# US 11,079,353 B2 · Method and sensor for detecting l-cysteine based on 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane

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- Number: US 11,079,353 B2
- Document ID: US11079353B2
- Status: Granted
- Kind: B2
- Application number: 16/955,797
- Filed: 2019-08-24
- Published: 2021-01-28
- Granted: 2021-08-03
- Earliest claimed: 2018-09-17
- Assignees: Changsha University of Science and Technology
- Applicants: Changsha University of Science and Technology
- Inventors: Zhong Cao; Yuyu Peng; Chen Liu; Ling Tang; Qin Zhu; Min Jin; Jinglin He; Zhongliang Xiao
- Web page: https://patentgrep.com/patent/US11079353B2

## CPC

- G01N 27/4145: {specially adapted for biomolecules, e.g. gate electrode with immobilised receptors}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

A method and a sensor for detecting L-cysteine based on a 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane are provided. The method includes: implanting a p-well and an N-type substrate on field effect transistor substrate, constructing a source electrode and a drain electrode at the p-well, constructing a silicon dioxide layer on the substrate, plating an aluminum-copper alloy layer, a chromium-palladium alloy layer, and a gold film layer on a polysilicon gate substrate, constructing a silicon nitride layer on the substrate and the silicon dioxide layer; extending a gate part; preparing an ethanol solution of disodium 3,3′-dithiobis (1-propanesulfonate), cleaning and soaking gate gold electrode in the solution, followed by soaking in an ethanol solution of mercuric nitrate, and then washing the gate gold electrode; connecting electrode interfaces, inserting the electrode into PBS, and connecting power interfaces to a stabilized voltage supply, connecting a signal output interface to a multimeter.

## Claims

### Claim 1

A method for detecting L-cysteine based on a 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane, comprising the following steps:
(1) implanting a p-well and an N-type substrate on a Si substrate of a field effect transistor, constructing a source electrode and a drain electrode at the p-well by a thermal evaporation and a magnetron sputtering, then constructing a silicon dioxide layer on the Si substrate after being implanted with the p-well and the N-type substrate and constructed with the source electrode and the drain electrode, followed by successively plating an aluminum-copper alloy layer, a chromium-palladium alloy layer and a gold film layer on a substrate of a polysilicon gate by the thermal evaporation and the magnetron sputtering, and next, constructing a silicon nitride layer on the substrate of the polysilicon gate and the silicon dioxide layer; subsequently, extending a gate part of the polysilicon gate by a distance of 0.1-500 mm to obtain an extended gate field effect transistor with a gate gold electrode;
(2) preparing an ethanol solution of disodium 3,3′-dithiobis (1-propanesulfonate), cleaning the gate gold electrode of the extended gate field effect transistor, soaking the gate gold electrode of the extended gate field effect transistor in the ethanol solution of disodium 3,3′-dithiobis (1-propanesulfonate) in a dark and dry environment, and putting the ethanol solution of disodium 3,3′-dithiobis (1-propanesulfonate) aside at 25° C., then taking out and washing the gate gold electrode of the extended gate field effect transistor, followed by soaking the gate gold electrode of the extended gate field effect transistor in an ethanol solution of mercuric nitrate, putting the ethanol solution of mercuric nitrate aside, and then washing the gate gold electrode of the extended gate field effect transistor after being soaked to obtain a 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane gate gold electrode modified by a 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane; and
(3) connecting an electrode interface of a reference electrode, an electrode interface of the 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane gate gold electrode, and an electrode interface of the extended gate field effect transistor to form a differential amplifier circuit with a high input impedance, inserting the reference electrode and the 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane gate gold electrode into a phosphate buffer solution (PBS), and connecting power interfaces of the extended gate field effect transistor to positive and negative poles of a stabilized voltage supply, respectively, connecting a signal output interface of the extended gate field effect transistor to a test port of a multimeter to form a complete sensing detection circuit; wherein a potential change of a system is detected sensitively by using an in-situ signal amplification of the extended gate field effect transistor; potential of the 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane gate gold electrode as a working electrode tends to be stable with an increase of time in the PBS, and after the potential is stable, samples to be tested containing different concentrations of L-cysteine are added, and then corresponding potential response data corresponding to the samples to be tested are obtained to complete a detection of L-cysteine in the samples to be tested.

