat to air-tightly seal the cup with the lid to obtain a closed cup compressible under high pressure at high temperature while maintaining the air-tight seal, and hot-pressing the closed cup to obtain a sintered compact. The covering member may include a porous lid closing the cup and a solder put on the porous lid.
U.S. Pat. No. 4,425,315 to Tsuji, et al. which is herein incorporated by reference for all that it contains, discloses a diamond sintered compact wherein diamond crystal particles are uniformly orientated in a particular direction and the method for producing the same, and has for an object to provide a diamond sintered compact having a high thermal conductivity particularly suitable for heat sink for use in the field of electronics. According to the invention, graphite is used as carbonaceous raw material, diamond crystal particles having such elongated shape that the ratio of the length of the long axis to that of the short axis is more than 2 being synthesized in such state that the greater part of the crystal particles have their long axes uniformly oriented in a particular direction, the crystal particles being sintered in the direction of the long axes thereof so that transformation of the graphite into diamond and sintering thereof may be accomplished synchronously. The invention has for an object to obtain a diamond sintered compact suitable for the aforesaid use by degassing reaction system raw material plugged into an air permeable container by heating it in vacuum in order to intercept gaseous components causing a decrease of thermal conductivity at the time of synthesizing diamond from carbonaceous material and a catalytic metal and sintering thereof, subsequently the air permeable part of the said container being sealed by means of soldering material preliminarily placed in contact with the said container.
U.S. Pat. No. 6,596,225 to Pope, et al. which is herein incorporated by reference for all that it contains, discloses sealing of the can by electron beam welding at high temperature and in a vacuum.
U.S. Patent Publication No. 2005/0044800 to Hall, et al. which is herein incorporated by reference for all that it contains, discloses an assembly for High-Pressure High-Temperature (HPHT) processing comprising a can, a cap, a meltable sealant and sealant barrier, and a superhard mixture comprising superhard particles. The superhard particles may be positioned adjacent a substrate of cemented metal carbide. The can and cap contain the superhard mixture with the sealant barrier positioned within the assembly so as to be intermediate the sealant and at least a portion of the mixture, thereby preventing the sealant from coming in contact with the mixture during processing. The assembly is placed within a vacuum chamber and heated to a temperature sufficient to cleanse the assembly and then melt the sealant providing a hermetic seal for the assembly in preparation for further HPHT processing.
U.S. Patent Publication No. 2008/0057145 to Hall, et al. which is herein incorporated by reference for all that it contains discloses an improved assembly for HPHT processing having a can with an opening and a mixture disposed within the opening. A sealant barrier is positioned atop the mixture. First and second lids are positioned atop the mixture. A meltable sealant positioned intermediate the second lid and a cap covering the opening.
Not withstanding the preceding patents, there remains a need in the art for an easier and more cost effective method of preventing meltable sealant contamination within the can.
In one embodiment of the present invention, an assembly for HPHT processing comprises a can with an opening. A powder mixture is disposed within the opening. A substrate is disposed within the opening adjacent the powder mixture. Paint is coated on a surface within the opening and opposite the mixture with respect to the substrate. A meltable sealant is disposed within the opening and opposite the substrate with respect to the surface and a cap is covering the opening.
The assembly for HPHT processing may further comprise an under lap component between the substrate and the meltable sealant. The under lap component may comprise a disc with a fold along a perimeter. At least a portion of the surface coated with paint may form part of the under lap component. At least a portion of the surface coated with paint may form an entire exterior of the under lap component. The fold of the disc may comprise an angle of substantially 180 degrees. The assembly for HPHT processing may further comprise a first metal disc disposed intermediate the substrate and the under lap component and a second metal disc disposed opposite the under lap component from the first metal disc. The first metal disc and second metal disc may comprise a melting temperature higher than the melting temperature of the meltable sealant. The first metal disc and second metal disc may be nonreactive with the substrate. At least a portion of the surface coated with paint may form part of the first metal disc. At least a portion of the surface coated with paint may form a periphery of the first metal disc.
The can may comprise a fold around a mouth of the can and may separate the metal disc from the under lap component. A portion of the second metal disc may contact the fold in the can. The fold in the under lap component may be urged by a resilient force against the fold in the can to form a tight seal. The meltable sealant may comprise a material selected from the group consisting of copper, nickel, cobalt, gold, silver, manganese, palladium, titanium, niobium, zinc, phosphorus, boron, aluminum, cadmium, chromium, tin, silicon, tantalum, alloys, compound mixtures, and combinations thereof. The paint may comprise isopropanol, plasticizer, polyethylene glycol, polyvinyl butyral resin, alcohol, anti-wetting material, or combinations thereof. A method of making a paint may comprise providing 500 ml of isopropanol, adding 20 ml of plasticizer and 20 ml of polyethylene glycol to the isopropanol, mixing the isopropanol, plasticizer and polyethylene glycol, further adding 40 gm of polyvinyl butyral resin and 400 ml of isopropanol, shaking all ingredients until all the polyvinyl butyral resin is dissolved and adding 1 gm of stop off per ml of all ingredients.
