CN103738007B - Glassware and preparation method thereof - Google Patents
Glassware and preparation method thereof Download PDFInfo
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- CN103738007B CN103738007B CN201310681148.1A CN201310681148A CN103738007B CN 103738007 B CN103738007 B CN 103738007B CN 201310681148 A CN201310681148 A CN 201310681148A CN 103738007 B CN103738007 B CN 103738007B
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Abstract
The present invention relates to a kind of glassware and preparation method thereof.This glassware comprises glass substrate and is laminated in the Hardening layer on described glass substrate, and the material of described Hardening layer comprises aluminium oxide and neodymium oxide.Above-mentioned glassware have hardness high, to be not easily scratched and feature that light transmittance is high, not only can be applied to the face glass of electronic product, showcase, glass tea table etc., improve service life and keep attractive in appearance, and diamond glass cutter glass-cutting can be replaced as glass cutter, apply comparatively extensive.
Description
Technical field
The present invention relates to glass technology field, particularly relate to a kind of glassware and preparation method thereof.
Background technology
Glassware is widely used in various occasion, as the face glass, showcase, glass tea table etc. of electronic product.Because the hardness of glassware is scratched not, easily, cause the life-span of the article of the goods applying glass shorter, or after a long time use, surface is scratched and affect attractive in appearance.
Summary of the invention
Based on this, be necessary for provide a kind of hardness higher, to be not easily scratched and glassware that light transmittance is high.
Further, a kind of preparation method of glassware is provided.
A kind of glassware, comprise glass substrate and be laminated in the Hardening layer on described glass substrate, the material of described Hardening layer comprises aluminium oxide and neodymium oxide.
Wherein in an embodiment, the mass ratio of described aluminium oxide and neodymium oxide is 95:5 ~ 99:1.
Wherein in an embodiment, the thickness of described Hardening layer is
~
.
Wherein in an embodiment, the thickness of described glass substrate is 0.3 millimeter ~ 20 millimeters.
A preparation method for glassware, comprises the steps:
Glass substrate is provided; And
Adopt magnetron sputtering to prepare Hardening layer on described glass substrate, obtain described glassware.
Wherein in an embodiment, before described employing magnetron sputtering prepares the step of Hardening layer on described glass substrate, also comprise the step that described glass substrate is cleaned, the step of described cleaning is: after described glass substrate is used pure water and caustic dip successively, then carries out two fluid spray, pure water spray and high-pressure spraying successively.
Wherein in an embodiment, described employing magnetron sputtering is prepared in the step of Hardening layer on described glass substrate, and the vacuum of described magnetron sputtering is 2.5 × 10
-1pa ~ 3.50 × 10
-1pa.
Wherein in an embodiment, described employing magnetron sputtering is prepared in the step of Hardening layer on described glass substrate, and the temperature of described glass substrate is 120 DEG C ~ 200 DEG C.
Wherein in an embodiment, the step that described employing magnetron sputtering prepares Hardening layer on described glass substrate adopts neodymium aluminium alloy target, and passes into oxygen and argon gas.
Wherein in an embodiment, the flow of described oxygen is 200sccm ~ 220sccm, and the total gas pressure of described oxygen and argon gas is 0.3Pa.
Above-mentioned glassware comprises glass substrate and is laminated in the Hardening layer on glass substrate, and the material of Hardening layer comprises aluminium oxide and neodymium oxide.This glassware has higher hardness, to be not easily scratched and the high feature of light transmittance, not only can be applied to the face glass of electronic product, showcase, glass tea table etc., improve service life and keep attractive in appearance, and diamond glass cutter glass-cutting can be replaced as glass cutter, apply comparatively extensive.
Accompanying drawing explanation
Fig. 1 is the structural representation of an embodiment glassware;
Fig. 2 is the flow chart of the preparation method of the glassware of an embodiment;
Fig. 3 is the SEM figure of the Hardening layer of the glassware of embodiment 1.
Detailed description of the invention
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
Refer to Fig. 1, the glassware 100 of an embodiment, the Hardening layer 40 comprising glass substrate 20 and be laminated on glass substrate 20.
Glass substrate 20 is preferably the good unorganic glass substrate of heat resistance.
The thickness of glass substrate 20 is preferably 0.3 millimeter ~ 20 millimeters.
The thickness of glass substrate 20 is more preferably 0.5 millimeter ~ 10 millimeters, to make glass substrate 20 have higher intensity, and glass-cutting comparatively easily when glassware 100 is used as glass cutter.
The material of Hardening layer 40 comprises aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3).Hardening layer 40 is aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3) rete that formed.
Hardening layer 40 has higher hardness and higher chemical stability.Further, the light transmittance of Hardening layer 40 is up to 95.0%.
The thickness of Hardening layer 40 is too little, and technique is difficult to control, and adhesive force on glass substrate 20 is too poor; The thickness of Hardening layer 40 is too large, and preparation cost is high.Therefore, preferably, the thickness of Hardening layer 40 is
~
.
