Apparatus for preparation of sintered ceramic body of large dimension
A spark plasma sintering tool. The tool comprises a die including an inner wall having a diameter that defines an inner volume configured to receive a ceramic powder, and an upper punch and a lower punch operably coupled with the die, wherein each of the upper and lower punches have an outer wall defining a diameter that is less than the diameter of the inner wall of the die thereby creating a gap from 10 μm to 100 μm wide between each of the punches and the inner wall of the die when at least one of the punches moves within the inner volume of the die. Also disclosed is a method of using the tool to create a large sintered ceramic body and a computer readable medium storing processor-executable instructions adapted to cause one or more computing devices to operate the tool.
1 . A spark plasma sintering tool having a central axis and creating sintered ceramic bodies having dimensions of about 100 mm to about 625 mm, the tool comprising:
a. a die comprising a sidewall comprising an inner wall and an outer wall, wherein the inner wall has a diameter that defines an inner volume configured to receive at least one ceramic powder having a specific surface area (SSA) of from 1 to 18 m 2 /g as measured according to ASTM C 127 4; and
b. an upper punch and a lower punch operably coupled with the die, wherein each of the upper punch and the lower punch have an outer wall defining a diameter that is less than the diameter of the inner wall of the die thereby creating a gap between each of the upper punch and the lower punch and the inner wall of the die when at least one of the upper punch and the lower punch moves within the inner volume of the die, wherein the gap is from 10 μm to 100 μm wide,
wherein the spark plasma sintering tool comprises on the inner wall of the die at least one conductive foil which has a minimum thickness of 25 μm and wherein the gap is measured from an inwardly facing surface of the conductive foil closest to the upper and lower punches to the outer wall of each of the upper and lower punches.
2 . The spark plasma sintering tool of claim 1 wherein the at least one conductive foil comprises graphite, niobium, nickel, molybdenum, or platinum.
3 . The spark plasma sintering tool of claim 1 wherein the die, the upper punch, and the lower punch comprise at least one graphite material.
4 . The spark plasma sintering tool of claim 3 , wherein the at least one graphite material has a grain size selected from the group consisting of from 1 to 50 μm, from 1 to 40 μm, from 1 to 30 μm, from 1 to 20 μm, from 5 to 50 μm, from 5 to 40 μm, from 5 to 30 μm, from 5 to 20 μm, from 5 to 15 μm, and from 5 to 10 μm; and the graphite material has a density selected from the group consisting of from 1.45 to 2.0 g/cc, from 1.45 to 1.9 g/cc, from 1.45 to 1.8 g/cc, from 1.5 to 2.0 g/cc, from 1.6 to 2.0 g/cc, from 1.7 to 2.0 g/cc, and from 1.7 to 1.9 g/cc.
5 . The spark plasma sintering tool of claim 3 wherein the at least one graphite material includes an average coefficient of thermal and a radial deviation from the average coefficient of thermal expansion varies about the central axis of the tool by at least one amount selected from the group consisting of 0.3×10 −6 ppm/° C. and less, 0.25×10 −6 ppm/° C. and less, 0.2×10 −6 ppm/° C. and less, 0.18×10 −6 ppm/° C. and less, 0.16×10 −6 ppm/° C. and less, 0.14×10 −6 ppm/° C. and less, 0.12×10 −6 ppm/° C. and less, 0.1×10 −6 ppm/° C. and less, 0.0 8×10 −6 ppm/° C. and less, and 0.06×10 −6 ppm/° C. and less.
6 . The spark plasma sintering tool of claim 5 wherein the radial deviation from the average coefficient of thermal expansion of the at least one graphite material is maintained across a rotational position of from 0 to 360 degrees with respect to the rotational position of the die and upper and/or lower punches.
7 . The spark plasma sintering tool of claim 1 wherein at least one of the upper punch and the lower punch is coupled to an electrode and at least one of the upper punch and the lower punch is in ohmic contact with the die.
