CN102353610A - Capacitance micro-machining ultrasonic sensor for measuring density and production method thereof - Google Patents
Capacitance micro-machining ultrasonic sensor for measuring density and production method thereof Download PDFInfo
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- CN102353610A CN102353610A CN2011101560609A CN201110156060A CN102353610A CN 102353610 A CN102353610 A CN 102353610A CN 2011101560609 A CN2011101560609 A CN 2011101560609A CN 201110156060 A CN201110156060 A CN 201110156060A CN 102353610 A CN102353610 A CN 102353610A
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Abstract
The invention provides a capacitance micro-machining ultrasonic sensor for measuring density and a production method thereof. The capacitance micro-machining ultrasonic sensor comprises a monocrystalline silicon substrate, a cavity formed by corrosion arranged on the monocrystalline silicon substrate, a first silica thin layer arranged on the upper end surface of the monocrystalline silicon substrate and sealing the cavity, a metal electrode layer formed by sputtering on the silica thin layer, and a silicon nitride thin layer and a second silica thin layer formed by successively etching on the metal electrode layer. The sensor disclosed herein has the characteristics of insulation, corrosion resistance and high temperature resistance, and can guarantee the reliability of CMUT in different measurement environments and the measurement precision.
Description
Technical field
The present invention relates to MEMS technology and liquid rerum natura parameter testing technical field, particularly a kind of electric capacity micromachined ultrasonic transducer that is used for density measure and preparation method thereof.
Background technology
At present, the liquid density sensor of technology maturation and widespread use mainly contains in actual measurement: oscillatory type, radioactive isotope formula, floatage-type, static pressure type, gravity type, velocity of sound formula etc.These traditional density sensors all have a common defective, promptly can not satisfy on-line measurement.When liquid density measurement, need to extract earlier sample off-line measurement again, but because test environment and the difference of actual condition at aspects such as temperature, pressure, can cause between measured value and the actual environment measured value of density existence than mistake.In addition, required sample was many when traditional density sensing was measured, if will obtain the Changing Pattern of testing liquid density under the different condition, just needed the multi-point sampling analysis, and workload is big, and length consuming time, efficient are low.In addition, traditional density sensor complex structure, volume is big, is not easy to carry, and is not suitable for the measurement of micro liquid density, and used sample liquids can not utilize mostly once more, and waste is serious.
In order to overcome the problems referred to above that traditional density sensor exists in measurement, domestic and international many scholars have carried out the research based on the miniature density sensor of MEMS (Micro Electro-Mechanical Systems is called for short MEMS) technology.There is a kind of rectangle silicon micro-cantilever vibratory drilling method to measure the sensor of fluid density, under the condition of 150 ℃ of high temperature, high pressure 68MPa, realizes that the measuring accuracy of density is ± 1% based on the MEMS technology; But, cause its sensitivity not high because the silicon micro-cantilever is a rectangular configuration; Simultaneously owing to adopting o, to such an extent as to the sensor bulk after the encapsulation is bigger as exciting device.
Except that above-mentioned microsensor based on the MEMS technology, capacitance type micromachined ultrasonic transducer (CMUTs) also is based on one of MEMS Study on Technology focus.CMUTs has that size is little, in light weight, electromechanical properties good (electromechanical coupling factor can reach 0.85), highly sensitive, bandwidth is wide (20kHz～2MHz), noise is low, operating temperature range is wide advantages such as (maximum operating temperature can reach 500 ℃).In addition, CMUT can make, form high density arrays in batches, is prone to be integrated on the same silicon chip with electronic component.Nowadays, CMUT successfully is used for medical imaging, nondestructive examination, object distance detection and fluid-velocity survey field, and ripe commercial product is arranged on market.The plurality of advantages of the above CMUT and successful Application experience thereof are that the research of electric capacity micromachined ultrasonic transducer aspect liquid density measurement provides advantage.