Neodymium is rare earth metal, and price costly.Under the prerequisite meeting performance requirement, the content of neodymium is lower, and the price of this glassware 100 is lower.Preferably, the mass ratio of aluminium oxide and neodymium oxide is 95:5 ~ 99:1, and to make, the hardness of Hardening layer 40 is comparatively large, light transmission is good, chemical stability is good, and can be cost-saving.More preferably, the mass ratio of aluminium oxide and neodymium oxide is 98:2.
Be provided with Hardening layer 40, make the hardness of glassware 100 higher, anti-scratch performance is good, and can meet the demand of glass-cutting, makes this glassware 100 can as glass cutter for glass-cutting.
At the glass substrate 20 Hardening layer 40 that stacked hardness is higher on the surface, can cover glass substrate 20 preferably, prevent glass substrate 20 surface to be scratched, be conducive to improving the life-span of the product using this glassware 100 and keep continuation aesthetic.
Due to above-mentioned glassware 100 have hardness high, be not easily scratched with light transmittance high, various occasion can be widely used in, as the face glass of electronic product, showcase, glass tea table etc.
Further, this glassware 100 may be used for cutting various glass, can processing and manufacturing ultra-large type high rigidity product, is applicable to suitability for industrialized production.Such as, for glass-cutting prepare touch-screen face glass, cut other large-scale anti-scratch glass etc.
When using as glass cutter, above-mentioned glassware 100 is relative to price diamond glass cutter costly, and its price is lower.
Refer to Fig. 2, the preparation method of the glassware of an embodiment, comprise the steps S110 and step S120.The preparation method of this glassware is for the preparation of above-mentioned glassware 100.
Step S110: glass substrate is provided.
Preferably, thickness is provided to be the glass substrate of 0.3 millimeter ~ 20 millimeters.
In order to ensure that glass substrate cleans, before carrying out step S110, first glass substrate is cleaned.The step of cleaning is: after glass substrate is used pure water and caustic dip successively, then carries out two fluids (BJ) spray, pure water spray and high-pressure spraying successively.
Alkali lye is alkaline detergent solution, if alkalescence is as washing powder solution, alkaline liquid detergent solution etc.
High-pressure spraying refers to and to spray with High Pressure Pure Water.Preferably, the pressure of pure water is 1.2kg/cm
2~ 1.7kg/cm
2, fully to remove the pollutant such as dust, greasy dirt on glass substrate, but do not damage glass substrate.More preferably, the pressure of pure water is 1.5kg/cm
2.
After cleaning glass substrate is clean, use cold wind and heated-air drying successively, then check glass baseplate surface cleaning quality, qualified, for subsequent use.
Step S120: adopt magnetron sputtering to prepare Hardening layer on the glass substrate, obtain glassware.
Clean, dry glass substrate are put on the specimen holder of magnetron sputtering plating room, magnetron sputtering plating room is evacuated to certain vacuum degree, and glass substrate is heated to uniform temperature, and remain on this temperature, pass into oxygen and argon gas, start magnetron sputtering plating, prepare Hardening layer on the glass substrate.
The material of Hardening layer comprises aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3).Aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3) mass ratio be preferably 95:5 ~ 99:1, be more preferably 98:2.
Preferably, the vacuum of magnetron sputtering plating room is 2.5 × 10
-1pa ~ 3.50 × 10
-1pa.
Preferably, glass substrate is heated to 120 DEG C ~ 200 DEG C, and maintains 120 DEG C ~ 200 DEG C and carry out plated film.The temperature of glass substrate is too high then to be required high to the heatproof of glass substrate, and Glass breadks easily splits; The too low rete that will cause of temperature loosens, and affects stability and hardness.Therefore, the temperature of glass substrate is preferably 120 DEG C ~ 200 DEG C, is more preferably 150 DEG C.
Further, employing glass substrate is that the coating process of 150 DEG C makes chemical durability of layers good, and require low to storage condition, it is convenient to store.
Preferably, in 720 seconds, glass substrate is heated to 120 DEG C ~ 200 DEG C, to avoid glass substrate to be acutely heated, is conducive to preventing breaking glass panel.
Adopt neodymium aluminium alloy target, and pass into oxygen and argon gas.Oxygen is as reacting gas, and argon gas is as process gas.Oxygen and reactive aluminum generate aluminium oxide, and oxygen and neodymium react and generate neodymium oxide.The performance of flow-control to Hardening layer of oxygen plays material impact.
The neodymium of neodymium aluminium alloy target and the mol ratio of aluminium are 27:144.
Adopt suitable oxygen flow, the Hardening layer that compactness is good, hardness is high, stable chemical performance, adhesion property are good can be prepared.Preferably, the flow of oxygen is 200sccm ~ 220sccm.The total gas pressure of oxygen and argon gas is 0.3Pa.