8 . The spark plasma sintering tool of claim 7 wherein the at least one ceramic powder is selected from the group consisting of yttrium oxide, aluminum oxide, sapphire, yttrium aluminum monoclinic (YAM), yttrium aluminum garnet (YAG), yttrium aluminum perovskite (YAP), zirconium oxide, titanium oxide, cordierite, mullite, cobaltite, magnesium aluminate spinel, silicon dioxide, quartz, calcium oxide, cerium oxide, ferrite, spinel, zircon, nickel oxide, copper oxide, strontium oxide, scandium oxide, samarium oxide, lanthanum oxide, lutetium oxide, erbium oxide, erbium aluminum garnet (EAG), hafnium oxide, vanadium oxide, niobium oxide, tungsten oxide, manganese oxide, tantalum oxide, terbium oxide, europium oxide, neodymium oxide, zirconium aluminate oxide, zirconium silicate oxide, hafnium aluminate oxide, hafnium silicate oxide, titanium silicate oxide, lanthanum silicate oxide, lanthanum aluminate oxide (LAO), yttrium silicate oxide, titanium silicate oxide tantalum silicate oxide, yttrium nitride, yttrium oxynitride, aluminum nitride, aluminum oxynitride, silicon nitride, silicon oxyni-tride, sialon materials, boron nitride, beryllium nitride, titanium nitride, tungsten nitride, forsterite, steatite, cordierite, mullite, barium titanate, lead titanate, lead zirconate titanate, Mn—Zn ferrite, Ni—Zn ferrite, and sialon.
9 . The spark plasma sintering tool claim 1 wherein the die, the upper punch, and the lower punch create a homogeneous temperature distribution in the at least one ceramic powder.
10 . The spark plasma sintering tool of claim 1 wherein the at least one ceramic powder has a specific surface area (SSA) selected from the group consisting of from 2 to 18 m 2 /g, from 3 to 18 m 2 /g, from 4 to 18 m 2 /g, from 5 to 18 from 6 to 18 m 2 /g, from 1 to 16 m 2 /g, from 2 to 16 m 2 /g, from 4 to 16 m 2 /g, from 6 to 16 m 2 /g, from 1 to 14 m 2 /g, from 1 to 12 m 2 /g, from 1 to 10 m 2 /g, from 1 to 8 m 2 /g, from 2 to 12 m 2 /g, from 2 to 10 m 2 /g, from 6 to 8 m 2 /g, and from 3 to 8 m 2 /g; and the at least one ceramic powder contains less than 100 ppm of total impurities; and the at least one ceramic powder has a resistivity of at least from about 1×10 +10 ohm-cm.
11 . The spark plasma sintering tool of claim 1 further comprising: a vacuum chamber applying a vacuum to the die, the upper punch, and the lower punch;
an upper punch electrode connected to the upper punch and a lower punch electrode connected to the lower punch;
a power source providing an electric current to the upper punch electrode and to the lower punch electrode;
a pressurizing system applying pressure to the upper punch and the lower punch; and a controller operating the various components of the tool.
12 . The spark plasma sintering tool of claim 1 wherein the gap is axisymmetric about the central axis.
13 . The spark plasma sintering tool of claim 1 wherein the gap is asymmetric about the central axis.
14 . The spark plasma sintering tool of claim 1 wherein the gap has a width selected from the group consisting of from 10 μm to 70 μm, from 20 μm to 70 μm, from 30 μm to 70 μm, from 40 μm to 70 μm, from 50 μm to 70 μm, from 60 μm to 70 μm, from 10 to 60 μm, from 10 to 50 μm, and from 10 to 40 μm.
15 . A computer readable medium storing processor-executable instructions adapted to cause one or more computing devices to create sintered ceramic bodies having dimensions of about 100 mm to about 625 mm by a method comprising:
a. disposing at least one ceramic powder having a specific surface area of from 1 to 18 m 2 /g as measured according to ASTM C 127 4 inside an inner volume of a spark plasma sintering tool, wherein the spark plasma sintering tool comprises a die comprising a sidewall comprising an inner wall and an outer wall, wherein the inner wall has a diameter that defines the inner volume, an upper punch and a lower punch operably coupled with the die, wherein each of the upper punch and the lower punch have an outer wall defining a diameter that is less than the diameter of the inner wall of the die thereby creating a gap from 10 μm to 100 μm wide between each of the upper punch and the lower punch and the inner wall of the die when at least one of the upper punch and the lower punch moves within the inner volume of the die,
wherein the spark plasma sintering tool comprises on the inner wall of the die at least one conductive foil which has a minimum thickness of 25 μm and wherein the distance of the gap is measured from the inwardly facing surface of the conductive foil closest to the upper and lower punches to the outer wall of each of the upper and lower punches;
b. moving at least one of the upper punch and the lower punch to apply pressure to the ceramic powder while heating the ceramic powder to a sintering temperature and sintering the ceramic powder to form the sintered ceramic body; and
c. lowering the temperature of the sintered ceramic body.