High frequency piezoelectric crystal composites, devices, and methods for manufacturing the same
10230040 ยท 2019-03-12
Assignee
Inventors
- Pengdi Han (New Castle, WA, US)
- Jian Tian (Naperville, IL, US)
- Kevin Meneou (Downers Grove, IL, US)
- Brandon Stone (Elgin, IL, US)
Cpc classification
H10N30/852
ELECTRICITY
G03H3/00
PHYSICS
C04B2235/3286
CHEMISTRY; METALLURGY
C04B2235/96
CHEMISTRY; METALLURGY
C04B2235/3296
CHEMISTRY; METALLURGY
C04B2235/76
CHEMISTRY; METALLURGY
A61B8/4483
HUMAN NECESSITIES
C04B2235/3206
CHEMISTRY; METALLURGY
C04B2235/3215
CHEMISTRY; METALLURGY
C04B2235/3298
CHEMISTRY; METALLURGY
C04B2235/3255
CHEMISTRY; METALLURGY
C30B29/32
CHEMISTRY; METALLURGY
H03H9/02015
ELECTRICITY
C04B35/491
CHEMISTRY; METALLURGY
Y10T29/42
GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
C04B35/495
CHEMISTRY; METALLURGY
C01G33/006
CHEMISTRY; METALLURGY
C04B2235/3224
CHEMISTRY; METALLURGY
C04B2235/3249
CHEMISTRY; METALLURGY
International classification
G03H3/00
PHYSICS
C30B29/32
CHEMISTRY; METALLURGY
A61B8/00
HUMAN NECESSITIES
Abstract
The present invention generally relates to high frequency piezoelectric crystal composites, devices, and method for manufacturing the same. In adaptive embodiments an improved imaging device, particularly a medical imaging device or a distance imaging device, for high frequency (>20 MHz) applications involving an imaging transducer assembly is coupled to a signal imagery processor. Additionally, the proposed invention presents a system for photolithography based micro-machined piezoelectric crystal composites and their uses resulting in improved performance parameters.
Claims
1. A piezoelectric PMN-PT based crystal composite, said piezoelectric crystal composite having a crystal composition represented by the formula:
x*Pb(B.sub.1/2B.sub.1/2)O.sub.3-y*PbTiO.sub.3-(1xy)*Pb(Mg.sub.1/3Nb.sub.2/3)O.sub.3; wherein, x is defined as molar % 0.00 to 0.50; y is defined as molar % 0.00 to 0.50; B represents Indium (In), Ytterbium (Yb), Scandium (Sc), Zirconium (Zr), or Iron (Fe); and B represents Niobium (Nb) or Tantalum (Ta).
2. A piezoelectric crystal composite, according to claim 1, in further combination with: an additive, said additive being selected from the group consisting of: Manganese (Mn) of up to 5% (wt %) and Cerium (Ce) of up to 10% (wt %) of a total batch weight.
3. A piezoelectric crystal composite, according to claim 1, wherein: said crystal composite has a thickness electromechanical coupling factor k.sub.t of about 0.65 to 0.90.
4. A piezoelectric crystal composite, according to claim 1, wherein: said crystal composite is operative at a frequency of at least 20 MHz.
5. A piezoelectric crystal composite, according to claim 1, wherein: said crystal composite is operative at a frequency of at least 80 MHz.
6. A piezoelectric crystal composite, according to claim 1, in further combination with: a medical imaging device configured for operative ultrasound imaging.
7. A piezoelectric crystal composite, according to claim 1, wherein: said crystal composite is (001) cut and <011> poled and provides zero strain in the direction of +/32.5 (+/2.5) away from the <011> direction according to the coordinate rotation d.sub.31 formula:
d.sub.31=d.sub.31*Cos()*Cos()+d.sub.32*Sin()*Sin().
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1)
(2)
(3)
(4)
(5) composite for a transducer having a hexagonal structure, <001> cut, noting directional orientation and epoxy polymer and crystal designations with no impact on clamping direction due to <001> cut.
(6)
(7)
(8)
(9)
(10)
(11)
(12)
(13)
(14)
(15)
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
(16) Reference will now be made in detail to embodiments of the invention. Wherever possible, same or similar reference numerals are used in the drawings and the description to refer to the same or like parts or steps. The drawings are in simplified form and are not to precise scale. For purposes of convenience and clarity only, directional (up/down, etc.) or motional (forward/back, etc.) terms may be used with respect to the drawings. These and similar directional terms should not be construed to limit the scope of the invention in any manner,
(17) As will be used herein the Miller Indices identifiers serve as vector representations for orientation of an atomic plane in a crystal lattice having three axes represented by a set of 3 integer numbers, for example such conventional identifiers as, for example <010> or <10{tilde over (1)}>, are used.
