 
                 Patent Grant
 Patent Grant
                     8421170
 8421170
                    This invention relates generally to capacitive micromachined ultrasonic transducers (CMUTs), particularly to those comprising diamond or diamond like carbon (will be referred to as diamond) membranes and a method of microfabrication of such CMUTs.
Capacitive micromachined ultrasonic transducers (CMUTs) are electromechanical energy conversion devices used to transmit and receive ultrasound. CMUTs used in immersion are generally composed of vacuum-sealed cavities formed by a membrane material. The vacuum-sealed cavities are conventionally realized by two techniques. First one is the sacrificial release process where sacrificial material deposited before the membrane material is etched through the etch holes, and etch holes are filled by deposition under low pressure to form the cavity. CMUTs fabricated by sacrificial release process mostly feature Si3N4 membranes. The limitations of sacrificial release process to achieve very large membranes without breaking or very small membranes with high fill factor adversely affect the precise engineering of the transducer physical parameters. The Si3N4 membranes are also hard to present well-controlled deflection profiles due to the process-dependent residual stress in the membrane material. The second one is direct wafer bonding method where two wafers (one having cavity patterning and the other having the membrane material) are bonded under elevated temperatures under vacuum.
Among these microfabrication methods, direct wafer bonding technology is more economical offering better process control, higher yield, and more novelties in CMUT designs than the sacrificial release process. Direct wafer bonding technology enabled development of single crystal silicon membrane CMUTs rather than silicon nitride membrane ones. As the membrane and the substrate material are both silicon, direct wafer bonding at high temperatures (1100° C.) is achieved without introducing any residual stress in the membrane. Furthermore, IC compatible direct wafer bonding at lower temperatures (400° C.) can be also utilized. This technology has significantly reduced the complexity and the time of the processing of CMUTs additionally offering superior process control, high yield, and improved uniformity compared to the already mature sacrificial release process. Best part of wafer bonding technology is to present a well-known silicon crystal material as a membrane, and to achieve vacuum sealed cavities without the need to open etch holes on the membrane, both of which directly translate into reliable operation in immersion. Recently, successful flip-chip bonding of IC and wafer-bonded 2-D CMUT arrays incorporating through wafer trench-isolated interconnects has been demonstrated. Therefore, recent developments enable the specifications of the CMUT design be comfortably satisfied facilitating the realization of industrial grade CMUT products using direct wafer bonding technology.
Energy conversion efficiency of CMUTs has been of primary importance for ultrasound applications, and improvement of this efficiency has been extensively studied for ultrasound transducers. Conventionally, the CMUT is biased at a voltage below the collapse voltage, and an AC signal is applied to generate ultrasound. The efficiency of the transducer is drastically improved as the bias voltage approaches the close vicinity of the collapse voltage. However, this high efficiency comes with a risk of membrane collapse onto the substrate. Additionally, the AC amplitude is limited to a small excitation voltage around a large bias voltage to prevent membrane collapse during operation. Therefore, the maximum output pressure of a CMUT is inherently limited by the requirements of the conventional operation.
For potential applications such as high intensity focused ultrasound (HIFU) in medical therapeutics, larger output pressures are essential. To offer unprecedented acoustic output pressure in transmit without the aforementioned limitations, novel CMUT operation modes of collapse and collapse-snapback are introduced. Both operation modes require the membrane to contact the substrate surface, which poses a problem on the durability of the membrane in terms of structural integrity and tribological property. Large membrane deflection at collapse increases the stress within the membrane, and change of stress at ultrasound frequencies causes reduced lifetime and compromised reliability in these high output pressure operation modes. Ultrasound applications require the transducer surface to be in contact with the acoustic medium. Because the surface is subject to environmental conditions as well as external pressures, the durability of the membrane defined by hardness is also a major criteria for CMUT performance. Because of electrostatic forces in addition to the atmospheric pressure due to the vacuum sealed cavities, Young's modulus of the membrane plays an important role in the membrane deflection profiles as well.
Collapse-snapback mode requires the collision of the contacting surfaces every cycle, and heat released needs to be dissipated quickly to maintain stable operation. Based on the additional requirements of these modes to reach high output transmit pressure at a sustainable transducer operation, diamond is proposed as the ultimate solution to be used as the membrane material. Mechanical (high Young's modulus, extreme hardness), thermal (large thermal conductivity, low thermal expansion coefficient), and electrical properties (insulator, large electrical breakdown field) of diamond are all in favor of its use in the microfabrication of CMUTs. Chemical inertness, biocompatibility and surface modification are further benefits of diamond for CMUTs to be utilized in corrosive environment and biological samples, respectively. For example, hydrophilic O2-terminated diamond surface, achieved by oxygen plasma or piranha wet processing, will withstand against the detrimental cavitation shock of bubbles in immersion. Because no wet chemical etchant of diamond exists, its use is best suited for extreme and harsh environments. Compared to all potential membrane materials as well as current membrane materials of Si3N4 and silicon, diamond distinguishes itself based on high Young's modulus and exceptional hardness (see Table 1 for material properties of Si3N4, Si, and diamond).
  
