Stoichiometric TiN Thin Films High-Temperature Sputtering

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Solution Overview

Problem

Existing thin film titanium nitride (TiN) coatings are not stable at temperatures higher than 100°C, and most studies on their electrical resistivity are conducted below this temperature range, limiting their application in high-temperature devices such as thermoelectric devices and electronics in harsh environments.

Innovation Solution

Sputtered stoichiometric TiN thin films are produced at high substrate temperatures (up to 800°C) and/or annealed at high temperatures, using a magnetron sputtering system with controlled argon and nitrogen gas flows, presputtering, and a thin adhesion layer to ensure nitrogen saturation and stability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If TiN films are deposited at low substrate temperature (room temperature), then deposition process is simple and fast, but the films exhibit poor thermal stability and non-linear resistivity above deposition temperature

Engineering Contradiction:
Improvethermal stabilityVSAvoiddeposition process complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The substrate is pre-heated to high temperature (up to 800°C) before deposition begins. This preliminary thermal preparation enables the TiN films to achieve stable crystalline structure and linear resistivity characteristics from the start, eliminating the need for post-deposition annealing and ensuring thermal stability above 100°C

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The substrate temperature parameter is changed from room temperature to high temperature (up to 800°C) during deposition. This parameter change fundamentally alters the film formation process, resulting in TiN films with enhanced thermal stability, linear resistivity-temperature relationship, and suitability for high-temperature applications

Inventive Principle:
Principle #35Parameter changes

2Reliability

If TiN films are annealed at high temperature to improve stability, then thermal stability improves, but the deposition and processing time increases

Engineering Contradiction:
Improvethermal stabilityVSAvoidprocessing time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The desired crystalline structure and stoichiometry are achieved during the deposition process itself by maintaining high substrate temperature (up to 800°C). This preliminary formation of stable structure eliminates the need for separate post-deposition annealing steps, reducing total processing time while ensuring thermal stability

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The deposition and annealing processes are merged into a single high-temperature deposition step. By combining structure formation and thermal stabilization into one process, the patent eliminates the sequential deposition-then-anneal workflow, reducing processing time while achieving both low resistivity and thermal stability

Inventive Principle:
Principle #5Merging (Combining)

3Ease of manufacture

If conventional sputtering methods are used, then deposition is straightforward, but the films show non-linear resistivity above deposition temperature

Engineering Contradiction:
Improvedeposition easeVSAvoidresistivity stability
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The substrate temperature parameter is elevated to high values (up to 800°C) during sputtering. This parameter change transforms the film properties, ensuring linear resistivity-temperature relationship and eliminating the non-linear behavior that occurs in conventionally deposited films when temperature exceeds deposition temperature

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The substrate is maintained at uniformly high temperature throughout the deposition process. This localized thermal condition ensures consistent atomic mobility and film formation across the entire substrate surface, resulting in uniform resistivity characteristics and linear temperature dependence throughout the film

Inventive Principle:
Principle #3Local quality

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The resulting TiN films exhibit excellent long-term high-temperature thermal stability, low resistivity, and a high temperature coefficient of resistivity, making them suitable for high-temperature applications like thermoelectric devices and resistive temperature sensors up to 600°C.

Implementation Method 1

Sputtered stoichiometric TiN thin films are produced at high substrate temperatures (up to 800°C) and/or annealed at high temperatures, using a magnetron sputtering system

Methodology Applied
Scientific EffectSputtering: Sputtering

Implementation Method 2

presputtering

Methodology Applied
Scientific EffectSputtering: Sputtering

Implementation Method 3

annealed at high temperatures

Methodology Applied
Scientific EffectAnnealing: Annealing

Data Source

PatentUS11072848B2High temperature sputtered stoichiometric titanium nitride thin films
Publication Date: 2021.07.27 THE GOVERNMENT OF THE UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY DEPARTMENT OF HEALTH & HUMAN SERVICES
  • US11072848B2 patent drawing
  • US11072848B2 patent drawing
  • US11072848B2 patent drawing

AI summary

A method for producing high-temperature sputtered stoichiometric TiN thin films. A substrate is placed in a sputtering chamber a Ti target to be sputtered and the substrate temperature is controlled to be between room temperature and about 800° C. The sputtering chamber is evacuated to a base pressure of 2×10−7 Torr or lower, The Ti target is presputtered under an Ar gas flow at a pressure of 2-15 mTorr in a radio frequency (RF) power of 50-200 W. The Ti is then sputtered onto the substrate in the presence of N2 and Ar gas flows under the same pressure and RF power, with the ratio of N2 to Ar favoring N to ensure that the film is nitrogen-saturated.