# US 11,305,253 B2 · High surface area coatings for solid-phase synthesis

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- Number: US 11,305,253 B2
- Document ID: US11305253B2
- Status: Granted
- Kind: B2
- Application number: 16/597,799
- Filed: 2019-10-09
- Published: 2021-04-15
- Granted: 2022-04-19
- Earliest claimed: 2019-10-09
- Assignees: Microsoft Technology Licensing, LLC
- Applicants: Microsoft Technology Licensing, LLC
- Inventors: Bichlien Hoang Nguyen; Karin Strauss; Hsing-Yeh Parker
- Web page: https://patentgrep.com/patent/US11305253B2

## CPC

- B01J 19/0046: {Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays (synthesis methods per se C40B50/00)}
- C07K 1/042: {characterised by the nature of the carrier}
- C25D 5/16: Electroplating with layers of varying thickness
- C25D 5/48: After-treatment of electroplated surfaces
- C25D 17/10: Electrodes {, e.g. composition, counter electrode}
- B01J 2219/0059: Sequential processes
- B01J 2219/00497: Features relating to the solid phase supports
- B01J 2219/00596: Solid-phase processes
- B01J 2219/00612: the surface being inorganic
- B01J 2219/00722: Nucleotides
- B01J 2219/00725: Peptides
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C07K: PEPTIDES (peptides in foodstuffs A23; obtaining protein compositions for foodstuffs, working-up proteins for foodstuffs A23J; preparations for medicinal purposes A61K; peptides containing beta-lactam rings C07D; cyclic dipeptides not having in their molecule any other peptide link than those which form their ring, e.g. piperazine-2,5-diones, C07D; ergot alkaloids of the cyclic peptide type C07D519/02; macromolecular compounds having statistically distributed amino acid units in their molecules, i.e. when the preparation does not provide for a specific; but for a random sequence of the amino acid units, homopolyamides and block copolyamides derived from amino acids C08G69/00; macromolecular products derived from proteins C08H1/00; preparation of glue or gelatine C09H; single cell proteins, enzymes C12N; genetic engineering processes for obtaining peptides C12N15/00; compositions for measuring or testing processes involving enzymes C12Q; investigation or analysis of biological material G01N33/00)
- C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR

## Abstract

High surface area coatings are applied to solid substrates to increase the surface area available for solid-phase synthesis of polymers. The high surface area coatings use three-dimensional space to provide more area for functional groups to bind polymers than an untreated solid substrate. The polymers may be oligonucleotides, polypeptides, or another type of polymer. The solid substrate is a rigid supportive layer made from a material such as glass, a silicon material, a metal material, and plastic. The coating may be thin films, hydrogels, microparticles. The coating may be made from a metal oxide, a high-κ dielectric, a low-κ dielectric, an etched metal, a carbon material, or an organic polymer. The functional groups may be hydroxyl groups, amine groups, thiolate groups, alkenes, n-alkenes, alkalines, N-Hydroxysuccinimide (NHS)-activated esters, polyaniline, aminosilane groups, silanized oxides, oligothiophenes, and diazonium compounds. Techniques for applying coatings to solid substrates and attaching functional groups are also disclosed.

## Claims

### Claim 1

A stack for solid-phase polymer synthesis comprising:
a solid substrate;
a coating that has a three-dimensional structure which increases available surface area relative to the solid substrate, the coating covering at least a portion of the solid substrate;
a second coating which further increases the available surface area relative to the coating, wherein the second coating comprises microparticles baked into a porous coating; and
a functional group attached to the coating.

### Claim 2 (depends on 1)

The stack of claim 1, further comprising a polymer covalently bound to the functional group, wherein the polymer is comprised of an oligonucleotide or a polypeptide.

### Claim 3 (depends on 1)

The stack of claim 1, wherein the solid substrate comprises a silicon material, a metal material, or a plastic.

### Claim 4 (depends on 1)

The stack of claim 1, wherein the coating comprises a metal oxide, an etched metal, a high-κ dialectric, a low-κ dialectric, a carbon material, or an organic polymer.

### Claim 5 (depends on 1)

The stack of claim 1, wherein a structure of the coating is a thin film, a hydrogel, or a microparticle.

### Claim 6 (depends on 1)

The stack of claim 1, wherein the functional group comprises a hydroxyl group, an amine group, a thiolate group, an alkene, a n-alkene, an alkaline, a N-Hydroxysuccinimide (NHS)-activated ester, polyaniline, a silanized oxide, an oligothiophene, or a diazonium compound.

### Claim 7

A stack for solid-phase polymer synthesis comprising:
a silicon substrate patterned with a noble metal;
a coating that has a three-dimensional structure with an available surface area that is greater than the silicon substrate, the coating selected from the group comprising silicon dioxide, silicon dioxide microparticles, aluminum oxide, porous anodic aluminum oxide (AAO), and agarose, wherein the coating covers the silicon substrate and does not cover the noble metal; and
a functional group present on the coating, the functional group selected from the group comprising an aminosilane group and a hydroxyl group.

### Claim 8 (depends on 7)

The stack of claim 7, wherein the coating comprises the porous AAO and the functional group comprises the aminosilane group.

### Claim 9 (depends on 7)

The stack of claim 7, wherein the coating comprises silicon dioxide microparticles and the functional group comprises the aminosilane group.

### Claim 10 (depends on 7)

The stack of claim 7, wherein the coating comprises agarose and the functional group comprises the hydroxyl group present on the agarose as a free hydroxyl group.

### Claim 11

A method of making a stack for solid-phase polymer synthesis comprising:
sputtering an aluminum coating on to a solid substrate;
electrochemically etching the aluminum coating to create porous AAO, the coating having an available surface area that is greater than the solid substrate; and
functionalizing the coating with a functional group that forms a covalent bond to a monomer subunit of a polymer.

### Claim 12 (depends on 11)

The method of claim 11, further comprising patterning the solid substrate with a metal or a semiconductor.

### Claim 13 (depends on 11)

The method of claim 11, wherein the functionalizing the coating comprises silanization, chemical grafting, electro-grafting, photochemical grafting, or electrochemical polymerization.

### Claim 14 (depends on 11)

The method of claim 11, further comprising, depositing a second coating on the coating, the second coating having an available surface area that is greater than the coating.

### Claim 15 (depends on 14)

The method of claim 14, wherein the second coating comprises nanoparticles.

### Claim 16 (depends on 13)

The method of claim 13, wherein functionalizing the coating comprises silanization by submersion in 3-aminopropyltriethoxysilane in ethanol.

### Claim 17 (depends on 1)

The stack of claim 1, wherein the functional group is also attached to the second coating.

### Claim 18 (depends on 1)

The stack of claim 1, wherein the second coating comprises silicon dioxide nanoparticles baked into a porous silicon dioxide coating.

### Claim 19 (depends on 1)

The stack of claim 1, wherein the wherein the microparticles comprise silicon dioxide microparticles.

### Claim 20 (depends on 1)

The stack of claim 1, wherein the microparticles are nanoparticles.