Summary of the invention
Technical matters to be solved by this invention provides little, highly sensitive, simple in structure, portative electric capacity micromachined ultrasonic transducer that is used for density measure of a kind of size and preparation method thereof, satisfies the requirement of on-line measurement density, and can realize trace measurement.
The present invention is used for the electric capacity micromachined ultrasonic transducer of density measure; Comprise the CMUT array element, this CMUT array element comprises silicon dioxide stress matching layer, silicon nitride dielectric layer, metal electrode, silica membrane and monocrystal silicon substrate from top to bottom successively, wherein; Metal electrode is a top electrode; Monocrystal silicon substrate is a bottom electrode, and said monocrystal silicon substrate is provided with cavity, and silica membrane seals cavity.
The useful area of said metal electrode is the half the of silica membrane useful area; The thickness of said silica membrane is less than 1 μ m; The thickness of said metal electrode is 0.5 μ m～2 μ m; The gross thickness of said silicon nitride dielectric layer and silicon dioxide stress matching layer is less than 1 μ m.
The preparation method that the present invention is used for the electric capacity micromachined ultrasonic transducer of density measure comprises: second monocrystalline silicon of getting heavily doped first monocrystalline silicon of n type < 111>crystal face boron ion and n type < 100>crystal face; On first monocrystalline silicon, adopt the plasma etching technology etched recesses; Form cavity, oxidation second monocrystalline silicon also descends the two sides to form silica membrane respectively above that; The upper surface of first and second monocrystalline silicon after step (1) handled carries out polishing, under the high-temperature vacuum environment, the polished surface of first and second monocrystalline silicon is carried out bonding then, and wherein second monocrystalline silicon is positioned at the top of first monocrystalline silicon; Adopt the plasma etching technology photoetching to fall the silicon dioxide layer on upper strata, erode the first half of second monocrystalline silicon then, only stay the silica membrane of second monocrystalline silicon below, be silica membrane; The sputter gold forms metal electrode after the etching on silica membrane; On the metal electrode after the etching, adopt low-pressure vapor phase deposition technology deposit silicon nitride insulation course and silicon dioxide stress matching layer successively, adopt plasma etching technology etching silicon dioxide stress matching layer and silicon nitride dielectric layer successively then, expose metal pad.
In step (3), the mass concentration that adopts heating when eroding the first half of second monocrystalline silicon is that 25% potassium hydroxide solution corrodes.
The electric capacity micromachined ultrasonic transducer that the present invention is used for density measure has the following advantages at least: at sensor of the present invention; Said silicon dioxide stress matching layer, silicon nitride dielectric layer, metal electrode and silica membrane form the vibration film of CMUT unit jointly; This structure has insulation, corrosion-resistant and realize the effect of thermal stress coupling simultaneously, can guarantee the reliability and the accuracy of sensor on-line measurement fluid density.Because during on-line measurement, fluid to be measured possibly or be a high-temp liquid etc. for electric conductivity or corrosive liquids, and this just requires sensor designed can prevent effectively that suchlike undesirable element is to the influence of measuring or reduce to its influence minimum.And in the present invention; Silicon dioxide and silicon nitride are insulativity and corrosion resistance material; The thermal expansivity of metal electrode, silicon nitride, silicon dioxide reduces successively simultaneously, in hot environment, can effectively realize the stress coupling, reduce the CMUT cellular construction distortion that is caused by thermal stress.Thereby sensor of the present invention has insulation, corrosion-resistant and resistance and high temperature resistance property simultaneously, can guarantee the reliability that CMUT works in the different measuring environment and the precision of measurement thereof.
Description of drawings
Fig. 1 is used for the structural representation of the electric capacity micromachined ultrasonic transducer of density measure for the present invention;
Fig. 2 is the section of structure of CMUT unit among Fig. 1;
Fig. 3 is the manufacturing process flow diagram of CMUT unit among Fig. 1;
Fig. 4 is the equivalent circuit diagram of CMUT unit among Fig. 1.
