EP1842227A2 - Dispositifs medicaux en diamant - Google Patents

Dispositifs medicaux en diamant

Info

Publication number
EP1842227A2
EP1842227A2 EP06717944A EP06717944A EP1842227A2 EP 1842227 A2 EP1842227 A2 EP 1842227A2 EP 06717944 A EP06717944 A EP 06717944A EP 06717944 A EP06717944 A EP 06717944A EP 1842227 A2 EP1842227 A2 EP 1842227A2
Authority
EP
European Patent Office
Prior art keywords
diamond
cvd
void
ion implantation
species
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP06717944A
Other languages
German (de)
English (en)
Inventor
Inc. Apollo Diamond
Robert C. Linares
Patrick J. Doering
Bryant Linares
Alfred R. Genis
William W. Dromeshauser
Michael Murray
John M. Abrahams
Alicia E. Novak
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Apollo Diamond Inc
Original Assignee
Apollo Diamond Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US11/056,338 external-priority patent/US20050181210A1/en
Priority claimed from US11/178,623 external-priority patent/US7122837B2/en
Application filed by Apollo Diamond Inc filed Critical Apollo Diamond Inc
Publication of EP1842227A2 publication Critical patent/EP1842227A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/20—Doping by irradiation with electromagnetic waves or by particle radiation
    • C30B31/22—Doping by irradiation with electromagnetic waves or by particle radiation by ion-implantation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
    • B81C1/00047—Cavities
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/0405—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising semiconducting carbon, e.g. diamond, diamond-like carbon
    • H01L21/041—Making n- or p-doped regions
    • H01L21/0415—Making n- or p-doped regions using ion implantation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/0405—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising semiconducting carbon, e.g. diamond, diamond-like carbon
    • H01L21/042—Changing their shape, e.g. forming recesses

Definitions

  • Diamond appears to be highly biocompatible with living tissue.
  • Diamond does not appear to exhibit carcinogenetic or toxicity for in situ applications, and it appears to be biologically inert in bulk form. Diamond may be synthesized in a variety of ways. However, it is a difficult material to work with, and new techniques may be required for forming structures for handling biological materials.
  • Modern semiconductors are typically based on silicon, with various elements doped to change their electrical properties. For example, doping silicon with phosphorous creates a surplus of electrons resulting in n-type semiconductor material due to the fifth valence electron not present in silicon, which has only four valence electrons. Similarly, doping silicon with boron creates p-type silicon having a surplus of "holes", or an absence of electrons, because boron has only three valence electrons which is one fewer than silicon. [0004] When n-type and p-type silicon are in contact with one another, electricity flows in one direction across the junction more easily than in the other direction. More complex configurations of n-type and p-type material can be assembled to form various types of transistors, integrated circuits, and other such devices.
  • Masked and controlled ion implants are used in CVD formed single crystal diamond to create structures for both optical applications, nanoelectromechanical device formation, and medical device formation.
  • Ion implantation is employed to deliver one or more atomic species into and beneath the diamond growth surface in order to form an implanted layer with a peak concentration of atoms at a predetermined depth beneath the diamond growth surface.
  • the composition is heated in a non- oxidizing environment under suitable conditions to cause separation of the diamond proximate the implanted layer.
  • Further ion implants may be used in released structures to straighten or curve them as desired. Boron doping may also be utilized to create conductive diamond structures.
  • a nanochannel is formed by implanting ions in a diamond at a point where the nanochannel is desired.
  • Masks may be used to control a width and length of the implant, and selected implant power levels can be utilized to control the depth of the implant. Heating the diamond causes a separation to occur at or about the implant. Such separation may be used as a nanochannel for conveying fluids, or as a low refractive index portion of a waveguide.
  • Further implants may be sized and shaped to form an etalon, optical filter, or optical deflector when heated to cause separation.
  • An approximately 500nm circular shape is used in one embodiment.
  • Using a progression of masks and implant depths can provide for formation of many different mechanical structures, such as those that may be formed in silicon. Further layers of synthetic diamond of one or more diamond layers may be grown following the implants.
  • device formed of materials other than diamond such as silicon or germanium based devices are coated with CVD diamond, providing a highly biocompatible device protected from oxidation.
  • FIG. 1 is a block representation of a diamond having a Nv- center according to an example embodiment.
  • FIG. 2 is a side view cross sectional representation of a diamond illustrating a masked ion implant process according to an example embodiment.
  • FIG. 3 is a top view of the diamond of FIG. 2, illustrating the mask for ion implantation according to an example embodiment.
  • FIG. 4 is a side view cross sectional representation of the diamond of FIG. 2 following the ion implant and heating according to an example embodiment.
  • FIG. 5 is a side view cross sectional representation of a diamond illustrating a masked ion implant process for forming a cantilever according to an example embodiment.
  • FIG. 6 is a top view representation of an ion implantation mask used to form a cantilever according to an example embodiment.
  • FIG. 7 is a side view cross sectional representation of a released cantilever according to an example embodiment.
  • FIG. 8 is a side view cross sectional representation of a masked diamond for forming optical structures according to an example embodiment.
  • FIG. 9 is a top cross sectional view of the diamond of FIG. 8 illustrating optical structures formed according to an example embodiment.
  • FIG. 10 is a top view representation of a drug pump according to an example embodiment.
  • FIG. 11 is a side cross section view of a multilevel capillary system according to an example embodiment.
