# US 12,179,204 B2 · Sample well fabrication techniques and structures for integrated sensor

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- Number: US 12,179,204 B2
- Document ID: US12179204B2
- Status: Granted
- Kind: B2
- Application number: 16/580,877
- Filed: 2019-09-24
- Published: 2020-06-04
- Granted: 2024-12-31
- Earliest claimed: 2018-12-03
- Assignees: Quantum-Si Incorporated
- Applicants: Quantum-Si Incorporated
- Inventors: Guojun Chen; James Beach; Kathren Fink Croce; Jeremy Lackey; Gerard Schmid
- Web page: https://patentgrep.com/patent/US12179204B2

## CPC

- B01L 3/508: {Rigid containers without fluid transport within}
- B01L 3/5085: {for multiple samples, e.g. microtitration plates}
- G02B 6/132: by deposition of thin films
- G02B 6/136: by etching
- B01J 2219/00317: Microwell devices, i.e. having large numbers of wells
- B01J 2219/00621: by physical means, e.g. trenches, raised areas
- B01J 2219/00637: by coating it with another layer
- B01L 2200/12: Specific details about manufacturing devices
- B01L 2300/0636: Integrated biosensor, microarrays
- B01L 2300/0829: Multi-well plates; Microtitration plates
- B01L 2300/0851: Bottom walls
- B01L 2300/0858: Side walls
- B01L 2300/0887: Laminated structure
- B01L 2300/12: Specific details about materials
- G02B 2006/12138: {Sensor}
- B01L: CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- G02B: OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

A method of forming an integrated device includes forming a sample well within a cladding layer of a substrate; forming a sacrificial spacer layer over the substrate and into the sample well; performing a directional etch of the sacrificial spacer layer so as to form a sacrificial sidewall spacer on sidewalls of the sample well; forming, over the substrate and into the sample well, a functional layer that provides a location for attachment of a biomolecule; and removing the sacrificial spacer material.

## Claims

### Claim 1

A method of forming an integrated device, the method comprising:
forming a sample well within a cladding layer of a substrate;
forming a sacrificial spacer layer over the substrate and into the sample well;
performing a directional etch of the sacrificial spacer layer so as to form a sacrificial sidewall spacer on sidewalls of the sample well;
forming, over the substrate and into the sample well, a functional layer that comprises at least one functional moiety and provides a location for attachment of a biomolecule, wherein functional material of the functional layer bonds to sacrificial spacer material of the sacrificial spacer layer; and
after forming the functional layer, removing completely the sacrificial spacer material thereby removing the functional material bonded to the sacrificial spacer material, resulting in the functional layer disposed only on a bottom surface of the sample well.

### Claim 2 (depends on 1)

The method of claim 1, wherein the sacrificial spacer layer comprises Al2O3.

### Claim 3 (depends on 1)

The method of claim 1, wherein forming the sample well further comprises:
forming a metal stack on the cladding layer of the substrate;
forming an aperture in the metal stack;
forming a conformal spacer layer over the metal stack and into the aperture;
performing a directional etch of the conformal spacer layer so as to form protective sidewall spacers on an exposed sidewall of at least one metal layer of the metal stack; and
etching into the cladding layer.

### Claim 4 (depends on 3)

The method of claim 3, wherein the metal stack comprises at least one aluminum containing layer and at least one titanium containing layer.

### Claim 5 (depends on 3)

The method of claim 3, wherein the conformal spacer layer is formed by plasma enhanced chemical vapor deposition (PECVD).

### Claim 6 (depends on 5)

The method of claim 5, wherein the conformal spacer layer is selected from the group of: amorphous silicon (α-Si), SiO2, SiON, and SiN.

### Claim 7 (depends on 3)

The method of claim 3, wherein the conformal spacer layer is formed by atomic layer deposition (ALD).

### Claim 8 (depends on 7)

The method of claim 7, wherein the conformal spacer layer is selected from the group of: TiO2, Al2O3, SiO2, and HfO2.

### Claim 9 (depends on 1)

The method of claim 1, wherein the functional layer comprises biotin functional sites for attachment of a streptavidin-labeled biomolecule.