Label among the figure is represented as follows:
| 1 | |
2 | |
| 3 | |
4 | |
| 5 | Silicon nitride |
6 | Silicon dioxide stress matching |
| 8 | Voltage source | 9 | Divider resistance |
| 10 | Matching capacitance | 11 | The impedance bioelectrical measurement end |
Embodiment
Below in conjunction with accompanying drawing, to the present invention be used for density measure the electric capacity micromachined ultrasonic transducer (Capacitivemicrofabricated ultrasonic transducer, CMUT) and preparation method thereof do detailed description:
Electric capacity micro-machined ultrasonic density sensor of the present invention is used to measure the density of fluid, realize satisfying on-line measurement by trace measurement, and have that Measuring Time is short, precision is high, good operating stability, advantage that reliability is high.Said sensor comprises the CMUT array element; This CMUT array element comprises silicon dioxide stress matching layer 6, silicon nitride dielectric layer 5, metal electrode 4, silica membrane 3 and monocrystal silicon substrate 1 from top to bottom successively; Wherein, Metal electrode 4 is a top electrode, and monocrystal silicon substrate 1 is a bottom electrode, and said monocrystal silicon substrate is provided with cavity 2; Silica membrane 3 is cavity sealing, said silicon dioxide stress matching layer 6, silicon nitride dielectric layer 5, metal electrode 4 and the silica membrane 3 common vibration films that form the CMUT unit.
1.
The explanation of CMUT array
Referring to shown in Figure 1, wherein, 1 is monocrystal silicon substrate, is the basis of CMUT array.On the one hand, the silicon base corrosion forms cavity and bottom electrode; On the other hand, for the CMUT unit provides support and protects and is used to realize the electrical connection between the CMUT unit, its size can be confirmed according to the planform size of CMUT unit and the number of CMUT array.Vibration film is done mechanical vibration under the alternating voltage effect, produce ultrasound wave.Its rigidity of the thickness of film and effect length, and then the resonant frequency of decision CMUT unit, therefore the design through film thickness and length can be set in the natural reonant frequency of CMUT desired frequency range.Be used as bottom electrode with silicon pedestal in this embodiment; Top electrode forms through the gold of sputter on vibration film; Its surface area is the half the of film useful area; The thickness value should satisfy under the prerequisite of electromechanical conversion efficiency as far as possible more greatly, to reduce resistance in series, to cut down the consumption of energy, generally gets 1～2 μ m.
2.
The interlock circuit explanation
8 is voltage source, to said CMUT array AC signal is provided.CMUT of the present invention works under the working method of not subsiding, the amplitude of AC signal and bias voltage should try one's best near but all the time less than the voltage that subsides (the critical bias voltage between the CMUT upper/lower electrode that is added in when under the electrostatic attraction effect, making vibration film generation deformation touch bottom electrode).The magnitude of voltage that subsides can obtain according to relevant simulation software and experiment.9 is divider resistance, is mainly used in the magnitude of voltage of regulating in the array, in order to avoid voltage source directly acts on the CMUT unit, and with its damage, its resistance can adjust accordingly according to the impedance of applied voltage source and CMUT, and overall trend gets the small value.10 is matching capacitance, plays the logical effect that exchanges of stopping direct current, and its value should be as far as possible little under the situation that guarantees operate as normal, to reduce energy loss.11 is the impedance bioelectrical measurement end of CMUT; Confirm the electrical impedance smallest point of CMUT array in alternating voltage change of frequency process through electric impedance analyzer; And obtain inductance value in circuit this moment simultaneously, and then try to achieve fluid to be measured density through the funtcional relationship between fluid density and the inductance value.
