CN100560525C - The method of depositing TiN thin film on glass substrate - Google Patents

Abstract

The invention discloses the method for depositing TiN thin film on glass substrate, what adopt is chemical Vapor deposition process, by the shower nozzle in conditioned reaction gas inlet pipe road and the distance between glass substrate, realize that control is deposited on the resistivity of TiN film on the glass substrate and surface topography, optical property etc.The performance technologies such as resistivity that the inventive method is controlled film than traditional flow that passes through conditioned reaction temperature and reactant are simple, easily row.

Description

The method of depositing TiN thin film on glass substrate

Technical field

The present invention relates to a kind of on glass substrate the method for depositing TiN thin film.

Background technology

Along with global science and technology and economic fast development, the consumption of the energy is day by day significantly increased, make problem of energy crisis become increasingly conspicuous, energy-conservationly caused the extensive concern of countries in the world as a national strategy problem.And the development of Building technology makes that the shared under construction ratio of glass is increasing, even some Highrise buildings adopted the structure of full glass outer wall, in the hope of obtaining the modern architecture aesthetic effect of elegance attractive in appearance.Common flint glass is a kind of good material of construction, do window with it, both beautiful and practical, can see through about 90% solar radiation, but when it sees through visible light, also seen through near infrared ray and mid and far infrared line part, the transmissison characteristic that this nothing is selected makes simple glass become the main source of leaks of building energy consumption.

In order to reduce the energy loss that causes because big area adopts glass in the modern architecture industry, develop and a kind ofly plate one deck functional materials film in surface of ordinary glass, make glass can absorb selectively or reflect to visible region in the solar radiation and infrared region, be called low radiation film glass, the then corresponding low radiation film that is called of functional materials film on glass through the glass after this kind processing.

The TiN film makes it can be used to the low radiation film glass art because its distinctive photoelectric properties have high transmittance and near infrared region higher reflectivity arranged at visible region.The optical property of TiN film is closely related with its electric property, in the process that adopts aumospheric pressure cvd method (APCVD) preparation film, can control the resistivity of film and and then control its optical property by the flow of conditioned reaction temperature and reactant.But adopt these methods to control film performance, its operating process is comparatively loaded down with trivial details.The method that needs a kind of more easy control film performance.

Summary of the invention

The purpose of this invention is to provide the simply method of depositing TiN thin film on glass substrate of a kind of technology.

Of the present invention on glass substrate the method for depositing TiN thin film, employing be chemical Vapor deposition process, step is as follows:

1) with 10% hydrofluoric acid clean glass substrate;

2) glass substrate is put on the graphite support of chemical vapor deposition unit reaction chamber, reaction chamber is evacuated to-0.02Mpa, and feeds N ₂Reaction chamber is cleaned;

3) distance range of regulating between intake ducting shower nozzle and the glass substrate is 5～25cm;

4) reaction chamber is heated to 600 ℃;

5) with TiCl ₄, NH ₃And N ₂Reactant gases feeds reaction chamber, wherein TiCl ₄Flow be 300sccm, NH ₃Flow be 150sccm, N ₂Flow be 900sccm, the pressure of reaction chamber is-0.02MPa, deposits under 600 ℃ temperature condition, the reaction times is 90s, deposition finishes, and stops to feed gas, cooling gets final product.

Beneficial effect of the present invention is: by the shower nozzle in conditioned reaction gas inlet pipe road and the distance between glass substrate, can control the resistivity that is deposited on TiN film on the glass substrate and surface topography, optical property etc. easily.The performance technologies such as resistivity of controlling film than traditional flow that passes through conditioned reaction temperature and reactant are simple, easily row.

Description of drawings

Fig. 1 is field emission scanning electron microscope (FESEM) photo of the TiN film for preparing.

Embodiment

Further specify the present invention below in conjunction with specific examples.