  • FIG. 12 is a block cross section view of a CVD diamond coated optical device according to an example embodiment.
  • FIG. 13 is a top view of a porous CVD diamond membrane according to an example embodiment.
  • FIG. 14 is a block diagram representation of a structure coated with CVD diamond.
  • FIG. 17 shows a boron-doped diamond seed crystal with grown diamond separated at a hydrogen implant level, consistent with an example embodiment of the present invention.
  • FIG. 20 shows an integrated circuit having first and second boron-doped diamond semiconductor regions, consistent with an example embodiment of the present invention.
  • a first section of the application describes the ability to create
  • Nv- centers in single crystal diamond in a controlled manner.
  • Various ion implant processes are described that allow the creation of structures in single crystal diamond. These processes may then be used to create structures in other contexts, as described in a medical devices section. Further description is provided with respect to doping of single crystal diamond to obtain various semiconductor and conducting properties, which may be used in conjunction with nano and micromechanical devices formed in the diamond.
  • N-V centers in diamond can be created in a controlled manner.
  • a single crystal diamond is formed using a CVD process with nitrogen included in the growth process, and then annealed to remove N-V centers.
  • a thin layer of single crystal diamond is then formed with a controlled number of N-V centers. The N-V centers form Qubits for use in electronic circuits.
  • Qubit devices are formed in diamond having highly controlled purity.
  • a highly controlled number of N-V centers can be produced, and the N- V centers are isolated from each other and from other elements having a magnetic spin such as N-VO, Ns and 13C ( carbon 13).
  • single, isolated N-V centers are used to obtain information from individual atoms rather than from clusters.
  • the diamond has high crystal perfection since imperfections lead to shorter spin lifetimes and nitrogen tends to segregate at imperfections such as dislocations giving the effect of a higher concentration and the attendant interaction between adjacent spins and reduction of lifetime.
  • light is able to enter and leave the diamond host material in a controlled manner.
  • a Qubit emits light
  • the light will be emitted over a spherical surface and the light intensity at any point will be very low and difficult to detect.
  • the Qubit is contained within an optical waveguide which traps and directs the light in a minimum number of directions.
  • Diamond is ideal for such a waveguide since it has a very high index of retraction (2.4 in the visible range).
  • a thin layer of diamond in contact with air or vacuum on both sides provides such a waveguide.
  • Diamond has a significantly higher index of refraction than air, such that a light beam propagating down the waveguide is internally reflected by the walls of the diamond waveguide and be confined to the diamond waveguide.
  • Qubit With the Qubit within the diamond waveguide, most of the light emitted by the Qubit will be transmitted down the waveguide and be readily collected and detected. Other forms of transmission may also be utilized, such as by means of a plasma waveguide or slot waveguide. In still further embodiments, small metal wires are utilized to draw light from a Qubit. The light propagates on the outside of the wire within a diamond cladding.
  • One method for building a Qubit device involves growing single crystals by the HPHT method, incorporating a desired amount of nitrogen atoms which will all be Ns, irradiating the diamond to generate carbon vacancies and annealing to diffuse the carbon vacancies to the nitrogen atoms thereby causing N-V centers. This method may result in irradiation causing a significant level of crystal damage which decreases Qubit lifetime.
  • Another method of producing N-V centers in HPHT diamond involves growing the diamond with a titanium or aluminum getter to remove all of the nitrogen from the diamond and put nitrogen into the diamond later by ion implantation into selected spots. This method may not lend itself well to production of large size diamond wafers which would be suitable for device production.
  • FIG. 1 is a block representation of a diamond crystal lattice 100 having an N-V " center 110 according to an example embodiment.
  • Center 110 is also representative of N-V centers with different charge states.
  • an N-V " center 110 is nitrogen 115 in a substitutional site in diamond which is adjacent to a carbon vacancy 120.
  • the N-V " center 110 is isolated from other N-V centers such that spins of other centers and other structures do not interfere with the isolated N-V " center, thus forming a Qubit.
  • the N-V- center 110 in diamond has several attributes which make it desirable for Qubit based devices. It is easily pumped using low power microwaves. It is also easily detected (emission at 675 nanometers wavelength). Such N-V " centers in diamond have long lifetimes (60 to 500 microseconds) and room temperature operation. Diamond also has a high degree of optical transparency and a high optical index of refraction, enabling construction of optical waveguides and other optical structures.
  • N-V centers One method of producting N-V centers involves the use of CVD grown diamond.
  • CVD diamond can be grown in large sizes with highly controlled purity as seen in (see US Patent No. 6,582,513) and with layers of controlled purity, thickness and properties.
  • CVD diamond may be grown with high or low nitrogen concentrations, thin layers with or without 13C.
  • N-V center formation may be controlled by several means.
  • CVD diamond grows under conditions where N-V " , N-V 0 and Ns are all stable. Furthermore the ratios of these states can be varied by the growth conditions, the concentration and by heat treatment after growth. Moreover, it is possible to grow a substrate which is essentially free of all states of nitrogen and then grow a film of diamond which has only the desired level of nitrogen. Since the number of atoms of nitrogen in the film will be a function of concentration and thickness, N-V " centers may be isolated from all other centers. In other words, given a known concentration of N-V centers that will be formed in a given volume of CVD grown diamond, making the diamond layer very thin assures that very few N-V centers are formed, and are thus isolated from each other.
