CN102529209A - Enhanced protection type toughened low-radiation coated glass and manufacturing process thereof - Google Patents
Enhanced protection type toughened low-radiation coated glass and manufacturing process thereof Download PDFInfo
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- CN102529209A CN102529209A CN2011104271263A CN201110427126A CN102529209A CN 102529209 A CN102529209 A CN 102529209A CN 2011104271263 A CN2011104271263 A CN 2011104271263A CN 201110427126 A CN201110427126 A CN 201110427126A CN 102529209 A CN102529209 A CN 102529209A
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Abstract
A medium protecting layer is added to the outermost layer of ordinary low-radiation coated glass to serve as an enhanced protecting layer so that the ordinary low-radiation coated glass has high chemical stability, abrasion resistance and oxidation resistance and low friction coefficient and particularly improves scratch resistance, toughened low-radiation coated glass is convenient and simple to transport and process, and the finished product rate of production is greatly improved. In particular, the lowered processing requirements enable more small glass deep-processing enterprises to produce the low-radiation coated glass, and a foundation is established for popularization of environment-friendly energy-saving products. In addition, a metal absorbing layer is first coated on the glass, reflectivity of coated products can be greatly reduced, the problem of light pollution of the toughened low-radiation coated glass with low light transmittance is solved, and the toughened low-radiation coated glass products can meet the requirements of the market at present.
Description
Technical field
The present invention relates to the coating technique field in the glass deep processing, specifically is a kind of enhance protection type radiation coated glass capable of being toughened and manufacturing process thereof.
Background technology
At present, on the domestic market radiation coated glass capable of being toughened with its cheap price, do not fail in the performance of common low emissivity glass and the production cycle that shortens greatly, more and more receive client's favor.But; Long-distance transport and numerous following process links behind the plated film; The integrated yield that often causes producing is on the low side, and the particularly scuffing of rete, scratch and oxidation often causes a large amount of defective works; Therefore the protection effect that strengthens rete is extremely urgent, and the DLC diaphragm becomes optimal selection with the character of its high rigidity, high chemical stability, low-friction coefficient.
DLC (Diamond-like Carbon, DLC) film is owing to contain the carbon of sp3 hydridization and sp2 hydridization in its composition; Thereby show the various character between diamond and graphite; Be embodied as: high rigidity, wear-resistant, surface smoothness is high; Low-resistivity, high transmission rate and chemical inertness etc.It has been widely used in machinery, electronics, optics, magnetizing mediums protection and medical domain.Up to the present, the preparation method of diamond-film-like is broadly divided into two types: physical vaporous deposition such as magnetically controlled DC sputtering (DMS) method, radio-frequency sputtering (RFS) method; Ion beam enhanced depositing (IBED) method; Ion beam depositing (IBD) method, vacuum arc (VARC) method, laser-arc (LARC) method etc.; Plasma auxiliary chemical vapor deposition (PECVD), like direct current glow discharge method (DG) method, heated filament discharge (HFG) method, radio frequency glow discharge (RFG) method etc.Dijection glow discharge (RF-RF) the frequently method that has occurred high deposition rate and big depositional area this year again, radio frequency-direct current glow discharge (RF-DC) method and microwave-radio frequency (MW-FR) method etc.With data by MoM and MEI, RF-PECVD has low-temperature epitaxy, and sedimentation rate is high, can realize superiority such as large area deposition, is widely used.
Summary of the invention
Technical purpose of the present invention is to solve in the prior art to have problems, and a kind of anti-oxidant, enhance protection type radiation coated glass capable of being toughened and manufacturing process thereof that wearability is high are provided.
Technical scheme of the present invention is:
A kind of enhance protection type radiation coated glass capable of being toughened comprises glass substrate and is coated on the multicoating on the glass substrate, it is characterized in that, said plated film comprises and is arranged on outermost medium protective layer.
As preferably, said medium protective layer is Si
3N
4The combination layer of rete and C rete, or Si
3N
4Rete and CN
4The combination layer of rete, or Si
3N
4Rete, C rete and CN
4The combination layer of rete.