(18) As will be further used herein, for example regarding the images of the present invention wherein polymeric (epoxy) regions are filled with a piezoelectrically non-active material, that the use of the phrase kerf is not limited to a region formed by a mechanical saw of any kindinstead the phrase kerf will be understood broadly by ones skilled in the art to represent the region between piezoelectric posts which receiving polymeric material, whether or not the actual region is formed by a saw, or by any other manufacturing process discussed herein.
(19) Additionally, a description methodology (the M-N labeling convention) is used to describe the number of directions which each section of the piezoelectric material and polymeric material continuously extend, wherein M represents the number of continuous directions in which the piezoelectric (PMN-PT) material extends and N represents the number of directions in which the polymeric (epoxy) material continuously extends. While those of skill understand this convention, however as modified herein, the structures suggested herein have never been subjected to the M-N convention and therefore applicant requires a hybrid understanding wherein the directional extensions generally remain, but are discontinuous or interrupted, for example, by intersection with a cross directional polymeric material extending in a different and also discontinuous direction. In this manner, it will be understood that the (as later described) hexagonal structure involves discontinuous, interrupted, or hybrid polymeric (epoxy) material directions where the polymeric material direction is linear in only one direction along the length of the piezoelectric material itself and the other polymeric (epoxy) directions are interrupted-in-direction or discontinuous-in-direction by encountering piezoelectric material. One embodiment of the invention further has a structure the result of the piezoelectric material elements having discontinuous or interrupted side alignments with respective sides/edges of proximate piezoelectric material elements, so that sides/edges may not be coplanar (on the same plane) but may extend on parallel planes. Still a further embodiment of the invention does not contain simple regular unit elements (
(20) This invention relates to the 20 MHz to >100 MHz high frequency piezoelectric single crystal composes/composite crystal elements and the process for the preparation thereof. The novel high-coupling factor crystal composites can broadly replace the legacy materials such as piezoelectric ceramics, single crystal and traditional crystal composite for high frequency transducers.
(21) Referring now to
(22) The crystal composite and the composite crystal elements have novel structures and/or new crystallographic cut directions. The crystal composites cat be fabricated by proprietary procedures including photolithography, deep reactive ion etching, fine mechanical finishing and electrode coating.
(23) The plate (not shown) is preferably lapped on both sides and polished on one of the sides. The lapped and unpolished side can then be bonded to a glass carrier (not shown), which is bonded to a silicon, Si, wafer (not shown). The dimensions of the plate are in the range of ten (10) millimeters (mm)ten (10) mm0.20 mm-to-1.20 mm in thickness; however, the dimensions could be of any size.
(24) The material of the plate is a single crystal with electroded faces oriented along the <001> or <011> crystallographic directions. As one of ordinary skill in the art would appreciate, a single crystal structure can desirably have a high piezoelectric coefficient (e.g., d.sub.33>2000 pC/N, d.sub.33>0.8, d.sub.33>0.7). The plate preferably has a dielectric constant in the range of approximately 4000 to >7700 and a dielectric loss of less than 0.01.
(25) It will be recognized that the plate piezoelectric single crystal is a ternary crystal formed, according to the following formulas I or II:
(26) Formula I: x*Pb(B1/2B1/2)O3-y*PbTiO3-(1xy)*Pb(Mg1/3Nb2/3)O3, where, x is defined as molar % 0.00 to 0.50; and y is defined as molar % 0.00 to 0.50, B represents Indium (In), Ytterbium (Yb), Scandium (Sc) or Iron (Fe), B represents Niobium (Mb) or Tantalum (Ta). Additionally, formula I may be combined with additives Manganese (Mn) of up to 5% (wt %) and/or Cerium (Ce) of up to 10% (wt %) of a total batch weight.
(27) Formula II: x*ABO3-y*PbTiO3-(1xy)*Pb(Mg1/3Nb2/3)O3, where, x is defined as molar % 0.00 to 0.50; and y is defined as molar % 0.00 to 0.50. A represents Lead (Pb) or Bismuth (Bi), B represents Indium (In), Ytterbium (Yb), Iron (Fe), Zirconium (Zr), Scandium (Sc), Niobium (Nb), Tantalum (Ta), or a combination of the above elements. Additionally, formula II may be combined with additives Manganese (Ma) of up to 5% (wt %) and/or Cerium (Ce) of up to 10% (wt %) of a total batch weight.