  • each layer can be designed as a waveguide as described below, and have multiple and separated functions.
  • N-V centers may be randomly placed in the volume of the crystal, but can be readily found and marked for detection during the operation of the device.
  • different types of diamond may be used, such as natural, mined diamonds, high pressure, high temperature manufactured diamonds, CVD formed diamonds or others. Such diamond may then be annealed to destroy N-V centers, followed by implantation to create desired densities of N-V centers, and further implantation to form waveguides.
  • An alternate method utilizes very pure bulk crystal with or without the film of desired isotopic purity, heat treat to destroy all residual N-V centers and then implant single, isolated, N-V centers at desired locations. A capping layer of highly pure diamond may then be grown on the layer.
  • Waveguides may be formed proximate the N-V centers and optically coupled to them.
  • Hydrogen is implanted in the diamond in stripes, followed by heat treating the structure to create a cavity which separates the strip of diamond from the underlying diamond.
  • the strip of diamond is essentially surrounded by air and is used as an optical waveguide for bringing signals into and out of the diamond structure. It provides a highly isolated optical signal in and out and allows for multiple channels for optical in and out on a single diamond chip. Furthermore multiple functions may be provided, such as amplifiers, storage and computing all on one optical chip. Implant of multiple energies may provide multiple strips with separation layers from each other, in depth, allowing production of three dimensional, optically isolated Qubit structures. Such structures may significantly decrease the size of such devices since much of the volume could be utilized. Slot waveguides may also be formed.
  • the waveguide can be altered in its properties by causing the waveguide to rise or fall in spots or along its length by application of heat or voltage cycling. This is in essence a fully attached device. This can be used as a switch to turn off or on the light or as a switch to move the light to another channel.
  • Qubits, optical switching and MEMS technology are combined into the same chip with its attendant applications.
  • the use of masked or otherwise patterned implantation and lift-off technology permits the building of a range of waveguide structures such as sheets, plates, wires, disks and multiples of these shapes all with the possibility of modulation and switching as in optoelectronic and MEMS devices. It is also possible to build either normally open or normally closed switches and mixers by design of the proximity and shape of such waveguides.
  • Diamond Qubits may also be formed in conjunction with other semiconductors.
  • Diamond may be bonded to other semiconductors such as silicon, gallium arsenide, gallium nitride, silicon carbide or III-IV alloys.
  • the semiconductors can also be grown onto the diamond substrate.
  • optoelectronic devices such as lasers, detectors and associated circuitry to be directly integrated with the diamond QBIT to provide input and output to and from conventional sources, devices and systems. This will provide the basis for optical busses for higher speed interconnects in conventional computers and future QBIT based computers, hi fact a whole new family of integrated Qubit-Semiconductor devices (QSD) will be possible by combining the technologies and methods discussed.
  • QSD Qubit-Semiconductor devices
  • a diamond substrate 210 is covered with a mask 215 in one embodiment.
  • the mask 215 is formed of a material sufficient to screen out ions 220 being implanted at desired energy levels.
  • the mask may take many different shapes, but one such shape is shown in top view FIG. 3 at 310. In this embodiment, the mask is in the shape of a long, thin rectangle, resulting in a long thin implant 225 at a desired depth.
  • FIG. 4 is a side view cross sectional representation of the diamond 210 of FIG. 2 following the ion implant and heating to form an open space 410 within the diamond 210.
  • Open space 410 provides a low refractive index region on one side of a strip of diamond indicated at 420.
  • the other side of the strip 420 is essentially the top of the diamond 210, which may be exposed to air, also having a low refractive index compared to the index of refraction of the diamond strip 420.
  • the diamond strip 420 forms a waveguide.
  • a Qubit 430 is formed within the strip 420, and the strip provides a mechanism to capture and provide light to the Qubit to both detect and effect changes in the Qubit.
  • the strip 420 may be formed in different shapes, in order to conduct the light to a desired light source 440 and a light detector 450 which may each be further connected to processing circuitry, formed either, within, on, or off of the diamond substrate.
  • the source 440 and light detector 450 may also be within, on, or off the diamond substrate in various embodiments.
  • Optical fiber connections or optical couplers may be formed to conduct light to an from the waveguide strip 420.
  • patterned ion implantation is employed to deliver one or more atomic species into and beneath the diamond growth surface in order to form an implanted layer with a peak concentration of atoms at a predetermined depth beneath the diamond growth surface.
  • the composition is heated in a non-oxidizing environment under suitable conditions to cause separation of the synthetic diamond structure.
  • Such a non-oxidizing atmosphere generally includes any atmosphere not containing a sufficient concentration of oxygen so as to be reactive through oxidation.
  • atmospheres include inert (e.g., helium, neon, argon, etc.) and other non-oxygen containing gases (e.g., hydrogen, nitrogen, etc.). Environments used to provide such atmospheres can include plasmas, vacuums, and the like.
  • various initial steps can be performed prior to or concurrent with the ion implantation stage.
  • One such step involves choosing a substrate.
  • such substrate may be a single crystalline diamond.
  • at least one major surface of the substrate can be identified, and optionally prepared, for ion implantation.
  • Preparation of the diamond surface can include any suitable means for affecting the chemical and/or physical make-up of the surface, for instance, by polishing using conventional polishing methods. Preparation of this sort can be accomplished in advance of the ion implantation.