3. working sensor principle
When the upper/lower electrode of CMUT array applies bias direct current voltage and alternating voltage; The CMUT film produces the vibration identical with a-c cycle in liquid; Because capillary effect; The solution layer that film surface adhered to also vibrates along with film together, and its result is equivalent to the increase of film quality, thereby changes the CMUTs resonant frequency.The density of solution is high more, and corresponding liquid layer quality is big more, and the equivalent mass increase of film is many more, and resonant frequency changes big more.The equivalent circuit diagram of CMUT is as shown in Figure 4, and wherein, m is film and the liquid layer quality sum that resonates with film, and k is the rigidity of sensor surface, and b is fluid damping, wherein R
s=b/N
u 2, C
s=N
u 2/ k, L
s=m/N
u 2, wherein, N
uBe dynamo-electric transformation efficiency.Change the frequency of input ac voltage, when CMUT resonated, its impedance was minimum, measured electric parameter (impedance Z, the resistance R of CMUT this moment
s, capacitor C
sAnd inductance L
s), according to the funtcional relationship ρ=CL of density and electric parameter
s+ D realizes the measurement of fluid density.ρ is a detected fluid density in the formula, and C and D are calibrating parameters, through measuring known fluid, can confirm its numerical value like the density of water, gasoline.
Structure below in conjunction with novel C MUT unit among 2 couples of the present invention of accompanying drawing describes:
1 is monocrystal silicon substrate; Monocrystalline silicon is formed by etching cavity 2; Directly with the bottom electrode of this monocrystalline silicon as the CMUT unit; In order to reduce in hot environment because of the influence of thermal stress to CMUT unit measurement stability, depositing insulating layer not on bottom electrode, but correspondingly change the security that cavity height and control bias voltage guarantee its work.2 is cavity, as hyperacoustic emissive source, for improving ultrasonic intensity, should increase cavity height, and the height of this embodiment cavity 2 is controlled at about 1 μ m.3 is silica membrane, directly influences resonant frequency and the electromechanical coupling factor of CMUT as its thickness of vibration film and geomery, and the thickness of silica membrane is less than 1 μ m in this embodiment, and width is less than 100 μ m.4 is metal electrode, forms through the plasma sputtering gold, and its area is the half the of film useful area, and for reducing resistance in series, its thickness should be slightly more greatly, and its span is 0.5 μ m～2 μ m.5,6 be respectively silicon nitride dielectric layer and silicon dioxide stress matching layer.On the one hand, the two is has good insulation properties and corrosion resistance material, satisfies the requirement of in electric conductivity and corrosive liquids, carrying out liquid density measurement.On the other hand; Reduce successively to its thermal expansivity of silicon dioxide from gold, silicon nitride, can realize the stress coupling when in hot environment, measuring, make CMUT minimum because of the thermal strain that temperature rise produces; Thereby the precision of measurement and reliability are effectively guaranteed; But consider that topmost thin film is more, should make the thickness of this double-layer films as far as possible little, the thickness sum of two membranes is controlled within 1 mu m range under this embodiment.The main structure parameters scope of novel C MUT unit is as follows:
● film effective width: 15 μ m～100 μ m
● overall film thickness: 1 μ m～4 μ m
● cavity height: 0.4 μ m～1.2 μ m
● metal electrode thickness: 0.5 μ m～2 μ m
● the CMUT array sizes of designing :≤1 * 5mm
2
The manufacturing process flow of novel C MUT unit among the present invention is described below in conjunction with Fig. 3:
(1) left side is heavily doped first monocrystalline silicon 11 of 4 inches n types < 111>crystal face boron ion, and resistivity is 0.01～0.02 Ω cm, and the right side is second monocrystalline silicon 13 of 4 inches n types < 100>crystal face, and resistivity is 10 Ω cm;
(2) first monocrystalline silicon 11 in plasma etching left side is made the array grooves, and second monocrystalline silicon 13 on oxidation right side also forms silica membrane 3 respectively at upper and lower surface;
(3) upper surface to first and second monocrystalline silicon 11,13 of both sides carries out chemically mechanical polishing;
(4) under the high-temperature vacuum environment, the polished surface of first and second monocrystalline silicon 11,13 of both sides is carried out bonding, wherein, second monocrystalline silicon is positioned at the top;
(5) silicon dioxide layer 3 on the employing plasma etching technology photoetching second monocrystalline silicon upper strata;
(6) using the mass concentration of heating is the monocrystalline silicon that 25% potassium hydroxide solution erodes second monocrystalline silicon, 13 upper stratas; The silica membrane that only keeps second monocrystalline silicon below; Form silica membrane, like this, first monocrystalline silicon 11 is monocrystal silicon substrate 1 of the present invention;
(7) sputter gold on silica membrane 3 forms metal electrode 4 after the etching;
(8) adopt low-pressure vapor phase deposition technology deposit silicon nitride insulation course 5 and silicon dioxide stress matching layer 6 on metal electrode 4 or silica membrane 3 successively; Adopt plasma etching technology etching silicon dioxide stress matching layer and silicon nitride dielectric layer successively then, expose metal pad.