Further; In order to satisfy client's needs better; The inconvenience of avoiding light pollution to bring to the client; The present invention optimizes the glass rete, and said plated film outwards comprises from glass substrate successively: metal absorbed layer, first dielectric combination layer, first protective layer, infrared ray barrier layer, second protective layer, second dielectric combination layer, medium protective layer.
As preferably, said metal absorbed layer is the SST rete, and the preferred thickness range of said metal absorbed layer is 5-20nm;
Said first dielectric combination layer is Si
3N
4, a kind of among the TixO, thicknesses of layers is 10-40nm;
Said first protective layer, second protective layer are the NiCr rete, and thicknesses of layers is 1-10nm;
Said infrared ray barrier layer is the Ag layer, and thicknesses of layers is 5-15nm;
Second dielectric combination layer is Si
3N
4Layer, or ZnSnO
3Layer and Si
3N
4The combination layer of layer, thicknesses of layers is 10-40nm;
The thicknesses of layers of said medium protective layer is 5-20nm.
A kind of manufacturing process that is used to make above-mentioned enhance protection type radiation coated glass capable of being toughened adopts vacuum magnetic-control sputtering method and radio frequency plasma to strengthen the chemical vapour deposition technique plated film, it is characterized in that, may further comprise the steps:
Step 1, cleaning, dry glass substrate;
Step 2, on glass substrate, adopt magnetron sputtering method to be coated with the metal absorbed layer;
On the metal absorbed layer, adopt magnetron sputtering method to be coated with first dielectric combination layer;
On first dielectric layer, adopt magnetron sputtering method to be coated with first protective layer;
On first protective layer, adopt magnetron sputtering method to be coated with the infrared ray barrier layer;
On the infrared ray barrier layer, adopt magnetron sputtering method to be coated with second protective layer;
On second protective layer, adopt magnetron sputtering method to be coated with second dielectric combination layer;
Said metal absorbed layer, through the sputter in the straight argon atmosphere of direct current planar negative electrode, cathode targets is a kind of in Ti, SST, Cr, Ni, the NiCr alloy;
Said infrared ray barrier layer, through the sputter in argon atmosphere of direct current planar negative electrode, a kind of in the optional Ag of cathode targets, AgCu alloy, AgNi alloy, the AgTi alloy;
Said first, second dielectric combination layer, through the sputter in nitrogen argon, oxygen argon or nitrogen oxygen argon atmosphere of rotation interchange negative electrode, cathode targets is one or more among SiAl, Sn, ZnSn, TxO, Zn, AZO, the NbxO;
Said first, second protective layer, through the sputter in the straight argon atmosphere of direct current planar negative electrode, cathode targets is a kind of in Ti, SST, Cr, Ni, the Ni Cr alloy.
The beneficial effect of each rete of the present invention:
Said metal absorbed layer, its effect are to reduce reflection through the absorption that increases rete;
Said first, second dielectric combination layer, its effect is a, between silver layer and dielectric layer, absorption affinity is provided; B, protect whole film layer structure, reduce oxidation, improve the physics and the chemical property of product; The optical property and the color of c, controlling diaphragm system;
Said infrared ray barrier layer, its effect is: reduce radiance,, heat preservation effect heat insulation to play;
Said first, second protective layer, go the effect be: a, the protection silver layer not oxidized; B, increase the adhesion of silver layer with other rete;
The effect of said medium protective layer is that the whole rete of protection is not scratched, scratch and oxidation.
The medium protection film that the present invention adopts radio frequency plasma to strengthen the chemical deposition deposition is a kind of DLC film; Hardness, chemical stability and lower coefficient of friction that its tool is high; Make product of the present invention all be greatly improved aspect scratch resistance, the anti-oxidant and wearability; But thereby avoided tempering plated film product in follow-up cutting, wash the problems such as scuffing, scratch and oxidation in mill, the tempering process, the finished product rate is greatly improved, the production cycle shortens greatly.The medium protection film that the present invention adopts radio frequency plasma to strengthen the chemical deposition deposition will volatilize in the tempering process voluntarily; Do not stay any vestige, the reflectivity of rete, transmitance, color, performance are equal to data consistent behind the tempering of the composite film that does not plate this medium protective layer behind the tempering.
