CN102432190A - Method for preparing high transmissivity titanium nitride coated glass - Google Patents

Abstract

The invention discloses a method for preparing high transmissivity titanium nitride coated glass, which comprises the steps of: placing a cleaned glass substrate in a vapor phase deposition reaction chamber, vacuumizing the reaction chamber and introducing N2 to clean; heating the reaction chamber to 600 DEG C and introducing N2, NH3 and TiCl4 which is preheated to 41.2 DEG C to the reaction chamber by using an inert gas as a carrier; under the pressure of -0.02 MPa, naturally cooling the sample to the room temperature after depositing a titanium nitride thin film layer on the glass substrate; and then performing heat treatment for 15-120 min at 400-600 DEG C under atmosphere. The titanium nitride thin film prepared by the invention is uniformly compact and combined with the glass substrate well, and not only has high reflectivity both in a near infrared region and a far infrared region, but also has better transmissivity in a visible light region with performances of solar control and low radiation, and represents excellent energy-saving performance. The invention has simple preparation process, low production cost and high production efficiency.

Description

The method for preparing high permeability titanium nitride coating glass

Technical field

The present invention relates to the method for the novel energy-conserving glass energy-saving performance that a kind of improvement is used for building.

Background technology

Along with the develop rapidly of human social economy with civilization, the raising of the science and technology and the level of the productive forces, people's living standard is enhanced.The raising with people's living standard of advancing by leaps and bounds of science and technology directly cause human to natural resources utilization and the spending rate of the energy increased sharply thereupon, incident is increasing environmental problem and energy shortage problem.In various energy consumptions, 1/5th of building energy consumption account total energy consumption, and in building energy consumption, the energy consumption that causes through glass door and window accounts for 56% of whole buildings heat dissipation capacity, in the curtain buildings especially up to more than 90%.Building energy conservation is to need one of important topic of solution badly in the present Economic development.

TiN is a kind of typical transition metal nitride, and it has certain transmittance at visible region, near infrared and mid and far infrared district higher reflectivity is arranged also, and titanium nitride coating glass is a kind of energy-saving glass that has low radiance and sunlight control characteristics concurrently.But the greatest problem that the energy-conservation coated glass of titanium nitride faces is that visible light transmissivity is on the low side at present.Though through optimal preparation technology, as changing depositing temperature, depositing time, conditioned reaction logistics capacity wait and improve its visible light transmissivity, effect is undesirable.

Summary of the invention

The purpose of this invention is to provide a kind of method for preparing high permeability titanium nitride coating glass, can improve the daylighting effect of titanium nitride coating glass in the building glass door and window, improve the energy-efficient performance of coated glass.

The method for preparing high permeability titanium nitride coating glass of the present invention, step is following:

The glass substrate that 1) will pass through cleaning is put into phase depositing reaction chamber, and reaction chamber vacuumizes, and feeds N ₂The cleaning reaction chamber;

2) reaction chamber is heated to 600 ℃, with N ₂, NH ₃With the TiCl that is preheating to 41.2 ℃ ₄With the rare gas element is that carrier gas feeds reaction chamber, control N ₂: NH ₃: TiCl ₄Throughput ratio be 300:25:3; Keep pressure in the reaction chamber in-0.02 MPa, cvd nitride ti thin film layer on glass substrate, reaction times 90s; Close gas circuit then; Be evacuated to-0.02 MPa again, sample naturally cooled to room temperature, under air atmosphere in 400-600 ℃ of thermal treatment 15-120min.

Among the present invention, the visible light transmissivity of titanium nitride coating glass can be controlled through changing thermal treatment temp and time.

Beneficial effect of the present invention is:

The titanium nitride membrane of the present invention preparation is fine and close evenly, combine well with glass substrate; Film not only all has high-reflectivity in near-infrared region and mid and far infrared district; And have transmitance preferably at visible region, and have sunlight control and low radiance concurrently, show excellent energy-efficient performance.Preparation technology of the present invention is simple, and production cost is low, and production efficiency is high.

Description of drawings

Fig. 1 is the transmitted spectrum of titanium nitride membrane before and after the thermal treatment;

Fig. 2 is the reflection spectrum of titanium nitride membrane before and after the thermal treatment.