When practical application, also need insulate and corrosion-resistance treatment, such as being coated in the silicon pedestal surface with insulating material to realize the insulation with conductive liquid to structures such as the exposed silicon pedestals, metal lead wire outside of CMUT array.Also need encapsulate one-piece construction, can design different encapsulating structures voluntarily according to reality.
The present invention is not limited to said embodiment, said CMUT array structure size, CMUT unit columns, distribution form; Film shape, the size of said CMUT unit, electrode shape, size, the size of cavity; Resistance value, capacitance all can adjust accordingly according to actual in the subsequent conditioning circuit, and its principle is to make electromechanical coupling factor height, the energy consumption of CMUT unit little.
The key technical indexes of the present invention is following:
● measuring media: Newtonian liquid
● density measure scope: 500Kgm
-3～1500Kgm
-3
● density measurement accuracy: be superior to 1%FS
● working temperature :-20 ℃～150 ℃
● environment static pressure :≤60MPa
In sum, sensor of the present invention has the following advantages:
(1) the present invention has designed the CMUT structure towards on-line measurement, has realized the on-line measurement of fluid density;
(2) workload is few when measuring, efficiency of measurement is high and the measurement result precision is high for sensor of the present invention;
(3) the present invention can be implemented in the density measure under the rugged surroundings, and like the measurement in the environment such as corrosivity, high temperature, applied range, stability and reliability are high;
(4) said CMUT cellular construction and manufacture craft thereof are simple, with short production cycle, efficient is high;
(5) the present invention realizes the microminiaturization of sensor, realizes the waste of trace measurement, minimizing fluid to be measured.
The above is merely one embodiment of the present invention; It or not whole or unique embodiment; The conversion of any equivalence that those of ordinary skills take technical scheme of the present invention through reading instructions of the present invention is claim of the present invention and contains.
Claims (7)
1. electric capacity micromachined ultrasonic transducer that is used for density measure; It is characterized in that: comprise the CMUT array element, this CMUT array element comprises silicon dioxide stress matching layer (6), silicon nitride dielectric layer (5), metal electrode (4), silica membrane (3) and monocrystal silicon substrate (1) from top to bottom successively, wherein; Metal electrode is a top electrode; Monocrystal silicon substrate is a bottom electrode, and said monocrystal silicon substrate is provided with cavity (2), and silica membrane (3) seals cavity.
2. the electric capacity micromachined ultrasonic transducer that is used for density measure as claimed in claim 1 is characterized in that: the useful area of said metal electrode (4) is the half the of silica membrane (3) useful area.
3. the electric capacity micromachined ultrasonic transducer that is used for density measure as claimed in claim 1 is characterized in that: the thickness of said silica membrane (3) is less than 1 μ m.
4. the electric capacity micromachined ultrasonic transducer that is used for density measure as claimed in claim 1 is characterized in that: the thickness of said metal electrode (4) is 0.5 μ m～2 μ m.
5. the electric capacity micromachined ultrasonic transducer that is used for density measure according to claim 1: it is characterized in that: the gross thickness of said silicon nitride dielectric layer (5) and silicon dioxide stress matching layer (6) is less than 1 μ m.
