Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B21/00—Nitrogen; Compounds thereof
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
  • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
  • B01J19/122—Incoherent waves
  • B01J19/126—Microwaves
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/25—Diamond
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/25—Diamond
  • C01B32/26—Preparation
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
  • C30B25/02—Epitaxial-layer growth
  • C30B25/10—Heating of the reaction chamber or the substrate
  • C30B25/105—Heating of the reaction chamber or the substrate by irradiation or electric discharge
• • C—CHEMISTRY; METALLURGY
  • C30—CRYSTAL GROWTH
  • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
  • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
  • C30B29/02—Elements
  • C30B29/04—Diamond
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
  • B01J2219/12—Processes employing electromagnetic waves
  • B01J2219/1203—Incoherent waves
  • B01J2219/1206—Microwaves
  • B01J2219/1209—Features relating to the reactor or vessel
  • B01J2219/1212—Arrangements of the reactor or the reactors
  • B01J2219/1218—Multiple reactors
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
  • B01J2219/12—Processes employing electromagnetic waves
  • B01J2219/1203—Incoherent waves
  • B01J2219/1206—Microwaves
  • B01J2219/1209—Features relating to the reactor or vessel
  • B01J2219/1221—Features relating to the reactor or vessel the reactor per se
  • B01J2219/1224—Form of the reactor
  • B01J2219/123—Vessels in the form of a cup
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
  • B01J2219/12—Processes employing electromagnetic waves
  • B01J2219/1203—Incoherent waves
  • B01J2219/1206—Microwaves
  • B01J2219/1209—Features relating to the reactor or vessel
  • B01J2219/1221—Features relating to the reactor or vessel the reactor per se
  • B01J2219/1239—Means for feeding and evacuation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
  • B01J2219/12—Processes employing electromagnetic waves
  • B01J2219/1203—Incoherent waves
  • B01J2219/1206—Microwaves
  • B01J2219/1287—Features relating to the microwave source
  • B01J2219/129—Arrangements thereof
  • B01J2219/1293—Single source