### Claim 10 (depends on 1)

The method of claim 1, wherein the functional layer comprises an intermediate coupling agent for subsequent attachment of a biotin functional site.

### Claim 11 (depends on 10)

The method of claim 10, wherein the intermediate coupling agent comprises an alkyne coupling agent for attachment of a biotin-azide.

### Claim 12 (depends on 10)

The method of claim 10, wherein the intermediate coupling agent comprises an isocyanate coupling agent for attachment of a biotin-thiol.

### Claim 13 (depends on 10)

The method of claim 10, wherein the intermediate coupling agent comprises an epoxy coupling agent for attachment of a biotin-thiol.

### Claim 14 (depends on 1)

The method of claim 1, wherein the functional layer is selected to facilitate biotin-silane bonding directly to material of the cladding layer.

### Claim 15 (depends on 1)

The method of claim 1, wherein the functional layer comprises more than one component, with at least one component selected to provide antifouling properties for a bottom surface of the sample well.

### Claim 16 (depends on 1)

The method of claim 1, further comprising using a silane chemistry to attach the functional layer to an exposed bottom surface of the sample well.

### Claim 17 (depends on 16)

The method of claim 16, wherein the silane chemistry comprises an alkoxysilane chemistry configured to obtain selective attachment to SiO2 surfaces relative to metal oxide surfaces.

### Claim 18 (depends on 17)

The method of claim 17, further comprising the functional layer using a liquid phase process.

### Claim 19 (depends on 17)

The method of claim 17, further comprising the functional layer using a vapor phase process.

### Claim 20 (depends on 1)

The method of claim 1, further comprising forming an antifouling film over the substrate and into the sample well.

### Claim 21

An integrated device, comprising:
a cladding layer;
a metal stack formed on the cladding layer, the metal stack having a first metal layer and a second metal layer;
a sample well formed through the metal stack and into at least a portion of the cladding layer, the sample well having sidewalls and a bottom surface comprising a same material;
an encapsulating spacer material filling an undercut region of at least one of the first and second metal layers, wherein the sample well is completely free of any spacer material on all exposed surfaces of the sidewalls; and
a biotin functional moiety selectively formed only on the bottom surface of the sample well, wherein the biotin functional moiety is configured for attachment of a biomolecule thereto and the sample well is completely free of any functional material on all exposed surfaces of the sidewalls.

### Claim 22 (depends on 21)

The device of claim 21, wherein the metal stack comprises at least one aluminum containing layer and at least one titanium containing layer.

### Claim 23 (depends on 21)

The device of claim 21, wherein the encapsulating spacer material is selected from the group of: amorphous silicon (α-Si), SiO2, SiON, and SiN.

### Claim 24 (depends on 21)

The device of claim 21, wherein the encapsulating spacer material is selected from the group of: TiO2, Al2O3, SiO2, and HfO2.

### Claim 25 (depends on 21)

The device of claim 21, wherein the biotin functional moiety is configured for attachment of a streptavidin-labeled biomolecule.

### Claim 26 (depends on 21)

The device of claim 21, wherein the biotin functional moiety comprises an intermediate coupling agent for subsequent attachment of a biotin functional site.

### Claim 27 (depends on 26)

The device of claim 26, wherein the intermediate coupling agent comprises an alkyne coupling agent for attachment of a biotin-azide.

### Claim 28 (depends on 26)

The device of claim 26, wherein the intermediate coupling agent comprises an isocyanate coupling agent for attachment of a biotin-thiol.

### Claim 29 (depends on 26)

The device of claim 26, wherein the intermediate coupling agent comprises an epoxy coupling agent for attachment of a biotin-thiol.

### Claim 30 (depends on 21)

The device of claim 21, wherein the biotin functional moiety is bonded directly to material of the cladding layer.

### Claim 31 (depends on 21)

The device of claim 21, wherein a functional layer used to form the biotin functional moiety comprises more than one component, with at least one component selected to provide antifouling properties for the bottom surface of the sample well.

### Claim 32 (depends on 21)

The device of claim 21, further comprising an antifouling film formed over the substrate and into the sample well.