Description of drawings
Fig. 1 is each film layer structure sketch map of the present invention;
Fig. 2 is the process flow diagram that the present invention is coated with each rete;
Fig. 3 is the process flow diagram that the present invention is coated with rete.
The specific embodiment
In order to illustrate technical scheme of the present invention and technical purpose, the present invention is done further introduction below in conjunction with the accompanying drawing and the specific embodiment.
The present invention strengthens the chemical deposition medium protective layer with radio frequency plasma and is incorporated in the large tracts of land low emissivity glass plated film; The tempered and low-radiation plated film is prone to scratch, scratch reaches the shortcoming that is prone to oxidation but solved at present; On glass substrate 10, plate layer of metal absorbed layer 11 in addition earlier; Can produce the sunshade type product of low reflection, avoid " light pollution " problem to bring client's inconvenience, more more options are provided to the client.
Like Fig. 2, shown in Figure 3, the practical implementation step of a kind of enhance protection type of the present invention radiation coated glass capable of being toughened process for plating is:
Execution in step S1: cleaning, dry glass substrate 10;
Execution in step S2: adopt the physics magnetron sputtering plating;
Execution in step S21: carry out the forevacuum transition;
Execution in step S22: on glass substrate 10, adopt magnetron sputtering method to be coated with metal absorbed layer 11;
Execution in step S23: on metal absorbed layer 11, adopt magnetron sputtering method to be coated with first dielectric combination layer 12;
Execution in step S24: on the first dielectric layer combination layer 12, adopt magnetron sputtering method to be coated with first protective layer 13;
Execution in step S25: on first protective layer 13, adopt magnetron sputtering method to be coated with infrared ray barrier layer 14;
Execution in step S26: on infrared ray barrier layer 14, adopt magnetron sputtering method to be coated with second protective layer 15;
Execution in step S27: on second protective layer 15, adopt magnetron sputtering method to be coated with second dielectric combination layer 16;
Execution in step S3: adopt radio frequency plasma to strengthen chemical vapour deposition technique and be coated with medium protective layer 17.
In the above-mentioned steps, said metal absorbed layer 11 is through the sputter in the straight argon atmosphere of direct current planar negative electrode, a kind of in the optional Ti of cathode targets, SST, Cr, Ni, the Ni Cr alloys target, and thicknesses of layers is: 5-20nm;
Said first, second dielectric combination layer exchanges negative electrode sputter in nitrogen argon, oxygen argon or nitrogen oxygen argon atmosphere through rotation, one or more among the optional SiAl of cathode targets, Sn, ZnSn, TxO, Zn, AZO, the NbxO, and thicknesses of layers is: 10-40nm;
Said infrared ray barrier layer 14 is through the sputter in argon atmosphere of direct current planar negative electrode, a kind of in the optional Ag of cathode targets, AgCu alloy, AgNi alloy, the AgTi alloy, and thicknesses of layers is 5-15nm;
Said first, second protective layer, through the sputter in the straight argon atmosphere of direct current planar negative electrode, a kind of in the optional Ti of cathode targets, Cr, Ni, the NiCr alloy, thicknesses of layers is: 1-10nm;
Said medium protective layer 17 adopts radio frequency plasma to strengthen the chemical vapour deposition technique deposition, and thickness is: 10-15nm.This radio frequency plasma strengthens chemical vapour deposition technique at 1*10
-6In the mbar background vacuum environment, charge into CH
4, H
2, N
2Deng gas, CH wherein
4And H
2Flow percentage be 30%-80%, gas purity is 99.99%, deposition pressure is 2～3*10
-3Mbar, the radio-frequency power supply frequency is 13.56MHz, and radio-frequency power is 5.5KW, and polar plate spacing is 60mm.
Embodiment 1:
Present embodiment adopts the magnetron sputtering embrane method to be coated with single silver low radiation coated glass earlier, adopts radio frequency plasma to strengthen chemical vapour deposition technique then, and in outermost layer deposition one deck medium protective layer 17 of single silver low radiation plated film, step is following:
Execution in step S1: cleaning, dry glass substrate 10;
Execution in step S2: adopt magnetically controlled sputter method to be coated with metal absorbed layer 11, first dielectric combination layer 12, first protective layer 13, infrared ray barrier layer 14, second protective layer 15, the combination of second dielectric layer by layer 16 successively;
Execution in step S3: adopt radio frequency plasma to strengthen chemical vapour deposition technique deposition medium protective layer 17.