### Claim 2 (depends on 1)

The method according to claim 1, wherein, in step (1), during successively plating the aluminum-copper alloy layer, the chromium-palladium alloy layer, and the gold film layer on the substrate of the polysilicon gate by the thermal evaporation and the magnetron sputtering, a plating vacuum degree is less than or equal to 5.0×10−6 torr, a plating speed is less than or equal to 2.0 Å/s, and a passivation is carried out with Si3N4; the aluminum-copper alloy layer includes the following components by weight: 40-68 parts of Al, 30-60 parts of Cu, 2-12 parts of Ni, 1-8 parts of Fe, 1-6 parts of Ti, and 0.01-0.50 parts of Nb; the chromium-palladium alloy layer includes the following components by weight: 40-80 parts of Cr, 10-40 parts of Pd, 2-12 parts of Ni, 1-8 parts of Fe, 1-6 parts of Ti, and 0.01-0.50 parts of Nb; a thickness of the aluminum-copper alloy layer is 20-600 nm, a thickness of the chromium-palladium alloy layer is 20-600 nm, and a thickness of the gold film layer is 20-1000 nm.

### Claim 3 (depends on 1)

The method according to claim 1, wherein, in step (2), a concentration of the ethanol solution of disodium 3,3′-dithiobis (1-propanesulfonate) is 1.0-10.0 mmol/L; in the ethanol solution of mercuric nitrate, a volume ratio of a mercuric nitrate aqueous solution to anhydrous ethanol is 1:1, and a concentration of the mercuric nitrate aqueous solution is 0.1-50.0 mmol/L.

### Claim 4 (depends on 1)

The method according to claim 1, wherein, in step (2), the gate gold electrode of the extended gate field effect transistor is soaked in the ethanol solution of disodium 3,3′-dithiobis (1-propanesulfonate) for 1-72 h, and soaked in the ethanol solution of mercuric nitrate for 1-72 h.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the reference electrode in step (3) is a saturated calomel electrode or an Ag/AgCl electrode integrated with a saturated KCl solution, and the working electrode is the 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane gate gold electrode.

### Claim 6 (depends on 1)

The method according to claim 1, wherein, in step (3), the PBS has a pH value of 3.0-11.0 and a concentration of 0.1 mol/L.

### Claim 7

A sensor for detecting L-cysteine, comprising a field effect transistor, wherein the field effect transistor is provided with an extended gate gold electrode; in the extended gate gold electrode, a gate part is extended by 0.1-500 mm, and a surface of a gold film layer of the extended gate gold electrode is assembled with a 3,3′-dithiobis (1-propanesulfonate)-mercury composite membrane.

### Claim 8 (depends on 7)

The sensor according to claim 7, wherein the field effect transistor comprises a Si substrate and a polysilicon gate provided on the Si substrate, a p-well and an N type substrate are implanted on the Si substrate, and a source electrode and a drain electrode are provided at the p-well, a silicon dioxide layer is provided on the Si substrate after being implanted with the p-well and the N-type substrate and constructed with the source electrode and the drain electrode, a substrate of the polysilicon gate is successively plated with an aluminum-copper alloy layer, a chromium-palladium alloy layer, and a gold film layer, and a silicon nitride layer is provided on the substrate of the polysilicon gate and the silicon dioxide layer.

### Claim 9 (depends on 8)

The sensor according to claim 8, wherein a thickness of the aluminum-copper alloy layer is 20-600 nm, a thickness of the chromium-palladium alloy layer is 20-600 nm, and a thickness of the gold film layer is 20-1000 nm.

### Claim 10 (depends on 7)

The sensor according to claim 7, wherein the sensor has an ultra Nernst response to L-cysteine with a linear range of 1.0×10−7-1.0×10−4 mol/L, a response sensitivity of 123.4 mV·pc−1, and a detection limit of 8.32×10−8 mol/L.

### Claim 11 (depends on 8)

The sensor according to claim 8, wherein the sensor has an ultra Nernst response to L-cysteine with a linear range of 1.0×10−7-1.0×10−4 mol/L, a response sensitivity of 123.4 mV·pc−1, and a detection limit of 8.32×10−8 mol/L.

### Claim 12 (depends on 9)

The sensor according to claim 9, wherein the sensor has an ultra Nernst response to L-cysteine with a linear range of 1.0×10−7-1.0×10−4 mol/L, a response sensitivity of 123.4 mV·pc−1, and a detection limit of 8.32×10−8 mol/L.