CN103614696B - A kind of preparation method of etching resistant film - Google Patents

Abstract

The invention discloses a kind of preparation method of etching resistant film, comprising: A, direct supply sputtering Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate₂o₃layer; B, AC power sputtering titanium oxide ceramics rotary target, at Bi₂o₃magnetron sputtering TiO on layer_xlayer; C, direct supply sputtering chromium planar target, at TiO_xmagnetron sputtering C rN on layer_xlayer; D, direct supply sputtering copper planar target, at CrN_xmagnetron sputtering C u layer on layer; E, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Cu layer; F, AC power sputtering ZnSn alloy rotary target, magnetron sputtering ZnSnO on NiCr layer₃layer.The object of the invention is to overcome weak point of the prior art, providing a kind of technique simple, easy to operate, the preparation method of the etching resistant film that production cost is relatively low.

Description

A kind of preparation method of etching resistant film

Technical field

The present invention relates to a kind of preparation method of etching resistant film.

Background technology

Low emissivity glass refers to have high-reflectivity to ir radiation, visible ray is had to the flat plate film coating glass of good transmissivity.Low emissivity glass has good printing opacity, insulation, heat-proof quality, is widely used in the places such as window, fire door, refrigerator door.

Low emissivity glass more common in the market has single silver-layer low-radiation glass, two silver-layer low-radiation glass, thermal control low emissivity glass and titanium base low emissivity glass etc.These four kinds of low emissivity glasses existing are not high enough in the visible wavelength range internal transmission factor of 380 ~ 780 nanometers, are only about 50%; Higher in infrared radiation wavelength scope internal transmission factor, be especially between 10 ~ 20% in the wavelength region internal transmission factor of 900 ~ 1100 nanometers.In addition, the wear resistance of these glass is usually excellent not.

And the rotproofness of existing transparent substrate is relative with thermotolerance poor, so existing transparent substrate awaits progressive perfect.

Summary of the invention

The object of the invention is to overcome weak point of the prior art, providing a kind of technique simple, easy to operate, the preparation method of the etching resistant film that production cost is relatively low.

In order to achieve the above object, the present invention adopts following scheme:

A preparation method for etching resistant film, is characterized in that comprising the following steps:

A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate₂o₃layer;

B, employing argon gas are as reactant gases, and AC power sputters titanium oxide ceramics rotary target, Bi in step₂o₃magnetron sputtering TiO on layer_xlayer;

C, employing nitrogen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters chromium planar target, TiO in stepb_xmagnetron sputtering C rN on layer_xlayer;

D, employing argon gas are as reactant gases, and direct supply sputters copper planar target, the CrN in step C_xmagnetron sputtering C u layer on layer;

E, adopt argon gas as reactant gases, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Cu layer in step D;

F, employing oxygen are as reactant gases, and argon gas is as shielding gas, and AC power sputters ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e₃layer.

The preparation method of a kind of etching resistant film as above, is characterized in that Bi described in steps A₂o₃the thickness of layer is 10 ~ 15nm, and the volume ratio of oxygen and argon gas is 1:2, and the sputtering power of described direct supply is 15 ~ 20KW.

The preparation method of a kind of etching resistant film as above, is characterized in that TiO described in step B_xthe thickness of layer is 10 ~ 15nm, the sputtering power 50 ~ 75KW of described AC power.

The preparation method of a kind of etching resistant film as above, is characterized in that CrN described in step C_xthe thickness of layer is 3 ~ 5nm, and the volume ratio of described nitrogen and argon gas is 1:2, the sputtering power 3 ~ 6KW of described direct supply.

The preparation method of a kind of etching resistant film as above, is characterized in that the thickness of Cu layer described in step D is 10 ~ 20nm, the sputtering power 3 ~ 6KW of described direct supply.

The preparation method of a kind of etching resistant film as above, is characterized in that the thickness of the layer of NiCr described in step e is 3 ~ 5nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 3 ~ 5KW of described direct supply.