After being coated with completion, wherein, said metal absorbed layer 11 is a stainless steel material, preferred SST film, and thicknesses of layers is: 5nm;
Said first dielectric combination layer 12 is a silicon nitride material, is specially Si
3N
4Film, thicknesses of layers is: 28.4nm;
Said first protective layer 13 is the nickel-cadmium material, is specially the NiCr film, and thicknesses of layers is: 4.2nm;
Said infrared ray barrier layer 14 is an ag material, i.e. Ag film, and thicknesses of layers is: 11.8nm;
Said second protective layer 15 is the nickel-cadmium material, is specially the NiCr film, and thicknesses of layers is: 4.2nm;
Said second dielectric combination layer 16 is a silicon nitride material, is specially Si
3N
4Film, thicknesses of layers is: 28.7nm;
Said medium protective layer 17 is the combination layer of silicon nitride film layer and carbon film layer, or the combination layer of silicon carbide film layer and nitrogenize carbon-coating, or the combination layer of silicon nitride film layer, carbon-coating and nitrogenize carbon-coating, is specially Si
3N
4+ C or Si
3N
4+ CN
4Or Si
3N
4+ C+CN
4, thicknesses of layers is: 10nm.
To sum up, concrete glass-film layer architecture is: SST/Si
3N
4/ NiCr/Ag/NiCr/Si
3N
4/ Si
3N
4+ C or Si
3N
4+ CN
4Or Si
3N
4+ C+CN
4
Below each table for the glass rete be coated with before and after the parameter comparison of product, print 1 is not for plating the radiation coated glass capable of being toughened of medium protective layer 17, print 2 is for plating the radiation coated glass capable of being toughened of medium protective layer 17.
Color distinction before and after the table 1. plating medium protective layer
| Rg | a* | b* | Rf | a* | b* | Tr | a* | b* | |
| 1 | 8.5 | -1.4 | -3.6 | 4.5 | 15.9 | 13.8 | 50.5 | -3.3 | 4.4 |
| 2 | 12.0 | -4.7 | 2.8 | 2.4 | 14.5 | -26.1 | 49.1 | -3.0 | 2.4 |
The comparison of transmitance (Tr) before and after table 2. grinds
| Revolution | Tr before grinding | Grind back Tr | ΔTr | |
| 1 | 50 | 50.54 | 49.32 | -1.22 |
| 2 | 50 | 49.26 | 48.61 | -0.65 |
| 2 | 100 | 49.12 | 48.72 | -0.38 |
| 2 | 200 | 49.43 | 48.68 | -0.75 |
Can find out from table 2 no matter the radiation coated glass capable of being toughened of plating medium protective layer 17 is to grind 50 to change, and still grinds 200 and changes, the variation of transmitance (Tr) is all less.
Anti oxidation time before and after the table 3. plating medium protection film:
| The autoxidation time (H) | Damp and hot machine oxidization time (H) | |
| 1 | 528 | 312 |
| 2 | 912 | 630 |
| Time expand | 384 | 318 |
Can find out from table 3 no matter the radiation coated glass capable of being toughened of plating medium protective layer 17 is autoxidation, still the oxidization time of damp and hot machine oxidation all significantly prolongs.
Microhardness contrast before and after the table 4. plating medium protective layer:
| Pressure head is got numbering ready | 1 | 2 | 3 | Mean value |
| 1 composite hardness (kgf/cm 2) | 395.2 | 376.5 | 382.1 | 384.6 |
| 2 composite hardness (kgf/cm 2) | 487.3 | 530.5 | 504.2 | 507.3 |
Can find out that from table 4 hardness of the radiation coated glass capable of being toughened of plating medium protective layer 17 is apparently higher than the glass that does not plate medium protective layer 17.