  • ions are implanted in a manner at a set distance and even flux across the diamond growth surface, such that the configuration of the implanted species layer will itself replicate the surface profile of the substrate.
  • any defects on an implanted surface of the substrate will typically have a corresponding influence on the implant profile, including on the configuration of the predetermined peak atomic layer.
  • Such structures may actually be substantially polished if the surface of the diamond is polished. Preparation of the substrate can be important to initially remove such defects.
  • surfaces are thoroughly cleaned for ion implanting, for instance, using solvents or other suitable methods known in the art, including plasma etching, gas phase etching and the like. Polishing damage may result in creation of undesired N-V centers. The surface of the polished diamond may be further etched to remove such damage and N-V centers.
  • the depth of implantation is generally accomplished with adjustments made to the electric field. Typically, as one increases the voltage of the electric field, the energy of the species is increased, which ultimately results in a deeper implantation by the species into the substrate.
  • the substrate may be any of a variety of crystalline shapes.
  • the substrate may be of any predetermined geometry including a cube, cone, prism, pyramid, wedge, or other geometries, as well as frustums of each.
  • the species generally penetrates the upper surface of the substrate until reaching a zone, such as zone 225 within the substrate.
  • a peak concentration of the species is at a certain depth generally known as the end of range depth. While the species is only shown at the one depth (the end of range depth), it should be appreciated that this is done for simplicity.
  • the species is generally distributed throughout the zone at and proximate to the end of range depth.
  • the species to be implanted Before ion implantation is started, the species to be implanted must be selected. Many variables are considered in selecting a species, such as cost and availability, as well as concern for how much damage the species is expected to cause to the substrate lattice, as described below. [0061]
  • the implanted portion of the lattice by directing the species (of ionized atoms) into the crystal lattice of the substrate, the implanted portion of the lattice generally dilates or expands. Excessive dilation of the lattice in this manner generally leads to strain within the implanted layer. Consequently, excessive strain can cause damage to the implanted layer. This damage is generally represented by dislocations, or cracking, within the implanted layer.
  • These dislocations can generally create an unfavorable outer substrate surface for growing quality synthetic diamond (e.g., producing diamond via CVD having no defects or dislocations, or insignificant amounts thereof).
  • quality synthetic diamond e.g., producing diamond via CVD having no defects or dislocations, or insignificant amounts thereof.
  • lattice dilation can be controlled in a number of ways, and in fact, relied upon.
  • hydrogen ions are implanted within a diamond substrate using the conventional techniques of ion implantation. Since the covalent radius of hydrogen is small, only a small amount of lattice dilation occurs within the implanted layer. Consequently, there is little strain (and little damage) within the implanted layer. Generally, as the covalent radius of the implanted species increases, the potential for creating such a favorable surface (e.g., having limited defects or dislocations) decreases. [0063] Generally, any species can be used for ion implanting in the inventive process so long as the species is suitable for subsequently enabling separation of a portion of the implanted layer from the substrate. As such, the species is selected so as to allow for suitable implantation within the substrate.
  • the substrate is also used for growing a synthetic diamond thereon.
  • the species preferably allows for suitable implantation within the substrate to enable separation, and allows for suitable formation of a favorable growth surface on the substrate from which a quality synthetic diamond can be grown. Therefore, the species is selected so as to allow for suitable implantation within the substrate without undesirably damaging the substrate.
  • Small- to medium-sized species (having small- to medium-sized covalent radiuses) are generally preferred. Examples include atomic species such as helium, lithium, boron, carbon, oxygen, phosphorous, and sulfur.
  • embodiments of the process can also involve large-sized species (having large-sized covalent radiuses).
  • the extent of lattice damage to the implanted portion can be limited by the dose quantity of the species implanted, with the dose being defined as the area density of atoms (atoms/cm 2 ) which are implanted into the substrate. For example, if the species is implanted using a high dose, the species will generally cause more damage to the substrate upon implantation than if a species were implanted using a lower dose. As the species (of ionized atoms) travels through the substrate, the damage to the substrate lattice is generally maximized near the end of the species range into the substrate (generally referred to as "end of range damage").
  • the degree of damage at the end of range is a function of the total dose at that level.
  • the ability to cause separation within the diamond crystal is also a function of the total dose.
  • the dose quantity is set in the range from about 1x1 Oe 1 atoms/cm 2 to about 1x1 Oe atoms/cm , and even more preferably, is set in the range from about IxIOe 15 atoms/cm 2 to about IxIOe 18 atoms/cm 2 .
  • any dose quantity within the range is generally suitable.
  • the extent of lattice damage to the diamond growth surface can be controlled by modifying the voltage of the electric field used in ion implantation. As one increases the voltage of the electric field, the energy of the species increases as well, ultimately resulting in a deeper implantation by the species into the substrate. In turn, the energy level can be selected for a specific species so as to implant a peak concentration of the species at about a certain implantation depth within the substrate (the end of range depth). This depth may range anywhere from about 500 angstroms to about 20,000 angstroms. While the end of range depth for the species can be limited by decreasing the species energy, one ought not limit the energy too severely.
  • the energy level is set in the range from about 10 KeV to about 10,000 KeV, and in another embodiment, is set in the range from about 50 KeV to about 500 KeV.
  • the species dose rate may affect the temperature of the substrate during the implant.