In another embodiment of the present invention, a method of sealing an assembly for HPHT processing comprises a can with an opening. A powder mixture is disposed within the opening. A substrate is disposed within the opening adjacent the powder mixture. A meltable sealant is disposed within the opening and opposite the powder mixture with respect to the substrate. A cap covers the opening. A surface within the opening and between the meltable sealant and the substrate is coated with paint. The can is heated such that a substantial portion of impurities are driven from the can. The can is further heated such that the meltable sealant melts. The meltable sealant is blocked from accessing the powder mixture with the paint and the can is cooled such that the meltable sealant solidifies. The coating of the surface with paint may comprise dipping the surface into paint before disposing it inside the can. The coating the surface with paint may comprise applying the paint on the surface with a paintbrush. The coating the surface with paint may comprise applying the paint on the surface with a swab.
In another embodiment of the present invention, an assembly for HPHT processing comprises a can with an opening, a powder mixture disposed within the opening, a substrate disposed within the opening adjacent and above the powder mixture, a formable sealant barrier within the opening above the substrate, a meltable sealant within the opening above the formable sealant barrier, and a cap covering the opening.
In another embodiment of the present invention, the assembly may comprise a can with an opening, a powder mixture disposed within the opening, a substrate disposed within the opening adjacent and above the powder mixture, a first layer of formable sealant barrier within the opening above the substrate, a lower niobium disc within the opening above the first layer of formable sealant barrier, a second layer of formable sealant barrier within the opening above the lower niobium disc, an under lap component within the opening above the second layer of formable sealant barrier, a steel disc within the opening above the underlap component, a meltable sealant within the opening above the steel disc, and cap placed on the assembly. The can may additionally comprise a fold. The fold may form a lid within the can.
In another embodiment, the assembly may comprise a ram disposed within the opening adjacent the formable sealant barrier. The ram may displace a portion of the formable sealant barrier.
The formable sealant barrier may comprise a formable structure such as a powder, a gel, an oil, a putty, or a combination thereof. The formable sealant barrier may also comprise a composition of aluminum oxide or boron nitride.
The meltable sealant may be a material selected from the group consisting of copper, nickel, cobalt, gold, silver, manganese, palladium, titanium, niobium, zinc, phosphorus, boron, aluminum, cadmium, chromium, tin, silicon, tantalum, alloys, compound mixtures, and combinations thereof having a melting point, or melting range, at least partially higher than the temperature required to cleanse the assembly.
In another embodiment of the present invention, a method of preparing an assembly for HPHT processing uses the steps of providing an assembly comprising a can with an opening and a powder mixture disposed within the opening, a substrate being adjacent and above the powder mixture, a formable sealant barrier positioned above the substrate, a meltable sealant disposed intermediate the sealant barrier and a cap covering the opening; next heating the assembly to a cleansing temperature for a first period of time; then further heating the assembly to a sealing temperature for a second period of time.
The assembly may be heated in a vacuum. The assembly may be further heated in an inert gas and brought back to atmospheric pressure at a temperature sufficient to melt the sealant.
The cleansing temperature may be between 800° C. and 1050° C. The sealing temperature may be between 1000° C. and 1200° C. The first period of time may be between 15 minutes and 60 minutes and the second period of time may be between 2 minutes and 25 minutes.
a is a cross-sectional diagram of another embodiment of an assembly for HPHT processing.
b is a cross-sectional diagram of another embodiment of an assembly for HPHT processing.
a is a cross-sectional diagram of another embodiment of an assembly for HPHT processing.
b is a cross-sectional diagram of another embodiment of an assembly for HPHT processing.
a is a cross-sectional diagram of an embodiment of a container filled with paint.
b is a cross-sectional diagram of an embodiment of a container filled with stop off.
a is a perspective diagram of an embodiment of an under lap component.
b is a perspective diagram of an embodiment of a paintbrush.
c is a perspective diagram of an embodiment of a swab.
a is a cross-sectional diagram of another embodiment of an assembly for HPHT processing.
b is a cross-sectional diagram of another embodiment of an assembly for HPHT processing.
c is a cross-sectional diagram of another embodiment of an assembly for HPHT processing.
It is to be appreciated that directional language used throughout this application, such as above or below, is with reference to the figures and is not limiting of the claims. In practice, embodiments may be oriented differently from the orientations shown in the figures.