Definitions

• the present invention relates to methods and apparatus for performing the combinatorial synthesis of the heterodiamond unit cell and a heterodiamond mass therefrom.
• it relates to methods and apparatus for controllably producing a heterodiamond molecule having the tetrahedral structure of the diamond unit cell with a heteroatom controllably, and with precise stoichiometry, substituted into the diamond unit cell thereby replacing a carbon atom.
• heterodiamond is conventionally defined to mean a super hard material containing boron, carbon and nitrogen (BCN). It is formed at high temperatures and high pressures, e.g., by application of an explosive shock wave to a mixture of diamond and cubic boron nitride.”
• BCN boron, carbon and nitrogen
• the heterodiamond of the present invention is produced using combinatorial l synthesis reactions at or around ambient pressure.
• heterodiamond of the present invention synthesized controllably and with precise stoichiometry, can be exclusively either aza-diamond or bora-diamond. This is the definition and meaning of the term “heterodiamond” as used in the present specification, which is not to be confused with the conventionally used term “heterodiamond,” which is BCN as already noted.
• diamond molecule has been incorrectly used for diamondoid molecules and masses of diamondoid molecules such as adamantine.
• adamantane is a hydrocarbon whose structure is unrelated to that of the diamond unit cell: the diamond molecule.
• Zhao et al. in US 7,938,997, disclose the preparation of a bulk superhard B-C-N nanocomposite compact. This is done by first ball-milling a mixture of graphite and hexagonal boron nitride, which is then encapsulated in a pressure range of 15 GPa to about 25 GPa and sintered at a temperature ranging from 1 ,800 to 2,500 K. These compacts include both boron and nitrogen.
• the heterodiamond of the present invention is produced by a combinatorial synthesis reaction at generally ambient conditions. Furthermore, the present invention controllably yields either bora-diamond or aza-diamond individually with precise stoichiometries. Popov et al.
• Goglio et al. disclose the decomposition of commercial thiosemicarbazide at 600°C under nitrogen flow to produce carbon nitrides. This is different from the present invention wherein a carbon of the diamond unit cell is substituted with a heteroatom to produce a heterodiamond unit cell using a combinatorial synthesis.
• heterodiamond wherein a heteroatom becomes an integral atom in the unit cell, occupying either an apical position or center, "cage,” position of the unit cell.
• the diamond unit cell is the smallest assembly of carbon atoms that make up diamond. It is, essentially, the diamond molecule.
• the diamond unit cell is a tetrahedral structure comprising five carbon atoms with a carbon atom at each of the four apices and one in the center, "cage" position. Each carbon atom is bonded to each other carbon atom of the diamond unit cell.
• the bonds in diamond are short, strong sp3 bonds, which render the three-dimensional, solid structure of diamond, as opposed to graphite, another allotrope of carbon, which has sp2 bonds and is planar.
• the preparation of the diamond unit cell whose structure is shown below, is described in U.S. 8,778,295 and U.S. 9,061 ,917:
• Diamond produced conventionally has several disadvantages including the following three.
• As a material, diamond has many desirable properties that make it ideal for microelectronic, optics, and other technological applications. These include extreme hardness, high index of refraction, high dielectric constant, extremely broad transparency bandwidth, band gap energy of around 5.45 ev, and others.
• diamond is an excellent electrical insulator, it is also one of the best heat conductors, more than four times better than copper.
• conventional methods of producing diamond have not been able to exploit these properties sufficiently to meet the large potential industrial demand that diamond, as a technological material, deserves.
• no method and apparatus to date has been able to produce reliably and controllably an identifiable diamond unit cell wherein a carbon atom is substituted by a heteroatom to produce "heterodiamond" as defined herein.
• a diamond p-type semiconductor can be produced by doping diamond with boron.
• boron is introduced into the gas stream of the reactor to form a boron impurity (i.e., dopant) that is incorporated into the diamond.
• This boron is not controllably substituted for a carbon of the diamond unit cell, thus controllably and predictably yielding a heterodiamond unit cell. Rather, as an impurity, it is essentially a useful defect in the diamond crystal lattice. It is also known that nitrogen can be contained within CVD-produced diamond.
• diamond has been used conventionally, albeit incorrectly, for a very hard material containing boron, carbon and nitrogen (BCN) usually formed by applying a shock wave to a mixture of diamond and cubic boron nitride.
• BCN boron, carbon and nitrogen
• heterodiamond has been used conventionally to describe a ceramic material, which is not structurally related to diamond.
• These ceramic materials do not reliably, controllably, and consistently comprise a diamond unit cell that has been modified to include a heteroatom such as boron or nitrogen substituting for a carbon atom of the diamond unit cell to produce a heterodiamond unit cell.
• the present invention is directed to a diamond unit cell having a carbon replaced by a single heteroatom such as nitrogen or boron resulting in a heterodiamond unit cell.
• the term “heterodiamond” is used to mean a material comprising at least one diamond unit cell wherein a heteroatom, such as nitrogen or boron, replaces a carbon atom: the heterodiamond unit cell.
• a heteroatom such as nitrogen or boron
• the homo-penta-atomic molecule having five carbon atoms in a tetrahedral configuration with one carbon atom occupying the center "cage" position and four carbon atoms deployed apically is designated the “homodiamond unit cell.”
• the heteroatoms of the present invention are structurally a part of the crystal lattice because they are structural elements of the heterodiamond unit cells and of the heterodiamond mass which they comprise.
• a heteroatom can occupy one of two positions of the heterodiamond unit cell, the center "cage" position or an apex position of the tetrahedron.
• a geometric analysis can be performed relating to atoms with sizes that are close to that of carbon.
• carbon is flanked by the III, V elements boron and nitrogen, respectively.
• Carbon has an atomic radius of 70 pm, while boron and nitrogen have atomic radii of 85 pm and 65 pm, respectively.
• the covalent radii of carbon, boron and nitrogen are 77 pm, 83 pm, and 75 pm, respectively.
• nitrogen is small enough to occupy the center "cage" position of the diamond unit cell.
• the atomic radius and covalent radius of boron are such that it can occupy an apical position of the heterodiamond unit cell.
• Heterodiamond unit cells which are the subject of the present invention, include aza-diamond, in which the
• heteroatom is nitrogen, and bora-diamond, in which the heteroatom is boron. These are shown below:
• aza-diamond bora-diamond The skilled practitioner will also recognize that aza-diamond and bora-diamond, once formed, are charged monopoles, that is, species bearing charge with no counter charge.
• Still another object of the invention is producing a heterodiamond unit cell by a vapor phase reaction.