Embodiment 2:
Present embodiment adopts the magnetron sputtering embrane method to be coated with single silver low radiation coated glass earlier, adopts radio frequency plasma to strengthen chemical vapour deposition technique then, and in outermost layer deposition one deck medium protective layer of single silver low radiation plated film, step is following:
Execution in step S1: cleaning, dry glass substrate 10;
Execution in step S2: adopt magnetically controlled sputter method to be coated with metal absorbed layer 11, first dielectric combination layer 12, first protective layer 13, infrared ray barrier layer 14, second protective layer 15, second dielectric combination layer 16;
Execution in step S3: adopt radio frequency plasma to strengthen chemical vapour deposition technique deposition medium protective layer 17.
Wherein, metal absorbed layer 11 is a stainless steel material, is specially the SST rete, and thicknesses of layers is: 6nm;
First dielectric combination layer 12 is a titania meterial, is specially the TixO rete, and thicknesses of layers is: 58.2nm;
First protective layer 13 is the nickel-cadmium layer material, is specially the NiCr rete, and thicknesses of layers is: 3.5nm;
Infrared ray barrier layer 14 is a silver layer, and thicknesses of layers is: 12nm;
Second protective layer 15 is the nickel-cadmium material, is specially the NiCr rete, and thicknesses of layers is: 3.2nm;
Second dielectric combination layer 16 is the combination layer of zinc-tin oxide rete and silicon nitride film layer, is specially ZnSnO
3+ Si
3N
4The combination rete, ZnSnO
3The thicknesses of layers of layer is 8.2nm, Si
3N
4The thicknesses of layers of layer is 12.1nm;
Said medium protective layer 17 is Si
3N
4+ C or Si
3N
4+ CN
4Or Si
3N
4+ C+CN
4, thicknesses of layers is: 10nm.
Concrete rete framework is: SST/TixO/NiCr/Ag/NiCr/ZnSnO
3/ Si
3N
4/ Si
3N
4+ C or Si
3N
4+ CN
4Or Si
3N
4+ C+CN
4
Below each table for the glass rete be coated with before and after the parameter comparison of product, print 1 is not for plating the radiation coated glass capable of being toughened of medium protective layer 17, print 2 is for plating the radiation coated glass capable of being toughened after the medium protective layer 17.
Color distinction before and after the table 5 plating medium protective layer
| Rg | a* | b* | Rf | a* | b* | Tr | a* | b* | |
| 1 | 8.1 | -2.5 | -4.4 | 5.7 | 17.2 | 16.7 | 44.2 | -3.9 | -5.1 |
| 2 | 9.7 | -4.0 | 7.3 | 2.2 | 21.0 | -22.8 | 44.3 | -3.6 | 1.1 |
The comparison of transmitance (Tr) before and after table 6 grinds
| Revolution | Tr before grinding | Grind back Tr | ΔTr | |
| 1 | 50 | 44.32 | 42.28 | -2.04 |
| 2 | 50 | 44.57 | 43.89 | -0.68 |
| 2 | 100 | 44.15 | 43.78 | -0.37 |
| 2 | 200 | 44.42 | 44.01 | -0.31 |
Can find out from table 6 no matter the radiation coated glass capable of being toughened of plating medium protective layer 17 is to grind 50 to change, and still grinds 200 and changes, the variation of transmitance (Tr) is all less.
Anti oxidation time before and after the table 7 plating medium protective layer:
| The autoxidation time (H) | Damp and hot machine oxidization time (H) | |
| 1 | 480 | 260 |
| 2 | 880 | 630 |
| Time expand | 400 | 370 |
Can find out from table 7 no matter the radiation coated glass capable of being toughened of plating medium protective layer 17 is autoxidation, still the oxidization time of damp and hot machine oxidation all significantly prolongs.
Microhardness contrast before and after the table 8 plating medium protective layer:
| Pressure head is got numbering ready | 1 | 2 | 3 | Mean value |
| 1 composite hardness (kgf/cm2) | 276.5 | 319.7 | 288.3 | 294.8 |
| 2 composite hardness (kgf/cm2) | 498.3 | 520.6 | 476.7 | 498.5 |
Can find out that from table 8 hardness of the radiation coated glass capable of being toughened of plating medium protective layer 17 is apparently higher than not plating medium protective layer 17.
Those skilled in the art all should be appreciated that, under the situation that does not break away from the spirit or scope of the present invention, can carry out various modifications and variations to the present invention.Thereby, if when any modification or modification fall in the protection domain of appended claims and equivalent, think that the present invention contains these modifications and modification.