Referring now to the figures,
At least a portion of the can 101 may comprise niobium, a niobium alloy, a niobium blend, or combinations thereof. At least a portion of the cap 102 may comprise a metal or metal alloy. Line BB describes the plane of the cross section of some of the subsequent figures.
The assembly 100 may comprise a can 101 with an opening 200. A powder mixture 204 may be disposed within the opening 200. A substrate 202 may be disposed within the opening 200 adjacent the powder mixture 204. A first metal disc 207 may be placed within the opening 200 and opposite the mixture 204 with respect to the substrate 202. A second metal disc 209 may be placed opposite the first metal disc 207 with respect to the under lap component 253. A meltable sealant 206 may be disposed within the opening 200 on top of the second metal disc 209. A cap 102 may cover the opening 200 of the can 101.
The can 101 may then be heated to remove the impurities present in the powder mixture 204. After contaminants have left the powder mixture 204 the temperature may then be raised such that the meltable sealant 206 begins to melt. The meltable sealant 206 may seal the can 101 by binding the cap 102 to the walls of the can 101. It is believed that this seal may be able to maintain a sterile vacuum within the can 101. The sterile vacuum will in turn prevent the recontamination of the powder mixture 204.
The assembly 100 may further comprise paint coated on a surface 220 within the opening 200 and opposite the powder mixture 204 with respect to the substrate 202. At least a portion of the surface 220 coated with paint may form part of the under lap component 253. The under lap component 253 may be dipped into the paint. Similarly, at least a portion of the surface 220 coated with paint may form a part of the first metal disc 207. In one embodiment, the periphery of the first metal disc 207 may be coated with paint.
Referring to
a and 4b are cross-sectional diagrams of another embodiment of an HPHT processing assembly 100. The assembly 100 may comprise a first metal disc 207 and second metal disc 209 comprising a melting temperature higher than the meltable sealant 206. The first metal disc 207 and second metal disc 209 are believed to be nonreactive with the substrate 202. The first metal disc 207 and the under lap component 253 may comprise niobium, tantalum, or combinations thereof.
a and 7b are cross-sectional diagrams of embodiments of containers filled with paint 700 and filled with stop off 710 respectively. The paint 700 may comprise isopropanol, plasticizer, polyethylene glycol, polyvinyl butyral resin, alcohol, anti-wetting material, or combinations thereof. A method of making the paint 700 comprises filling a 1000 ml neoprene bottle with 500 ml of isopropanol. Further adding 20 ml of plasticizer and 20 ml of polyethylene glycol into the neoprene bottle and mixing together. Further mixing 40 gm of polyvinyl butyral resin and 400 ml of isopropanol and shaking until all the polyvinyl butyral resin is dissolved. Finally adding 1 gm of stop off 710 per ml of all ingredients. It is to be remembered that stop off 710 should be added an hour prior to using the paint 700. It is believed that leaving the paint 700 with stop off 710 for more than an hour may result in separation of the ingredients.
a is a perspective diagram of an embodiment of an under lap component 253 before rolling and forming a fold 300. The underside or exterior portion of the under lap component 253 may comprise a surface 220 coated with paint 700.
a is an exploded cross-sectional diagram of an embodiment of an assembly 900 for HPHT processing. The assembly 900 comprises a can 901 with an opening 902. A plurality of superhard particles 903 may be disposed within the opening 902 followed by a substrate 904. A first layer of a formable sealant barrier 905 may lie above and adjacent to the substrate 904. The first layer of formable sealant barrier 905 may lie substantially around the perimeter of the substrate 904. A lower niobium disc 906 may lie adjacent and above the first layer of sealant barrier 905. A second layer of formable sealant barrier 907 may lie above the lower niobium disc 906. An under lap component 908 may lie above the second layer of sealant barrier 907. The under lap component 908 may be coated in an anti-wetting material. A metal disc 909 may lie adjacent to and above the under lap component 908. A meltable sealant 910 may lie adjacent to and above the metal disc 909. A cap 915 may cover the opening 902 of the can 901.
The metal disc 909 and cap 915 may comprise steel. The metal disc 909 and cap 915 may aid the meltable sealant 910 in sealing the can 901 by forming a eutectic mixture with the meltable sealant 910.
The meltable sealant 910 may comprise a material selected from the group consisting of copper, nickel, cobalt, gold, silver, manganese, palladium, titanium, niobium, zinc, phosphorus, boron, aluminum, cadmium, chromium, tin, silicon, tantalum, alloys, compound mixtures, and combinations thereof having a melting point, or melting range, at least partially higher than the temperature required to cleanse the assembly. The meltable sealant 910 may have a melting point above the temperature at which contaminants begin to leave the can 901. After a substantial amount of contaminants have left the can 901 the temperature may then be raised such that the meltable sealant 910 begins to melt. The meltable sealant 910 may seal the can closed by binding the cap 915 to the can 901. It is believed that this seal may be able to maintain a sterile vacuum within the can 901. The sterile vacuum will in turn prevent recontamination.