(28) Several non-limited examples of formulae I and II are found in the following table. It will be recognized that any composition matching the formulae I or II is included herein by reference as a suitable composition.
(29) TABLE-US-00001 Formula I Formula II Example 1 31% PIN-46.7% 15% BiScO-58.6% PMN-20.8% PT PMN-26.4% PT Example 2 15% PIN-53.7% PMN-22.4% 15% BiScO-57.6% PMN- PT: 8.9% Ce 26.4% PT:1% Ce Example 3 25% PYbN-45.7% 10% BiScO-58.6% PMN- PMN-25% PT:2% Mn 26.4% PT:5% Mn Example 4 10% PZrT-64% 7% BaTiOs-61% PMN-24% PT:3% Mn PMN-PT-32% PT
(30) In a second step 20 of photolithography a thin metal (Nickel) seed layer was applied and then in a step 30 a mask was prepared by spincoating a photoresist on top of the seed layer. The mask defines the desired shape and/or pattern of imaging elements) within the piezoelectric composite material After baking, UV exposure, and development, a patterned photoresist was obtained.
(31) A Nickel mask of a predetermined thickness (here 10 microns, but can be any thickness from 1 to 30 microns) was electroplated thereon to have the inverse pattern of the mask of the photoresist, which was then stripped away using reactive ion etching. The use of hard or high molecular weight metals such as Ni and Pt, is desirable for selectivity to protect the covered underlying area of the plate from being later etched.
(32) The etching process, such as reactive ion etching (RIE) is used as noted, but other etching processes can be used, such as wet-etching. In one preferred embodiment chlorine, Cl.sub.2 based RIE etching is used, which has an etching rate of approximately from less than 3 microns/hour to 12 microns/hour and can cause a substantially vertical etching profile (e.g., >89 degree.). In the alternative, or in addition, to Cl.sub.2, sulfur hexafluoride, SF.sub.6, based etching can be used, which has similar etching properties to that of Cl.sub.2. The nickel, Ni, pattern protects the underlying portions of the plate covered by the pattern from the etching process.
(33) In a step 40 the crystal parts with the patterned etched mask were located into an ICP-plasma unit for deep reactive ion etching (DIRE) using the preferred Cl.sub.2 gas. As a result of step 40, one or more deep posts of the type discussed later are formed in the plate with one or more kerfs bounding each respective post, etched in the uncovered portions of the plate. The one or more kerfs can have a width in the range of approximately from less than one (<1) to twelve (12) microns, and preferably from 1 to 10 microns in width.
(34) The respective posts can have a width ranging from approximately 3 to 200 (or longer in length for the hybrid 2-2/1-3 configuration discussed herein) microns and have a height in the range of approximately less than five (<5) to more than seventy (>70) microns, such that in one embodiment it is preferable to have an aspect ratio (post height/post width) of at least one to dampen the effect of lateral modes. For the dimensions of the plate described above, the etching process can last approximately six (6) to eight or eighteen (8 or 8) hours. After the etching step 40, the plate is then rinsed with a solvent for cleaning.
(35) In the next step 50, the kerfs are filled with an epoxy, such as Epoxy 301 provided by Epo-Tek, although other epoxies may be employed without departing from the scope and spirit of the present invention. A vacuum (not shown) may be utilized to remove air bubbles and prevent any void within the kerfs. In the next step 60, after the epoxy cures, the top portion of the plate and epoxy are lapped to a thickness of approximately 25 microns. In a step 70, an electrode pattern is then applied to the plate to form the imaging transducer pattern. The electrode pattern is preferably comprised of gold (Au) and/or chromium (Cr). Moreover, as one of ordinary skill in the art would appreciate, electronic circuitry, such as imaging processing circuitry, (not shown) can be bonded to the electrodes (not shown). Further, the electrode pattern formed on the plate can define any pattern of imaging transducers, including an array, e.g., an imaging transducer at each post, or a single imaging transducer. An epoxy layer may be applied to the back of the plate.
(36) In a further step 80 the plate is dimensioned suitably as desired and then poled at 50 VDC. In a step 90 key dielectric and piezoelectric properties are measured and calculated with suitable equipment, for example Agilent 4294A Precision Impedance Analyzer.