6. the described preparation method who is used for the electric capacity micromachined ultrasonic transducer of density measure of claim 1 is characterized in that: may further comprise the steps:
(1) gets second monocrystalline silicon of heavily doped first monocrystalline silicon of n type < 111>crystal face boron ion and n type < 100>crystal face; On first monocrystalline silicon, adopt the plasma etching technology etched recesses; Form cavity, oxidation second monocrystalline silicon also descends the two sides to form silica membrane respectively above that;
(2) upper surface of first and second monocrystalline silicon after step (1) is handled carries out polishing, under the high-temperature vacuum environment, the polished surface of first and second monocrystalline silicon is carried out bonding then, and wherein second monocrystalline silicon is positioned at the top of first monocrystalline silicon;
(3) adopt the plasma etching technology photoetching to fall the silicon dioxide layer on upper strata, erode the first half of second monocrystalline silicon then, only stay the silica membrane of second monocrystalline silicon below, be silica membrane;
(4) sputter gold on silica membrane forms metal electrode after the etching;
(5) on the metal electrode after the etching, adopt low-pressure vapor phase deposition technology deposit silicon nitride insulation course and silicon dioxide stress matching layer successively; Adopt plasma etching technology etching silicon dioxide stress matching layer and silicon nitride dielectric layer successively then, expose metal pad.
7. the preparation method who is used for the electric capacity micromachined ultrasonic transducer of density measure according to claim 1; It is characterized in that: in step (3), the mass concentration that adopts heating when eroding the first half of second monocrystalline silicon is that 25% potassium hydroxide solution corrodes.
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| CN102621036A (en) * | 2012-03-31 | 2012-08-01 | 西安交通大学 | Method for quickly measuring fluid density on line by adopting piezoresistive micro-cantilever beam |
| CN102620878A (en) * | 2012-03-15 | 2012-08-01 | 西安交通大学 | Capacitive micromachining ultrasonic sensor and preparation and application methods thereof |
| CN103196613A (en) * | 2013-03-15 | 2013-07-10 | 西安交通大学 | High-temperature CMUT pressure sensor and preparation method thereof |
| CN103217228A (en) * | 2013-03-15 | 2013-07-24 | 西安交通大学 | Temperature sensor based on capacitive micromachined ultrasonic transducer (CMUT) and preparation and application method of temperature sensor |
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| CN108982291A (en) * | 2018-07-09 | 2018-12-11 | 西安交通大学 | A kind of comb-tooth-type CMUTs fluid density sensor and preparation method thereof |
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| CN109502541A (en) * | 2018-12-17 | 2019-03-22 | 智驰华芯(无锡)传感科技有限公司 | A kind of piezoelectric mems ultrasonic sensor and its manufacturing method |
| CN109502541B (en) * | 2018-12-17 | 2023-10-10 | 智驰华芯(无锡)传感科技有限公司 | Piezoelectric MEMS ultrasonic sensor and manufacturing method thereof |
| CN110057907A (en) * | 2019-03-22 | 2019-07-26 | 天津大学 | A kind of CMUT and preparation method for gas sensing |
| CN110057907B (en) * | 2019-03-22 | 2021-11-23 | 天津大学 | CMUT (capacitive micromachined ultrasonic transducer) for gas sensing and preparation method |
| CN110570836A (en) * | 2019-09-24 | 2019-12-13 | 中北大学 | Ultrasonic transducer and preparation method thereof |
| CN110570836B (en) * | 2019-09-24 | 2021-11-19 | 中北大学 | Ultrasonic transducer and preparation method thereof |
| CN114620673A (en) * | 2022-03-18 | 2022-06-14 | 浙江仙声科技有限公司 | Ultrasonic transducer cell with CMUT combined with MEMS pressure sensor, array and manufacturing method |
| CN114620673B (en) * | 2022-03-18 | 2022-11-15 | 浙江仙声科技有限公司 | Ultrasonic transducer unit and array with CMUT combined with MEMS pressure sensor and manufacturing method |
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Application publication date: 20120215 |