Claims (7)
1. an enhance protection type radiation coated glass capable of being toughened comprises glass substrate and is coated on the multicoating on the glass substrate, it is characterized in that, said plated film comprises and is arranged on outermost medium protective layer.
2. a kind of enhance protection type radiation coated glass capable of being toughened according to claim 1, it is characterized in that: said medium protective layer is Si
3N
4The combination layer of rete and C rete, or Si
3N
4Rete and CN
4The combination layer of rete, or Si
3N
4Rete, C rete and CN
4The combination layer of rete.
3. a kind of enhance protection type radiation coated glass capable of being toughened according to claim 1 and 2; It is characterized in that said plated film outwards comprises from glass substrate successively: metal absorbed layer, first dielectric combination layer, first protective layer, infrared ray barrier layer, second protective layer, second dielectric combination layer, medium protective layer.
4. a kind of enhance protection type radiation coated glass capable of being toughened according to claim 3 is characterized in that:
Said metal absorbed layer is the SST rete;
Said first dielectric combination layer is Si
3N
4, a kind of among the TixO;
Said first protective layer, second protective layer are the NiCr rete;
Said infrared ray barrier layer is the Ag layer;
Second dielectric combination layer is Si
3N
4Layer, or ZnSnO
3Layer and Si
3N
4The combination layer of layer.
5. a kind of enhance protection type radiation coated glass capable of being toughened according to claim 4 is characterized in that:
The thicknesses of layers of said first dielectric combination layer, second dielectric combination layer is 10-40nm;
The thicknesses of layers of said first protective layer, second protective layer is 1-10nm;
The thicknesses of layers of said infrared ray barrier layer is 5-15nm;
Said metal absorbed layer is 5-20nm;
The thicknesses of layers of said medium protective layer is 5-20nm.
6. the manufacturing process of an enhance protection type radiation coated glass capable of being toughened adopts vacuum magnetic-control sputtering method and radio frequency plasma to strengthen the chemical vapour deposition technique plated film, it is characterized in that, may further comprise the steps:
Step 1, cleaning, dry glass substrate;
Step 2, on glass substrate, adopt magnetron sputtering method to be coated with the metal absorbed layer;
On the metal absorbed layer, adopt magnetron sputtering method to be coated with first dielectric combination layer;
On first dielectric layer, adopt magnetron sputtering method to be coated with first protective layer;
On first protective layer, adopt magnetron sputtering method to be coated with the infrared ray barrier layer;
On the infrared ray barrier layer, adopt magnetron sputtering method to be coated with second protective layer;
On second protective layer, adopt magnetron sputtering method to be coated with second dielectric combination layer;
Step 3, on second dielectric layer, adopt radio frequency plasma to strengthen chemical vapour deposition technique deposition medium protective layer, at 1*10
-6In the mbar background vacuum environment, charge into CH
4, H
2And N
2Gas, wherein CH
4And H
2Flow percentage be 30%-80%, gas purity is 99.99%, deposition pressure is 2～3*10
-3Mbar, the radio-frequency power supply frequency is 13.56MHz, and radio-frequency power is 5.5KW, and polar plate spacing is 60mm.
7. the manufacturing process of a kind of enhance protection type radiation coated glass capable of being toughened according to claim 6 is characterized in that:
Said metal absorbed layer, through the sputter in the straight argon atmosphere of direct current planar negative electrode, cathode targets is a kind of in Ti, SST, Cr, Ni, the NiCr alloys target;
Said infrared ray barrier layer, through the sputter in argon atmosphere of direct current planar negative electrode, a kind of in the optional Ag of cathode targets, AgCu alloy, AgNi alloy, the AgTi alloy;
Said first, second dielectric combination layer, through the sputter in nitrogen argon, oxygen argon or nitrogen oxygen argon atmosphere of rotation interchange negative electrode, cathode targets is one or more among SiAl, Sn, ZnSn, TxO, Zn, AZO, the NbxO;
Said first, second protective layer, through the sputter in the straight argon atmosphere of direct current planar negative electrode, cathode targets is a kind of in Ti, SST, Cr, Ni, the NiCr alloy.
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