• Another object of the invention is to produce a heterodiamond unit cell by a solid state reaction.
• a further object of the present invention is to produce a mixture comprising both homodiamond unit cells and heterodiamond unit cells.
• Yet a further object of the present invention is an apparatus that can produce homodiamond unit cells, heterodiamond unit cells, and any combinations thereof.
• (A) shows a vapor phase reaction for producing homodiamond using tetrahedrane as the tetrahedranoidal reactant.
• (B) shows a vapor phase reaction that produces homodiamond using three other tetrahedranoidal reactants.
• Figure 2 shows three reactions for producing excited state atomic nitrogen and one reaction for producing excited state atomic boron.
• Figure 5 depicts a solid state reaction for forming aza-diamond.
• Figure 6 is a schematic diagram of an integrated, controlled system for producing heterodiamond and homodiamond unit cells and a mixture of any combination thereof.
• Figure 7 is a schematic diagram with added detail of a portion of the integrated, controlled system for producing heterodiamond and homodiamond unit cells and a mixture of any combination thereof.
• Figure 8 is a schematic diagram of a deposition chamber adapted to receive heterodiamond and homodiamond unit cells and a mixture of any combination thereof from the integrated, controlled system of Figures 6 and 7.
• Figure 9 illustrates a process for producing an aza-diamond mass using a solid state reaction.
• Field measurements means measurements of experimental variables, such as temperature, pressure, reactant flow rates and nozzle sizes, for example, that may be adjusted with routine skill in the art to achieve best results.
• Tetrahedranoidal molecules as used herein means benzvalene, 3,4- diazabenzvalene and 2,3,4-methynyl-cyclobutanone. One or more of these molecules may be preferred in the reactions as described hereinbelow.
• Combinatorial syntheses of the diamond unit cell are disclosed in US 8,778,295 and US 9,061 ,917, which are fully incorporated herein by reference in their entirety. These syntheses proceed by the reaction of an excited state carbon atom with a tetrahedranoidal molecule with concomitant ejection of leaving groups to form the diamond unit cell.
• the diamond unit cell produced by these combinatorial reactions is a homo-penta-atomic molecule being comprised of 5 carbon atoms. While not intending to be bound by theory, it is believed that the excited state carbon atom "inserts" into the unit cell cage position.
• Figures 1 (A) and 1 (B) illustrate the diamond unit cell forming reactions of the above cited references.
• Insertion of an excited state heteroatom into a tetrahedranoidal molecule can be accomplished by adapting the methods of diamond unit cell synthesis described in the above cited references by substituting a heteroatom for a carbon atom in the diamond unit cell.
• a heteroatom for a carbon atom in the diamond unit cell.
• the atomic radius of the hetero-atom must be similar to that of carbon.
• the heteroatom must be capable of forming four sigma bonds (bond order of 4). Both nitrogen and boron and nitrogen have such capability.
• the atomic radius of carbon is 70 picometers (pm).
• the nitrogen atom has a radius of 65 pm
• the boron atom has a radius of 85 pm.
• the heterodiamond unit cell so produced is aza-diamond.
• the heteroatom is boron
• the heterodiamond unit cell so produced is bora-diamond. Both are hetero-penta-atomic molecules having the tetrahedron structure of diamond.
• the heterodiamond unit cells as discussed are charge monopoles in that they bear a charge without a species bearing a charge of opposite sign.
• the aza-diamond unit cell bears a positive charge because nitrogen must donate its lone pair of electrons to form the fourth sigma bond to a carbon atom of the tetrahedranoidal molecule.
• the bora-diamond unit cell bears a negative charge because the vacant orbital of the boron atom receives electron density from a carbon atom of the tetrahedranoidal molecule to form the fourth sigma bond between carbon and boron.
• Quaternary ammonium compounds of nitrogen such as tetramethyl ammonium salts are well known to organic chemists.
• Quaternary boride anions such as the tetraphenyl boride anion are also well known to organic chemists. Unipolar molecules have been well studied.
• cubane is replaced by a source of excited state nitrogen atoms.
• three nitrogen atom sources may be used: dinitrogen, ammonia, and hydrazine, respectively.
• the microwave discharge used for obtaining excited state carbon atoms from vapor phase cubane may be used to obtain excited state nitrogen atoms from ammonia and hydrazine.
• a high voltage discharge is used (Rayleigh). The same method may also be used with ammonia and hydrazine (reactions 2 and 3).
• thermodynamically favored recombination of nitrogen atoms to form dinitrogen is also advantageous because excess atomic nitrogen will recombine rather than deposit into the diamond mass so produced.
• the stoichiometric considerations required for the heterodiamond unit cell forming reaction are exactly opposite of those for the homodiamond unit cell forming reaction.
• an excess of the excited state atom to be cage inserted relative to the tehrahedranoidal reactant is required.
• an excess of the tetrahedranoidal compound relative to the excited state carbon atom is required.
• the reactions for forming the aza-diamond unit cell are shown in Figure 3.
• the excited state nitrogen atoms in inert carrier gas are delivered by a nozzle disposed within the volume of the vaporous tetrahedranoidal molecule "cloud," and this nozzle is also the high energy discharge apparatus that is a conduit comprising an electrical insulator within which are a discharge electrode pair.
• Such an apparatus, into which are disposed the discharge electrodes (these can be metal foils such as Cu, Pt, Pd, Au, etc.), may comprise diamond prepared by the diamond unit cell forming methods disclosed by Newman et al. in US
• the nozzle material may also comprise glass or ceramic, but diamond by the unit cell process is preferred owing to its electrical insulating properties unavailable by diamond produced by conventional processes. Nitrogen atom flow rates, dispensing nozzle dimensions and geometry are best determined by field measurements for preferred results and control by
• Benzvalene is vaporized between 77 and 80°C at 760 mm pressure at a rate of not more than 5°C per minute. Reduced pressure may be used for benzvalene vaporization with concomitant decrease in vaporization temperature, but the rate of heating should not be altered from that which is used for atmospheric vaporization of
• Tetrahedranone may be used as the tetrahedranoidal reactant, but it should only be vaporized at atmospheric pressure and at about 37°C to avoid autogenous ejection of CO which leads to decomposition of tetrahedranone.
• the solid state homodiamond unit cell forming reaction proceeds by forming a homogeneous blend of benzvalene and cubane in an 8:1 benzvalene : cubane ratio having high stoichiometric precision to prevent the formation of carbonaceous impurities in the mass of diamond unit cells so produced due to an excess (or deficiency) of either cubane or benzvalene. Care must be taken during preparative manipulations of the homogeneous blend of reactants such that this precise stoichiometric ratio is not altered by the vapor pressures of the two blend constituents.
• Hydrazine freezes at 2.0°C, boils at 1 13.5°C, and has a vapor pressure of 10mm at 30.7°C.