  • the dose rate is set in the range from about 0.05 microamps/cm 2 to about 100 niilliamps/cm 2 , and in others, is set in the range from about 0.1 microamps/cm 2 to about 500 microamps/cm 2 .
  • implants at multiple levels, followed by heating are performed to create gaps at different levels of the substrate.
  • One example provides three such gaps by implanting H 2 at energy levels of 150, 155 and 160 KeV. This can provide three levels of structures, such as waveguides, with potential corresponding isolated N-V centers.
  • TRIM Transport of Ions in Matter
  • Table 1 lists the approximate end of range depths for various species at various energy levels, given a diamond seed being used as the substrate. Regardless of whether the diamond seed is HPHT, CVD, or natural diamond, the end of range depths for the species generally remain the same. As illustrated, as the energy level is increased for a species such as hydrogen, its end of range depth is also increased.
  • Heat treatments are provided on the diamond composition in the non-oxidizing atmospheres. Such treatments can be provided by any suitable method, including radiation, conduction, or convection sources, all generally known in the art. Generally, the temperature range of the heat treatments is preferably set in the range from about 1100 0 C to about 1800 0 C and, more preferably, about 1100 0 C to about 1500 0 C. The combination of the appropriate atmosphere and the temperature levels provides an ideal environment to cause spontaneous separation of the synthetic diamond and the implanted layer portion.
  • FIG. 5 is a side view cross sectional representation of a diamond illustrating a masked ion implant process for forming a cantilever according to an example embodiment.
  • a first mask is used to form a generally rectangular area which will end up defining the size of a cavity in which the cantilever will be released to be free to move.
  • shapes other than rectangular may be used.
  • the implantation depth may be varied, such that a sufficient density of ions are implanted in the entire area beneath the cantilever and to the sides of the cantilever to allow sufficient motion once the cantilever is released to move.
  • the mask extends at least slightly beyond the edges and released end of the cantilever.
  • FIG. 6 is a top view representation of an ion implantation mask 600 used to form a cantilever according to an example embodiment.
  • This mask allows implantation to the sides and past the released end of the cantilever, while defining the shape of the cantilever itself with projection 610.
  • the energy levels of implantation used with this mask are designed to implant a sufficient density of ions to the sides and released end of the cantilever.
  • This implant may vary the depth of implant from the surface of the diamond substrate to the cavity defined below the cantilever.
  • heating in a non-oxidizing environment released the cantilever as shown in FIG. 7, which is a side view cross sectional representation of a released cantilever beam 710 according to an example embodiment.
  • releasing may be performed using a carbon implant at the edges and etching by oxidation via heat, electrolysis or oxidizing acid.
  • cantilever beam 710 tends to curve upward when released. Further implants in the upper levels may be provided either prior to or after release of the cantilever beam. Such implants, depending on depth and density, will begin to straighten the cantilever by putting the surface in compression, and if continued, may actually cause the cantilever beam to curve downward.
  • FIG. 8 is a side view cross sectional representation of a masked diamond for forming optical structures according to an example embodiment.
  • the mask 800 comprises an array of one or more multiple round openings 810.
  • the disk like voids 910 may behave as a pump, or optical deflector in one embodiment.
  • the surface of the diamond bubbles up slightly. These bubbles can result in optical fringe effects, including color changes.
  • the disks are approximately 500 nm in diameter. Other shapes and sizes may easily be formed.
  • further masks and implants may be used to fully release the diamond above each of the disk like voids, to create small lens like structures.
  • Such structures may be of desired thicknesses tied to the implant levels.
  • the lenses are approximately 50 um thick, forming an etalon or optical filter. It should be noted that lasers and other method of releasing the lenses may be utilized in addition to varying depth implants and heat to release the lenses. In some embodiments, thicknesses of less than 1 um are utilized. The thickness may also be a function of the desired wavelength of operation of the optical device including such structures.
  • Diamond appears to be highly biocompatible with living tissue.
  • diamond does not appear to exhibit carcinogenetic or toxicity for in situ applications, and it appears to be biologically inert in bulk form.
  • Such medical structures may be formed from CVD diamond directly, using the above identified processes, or from materials that are currently used, and then coated with CVD diamond to provide enhanced biocompatibility.
  • the coating may be applied by coating desired surfaces, or the entire structures with nanocrystalline diamond, and the growing a thin layer of CVD diamond on such surfaces.
  • Such a diamond layer may be made conductive by including desired dopants, or may be non-conductive if desired.
  • a 50 nm coating of CVD diamond is sufficient to provide desired characteristics. Such characteristics include biocompatibility, as well as the ability to inhibit oxidation of the structures they are coating.
  • nanocrystalline diamond is used to seed the structure where desired.
  • the nanocrystalline diamond is commercially available, and may be suspended in alcohol for application to the structure. The structure may be dipped in the alcohol, and the alcohol allowed to evaporate, leaving a desired amount of diamond seed on the structure.
  • An adhesive carrier for the diamond seed may also be used, such as photoresist, which may then be evaporated.
  • the CVD diamond layer may be formed from the seed, such as growing from the seeds at various process temperatures, such as between 500 to 1000 0 C, or approximately 200 0 C depending on the thermal budget of the structures, or their tolerance to heat.
  • the CVD diamond is grown on the seeds sufficient to cover desired portions of the structure with CVD diamond. Multiple such coatings may be performed to cover the entire structure.
  • Some applications include surgical scalpels and drill bits.