    
      
        
        
        
          
            
            
          
        
        
          
            
            
          
          
            
            
          
        
      
      
        
        
        
        
        
          
            
            
            
            
          
          
            
          
        
      
      
        
        
        
        
        
          
            
            
            
            
          
          
            
            
            
            
          
          
            
            
            
            
          
          
            
            
            
            
          
          
            
          
        
      
    
  
Diamond is a perfect membrane material candidate based on its material properties. However, unmature single crystal diamond (SCD) deposition technologies prevented diamond membranes integration into CMUTs. Thin film SCD coated wafers are not commercially available for batch MEMS processes. Surface roughness of SCD is also high to be utilized for CMUT microfabrication based on direct wafer bonding technology.
Recently, with improvements in diamond material growth and technology, ultrananocrystalline diamond (UNCD) as a thin film was made commercially available.
UNCD shares a large portion of the benefits of the SCD with compromised features such as reduced resistivity due to graphitic forms enclosing polycrystalline diamond (SCD: insulator, UNCD: highly resistive). A remarkable feature of UNCD as a membrane material is its deposition as a thin film over a wafer surface with very low residual stress (i.e. <50 MPa). UNCD, featuring smaller grain size and surface roughness has been recently explored for microelectromechanical systems (MEMS) applications such as RF MEMS resonators and hybrid piezoelectric/UNCD cantilevers. However, there are no studies of CMUTs with diamond membranes.
In the documents U.S. Pat. No. 7,846,102B2 and U.S. Pat. No. 7,745,248B2 disclosing various improvements regarding CMUTs, it has been merely mentioned that diamond can be used in the membrane material amongst other materials such as silicon, silicon nitride or silicon carbide.
In the document U.S. Pat. No. 7,530,952B2, a CMUT incorporating direct wafer bonding between the membrane and the substrate is disclosed. It has also been mention in said document that the membrane material can be of diamond amongst other materials such as silicon, silicon nitride or sapphire.
The inventions disclosed in the above mentioned documents, U.S. Pat. No. 7,846,102B2, U.S. Pat. No. 7,745,248B2 and U.S. Pat. No. 7,530,952B2, are not concerned with providing a method to use diamond in the membrane and thus, neither the characteristics of the diamond material to be used nor the means for such use of diamond are not established.
An inconvenience arises in the use of diamond in a membrane to be joined to the substrate by direct wafer bonding, due to the surface properties of diamond layers grown on a substrate as is required for direct wafer bonding. The high surface roughness of such a diamond layer and the low chemical affinity between diamond and silicon dioxide hinders the establishment of the desired direct wafer bond. Moreover, applying conventional polishing methods on a diamond layer does not improve the direct wafer bonding abilities of the diamond layer.
The object of the invention is to achieve microfabrication of a CMUT employing a membrane having ultrananocrystalline diamond (UNCD) or nanocrystalline diamond (NCD). A membrane made of diamond advances the state of the art CMUT features due to several advantageous diamond material properties such as high Young's modulus, high hardness, high heat conductivity and low thermal expansion.
Another object of the invention is to achieve microfabrication of a diamond-based CMUT by plasma-activated direct wafer bonding of cavity-defined thermally oxidized silicon wafer and diamond coated silicon wafer having a thin high temperature oxide interlayer on top.
The method for microfabrication of a diamond-based CMUT having at least one CMUT cell, basically includes the steps
1. preparation of the base substrate by
2. preparation of the membrane substrate by
3. bonding of the base and the membrane substrates by
4. removing the substrate of the diamond layer;
5. and forming at least one second electrode on the membrane and at least one first electrode connection;
wherein the intermediate layer of step 2.b. is of a material with high chemical affinity towards the cavity wall material and by polishing the surface roughness of said intermediate layer is decreased after deposition, to below 0.5 nm thus providing a surface suitable for direct wafer bonding. The resulting thickness of said intermediate layer after being polished is determined such that the behavior of the membrane is determined by the diamond layer.
Preferably, for the diamond layer, diamond in the form of a nanocrystalline diamond (NCD) or an ultrananocrystalline diamond (UNCD) layer with a low residual stress below 50 MPa is obtained on a silicon or silicon dioxide wafer and then a high temperature oxide (HTO) to form the intermediate layer is applied on the diamond layer. The HTO is then chemically-mechanically polished (CMP) to obtain the desired surface roughness and thickness. Shaping of various layers can be performed using known masking, etching etc. methods.
Thus the CMUT according to the invention consists of a base wafer, a conductive layer to act as a first electrode on one surface of said base wafer, at least one cavity on said first electrode, an intermediate layer adjacent to said at least one cavity, a diamond membrane, at least one second electrode on the membrane and at least one first electrode connection.
The diamond layer may be undoped or doped. If the diamond used for the membrane is of a conductive form, then the membrane itself acts as a second electrode. Then, the intermediate layer serves also as an electrical insulator preventing the circuit from shorting through the first electrode.
The objectives and advantages of the present invention will be understood by reading the following detailed description in conjuction with the drawing, in which:
    