• stock solutions of benzvalene and hydrazine (substituted for cubane) in a solvent such as diethyl ether are prepared having a high degree of stoichiometric precision with respect to molar concentration. These solutions are combined in a ratio of 2:1
• a charge of opposite sign to that of the aza-diamond unit cell may be impressed upon the reaction vessel to mitigate like charge repulsions between the aza- diamond unit cells formed.
• the effect of a static electric field upon benzvalene has not been studied, to date. Accordingly, the reaction should be conducted in a sealed tube type of apparatus.
• the boron atomic radius is 85 pm and thus is unlikely to occupy the cage position of the diamond unit cell.
• anions are well known by both chemists and physicists to have radii larger than their neutral atom counterparts owing to the presence of excess electrons constituting the "noble gas shell.” Accordingly, a synthetic strategy for inserting a boron atom into the cage position of a tetrahedranoidal molecule should not be used. A different strategy is required because a different kind of heterodiamond unit cell is produced relative to the homodiamond unit cell or the aza-diamond unit cell.
• the bora-diamond unit cell must be prepared using an apical insertion strategy. This is unlikely to proceed using the method of US 9,061 ,917 using benzvalene.
• US 9,061 ,917 two other tetrahedranoidal reactants are disclosed: 3,4-diazabenzvalene and 2,3,4-methynyl-cyclobutanone ("tetrahedranone"). While their tetrahedranoidal structures are closely related to that of benzvalene structure, their stability is different. Both tetrahedranone and diazabenzvalene can decompose autogenously if care is not taken in storage and manipulations.
• Benzvalene does not decompose in the strict sense; rather, it re-arranges to benzene, which can be removed from benzvalene under reduced pressure.
• thermodynamically more stable re-arrangement product than cyclobutadiene This produces the bora-diamond unit cell by incorporating the boron atom apically.
• the preferred tetrahedranoidal molecule for this reaction is 2,3,4- methynyl-cyclobutanone because its counterpart, 3,4-diazabenzvalene, is only stable below -60°C.
• Tetrahedranone cannot be allowed to decompose autogenously; rather, this decomposition must be a result of the chemical interaction between tetrahedranone and an excited state boron atom. It is highly unlikely that an excited state boron atom will be able to react with an autogenous tetrahedranone decomposition transient. Thus, the conditions of the reaction must preserve the integrity of tetrahedranone in the vapor phase.
• bora- diamond must be prepared in the vapor phase following the procedures for vapor phase homodiamond unit cell synthesis of US 9,061 ,917 using tetrahedranone as the tetrahedranoidal compound and substituting diborane for cubane but maintaining temperature and pressure of the reaction within the narrow ranges detailed above to deter autogenous decomposition of tetrahedranone in favor of (excited state) boron atom interaction with tetrahedranone to form bora-diamond.
• Bora-diamond should preferably be formed by the reaction of tetrahedranone and an excited state boron atom. Accordingly, heat other than that used to vaporize the atomic boron source and tetrahedranone should not be applied to the reaction zone. Tetrahedranone is best vaporized at atmospheric pressure and at its vaporization temperature which is approximately 37°C. Higher temperatures are counter-indicated because tetrahedranone decomposes thermally. Pressures higher than one atmosphere would require a higher vaporization temperature for tetrahedranone which is likely to lead to autogenous and thermally induced decomposition of tetrahedranone.
• Reduced pressure can be used to reduce the heat required to vaoporize tetrahedranone, but this increases the likelihood of ejection of CO and concomitant decomposition of tetrahedranone.
• the proper use of reduced pressure to vaporize tetrahedranone to form the bora- diamond unit cell by the reaction of an excited state boron atom with vaporous tetrahedranone is preferably set by field measurements.
• reaction 4 the boron atom source may be diborane.
• the microwave discharge used for obtaining excited state carbon atoms from vapor phase cubane may be used to obtain excited state boron atoms from diborane.
• Reactions for forming the bora-diamond unit cell are shown in Figure 4.
• the boron source must be delivered to the system as a vapor in an inert carrier gas such as argon, helium, etc. Care must be taken to ensure that the boron atoms so produced are delivered to the reaction zone.
• the dispensing nozzle must be located within the "cloud" of vaporous tetrahedanoidal compound.
• the stoichiometric considerations required for the heterodiamond unit cell forming reaction using boron as the heteroatom are the same as those for the homo- diamond unit cell forming reaction.
• the excited state boron atoms in inert carrier gas are delivered by a nozzle disposed within the volume of the tetrahedranoidal molecule vapor.
• Boron atom flow rates, dispensing nozzle dimensions and geometry are determined by field measurements for optimization and control by appropriate hardware and software The same optimizations are done for the tetrahedranoidal molecule reactant to be used within the temperature and pressure ranges detailed above.
• bora-diamond unit cell The synthesis of the bora-diamond unit cell is limited to the vapor phase reaction. Synthetic chemists are well aware of the behavior of boron hydrides with carbonyl compounds. In synthetic organic chemistry, boranes are reducing agents for aldehydes and ketones. Hence, a blend of diborane and
• bora- diamond must be prepared in the vapor phase following the procedures for vapor phase diamond unit cell synthesis of US 9,061 ,917 substituting tetrahedranone for the tetrahedranoidal compound and diborane for cubane.
• heterodiamond seed nor does the produced bora-diamond unit cell and/or diamond mass contain any boron nitride.
• Figure 6 shows an apparatus configured to produce homodiamond unit cells and heterodiamond unit cells.
• the term "line” can mean one line or a plurality of lines.
• Reaction chambers 102, 104, and 106 are for producing bora-diamond, homodiamond, and aza-diamond, respectively.
• reaction chambers 102 and 106 are for producing
• heterodiamond unit cells and reaction chamber 104 is for producing
• Tetrahedranoidal reactant conduits 210, 212, and 214 define tetrahedranoidal reactant input ports into reaction chambers 102, 104, and 106, respectively.
• Reaction chambers 102, 104, and 106 receive boron, carbon, and nitrogen through conduit nozzles 200, 204, and 208, respectively, which define atomic reactant input ports.
• Inert gas source 126 provides, for example, argon as a carrier gas to the reaction chambers 102, 104, and 106 through carrier gas conduits 194, 202, and 196, respectively.
• inert gas such as nitrogen
• the inert gas is also provided to boron source container 120, carbon source container 122 and nitrogen source container 124. Details (e.g., conduits and flow control, etc.) for providing the inert gas to the source containers are not shown in Figure 6.
• Diborane is subjected to a high energy discharge (e.g., microwave discharge) within the boron source container 120 to produce excited state boron atoms.
• a microwave discharge is provided by microwave source 134, within boron source container 120.