  • CVD diamond coating provides increased durability.
  • drill bits such as dental, neuro, or orthopedic type drill bits
  • the CVD diamond structure or coating may provide increased durability, and in addition, can permit a desired level of sharpness without increased erosion of the drill bit.
  • a duller drill bit may have a desired property of providing increased control of drill rates.
  • orthopedic devices may have improved performance. Ball and socket or cub mechanisms forming artificial knee, hip, shoulder and elbow joints may be selectively coated with CVD diamond, or in some embodiments, entirely created from CVD diamond. Further devices, such as spinal disc replacements, screws, plates, nodes, etc may be formed of diamond, or coated with CVD diamond.
  • Cardiovascular applications for CVD diamond formed or coated devices include catheter systems, such as rotator blades for cleaning arteries, stents, and heat valves may all have increased lives because of associated reduction in wear and tear rates.
  • Nano medical applications include the use of CVD diamond to encase devices that deliver proteins, recombinant protein, and/or retrovirus, endovirus, and plasmid technologies.
  • a reservoir 1010 containing a drug is formed in diamond, silicon, or other substrate material using methods suitable for the corresponding materials.
  • many basic photolithographic techniques may be used to form structures. Sacrificial layers may be used to form the reservoir 1010, and a first tube or conduit 1015 to a pump 1020, which is a small, bubble-like structure having the ability to have its volume controlled by desired actuation.
  • the pump 1020 is further connected to an output tube or conduit 1025, for injecting fluids.
  • Pump 1020 may be actuated by application of voltage, or mechanically by use of piezoelectric material to cause the bubble to controllably collapse and reform. This results in a nanofluidic switch or pump.
  • the silicon device 1000 may then be coated with CVD diamond as described above. Two applications of CVD diamond may be used, with the device turned over for the second application to coat a bottom of the device.
  • a masked carbon ion implant of various energy levels may be used to create a via from the reservoir 1010 to the surface of the device 1000. This provide access for easier etching, and also for quicker loading of the device with desired drugs. Circuitry may also be provided to supply controlled voltages or suitable pressure to surfaces of the pump 1020, to provide actuation of the pump. In still further embodiments, an additional pump or bubble 1030 may be formed such that there are two pumps between the reservoir and exit conduit. When operated in the proper sequence, they ensure that fluid is pumped in the desired direction. While the shape of device 1000 is shown as rectangular, the actual shape may be varied as desired for compatibility with in situ applications. The sizes of tubes and reservoirs may also be varied to achieve desired operating parameters.
  • Multiple implants at varying energy levels may be used to form the via.
  • An anneal is used to open the capillaries, and may also serve to open the via.
  • etching as described above may be used to open the via.
  • the etchant may be provided through the open capillaries if desired. Electrolysis with water and a current applied between ends of the capillaries may also be used to remove the graphitic material.
  • Multiple capillaries and vias may be formed in and between multiple levels in various embodiments to form complex fluidic structures. The above bubbles may be integrated into the capillaries and operate as switches or pumps between intersecting capillaries or channels.
  • the capillaries may be formed with varying dimensions, such as from 5 to 10 urn wide to millimeter range widths. They may also be formed as long as desired. Both dimensions are controlled by masking the implantations used to form them.
  • capillary 1110 is formed with a portion of the capillary doped to make it conductive.
  • the doping may be provided during formation of the diamond device 1100 such that the top of capillary 1110 is conductive, with the remainder of the tube having insulative properties of undoped CVD diamond.
  • Electrical pulses may be used to close off the capillary or open it, thus operating as a switch, hi a further embodiment, electrodes may be placed on either end of the conductive portions of the capillary to measure conductivity of fluid within the capillary.
  • optical sensors and emitters may be embedded in a diamond, or coated with CVD diamond as shown in block diagram in FIG. 12.
  • a silicon substrate 1205 has an optical emitter 1210 coupled to an optical detector 1220 by a waveguide 1230.
  • a CVD diamond coating 1235 is used to encapsulate the silicon structures.
  • the diamond coating 1235 serves to protect the silicon structures and prevent oxidation of them. Thus, they may be used implanted into living beings and be biocompatible.
  • a conductive input path 1240 extends from optical detector 1210 through the diamond layer, such as by doping both the silicon and diamond layer to form an contact in the diamond layer.
  • a conductive output path is formed at 1245, and extends from the optical detector 1220 to the outside of the diamond coating 1235.
  • the input and output may be used as a neural conductor in some embodiments.
  • various combinations of silicon and diamond may be constructed as described below with respect to boron doping of diamond semiconductor.
  • Various other optical and electrical detectors formed of silicon or gallium arsenide or other semiconductor materials may also be encased or selectively coated with CVD diamond.
  • the diamond conductive portion extends from one end of the diamond to the other, providing a diamond based neural connector.
  • FIG. 14 is a representation of a structure 1410, such as one of the structures described above, including prosthetic devices, implantable medical devices, tools, etc. selectively coated with CVD diamond 1420. It is in block diagram form, since many of such structures are well known. While the entire structure 1410 is shown as coated, only a portion need be coated with CVD diamond.
  • the CVD diamond 1420 maybe single crystalline, nano-crystalline or poly crystalline depending on application.
  • One example embodiment provides first and second synthetic diamond regions doped with boron.
  • the second synthetic diamond region is doped with boron to a greater degree than the first synthetic diamond region, and in physical contact with the first synthetic diamond region.