    
    a) shows a top view of a single CMUT.
    
    b) shows a magnified view of a CMUT cell and its neighboring cells.
    
    a) shows a top view of a 16-element 1-D CMUT array.
    
    b) shows a magnified view of a portion of 5 neighboring 1-D CMUT array elements.
    
    c) shows a magnified view of a CMUT cell and its neighboring cells.
    
    a) shows an n-type silicon substrate with <100> crystal orientation.
    
    b) shows an n-type silicon substrate with phosphorous doped (n+-type) conductive surface layer.
    
    c) shows thermally oxidized silicon dioxide layer on top of n+-type surface layer.
    
    d) shows spin-coated photoresist layer on top of thermal silicon dioxide layer of 
    
    e) shows patterned photoresist layer of 
    
    f) shows patterned thermal silicon dioxide layer (protected via patterned photoresist) via reactive ion etching of silicon dioxide (RIE-SiO2) using CHF3/CF4 gas chemistry.
    
    g) shows cavity walls of thermal silicon dioxide formed over doped silicon substrate (photoresist removed via oxygen plasma).
    
    a) shows diamond deposited on silicon wafer.
    
    b) shows high temperature oxide (SiO2) deposited on silicon substrate in a low pressure chemical vapor deposition (LPCVD) furnace using dichlorosilane (SiH2Cl2) and nitrous oxide (N2O) gas chemistry.
    
    c) shows chemically mechanically polished (CMP) high temperature oxide layer (thinned) of 
    
    a) shows plasma-activated direct wafer bonded pair of top surfaces of substrates in 
    
    b) shows thinned substrate (mechanically supporting the diamond layer) of 
    
    c) shows plasma enhanced chemical vapor deposition (PECVD) of silicon dioxide on the bottom of the substrate having cavity walls.
    
    d) shows diamond membranes over cavity via wet chemically etched thinned substrate of 
    
    a) shows plasma enhanced chemical vapor deposition (PECVD) of silicon dioxide on top of the diamond membrane of 
    
    b) shows spray-coated photoresist layer on top of PECVD silicon dioxide of 
    
    c) shows patterned photoresist layer of 
    
    d) shows patterned PECVD silicon dioxide layer (protected via patterned photoresist) via reactive ion etching of silicon dioxide (RIE-SiO2) using CHF3/CF4 gas chemistry.
    
    e) shows patterned diamond layer (protected via patterned PECVD silicon dioxide layer) via reactive ion etching of diamond (RIE-C) using inductively coupled O2 plasma.
    
    f) shows opening of ground contact area on doped substrate and top electrode contact area on diamond membrane via reactive ion etching of silicon dioxide (RIE-SiO2) using CHF3/CF4 gas chemistry.
    
    a) shows aluminium deposited on top surface of 
    
    b) shows spray-coated photoresist layer on top surface of 
    
    c) shows patterned photoresist layer of 
    
    d) shows planar cross-sectional view of the final device having patterned aluminium layer (protected via patterned photoresist) via wet chemical etching, and removal of the patterned photoresist via oxygen plasma.
    
    a) is a graph showing the experimental and the theoretical deflection profiles of a CMUT with a nanocrystalline diamond membrane according to the invention.
    
    b) is a graph showing the experimental and the theoretical deflection profiles of a CMUT with a ultrananocrystalline diamond membrane according to the invention.
    
    a) is a graph of capacitance and resistance versus frequency for a CMUT according to the invention.
    
    b) is a graph showing the experimental and the theoretical deflection profiles versus bias voltage of a CMUT according to the invention.
    
    
    a) is a photo of aligned diamond-based CMUT and needle hydrophone in immersion. 2-D scan area in x and y coordinates are shown visually. Origin corresponds to the center of the CMUT.
    