Embodiment 1

1) with 10% hydrofluoric acid clean glass substrate;

2) glass substrate is put on the graphite support of chemical vapor deposition unit reaction chamber, reaction chamber is evacuated to-0.02Mpa, and feeds N ₂Reaction chamber is cleaned;

3) distance of regulating between shower nozzle and the glass substrate is 5cm;

4) reaction chamber is heated to 600 ℃;

5) with TiCl ₄, NH ₃And N ₂Reactant gases feeds reaction chamber, wherein TiCl ₄Flow be 300sccm, NH ₃Flow be 150sccm, N ₂Flow be 900sccm, the pressure of reaction chamber is-0.02MPa, deposits under 600 ℃ temperature condition, the reaction times is 90s, after reaction finishes, stops to feed gas, cooling gets final product.

The TiN film resiativity for preparing is 1.5 * 10 ⁴μ Ω .cm is 45% at the reflectivity of infrared region, and increases with wavelength, and the reflectivity of film is in rising trend.

Embodiment 2

1) with 10% hydrofluoric acid clean glass substrate;

2) glass substrate is put on the graphite support of chemical vapor deposition unit reaction chamber, reaction chamber is evacuated to-0.02Mpa, and feeds N ₂Reaction chamber is cleaned;

3) distance of regulating between shower nozzle and the glass substrate is 25cm;

4) reaction chamber is heated to 600 ℃;

5) with TiCl ₄, NH ₃And N ₂Reactant gases feeds reaction chamber, wherein TiCl ₄Flow be 300sccm, NH ₃Flow be 150sccm, N ₂Flow be 900sccm, the pressure of reaction chamber is-0.02MPa, deposits under 600 ℃ temperature condition, the reaction times is 90s, after reaction finishes, stops to feed gas, cooling gets final product.

The TiN film for preparing is non-conductive, is 35% at the reflectivity of infrared region, and increases with wavelength, and the emittance of film is on a declining curve.

Embodiment 3

1) with 10% hydrofluoric acid clean glass substrate;

2) glass substrate is put on the graphite support of chemical vapor deposition unit reaction chamber, reaction chamber is evacuated to-0.02Mpa, and feeds N ₂Reaction chamber is cleaned;

3) distance of regulating between shower nozzle and the glass substrate is 13cm;

4) reaction chamber is heated to 600 ℃;

5) with TiCl ₄, NH ₃And N ₂Reactant gases feeds reaction chamber, wherein TiCl ₄Flow be 300sccm, NH ₃Flow be 150sccm, N ₂Flow be 900sccm, the pressure of reaction chamber is-0.02MPa, deposits under 600 ℃ temperature condition, the reaction times is 90s, after reaction finishes, stops to feed gas, cooling gets final product.

The resistivity of the TiN film for preparing is 7.5 * 10 ³μ Ω .cm can reach more than 50% at the reflectivity of infrared region, and in rising trend with the increase of wavelength.

The field emission scanning electron microscope photo of the TiN film that above-mentioned examples preparation obtains as shown in Figure 1, as seen from the figure, the film for preparing is that columnar structure and homogeneity are better.

Claims (1)

1. the method for depositing TiN thin film on glass substrate, step is as follows:

1) with 10% hydrofluoric acid clean glass substrate;

2) glass substrate is put on the graphite support of chemical vapor deposition unit reaction chamber, reaction chamber is evacuated to-0.02Mpa, and feeds N ₂Reaction chamber is cleaned;

3) distance range of regulating between intake ducting shower nozzle and the glass substrate is 5～25cm;

4) reaction chamber is heated to 600 ℃;

5) with TiCl ₄, NH ₃And N ₂Reactant gases feeds reaction chamber, wherein TiCl ₄Flow be 300sccm, NH ₃Flow be 150sccm, N ₂Flow be 900sccm, the pressure of reaction chamber is-0.02MPa, deposits under 600 ℃ temperature condition, the reaction times is 90s, deposition finishes, and stops to feed gas, cooling gets final product.

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