  • the first and second synthetic diamond regions form a diamond semiconductor, such as a Schottky diode.
  • FIGS. 15-18 illustrate a method of producing a monocrystalline synthetic diamond Schottky diode, which is one example of a diamond semiconductor device such as can be produced using the present invention.
  • FIG. 15 illustrates a diamond seed crystal that is heavily doped with boron, which has only three valence electrons relative to carbon's four valence electrons, making the diamond a strongly p-type semiconductor material.
  • the absence of electrons in sites in the diamond that contain boron leaves a "hole” that is receptive to electrons, making what is in effect a mobile positive charge.
  • the negatively charged boron atom is fixed in the diamond lattice, meaning that the boron atoms cannot move but contribute holes as electron receptors to the electrical conduction process.
  • Hydrogen atoms are then implanted to a desired depth, as is shown in FIG. 15 at 102.
  • the hydrogen atoms are implanted under various conditions in various examples, but in one example are implanted at an angle of ten degrees relative to the diamond surface, and at a dose rate of approximately one microamp per square centimeter.
  • the electrons are implanted with an energy of approximately 200 KeV, until the total dose of approximately ten to the seventeenth atoms per square centimeter are implanted into the diamond 101. Varying the parameters of the hydrogen implant will vary the depth and density of the resulting hydrogen implant layer.
  • the hydrogen implant layer is shown as the dotted layer 102 of FIG. 15.
  • the diamond grown in one example is a monocrystalline synthetic diamond uses a stream of gas, such as methane or other gas, to provide the precursor material for the plasma reactor to produce a plasma that precipitates to form diamond.
  • the gas in some examples or in some layers of the diamond contains various impurities, such as boron dopants or various isotopes of carbon.
  • diamonds having a greater than average purity of carbon- 12 and a corresponding reduced concentration of carbon- 13 isotopes are known as isotopically enhanced, and are particularly thermally conductive. This makes them well-suited for applications such as semiconductor device fabrication, enabling higher power and higher density than can otherwise be achieved.
  • Isotopic enhancement of the diamond CVD precursor gases with carbon- 12 can result in a diamond having significantly less than the typical 1.1% carbon- 13 concentration, resulting in thermal conductivity as high as 3300W/mK.
  • Other examples of methods of producing synthetic diamond with high thermal conductivity include growing diamond in a low nitrogen environment, growing synthetic diamond in an environment rich in hydrogen, and using boron doping resulting in an increase in thermal conductivity.
  • diamond regions having boron or other dopants implanted will have somewhat larger or smaller lattice structures than undoped diamond as a result of placement of the dopant within the diamond crystal structure.
  • the lattice mismatch between diamonds having different doping concentrations or between doped and undoped diamonds is controlled in some embodiments by implantation of ions selected to give the desired lattice structure.
  • ions selected to give the desired lattice structure.
  • a lightly boron-doped diamond region will have a lattice structure somewhat expanded relative to undoped diamond made from primarily carbon- 12. Adding carbon- 13 to the boron-doped diamond shrinks the lattice structure, and is used in some embodiments to eliminate the lattice mismatch between diamond layers or to control the lattice mismatch or strain between diamond layers.
  • the seed 201 is polished flat before hydrogen implantation or at some other point before growth of the second synthetic diamond region 202, and is trimmed to a desired size or shape such as by laser cutting before or after growth of the second synthetic diamond region.
  • the top layer is grown to a desired thickness, such as 100 microns in one example, and is then polished and cut to form the diamond assembly shown in FIG. 16.
  • the assembly of FIG. 16 is then heated to a temperature sufficient to cause separation of the first diamond region 101 at the hydrogen implant level, resulting in a portion of the seed diamond region 101's becoming detached with the grown synthetic diamond region 202.
  • This operation results in a seed diamond 301 that is somewhat smaller than the original seed diamond 101, due to the more heavily boron-doped diamond portion 302 that is removed with the more lightly boron-doped portion 303.
  • the resulting structure of 302 and 303 in FIG. 17 forms the semiconductor portion of a Schottky diode, which is able to operate at particularly high voltage and power levels due to the characteristics of diamond when compared to other semiconductor materials such as silicon.
  • the grown region will be more heavily doped with boron than the seed region, the thicknesses of the diamond regions will differ, and other structural and design changes will be made.
  • FIG. 17 that was lifted off the diamond seed region at 401, with electrical leads attached at 402 and 403.
  • the metal attached is selected based on the metal's work function or fermi function and the desired characteristics of the Schottky diode, and will typically be a metal or metal alloy containing metals such as aluminum, platinum, gold, titanium, or nickel.
  • the terminal 403 is known as the anode
  • terminal 402 is known as the cathode.
  • the rectifying portion of the Schottky diode is actually the metal- to diamond semiconductor contact, rather than the interface between semiconductor materials as is the case in most other types of diodes such as p-n semiconductor diodes.
  • the theory of Schottky diode operation is well- understood but relatively complex, and results in a number of significant advantages over regular semiconductor diodes for many applications.
  • the forward voltage drop across a Schottky diode is typically much less than across a typical p-n junction semiconductor diode, with typical values of .2 Volts drop across a Schottky diode and . ⁇ -.7 Volts drop across a silicon p-n junction diode.
  • FIG. 19 is a flowchart of a method of making a boron-doped diamond semiconductor device such as that of FIG. 18.