• Microwave source 134 is controlled by control line 174, which connects through to the systems controller 390 via the main system bus 392 and controller bus 391.
• the excited state boron atoms exit the boron source container 120 through boron flow control valve 140.
• Boron flow control valve 140 is controlled by system controller 390 via valve control line 142, which connects to system controller 390 through main system bus 392 and controller bus 391.
• Additional inert gas flows from inert gas source 126 through carrier gas conduit 194 controlled by carrier gas valve 152 and converges and mixes with the excited state boron atom stream controllably flowing through boron flow control valve 140.
• Inert gas valve 152 is controlled by control line 154, which connects to system controller 390 through main system bus 392 and controller bus 391.
• the excited state boron atom and argon mixture flow through conduit nozzle 200, which serves as an input port into reaction chamber 102.
• Tetrahedranoidal molecule source container 108 provides tetrahedranoidal molecules to reaction chamber 102 through tetrahedranoidal reactant conduit 210, which flow is controlled by valve 168.
• Valve 168 is controlled by control line 170, which is connected to system controller 390 through main system bus 392 and controller bus 391.
• control line 170 is connected to system controller 390 through main system bus 392 and controller bus 391.
• tetrahedranone 2,3,4-methynyl-cyclobutanone
• the bora-diamond unit cell reaction of Figure 4(B) occurs in reaction chamber 102.
• excited state boron atom cloud 201 is shown mixing and reacting with tetrahedranone vapor 211.
• the resulting bora-diamond unit cells are conducted out of reaction chamber 102 through bora-diamond output conduit 216.
• the output flow of the bora-diamond unit cells through bora- diamond output conduit 216 is controlled by bora-diamond output valve 186, which is regulated by the systems controller 390 via control line 176, which connects to the systems controller 390 through main system bus 392 and controller bus 391.
• Bora-diamond unit cells are provided through bora-diamond output conduit 216 to manifold 112.
• the apparatus of Figure 6 is also configured to produce homodiamond unit cells. This is achieved with the reaction shown in Figure 1 (B). Cubane is subjected to a high energy discharge (e.g., microwave discharge) within the carbon source container 122 to produce excited state carbon atoms. This reaction is disclosed in US 9,061 ,917, which is incorporated fully herein by reference. As shown, a microwave discharge is provided by microwave source 132, within carbon source container 122. Microwave source 132 is controlled by control line 172, which connects through to the systems controller 390 via the main system bus 392 and controller bus 391.
• a microwave discharge is provided by microwave source 132, within carbon source container 122.
• Microwave source 132 is controlled by control line 172, which connects through to the systems controller 390 via the main system bus 392 and controller bus 391.
• Carbon flow control valve 144 is controlled by system controller 390 via valve control line 146, which connects to system controller 390 through main system bus 392 and controller bus 391.
• Additional inert gas (as shown, argon) flows from inert gas source 126 through carrier gas conduit 202, controlled by carrier gas valve 184 and converges and mixes with the excited state carbon atom stream controllably flowing through carbon flow control valve 144.
• Carrier gas valve 184 is controlled by control line 179, which connects to system controller 390 through main system bus 392 and controller bus 391.
• the excited state carbon atom and argon mixture flow through conduit nozzle 204, which serves as an input port into reaction chamber 104.
• Tetrahedranoidal molecule source container 110 Tetrahedranoidal molecule source container 110
• reaction chamber 104 provides tetrahedranoidal molecules to reaction chamber 104 through
• valve 160 tetrahedranoidal reactant conduit 212, which flow is controlled by valve 160.
• Valve 160 is controlled by control line 162, which is connected to system controller 390 through main system bus 392 and controller bus 391.
• the preferred tetrahedranoidal molecule is benzvalene.
• homodiamond unit cells are conducted out of reaction chamber 104 through homodiamond output conduit 218.
• the output flow of the homodiamond unit cells through homodiamond output conduit 218 is controlled by homodiamond output valve 188, which is regulated by the systems controller 390 via control line 178, which connects to the systems controller 390 through main system bus 392 and controller bus 391.
• Homodiamond unit cells are provided through
• the apparatus of Figure 6 is also configured to produce aza-diamond unit cells. This is achieved with the reaction shown in Figure 3(B).
• a nitrogen source is subjected to a high energy discharge (e.g., electrostatic discharge) to produce excited state nitrogen atoms.
• the Figure 2 reactions 1 , 2, or 3, which produce atomic nitrogen from molecular nitrogen, ammonia, and hydrazine, respectively, can be used to yield the excited state nitrogen atoms for synthesizing aza- diamond.
• hydrazine is used as a nitrogen atom source. Hydrazine exits nitrogen source container 124 through nitrogen flow control valve 148. Nitrogen flow control valve 148 is controlled by system controller 390 via valve control line 150, which connects to system controller 390 through main system bus 392 and controller bus 391. Additional inert carrier gas (as shown, argon) flows from inert carrier gas source 126 through carrier gas conduit 196 controlled by carrier gas valve 156 and converges and mixes with the excited hydrazine stream controllably flowing through nitrogen flow control valve 148. Inert gas valve 156 is controlled by control line 158, which connects to system controller 390 through main system bus 392 and controller bus 391.
• inert carrier gas as shown, argon
• the hydrazine mixed with the argon carrier gas mixture passes between electrostatic discharge electrode pair 182, which are powered by high voltage source 130 through power lines 181 , of which there are two (i.e., on line per electrode).
• High voltage source 130 is controlled by systems controller 390 through control line 131 , which connects through to systems controller 390 via main system bus 392 and controller bus 391.
• the electrodes of the discharge electrode pair 182 are located within conduit nozzle 208 and, when energized by voltage source 130, produce an electrostatic discharge between them. This electrostatic discharge causes hydrazine within conduit nozzle 208 to dissociate according to reaction 3 of Figure 2, thereby producing excited state nitrogen atoms, which flow into reaction chamber 106.
• Tetrahedranoidal molecule source container 110 provides tetrahedranoidal molecules to reaction chamber 106 through tetrahedranoidal reactant conduit 214, which flow is controlled by valve 164.
• Valve 164 is controlled by control line 166, which is connected to system controller 390 through main system bus 392 and controller bus 391.
• the preferred tetrahedranoidal molecule is benzvalene.
• the aza-diamond unit cell reaction of Figure 3(B) occurs in reaction chamber 106.
• excited state nitrogen atom cloud 209 is shown mixing and reacting with benzvalene vapor 215.
• the resulting aza- diamond unit cells are conducted out of reaction chamber 106 through aza- diamond output conduit 220.