One embodiment of a meltable sealant 910 may comprise a copper disc. The process of using copper to seal the assembly is known in the art. Copper functions as a sealant due to its melting temperature relative to the temperature at which contaminants escape the assembly 900. Copper melts at a temperature of 1084.62° C., which may be a higher temperature than the temperature required to remove impurities from the assembly 900. The higher melting temperature of copper may allow for the temperature of the assembly 900 to be raised such that contaminants exit the assembly 900. The temperature may then be further raised causing the copper to melt and seal the assembly 900.
The first layer of formable sealant barrier 905 may comprise a formable anti-wetting material. In one embodiment, the first layer of formable sealant barrier 905 may comprise a boron nitride powder. In the past, a sealant barrier comprising stop-off which contains aluminum oxide was placed adjacent to the carbide substrate 904. It is believed that the aluminum oxide reacted negatively with the carbide substrate 904 causing cracking and weakness within the carbide substrate 904. It is further believed that boron nitride may function as an anti-wetting material and may not react negatively with the carbide substrate 904. The first layer of sealant barrier 905 may allow contaminants to flow through the barrier while functioning as an anti-wetting agent and preventing the inflow of a meltable sealant 910 into the superhard particles 903.
The second layer of sealant barrier 907 may comprise aluminum oxide. A powder that comprises aluminum oxide that may be used is stop-off. A suitable powder stop-off is manufactured under the brand name Nicrobraz by the Wall Colmonoy Corporation, 101 W. Girard, Madison Heights, Mich. 48071. It is believed that stop-off comprising aluminum oxide may function as a better sealant barrier than boron nitride, however due to the possible negative reaction between aluminum oxide and carbide the stop-off may be isolated to the second layer of sealant barrier 907.
b depicts a close-up cross-sectional view of an embodiment of an assembly 900 for HPHT processing. After the various components are inserted into the assembly 900 a portion of the can wall 920 may be folded inward over the sides of the under lap component 908 causing the two sides to fold inward together. It is believed that having both the can 901 and the under lap component 908 folded inward that the pathway for contamination to the superhard particles 903 will be more torturous. The assembly 900 in
c depicts a close-up cross-sectional view of an embodiment of an assembly 900 for HPHT processing. The assembly 900 in
In one embodiment the assembly may be heated 1602 to the cleansing temperature in a vacuum and then brought back to atmospheric pressure in an inert gas. The assembly may then be further heated 1603 to the sealing temperature while in an inert gas. In other various embodiments, the cleansing temperature may be between 800° C. and 1050° C. and the sealing temperature may be between 1000° C. and 1200° C.
Whereas the present invention has been described in particular relation to the drawings attached hereto, it should be understood that other and further modifications apart from those shown or suggested herein, may be made within the scope and spirit of the present invention.
This application is a continuation of U.S. patent application Ser. No. 12/512,863; now U.S. Patent Publication No. 2009/0301391 now U.S. Pat. No. 7,927,085; filed on Jul. 30, 2009, which is a continuation-in-part of U.S. patent application Ser. No. 11/469,229; now U.S. Pat. No. 7,575,425; filed on Aug. 31, 2006 and entitled “Assembly for HPHT Processing,” which is herein incorporated by reference for all that it contains. This application also claims priority to U.S. Provisional Patent Application No. 61/164,956 filed on Mar. 31, 2009, and entitled “Formable Sealant Barrier” which is herein incorporated by reference for all that it contains.
| Number | Name | Date | Kind |
|---|---|---|---|
| 4333902 | Hara | Jun 1982 | A |
| 4333986 | Tsuji | Jun 1982 | A |
| 4412980 | Tsuji | Nov 1983 | A |
| 4425315 | Tsuji | Jan 1984 | A |
| 4723999 | Hasselstrom | Feb 1988 | A |
| 6596225 | Pope | Jul 2003 | B1 |
| 20050044800 | Hall | Mar 2005 | A1 |
| 20080057145 | Hall | Mar 2008 | A1 |
| Number | Date | Country | |
|---|---|---|---|
| 20090302501 A1 | Dec 2009 | US |
| Number | Date | Country | |
|---|---|---|---|
| 61164956 | Mar 2009 | US |
| Number | Date | Country | |
|---|---|---|---|
| Parent | 12512863 | Jul 2009 | US |
| Child | 12512889 | US |
| Number | Date | Country | |
|---|---|---|---|
| Parent | 11469229 | Aug 2006 | US |
| Child | 12512863 | US |