  • aboron-doped seed diamond is cx * eated. This can be achieved by ion implantation into a natural or synthetic diamond, by growing a synthetic diamond in an environment that is rich in boron, or by any other suitable method. Grown diamond can be produced by high pressure high temperature (HPHT) methods, by chemical vapor deposition, or by any other suitable method.
  • HPHT high pressure high temperature
  • the boron-doped seed diamond surface is polished at 502, to prepare a flat diamond crystal surface of a desired crystal orientation. For example, the diamond may be polished in the 100 plane, tilted two degrees toward the 110 plane, to produce a polished surface slightly off the 100 plane of the diamond.
  • the diamond is grown until a desired thickness is reached, such as 500 microns thickness, or between 10 and 15,000 microns thick.
  • a desired thickness such as 500 microns thickness, or between 10 and 15,000 microns thick.
  • the diamond assembly is removed from the grower, and edges are trimmed with a laser cutter at 505. In other examples, the edges are trimmed using other methods, and may be polished or ground. The edges of the seed are thereby also trimmed to desired dimensions, such as back to the original seed dimensions before growth on top of the seed diamond region.
  • the resulting diamond assembly is heated in a non-oxidizing environment, such as in hydrogen or an inert gas, to an elevated temperature designed to cause the seed diamond region of the diamond assembly to separate at the area of hydrogen implantation.
  • This separation occurs in one example at about 1200 degrees Celsius, while in other examples occurs within a range of 1100 to 2400 degrees Celsius.
  • the grown diamond-see diamond assembly remains, as is shown in FIG. 17, with a portion of the seed diamond above the hydrogen implant layer attached to the grown diamond.
  • the separation occurs spontaneously at elevated temperatures in some examples, but is cause by application of pressure across the hydrogen implant layer in other examples.
  • FIG. 20 This figure shows generally a diamond semiconductor substrate at 601, which has at least a region or portion 602 that is boron-doped. A second region 603 is grown, implanted, or otherwise formed in contact with the diamond region 602, but with a different boron doping density. This forms the semiconductor portion of a Schottky diode, but similar processes can be used to form transistors and various other components.
  • FIG. 21 illustrates an example of an electronic device that may be constructed, consistent with some example embodiments of the present invention.
  • a radar apparatus 701 uses Schottky diodes for low-level, high- frequency radio detection, and for mixing in further example applications such as Doppler radar.
  • the electronic device benefits from the increased performance possible with boron-doped diamond semiconductors, such as improved power handling, higher density, and higher performance relative to traditional semiconductors such as silicon.
  • Boron-doped diamond is also distinct from silicon-based semiconductors in that it is largely transparent, with a bluish tint. This makes boron-doped diamonds particularly well-suited for applications such as blue LED or laser semiconductor devices in configurations where light is emitted from other than an external surface of a semiconductor junction, in addition to other applications such as traditional LED or laser diodes.
  • boron-doped diamond conducts electricity to some extent, it is also used in a variety of applications where conductivity is desired, such as in electrodes, in an electrically conductive cutting tool where the condition or other characteristics of the cutting tool can be electrically monitored, in conductive heat sinks or heat spreaders, and in optical windows that can be heated or that have an index of refraction that can be altered by current flow.
  • Schottky barrier junctions are further usable in a variety of applications other than Schottky diodes, including in use in bipolar junction transistors where a Schottky junction is located between the base and collector of the transistor. This prevents the transistor from saturating too deeply, resulting in faster switching times for the transistor.
  • Metal-semiconductor field effect transistors also use a reverse-biased Schottky barrier to provide the depletion region in the transistor, ans works similarly to a JFET.
  • Still other devices, including high electron mobility transistors (HEMTs) use Schottky barriers in a heterojunction device to provide extremely high conductance in a transistor.

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Abstract

Selon l'invention, des implants ioniques masqués et contrôlés, couplés à la recuisson ou à l'attaque chimique, sont utilisés dans un diamant monocristallin formé par CVD afin de créer des structures pour des applications optiques, pour la formation de dispositifs nanoélectromécaniques et pour la formation de dispositifs médicaux. L'implantation ionique est utilisée pour délivrer une ou plusieurs espèces atomiques à l'intérieur de et sous la surface de croissance de diamant de manière à former une couche implantée présentant une concentration de pointe d'atomes à une profondeur prédéterminée sous la surface de croissance de diamant. La composition est chauffée dans un environnement non oxydant dans des conditions appropriées pour entraîner la séparation du diamant à proximité de la couche implantée. D'autres implants ioniques peuvent être utilisés dans des structures libérées afin de les redresser ou de les courber tel que souhaité. Le dopage au bore peut également être utilisé pour créer des structures en diamant conductrices.
EP06717944A 2005-01-11 2006-01-11 Dispositifs medicaux en diamant Withdrawn EP1842227A2 (fr)

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US64339005P 2005-01-11 2005-01-11
US11/056,338 US20050181210A1 (en) 2004-02-13 2005-02-11 Diamond structure separation
US11/178,623 US7122837B2 (en) 2005-01-11 2005-07-11 Structures formed in diamond
PCT/US2006/000808 WO2006076354A2 (fr) 2005-01-11 2006-01-11 Dispositifs medicaux en diamant

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CN101203939A (zh) 2008-06-18
CN101838844A (zh) 2010-09-22

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