• the output flow of the aza-diamond unit cells through aza-diamond output conduit 220 is controlled by aza-diamond output valve 190, which is regulated by the systems controller 390 via control line 180, which connects to the systems controller 390 through main system bus 392 and controller bus 391.
• Aza-diamond unit cells are provided through aza-diamond output conduit 220 to manifold 112.
• Manifold 112 can receive bora-diamond unit cells, homodiamond unit cells, and aza-diamond unit cells, singularly, or in any predetermined combinations of controlled proportions. During operation, concentrations of any of these three products can be kept constant or controllably varied in a predetermined sequence, according a program stored in the systems controller.
• the output of manifold 112 is through manifold output conduit 114, which control there through is regulated by manifold output valve 192.
• Manifold output valve 192 is controlled by the systems controller 390 via control line 198, which connects to the systems controller 390 through main system bus 392 and controller bus 391.
• Flow of unit cells out of manifold 112 can be stopped immediately by diverting the gaseous stream away from manifold output conduit 114 with a diversionary stream of inert gas (e.g., argon) that enters manifold output conduit 114 through diversion input port 116 and exits through diversion output port 118.
• inert gas e.g., argon
• Figure 7 provides greater detail of a portion of the apparatus of Figure 6.
• Atomic reactant source container 410 provides boron, carbon or nitrogen as highly excited atoms 530 to reaction chamber 404 through atomic reactant flow control valve 430 into conduit nozzle 406 where it converges and mixes with an inert carrier gas such as argon, which is introduced into conduit nozzle 406 through carrier gas conduit 402.
• Reaction chamber 404 can be flushed of all reactants and reaction byproducts by closing atomic reactant flow control valve 430 and allowing inert carrier gas to flow into reaction chamber
• Inlet port 516 provides for an inflow of inert carrier gas (e.g., argon), which is provided to reaction chamber 404 under controlled flow and pressure by inlet pump 518.
• inert carrier gas e.g., argon
• Inlet pump 518 is controlled by the systems controller 390 via control lines 520, which connects to the systems controller 390 through main system bus 392 and controller bus 391.
• Effluent leaves reaction chamber 404 through effluent port 504.
• effluent pump 506 controls flow of effluent from reaction chamber 404. There may be circumstances when effluent pump 506 is not used, and, thus, effluent exits reaction chamber 404 through effluent port 506 passively (e.g., due to the pressure from inlet pump 518) but through a
• Effluent pump 506 connects through to GC-MS 508 (gas chromatograph in tandem with a mass spectrometer), for effluent analysis. Effluent pump 506 may be separate from, or integrally a part, of GC-MS 508. When separate from mass GC-MS 508, effluent pump 506 is controlled by the system controller 390 through effluent pump control lines 512. When integrally a part of GC-MS 508, effluent pump 506 may be directly or indirectly controlled through GC-MS bus 510, which connects communicatively through to system controller 390 through main system bus 392 and controller bus 391.
• Conduit nozzle 406 functions as an input port into reaction chamber 404 for highly excited boron, carbon, or nitrogen atoms within an inert carrier gas flow.
• Atomic reactant flow control valve 430 is controlled by systems controller 390 via control line 498, which connects to systems controller 390 through controller bus 391 and main system bus 392.
• Tetrahedranoidal molecule source container 408 provides tetrahedranoidal molecules 532 in vapor phase to reaction chamber 404 through tetrahedranoidal reactant conduit 420 the flow of which is regulated by valve 422.
• Valve 422 is controlled by systems controller 390 via control line 492, which connects to systems controller 390 through controller bus 391 and main system bus 392.
• Product 428 of the reaction in reaction chamber 404 i.e., bora-diamond, homodiamond, or aza-diamond unit cells, exits through output conduit 424, which flow is regulated by output valve 426.
• Output valve 426 is controlled by systems controller 390 via control line 490, which connects communicatively to systems controller 390 through controller bus 391 and main system bus 392.
• Reaction chamber 404 provides a controlled environment specifically intended to maintain the physical and chemical conditions conducive to the production of homodiamond and heterodiamond unit ceils invention and to eliminate impurities formed by autogenous processes. Furthermore, physical and chemical conditions within tetrahedranoidal molecule source container 408 and atomic reactant source container 410 are also maintained so as to be conducive to the unit cell reactions of the present invention. The physical and chemical conditions within reaction chamber 404 are
• Sensor/actuator suite 444 communicatively connects through to systems controller 390 via sensor/actuator bus 494, main system bus 392, and controller bus 391.
• sensor/actuator suite 412 The physical and chemical conditions within tetrahedranoidal molecule source container 408 are maintained by sensor/actuator suite 412, which is controlled by systems controller 390. Sensor/actuator suite 412 communicatively connects through to systems controller 390 via sensor/actuator bus 500, main system bus extension 392a, main system bus 392, and controller bus 391.
• sensor/actuator suite 414 The physical and chemical conditions within atomic reactant source container 410 are maintained by sensor/actuator suite 414, which is controlled by systems controller 390. Sensor/actuator suite 414 communicatively connects through to systems controller 390 via sensor/actuator bus 502, main system bus extension 392a, main system bus 392, and controller bus 391.
• tetrahedranoidal reactant conduits 210, 212, and 214 of Figure 6 and tetrahedranoidal reactant conduit 420 of Figure 7 must be modified to include a heated catalytic frit so that acetylene can be converted to what we believe to be tetrahedrane.
• acetylene is sourced to the heated catalytic frit from tetrahedranoidal molecule source containers 108 and 110 of Figure 6 and tetrahedranoidal molecule source container 408 of Figure 7.
• the acetylene is provided within an inert carrier gas such as argon.
• Reaction chambers 104 and 106 of Figure 8 are shown sharing the same tetrahedranoidal molecule source container 110. If it is desired to use a different tetrahedranoidal molecule in reaction chamber 104 from that of reaction chamber 106, each chamber can be provided with its own tetrahedranoidal molecule source container and tetrahedranoidal reactant conduit.
• manifold 112 can be adapted to perform mixing to provide a uniform mixture of the unit cells.
• Figure 8 shows an exemplary use of the homodiamond unit cell and heterod amond unit ceil products of the apparatus of Figures 6 and 7.
• Deposition chamber 610 provides a controlled environment specifically intended to maintain the physical and chemical conditions conducive to the production of molecular diamond (i.e., the homodiamond unit cell and the heterodiamond unit cell) to yield useful, shapeabie diamond masses that can be components of products or products themselves.
• work piece holder 640 supports deposition substrate 604. Although only one work piece holder 640, is shown, a plurality of work piece holders with associated deposition substrates in a single depostion chamber 610 can be accommodated by the present invention.
