# US 10,319,553 B2 · Method for controllably growing ZnO Nanowires

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- Number: US 10,319,553 B2
- Document ID: US10319553B2
- Status: Granted
- Kind: B2
- Application number: 16/084,433
- Filed: 2017-03-14
- Published: 2019-03-14
- Granted: 2019-06-11
- Earliest claimed: 2016-03-16
- Assignees: Lightlab Sweden AB
- Applicants: Lightlab Sweden AB
- Inventors: Jonas Tirén; Jan-Otto Carlsson; Helena Tenerz; Patrik Hollman
- Web page: https://patentgrep.com/patent/US10319553B2

## CPC

- H01J 9/025: {of field emission cathodes}
- H10P 14/203: {using transformation of metal, e.g. oxidation or nitridation}
- H10P 14/3426: {Oxides}
- H10P 14/3462: {Nanowires}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- H01J 63/06: Lamps with luminescent screen excited by the ray or stream
- H01J 2201/30415: needle shaped
- H01J 2201/30446: characterised by the emitter material
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

The present invention relates to a method for controllably growing ZnO nanowires, for example to be used in relation to field emission lighting. In particular, the invention relates to a method of controlling thermal oxidation conditions to achieve steady-state conditions between an oxygen consumption rate by a growing oxide on a surface of a structure and the decomposition rate of the oxygen-carrying species within the chamber. The invention also relates to a corresponding field emission cathode.

## Claims

### Claim 1

A method for controllably growing zinc oxide (ZnO) nanowires on a surface of a structure by means of thermal oxidation, the structure comprising a zinc layer covering at least a portion of the structure, the method comprising:
arranging the structure within a thermal oxidation chamber, the chamber having a gas inlet and a gas outlet for allowing a gas flow through the chamber;
providing a gas comprising an oxygen-carrying precursor through the gas inlet of the chamber; and
controlling a concentration of oxygen along the surface of the structure by:
controlling a temperature within the chamber; and
controlling a gas flow of the gas comprising the oxygen-carrying precursor through the chamber,
such that steady-state conditions are achieved between an oxygen consumption rate by a growing oxide on the surface of the structure and the decomposition rate of the oxygen-carrying species within the chamber, thereby maintaining the same zinc oxidation conditions along the surface of the structure within the chamber.

### Claim 2 (depends on 1)

The method according to claim 1, wherein said gas comprises a plurality of oxygen carrying precursors.

### Claim 3 (depends on 1)

The method according to claim 1, further comprising controlling a gas pressure to provide substantially uniform growth conditions at the entire surface of the structure, at a given time.

### Claim 4 (depends on 1)

The method according to claim 1, further comprising controlling the gas flow such that a resulting concentration of oxygen is substantially uniform for the entire surface of the structure.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the oxygen-carrying precursor is selected from a group comprising of O2, CO2, N2O and H2O.

### Claim 6 (depends on 1)

The method according to claim 1, further comprising selecting a concentration of the oxygen precursor of the gas provided to the chamber.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the gas is a gas mixture further comprising at least one of nitrogen and argon.

### Claim 8 (depends on 1)

The method according to claim 1, wherein the temperature is controlled according to a predetermined temperature curve.

### Claim 9 (depends on 8)

The method according to claim 8, wherein the temperature curve is selected based on a decomposition rate of the oxygen-carrying precursor.

### Claim 10 (depends on 8)

The method according to claim 8, wherein the temperature curve comprises ramping up the temperature to an oxidation temperature using a fixed ramp, maintaining the oxidation temperature for a predetermined time, and ramping down the temperature using a fixed ramp.

### Claim 11 (depends on 8)

The method according to claim 8, wherein the temperature curve comprises:
ramping up the temperature to a first oxidation temperature using a first ramp rate;
performing thermal oxidation starting at the first oxidation temperature for a first period of time to form an initial oxide layer;
ramping up the temperature to a second oxidation temperature using a second ramp rate;
performing thermal oxidation at the second oxidation temperature for a predetermined period of time to initialize and to maintain nanowire growth;
ramping up the temperature to a third oxidation temperature using a third ramp rate and performing thermal oxidation during the temperature ramp to grow nanowires; and
when the third oxidation temperature is reached, ramping down the temperature to end the oxidation using a fourth ramp rate.

### Claim 12 (depends on 11)

The method according to claim 11, further comprising, when the third oxidation temperature is reached, ramping the temperature up or down to a fourth temperature using a fourth temperature ramp, and maintaining the fourth temperature for a predetermined period of time, before ramping down the temperature to end the oxidation using a fifth ramp rate.

### Claim 13 (depends on 1)

The method according to claim 1, wherein the third oxidation temperature within the chamber is equal to or lower than 625° C.

### Claim 14 (depends on 1)

The method according to claim 1, wherein a pressure within the chamber is a maximum of 1 atm.

### Claim 15 (depends on 1)

The method according to claim 1, further comprising:
preparing the structure by applying a predetermined thickness of a ZnO layer to the surface of the structure.

### Claim 16 (depends on 1)

The method according to claim 1, wherein the structure comprises at least one of copper and brass.

### Claim 17 (depends on 1)

The method according to claim 1, wherein the structure comprises a wire, a mesh or a plate.

### Claim 18 (depends on 1)

The method according to claim 1, wherein a length of the ZnO nanowires is selected to be between 2-100 um.

### Claim 19 (depends on 1)

The method according to claim 1, wherein a diameter of the ZnO nanowires is selected to be between 5-100 nm.

### Claim 20 (depends on 1)

A field emission light source comprising a structure provided with ZnO nanowires grown according to claim 1.

### Claim 21 (depends on 19)

The field emission light source according to claim 19, wherein the field emission light source is a UV light source.