Embodiment

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

Instance 1

1) with 10% hydrofluoric acid clean glass substrate, glass substrate is put on the graphite sample frame of phase depositing reaction chamber, reaction chamber vacuumizes, and feeds N ₂The cleaning reaction chamber;

2) keeping under the state that vacuumizes reaction chamber being heated to 600 ℃; With N ₂, NH ₃With the TiCl that is preheating to 41.2 ℃ ₄With the rare gas element argon gas is that carrier gas feeds reaction chamber, control N ₂Flow be 900sccm, NH ₃Flow be 75sccm, TiCl ₄Flow be 9sccm.Keep pressure in the reaction chamber at-0.02MPa, cvd nitride ti thin film layer on glass substrate, reaction times 90s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature;

3) after the sample cooling, bubbling air in phase depositing reaction chamber, reaction chamber are warmed up to 400 ℃, insulation 60min.Take out sample.

Titanium nitride membrane was as depicted in figs. 1 and 2 in the transmitted spectrum and the reflection spectrum in visible near-infrared district before and after prepared titanium nitride coating glass heat was handled; Visible by figure; Compare with the titanium nitride membrane before the thermal treatment, titanium nitride membrane has improved in the transmitance of visible region after the thermal treatment.Titanium nitride membrane in the transmitance of visible region near 30%.Film has good sunlight control characteristics and low radiance.

Instance 2

1) with 10% hydrofluoric acid clean glass substrate, glass substrate is put on the graphite sample frame of phase depositing reaction chamber, reaction chamber vacuumizes, and feeds N ₂The cleaning reaction chamber;

2) keeping under the state that vacuumizes reaction chamber being heated to 600 ℃; With N ₂, NH ₃With the TiCl that is preheating to 41.2 ℃ ₄With the rare gas element argon gas is that carrier gas feeds reaction chamber, control N ₂Flow be 900sccm, NH ₃Flow be 75sccm, TiCl ₄Flow be 9sccm.Keep pressure in the reaction chamber at-0.02MPa, cvd nitride ti thin film layer on glass substrate, reaction times 90s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature;

3) after the sample cooling, bubbling air in phase depositing reaction chamber, reaction chamber are warmed up to 400 ℃, insulation 120min.Take out sample.

The titanium nitride membrane of prepared titanium nitride coating glass in the transmitance of visible region near 25%.

Instance 3

1) with 10% hydrofluoric acid clean glass substrate, glass substrate is put on the graphite sample frame of phase depositing reaction chamber, reaction chamber vacuumizes, and feeds N ₂The cleaning reaction chamber;

2) keeping under the state that vacuumizes reaction chamber being heated to 600 ℃; With N ₂, NH ₃With the TiCl that is preheating to 41.2 ℃ ₄With the rare gas element argon gas is that carrier gas feeds reaction chamber, control N ₂Flow be 900sccm, NH ₃Flow be 75sccm, TiCl ₄Flow be 9sccm.Keep pressure in the reaction chamber at-0.02MPa, cvd nitride ti thin film layer on glass substrate, reaction times 90s closes gas circuit then, vacuumizes again, and sample is naturally cooled to room temperature;

3) after the sample cooling, bubbling air in phase depositing reaction chamber, reaction chamber are warmed up to 600 ℃, insulation 20min.Take out sample.

The titanium nitride membrane of prepared titanium nitride coating glass in the transmitance of visible region near 20%.

Claims (1)

1. the method for preparing high permeability titanium nitride coating glass is characterized in that step is following:

The glass substrate that 1) will pass through cleaning is put into phase depositing reaction chamber, and reaction chamber vacuumizes, and feeds N ₂The cleaning reaction chamber;

2) reaction chamber is heated to 600 ℃, with N ₂, NH ₃With the TiCl that is preheating to 41.2 ℃ ₄With the rare gas element is that carrier gas feeds reaction chamber, control N ₂: NH ₃: TiCl ₄Throughput ratio be 300:25:3; Keep pressure in the reaction chamber in-0.02 MPa, cvd nitride ti thin film layer on glass substrate, reaction times 90s; Close gas circuit then; Be evacuated to-0.02 MPa again, sample naturally cooled to room temperature, under air atmosphere in 400-600 ℃ of thermal treatment 15-120min.

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