• Work piece holder 640 includes a means for locally controlling the temperature and charge of the deposition substrate 604, the details for which are not shown.
• Temperature control lines 642 communicate data to and from the system controller 390 through sensor/actuator suite and interface 644, through sensor bus 645, main system bus 392, and controller bus 391.
• Sensor/actuator suite and interface 644, contains one or more temperature sensors and one or more pressure sensors. It can accommodate additional sensors.
• sensor/actuator suite and interface 644 is shown as a single, integrated module at one location in
• deposition chamber 610 alternatively, the sensors can be placed at disparate locations within deposition chamber 610.
• Sensor/actuator suite and interface 644 communicates data to and from the system controller 390 through
• Inlet port 684 provides for an inflow of inert carrier gas 652.
• Deposition chamber 610 may be pressurized by inlet pump 686 under the control of inlet pump control lines 688.
• Inlet pump 686 may be provided with dedicated flow sensor or sensors (preferably non-contact sensors) and/or pressure sensors that are not shown.
• Inlet pump control lines 688 communicate with system controller 390 through main system bus 392 and controller bus 391. It is also possible to maintain desired flow and pressure in deposition chamber 610 using the pressure of the inert carrier gas 652 storage tank and its regulator alone, making the inlet pump 686 unnecessary.
• Effluent leaves deposition chamber 610 through effluent port 660.
• effluent pump 662 controls flow of effluent from deposition chamber 610.
• effluent pump 662 connects through to GC-MS 666 (gas chromatograph in tandem with a mass spectrometer) for effluent analysis.
• Effluent pump 662 may be separate from or integrally a part of GC-MS 666.
• effluent pump 662 When separate from mass GC-MS 666, effluent pump 662 is controlled by the system controller 390 through effluent pump control lines 664. When integrally a part of GC-MS 666, effluent pump 662 may be directly or indirectly controlled through GC-MS bus 667, which connects communicatively through to system controller 390 through main system bus 392 and controller bus 391.
• Unit eel! inlet 614 provides homodiamond unit cells and/or heterodiamond unit cells, or any combination thereof, to deposition chamber 610. As shown, unit ceil inlet 614 is an extension of manifold output conduit 114 of Figure 6 or output conduit 424, of Figure 7.
• unit cells passing through unit cell inlet 614 are provided to delivery apparatus 612 through which they pass and are control!abiy directed at a predetermined location on deposition substrate 604.
• Unit cell stream 616 deposits unit cell mass 608 on deposition substrate 604.
• Unit cell stream 616 can comprise homodiamond unit ceils, heterodiamond unit cells, or a mixture thereof.
• Unit ceil mass 608 can be a localized mass (as shown) or a diffuse, uniform mass such as a thin film on deposition substrate 604.
• the relative position of delivery apparatus 612 is controlled by three dimensional position controller 694 (details not shown). Three dimensional position controller 694 is, in turn, controlled through position control lines 696, which communicate through to the systems controller 390 through main system bus 392 and controller bus 391.
• a single deposition chamber 610 can also accommodate multiple reactant delivery apparatuses. Delivery apparatus 612 can be
• FIG. 5 uses hydrazine as the source for highly excited nitrogen atoms.
• Figure 9 is a schematic that shows the formation of aza-diamond using this solid state reaction.
• a solution of benzvalene 700 and a solution of hydrazine 702 are combined to form a homogeneous solution 704 of benzvalene and hydrazine in a proportion of benzvalene to hydrazine of 2:1 .
• the solutions can be made in an organic solvent such as diethyl ether.
• the homogeneous solution 706 undergoes evaporation to form a homogeneous solid mixture 708 of benzvalene and hydrazine in a proportion of 2:1 respectively.
• Homogeneous solid mixture 708 is subjected to a high energy discharge (e.g., microwave) to yield aza-diamond mass 710.
• aza-diamond mass 712 retains the shape defined by the container.
• This reaction can be adapted for use with apparatus similar to that shown in Figures 8 and 10 of US 2015/0259790, which is fully incorporated herein by reference.
• this can be achieved by substituting a homogeneous solution of hydrazine and benzvalene for the homogeneous solution of cubane and benzvalene, which is disclosed in US 2015/0259790.
• sensors, actuators and control parameters of the systems controller are adjusted to be conducive to the reaction.
• the disclosed apparatus for producing bora-diamond, aza-diamond, and homodiamond unit cells is versatile.
• unit cells exiting from manifold output conduit 114 of Figure 6 or output valve 426 of Figure 7 can be used to build up thin films or layers of bora-diamond, aza-diamond, and homodiamond masses or masses comprising any combination mixed heterodiamond and/or homodiamond unit cells on a deposition substrate such as deposition substrate 604 of Figure 8.
• a deposition substrate such as deposition substrate 604 of Figure 8.
• Another exemplary use of bora-diamond, aza-diamond, and homodiamond unit cells, or various combinations thereof of the present invention, is as a dopant for other materials such as silicon, compound semiconductors, etc.
• the heterodiamond or homodiamond unit cell that is the dopant species, not the heteroatom per se.
• the bora-diamond unit cell and/or the aza-diamond unit cell can be the dopant species.
• the choice of substrate is not critical, and it is not necessary to heat the substrate as the energy of the substrate does not participate in the heterodiamond unit cell reaction.
• the heterodiamond unit cells so produced are charge monopoles (unipolar) having no associated species bearing charges of opposite sign (counter charges). For this reason, it can be beneficial to impress a charge of opposite sign onto the deposition substrate to minimize the potential for like charge repulsion phenomenon.
• Visser et al. disclose a method of manufacturing a semiconductor device in which photoresist on a silicon oxide layer on a semiconductor substrate is stripped using an oxygen plasma afterglow and a biased substrate.
• Nishioka et al. disclose a manufacturing method for silicon thin film solar batteries wherein a substrate can be biased negatively or positively.
• the control system of the apparatus comprises a computer system in
• Control system software for the computer is designed with a modular structure, although other schemes are also possible.
• Process control can employ previously determined, preferred parameters that are stored in memory maps for use with process control strategies such as closed-loop, fuzzy logic, etc., which are commercially available.
• the general structure applies to both vapor phase and solid state embodiments of the present invention.
• control system Generally, data are received from sensors in the apparatus and processed by the control system. When data indicate that a specific parameter's value has diverged from the desired set point, control signals are generated by the computer and routed through the control system interface to actuators in the apparatus. These signals correct for the difference between the actual measured parameter value and the target or desired value for that parameter.