    b) is a graph of measurement results of the normalized peak-to-peak pressure (in dB) for 2-D scan area. Theoretically calculated lines separating the main lobe and the side lobes are also shown with dotted lines on top of the measurement data.
    
    a) is a graph of experimental and theoretical results of the normalized peak-to-peak pressure on the normal of the CMUT surface.
    
    b) is a graph of experimental acoustic output pressure along the x-axis parallel to the CMUT surface at y=15 mm (Fresnel distance (S=1)), y=30 mm (S=2), and y=8.2 mm (S=0.5).
    
    c) is a graph of spectrum of the diamond-based CMUT with peak-to-peak AC amplitudes of 9 V, 36 V, and 54 V.
Although the following detailed description contains many specifics for the purposes of illustration, anyone of ordinary skill in the art will readily appreciate that many variations and alterations to the following exemplary details are within the scope of the invention.
Accordingly, the following preferred embodiment of the invention is set forth without any loss of generality to, and without imposing limitations upon, the claimed invention.
A CMUT cell produced according to the present invention is shown in 
The substrate electrode layer 102 can be n-doped or p-doped, using dopants such as phosphorus or boron respectively.
NCD consists of nanocrytalline diamond each of which having a grain size of 10 nm, whereas UNCD consists of ultrananocrystalline diamond each of which having a grain size of 3 to 5 nm.
During CMP, a reduction of 0.3 μm is sufficient to decrease the surface roughness of the intermediate layer 124 of HTO in 
The membrane electrode 156 and the substrate electrode connections 158 in 
The dimensions of the CMUT cell is determined according to the operational characteristics of the ultrasound transducer such as collapse voltage and center frequency.
The ratio of the thickness of the intermediate layer 144 to that of the diamond layer 142 cannot exceed 5 such that the behavior of the membrane is determined by the diamond layer 142. Said ratio is preferably 0.25.
Some dimensions have been marked on the CMUT cell depicted in 
For a CMUT cell according to the invention the above defined dimensions are
A CMUT producing ultrasound vibrations of a frequency of 1.74 MHz in air under a DC voltage of 100 V, fabricated according to the invention was used for testing purposes. The dimensions of each CMUT cell accordingly are
A single CMUT design in 
For the above mentioned CMUT, the method for microfabrication of a CMUT comprising a diamond membrane was performed through the steps:
1. preparation of the substrate by
2. preparation of the membrane by
3. assembling the membrane on the substrate, after activation of the respective surfaces with N2 plasma and at 550° C., under a vacuum of 10−4 mbar and a force of 10 kN for 7 hours, such that the intermediate layer 124 is facing cavities, by direct wafer bonding between the intermediate layer 124 and the cavity walls 114 as depicted in 
4. removing the membrane base wafer 118 by
5. and forming the membrane electrode 156 and the substrate electrode connections 158 by
During the deposition of HTO in step 2.b., SiH2Cl2 and N2O are employed. However, the N2O gas, being a strong oxidizer, can damage the diamond layer 120. Therefore this process is performed with a specific flow rate ratio of SiH2Cl2 to N2O equal to 1:2, leaving no excess N2O, whereas the conventional ratio is 1:5.
Removing of a membrane base wafer 118 of 500 μm solely by etching with tetramethylammonium hydroxide takes ten to twelve hours. Therefore the optional step 4.a. is incorporated thus decreasing the etching time to approximately two hours.
In an embodiment of the invention, the membrane electrode 156 consists of a titanium layer on the membrane to provide stiction, a platinum layer on said titanium layer to act as a diffusion barrier and a gold layer on said titanium layer.
The arrays of CMUT cells according to the invention can be of circular, polygonal or any other shape, and be arranged in various patterns by using masks of relevant shapes. Generally, the most efficient CMUT design, in terms of cells per area, would consist of regular hexagonal cells. Such an array with circular cells is depicted in 
The deflection profiles of two CMUTs fabricated according to the invention with membranes of NCD and UNCD are depicted in 
A CMUT having an inner radius of 2586 μm containing 1500 CMUT cells of a circular shape and a diameter of 120 μm was tested in air using a hydrophone. Capacitance and resistance of said CMUT was measured against a range of frequency, and the results are shown in 
A CMUT having an inner radius of 2586 μm containing 2708 CMUT cells of a circular shape and a diameter of 88 μm was tested in sunflower oil using a hydrophone as depicted in 
Various embodiments and applications employing the principles of the present invention can be implemented. Therefore the scope of the invention is not limited to the examples above but determined by the following claims.
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| Number | Date | Country | |
|---|---|---|---|
| 20120256517 A1 | Oct 2012 | US |