The preparation method of a kind of etching resistant film as above, is characterized in that ZnSnO described in F₃the thickness of layer is 20 ~ 30nm, and the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, the volume ratio of described argon gas and oxygen is 1:2, and the sputtering power of described AC power is 50 ~ 75KW.

The preparation method of a kind of etching resistant film as above, is characterized in that transparency and heat-proof substrate is transparent glass.

In sum, beneficial effect of the present invention:

Present invention process method is simple, and easy to operate, production cost is relatively low.Product erosion resistance is strong, less demanding to substrate clean level in production process, product transmittance T >=65% of the present invention, radiant ratio E≤0.15.

Embodiment

Below in conjunction with embodiment, the present invention is described further:

Embodiment 1

The preparation method of a kind of etching resistant film of the present invention, comprises the following steps:

A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate₂o₃layer; Wherein said Bi₂o₃the thickness of layer is 10nm, and the volume ratio of oxygen and argon gas is 1:2, i.e. oxygen: argon gas=500sccm:1000sccm, and the sputtering power of described direct supply is 15KW, and wherein said transparency and heat-proof substrate is transparent glass;

B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, Bi in step₂o₃magnetron sputtering TiO on layer_xlayer; Wherein said TiO_xthe thickness of layer is 10nm, the sputtering power 50KW of described AC power;

C, employing nitrogen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters chromium planar target, TiO in stepb_xmagnetron sputtering C rN on layer_xlayer; Wherein said CrN_xthe thickness of layer is 3nm, and the volume ratio of described nitrogen and argon gas is 1:2, i.e. nitrogen and argon gas=500sccm:1000sccm, the sputtering power 3KW of described direct supply;

D, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm direct supply sputtering copper planar target, the CrN in step C_xmagnetron sputtering C u layer on layer; The thickness of wherein said Cu layer is 10nm, the sputtering power 3KW of described direct supply;

E, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Cu layer in step D; The thickness of described NiCr layer is 3nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 3KW of described direct supply;

F, employing oxygen are as reactant gases, and argon gas is as shielding gas, and AC power sputters ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e₃layer; Described ZnSnO₃the thickness of layer is 20nm, and the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, the volume ratio of described argon gas and oxygen is 1:2, argon gas and oxygen=500sccm:1000sccm, and the sputtering power of described AC power is 50KW.

Embodiment 2

The preparation method of a kind of etching resistant film of the present invention, comprises the following steps:

A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate₂o₃layer; Wherein said Bi₂o₃the thickness of layer is 12nm, and the volume ratio of oxygen and argon gas is 1:2, i.e. oxygen: argon gas=500sccm:1000sccm, the sputtering power of described direct supply is 18KW, and wherein said transparency and heat-proof substrate is transparent glass;

B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, Bi in step₂o₃magnetron sputtering TiO on layer_xlayer; Wherein said TiO_xthe thickness of layer is 13nm, the sputtering power 60KW of described AC power;

C, employing nitrogen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters chromium planar target, TiO in stepb_xmagnetron sputtering C rN on layer_xlayer; Wherein said CrN_xthe thickness of layer is 4nm, and the volume ratio of described nitrogen and argon gas is 1:2, i.e. nitrogen and argon gas=500sccm:1000sccm, the sputtering power 5KW of described direct supply;

D, employing argon gas are as reactant gases, and direct supply sputters copper planar target, the CrN in step C_xmagnetron sputtering C u layer on layer; The thickness of wherein said Cu layer is 15nm, the sputtering power 4KW of described direct supply;

E, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Cu layer in step D; The thickness of described NiCr layer is 4nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 4KW of described direct supply;

F, employing oxygen are as reactant gases, and argon gas is as shielding gas, and AC power sputters ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e₃layer.Described ZnSnO₃the thickness of layer is 25nm, and the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, the volume ratio of described argon gas and oxygen is 1:2, argon gas and oxygen=500sccm:1000sccm, and the sputtering power of described AC power is 63KW.