(37) Imaging transducers having an operating frequency at above 20 MHz, e.g., 30 to >100 MHz, can be developed using photolithography based micromachining, such as the process 100 described above. The higher frequency of operation increases the resolution and image depth of an imaging transducer. Furthermore, the bandwidth of the imaging transducer, particularly when single crystal PMN-PT is employed as the piezoelectric, can be close to 100%, compared to only 70 to 80% for <20 MHz transducers made with PZT ceramic.
(38) The greater bandwidth improves the transducer's axial resolution, which increases the imaging depth. This is desirable for high frequency transducers, which have very limited imaging depth due the strong attenuation of high frequency ultrasound in tissue. When single crystal is used, these advantages can be achieved with sensitivities equivalent to or better than ceramic transducers. These high frequency transducers can be applied to a number of medical procedures including the imaging of the anterior region of an eye for monitoring surgical procedures such as cataract treatment by lens replacement and laser in situ keratomileusis (LASIK) and tumor detection (preferably up to sixty (60) MHz for fifty (50) .mu.m resolution); skin imaging for care of burn victims and melanoma detection (preferably twenty five (25) MHz for subcutaneous, fifty (50) MHz for dermis and one hundred plus (100+) MHz for epidermis); intra-articular imaging for detection of pre-arthritis conditions (preferably twenty five (25) to fifty (50) MHz); in-vivo mouse embryo imaging for medical research (preferably fifty (50) to sixty (60) MHz); Doppler ultrasound for determination of blood flow in vessels<one hundred (100) .mu.m in diameter (preferably twenty (20) to sixty (60) MHz); intracardiac and intravascular imaging (preferably ten (10) to fifty (50) MHz); and ultrasound guidance for the biopsy of tissue.
(39) As an example of such a medical device, we refer not to
(40) The present inventors have determined that the PMN-PT based piezoelectric crystals usually use (001)-cut and poling <001> which gives the highest d.sub.33 but the lateral clamping effect by the epoxy filled into kerfs cannot be avoided and his highly detrimental to performance for a variety of imaging systems and methods of use. We first use the hexagonal (bee nest) type hybrid shaped 1-3 type crystal composite. The advantage is significant in that the structure is mechanically much stronger and more stable than square-shaped pattern if the both piezo-effective volume is the same. It is much more practical/suitable for large scale fabrication.
(41) Referring now to
(42) We have induced the formula (1) to calculate the d.sub.31 by coordination rotation:
d.sub.31=d.sub.31*Cos()*Cos()+d.sub.32*Sin()*Sin() (1)
(43) From the 2-D plot of the d.sub.31, it is indicated that the micro strains are zero in the +/32.50 directions away from the <10{tilde over (1)}> direction. It is a significant advantage that the lateral strain-free arrangement will greatly enhance the electromechanical coupling factor and broaden the bandwidth permissible in an ultrasound device.
(44) Discussion of
(45) Referring now to
(46) Referring now to
(47) Referring now to
(48) As a result of preparing such composites according to the details herein throughout, a thickness electromechanical coupling factor k.sub.t of 0.65-0.90 is achieved.
(49) Referring now to
(50) Referring now to
(51) As noted herein with regards to
(52) It will be understood that the method of fabricating noted earlier may be used to fabricate one of more imaging transducers having any of the hybrid configurations with any composition shown herein without departing from foe scope of the entire disclosure. It will be understood that the compositions may be used in any configuration.
(53) It will be understood that an imaging device may be configured as discussed in
(54) It will be understood that the phrase hexagonal is a polygon with six edges or sides in a plan view, such that the hexagonal polygons of the type shown have six edges or sides and extend from an initial position.
(55) It will be understood that there are many different kinds of quadrilateral (four sided) polygons, and all have several things in common: two opposing sides are coplanar, have two diagonals, and the sum of their four interior angles equals 360 degrees, however as noted herein, the phrase parallelogram used herein reflects two parallel pairs of opposite sides without right angles, and a rhombus is merely such a parallelogram with equal length, sides (and may also be referred to as a diamond pattern or an oblique rhombus) with understanding by those of skill in the art.
(56) Having described at least one of the preferred embodiments of the present invention with reference to the accompanying drawings, it will be apparent to those skills that the invention is not limited to those precise embodiments, and that various modifications and variations can be made in the presently disclosed system without departing from the scope or spirit of the invention. Thus, it is intended that the present disclosure cover modifications and variations of this disclosure provided they come within the scope of the appended claims aid their equivalents. As a further example, each feature of one embodiment can be mixed and matched with other features shown in other embodiments, and similarly features may be added or removed such that the invention is recognized as not restricted except in view of the appended claims.