• the internal temperature and pressure of a reaction chamber or deposition chamber can be set to preferred values by adjusting the inert carrier gas temperature and/or flow rate based on the data received from temperature and pressure sensors.
• the inert gas can be, for example, argon gas with less than three parts per million O 2 , which is commercially available.
• the gas entering a reaction chamber first passes through a refrigeration device that includes a pump and one or more heat exchangers.
• the temperature of the inert gas is controlled by varying the heat exchanger's refrigerant temperature, which is managed by the system controller.
• the reaction chamber temperature is measured by one or more temperature sensors and the temperature data are provided to the system controller.
• One temperature sensor can be placed on a wall of the reaction chamber.
• Another one or two can be placed on or near the gas input port or ports of the reaction chamber.
• temperature can also be measured with a temperature sensor disposed on or near the reactant nozzle or dispenser.
• the work piece holder that holds the deposition substrate can be placed in intimate contact with a dedicated heat exchanger for heating and cooling the deposition substrate as required by the chosen process.
• a dedicated heat exchanger can have its own thermal fluid that is separate from that of the inert gas heat exchanger.
• Such apparatuses and their associated control systems are commercially available.
• the associated control system of the substrate heat exchanger is under the command and control of the general system controller.
• the pressure in a reaction chamber and deposition chamber can be controlled over a very wide range of values from fractions of an atmosphere up to many atmospheres. This is achieved by a combination of options that include using the high pressure of the inert gas in its storage cylinder or tank (passive pressure control) and/or an additional pressure pump in combination with a vacuum pump at the effluent port of the reaction chamber (active pressure control).
• passive pressure control the high pressure of the inert gas in its storage cylinder or tank
• active pressure control active pressure control
• pressurized gas from a high pressure tank is provided to the reaction chamber or deposition chamber, it flows through a gas pressure regulator, which provides a "step-down" in pressure as a first order of pressure control. Additional control is achieved through the use of a pressure sensor or sensors that are disposed within the reaction chamber.
• one pressure sensor can be placed on the reaction chamber wall but local to the general deposition area. In the placement of sensors, care is taken to avoid gas currents. If the reaction is performed at sub-atmospheric temperatures, a vacuum pump is used to maintain the lower pressure at the same time that inert gas continues to flow into the reaction chamber. If the reaction is performed above atmospheric pressures, passive pressure control (e.g., regulated tank pressure) and/or in combination of passive and active pressure control can be used. A valve can be used at the effluent port to control egress of the effluent gas.
• a vacuum pump is used to maintain the lower pressure at the same time that inert gas continues to flow into the reaction chamber.
• passive pressure control e.g., regulated tank pressure
• a valve can be used at the effluent port to control egress of the effluent gas.
• a controllable manifold can be used to provide kinetic energy to the gases to drive the heterodiamond and homodiamond forming reactions.
• the control system is able to set the preferred conditions for heterodiamond and homodiamond unit cell formation.
• flow control may be achieved with a non-contact flow sensor or sensors (e.g., ultrasonic flow sensor) in the inert gas input port or ports of reaction chamber. These sensors can be embedded in the walls of the conduits or nozzles.
• the feedback control loop for controlling flow is regulated by the system controller through a reactant gas pump and/or a throttling valve.
• precise amounts of homogeneous reactant solution can be delivered or dispensed by the use of well- calibrated metering pumps.
• Effluent ports are generally attached to the input port of a GC-MS spectrometer, which often has its own controllable pump system.
• the GC-MS spectrometer can monitor effluent either continually or periodically and provide effluent content data to the system controller. Process control may be based upon compositional data, physical parameter data, relative positional data, morphological data of the molecular diamond mass, etc.
• Mass spectrometer software is available both commercially and as open source programs that can be easily used in
• dispensers e.g., automated pipetting systems
• printing devices e.g., printing devices and other actuators and control systems therefor are well-developed
• FIGS. 6-8 of US 2015/0259790 A wide range of products for accomplishing the manufacturing processes shown in FIGS. 6-8 of US 2015/0259790, which is fully incorporated herein by reference, are available commercially and can be adapted to work in combination, and interface, with the control system of the present invention.
• the reactant delivery apparatuses of FIGS. 6-8 of US 2015/0259790 can be achieved using three-dimensional positioning devices (e.g., a 3 D printer gantry, etc.) and their associated control software.
• the control system software for the present invention not only maintains preferred reaction conditions but also controls the proper sequence of events.
• the switchable high-energy discharge apparatus can be actuated on and off depending on the effluent data provided by the mass spectrometer.
• the control system software can be written in a variety of programming languages, but it is particularly useful to use languages that provide bit-level addressing and manipulation, such as C or C++, because these allow for easy interfacing with input and output ports (e.g., reading from or writing to A/D and D/A converters directly, respectively). Otherwise, interface routines can be coded in assembly language and control processing can be done in a higher level language.
• instrument control software development systems are available commercially (e.g., LabVIEW or LabWindows/CVI from National Instruments) that can be adapted to develop the control system software for the present invention.

Landscapes

• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Life Sciences & Earth Sciences (AREA)
• Geology (AREA)
• Materials Engineering (AREA)
• Metallurgy (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Life Sciences & Earth Sciences (AREA)
• Crystallography & Structural Chemistry (AREA)
• General Chemical & Material Sciences (AREA)
• Physics & Mathematics (AREA)
• Electromagnetism (AREA)
• Health & Medical Sciences (AREA)
• General Health & Medical Sciences (AREA)
• Toxicology (AREA)
• Crystals, And After-Treatments Of Crystals (AREA)
• Carbon And Carbon Compounds (AREA)

Applications Claiming Priority (2)

Publications (2)

Family

ID=58662684

Family Applications (1)

Country Status (3)

Families Citing this family (1)

Family Cites Families (5)

• 2016
  • 2016-11-03 WO PCT/US2016/060249 patent/WO2017079388A1/en not_active Ceased
  • 2016-11-03 CA CA3003281A patent/CA3003281A1/en not_active Abandoned
  • 2016-11-03 EP EP16862934.3A patent/EP3370860A4/de not_active Withdrawn

Also Published As

Similar Documents

Legal Events