Embodiment 3

The preparation method of a kind of etching resistant film of the present invention, comprises the following steps:

A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate₂o₃layer; Wherein said Bi₂o₃the thickness of layer is 15nm, and the volume ratio of oxygen and argon gas is 1:2, i.e. oxygen: argon gas=500sccm:1000sccm, the sputtering power of described direct supply is 20KW, and wherein said transparency and heat-proof substrate is transparent glass;

B, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 800sccm, AC power sputtering titanium oxide ceramics rotary target, Bi in step₂o₃magnetron sputtering TiO on layer_xlayer; Wherein said TiO_xthe thickness of layer is 15nm, the sputtering power 75KW of described AC power;

C, employing nitrogen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters chromium planar target, TiO in stepb_xmagnetron sputtering C rN on layer_xlayer; Wherein said CrN_xthe thickness of layer is 5nm, and the volume ratio of described nitrogen and argon gas is 1:2, i.e. nitrogen and argon gas=500sccm:1000sccm, the sputtering power 6KW of described direct supply;

D, employing argon gas are as reactant gases, and direct supply sputters copper planar target, the CrN in step C_xmagnetron sputtering C u layer on layer; The thickness of wherein said Cu layer is 20nm, the sputtering power 6KW of described direct supply;

E, employing argon gas are as reactant gases, and the volumetric flow rate of argon gas is 1000sccm, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Cu layer in step D; The thickness of described NiCr layer is 5nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 5KW of described direct supply;

F, employing oxygen are as reactant gases, and argon gas is as shielding gas, and AC power sputters ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e₃layer.Described ZnSnO₃the thickness of layer is 30nm, and the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, the volume ratio of described argon gas and oxygen is 1:2, argon gas and oxygen=500sccm:1000sccm, and the sputtering power of described AC power is 75KW.

More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.

Claims (8)

1. a preparation method for etching resistant film, is characterized in that comprising the following steps:

A, employing oxygen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters Bi planar target, magnetron sputtering Bi on transparency and heat-proof substrate₂o₃layer;

B, employing argon gas are as shielding gas, and AC power sputters titanium oxide ceramics rotary target, Bi in step₂o₃magnetron sputtering TiOx layer on layer;

C, employing nitrogen are as reactant gases, and argon gas is as shielding gas, and direct supply sputters chromium planar target, magnetron sputtering C rNx layer on TiOx layer in stepb;

D, employing argon gas are as shielding gas, and direct supply sputters copper planar target, magnetron sputtering C u layer on the CrNx layer in step C;

E, adopt argon gas as shielding gas, direct supply sputtering NiCr alloy planar target, magnetron sputtering NiCr layer on Cu layer in step D;

F, employing oxygen are as reactant gases, and argon gas is as shielding gas, and AC power sputters ZnSn alloy rotary target, magnetron sputtering ZnSnO on the NiCr layer in step e₃layer.

2. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that Bi described in steps A₂o₃the thickness of layer is 10 ~ 15nm, and the volume ratio of oxygen and argon gas is 1:2, and the sputtering power of described direct supply is 15 ~ 20kW.

3. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that the thickness of the layer of TiOx described in step B is 10 ~ 15nm, the sputtering power 50 ~ 75kW of described AC power.

4. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that the thickness of the layer of CrNx described in step C is 3 ~ 5nm, and the volume ratio of described nitrogen and argon gas is 1:2, the sputtering power 3 ~ 6kW of described direct supply.

5. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that the thickness of Cu layer described in step D is 10 ~ 20nm, the sputtering power 3 ~ 6kW of described direct supply.

6. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that the thickness of the layer of NiCr described in step e is 3 ~ 5nm, the mol ratio 21:79 of Ni:Cr in described NiCr alloy, the sputtering power 3 ~ 5kW of described direct supply.

7. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that ZnSnO described in F₃the thickness of layer is 20 ~ 30nm, and the mol ratio 48:52 of Zn:Sn in described ZnSn alloy rotary target, the volume ratio of described argon gas and oxygen is 1:2, and the sputtering power of described AC power is 50 ~ 75kW.

8. the preparation method of a kind of etching resistant film according to claim 1, is characterized in that transparency and heat-proof substrate is transparent glass.