Preferably, the distance between neodymium aluminium alloy target and glass substrate is 20 millimeters.
Preferably, when magnetron sputtering prepares Hardening layer, the speed of service of glass substrate is 30 mm/second.
Preferably, the voltage of magnetron sputtering is 300V ~ 350V, and power is 800W ~ 1300W.
Be 2.5 × 10 in vacuum
-1pa ~ 3.50 × 10
-1the total gas pressure that Pa, glass substrate temperature are 150 DEG C, the flow of oxygen is 200sccm ~ 220sccm, oxygen and argon gas is 0.3Pa, distance between neodymium aluminium alloy target and glass substrate is 20 millimeters, the speed of service of glass substrate be 30 mm/second and voltage be 300V ~ 350V and power is under the process conditions of 800W ~ 1300W, and preparation-obtained Hardening layer has stable chemical performance, hardness height is not easily scratched, not easily occur that the fine and close height of cracking, not easily demoulding and rete not easily occurs the advantages such as spot.
The thickness of Hardening layer is preferably
~
.The plated film time is selected from according to required thickness.Be provided with thickness monitoring instrument in coating process and monitor thicknesses of layers in real time, to prepare the Hardening layer that thickness meets the demands.
When prepared glassware uses as glass cutter, the preparation method of its preparation method and traditional diamond glass cutter is generally in special metallic bond, add diamond abrasive, sinter under certain temperature, pressure, vacuum state, form through multiple manufacturing process Precision Machining, preparation technology is loaded down with trivial details.And preparation method's technique of above-mentioned glassware is simple, preparation efficiency is high, and without the need to adding metallic bond, preparation cost is lower.
And the preparation method of above-mentioned glassware, the temperature of glass substrate is only 150 DEG C, and relative to general magnetron sputtering plating, temperature is lower, and energy consumption is low.
The preparation method of above-mentioned glassware, can large-area coating film, can prepare large-scale high rigidity, light transmittance is high, stable chemical performance is high glassware.
Set forth further below by way of specific embodiment.
Embodiment 1
Prepare glassware
1, provide thickness to be the unorganic glass substrate of 2.0mm, after this glass substrate is used pure water and caustic dip successively, then carry out two fluid spray, pure water spray and high-pressure spraying successively, then cold wind and hot blast drying is used successively, inspection glass baseplate surface cleaning quality is qualified, for subsequent use;
2, clean, dry glass substrate are put on the specimen holder of magnetron sputtering plating room, magnetron sputtering plating room is evacuated to 2.5 × 10
-1pa, and in 720 seconds, glass substrate is heated to 150 DEG C, and the temperature maintaining glass substrate is 150 DEG C, passes into oxygen and argon gas, the flow of oxygen is 200ccm
2the total gas pressure of oxygen and argon gas is 0.3Pa, the speed of service of glass substrate is 30 mm/second, be 320V at voltage, power is under 950W, using aluminium neodymium alloy target (mol ratio of aluminium and neodymium is for 27:144) as sputtering target material, start magnetron sputtering plating, plated film 120 seconds, prepares Hardening layer on the glass substrate, obtains glassware.The material of Hardening layer comprises aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3), wherein, aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3) mass ratio be 98:2, the thickness of Hardening layer is
, light transmittance reaches 95%.
Preparation-obtained for the present embodiment 1 glassware is carried out moisture-proof experiment.By this glassware in 60 DEG C, place 24 hours in environment at relative humidity 90%RH, without falling film phenomenon, and Hardening layer surface inviolateness.
Preparation-obtained for the present embodiment 1 glassware is carried out heat resistance experiment.In air, toast this glassware 1 hour by 200 DEG C of temperature, Hardening layer is without cracking phenomena and other anomalies.
Preparation-obtained for the present embodiment 1 glassware is carried out solvent resistance experiment.This glassware is soaked 5 minutes in the alcohol of normal temperature, fall film phenomenon without bulk, and face is without color exception.
Preparation-obtained for the present embodiment 1 glassware is carried out alkali resistance experiment.Be soak this glassware 5 minutes in the NaOH of 2% in the mass fraction of normal temperature, fall film phenomenon without bulk, and face be without color exception.
Above-mentioned experiment proves, the chemical stability of Hardening layer is higher.
Inspection Hardening layer adhesive force on the glass substrate (3B ~ 5B is qualified), measurement result is 3B, qualified.
By the wearability of the 20 times test Hardening layers in erasing rubber friction Hardening layer surface under 1KG pressure, after test, rete, without cracking and obscission, illustrates that the wearability of this Hardening layer is better.
With 9H pencil eraser 5 under 1KG pressure, after test, rete is without cracking and obscission, and illustrate that the hardness of this Hardening layer is better, at more than 9H, therefore, the anti-scratch performance of this glassware is good, and can be used in glass-cutting.
Fig. 3 is the SEM picture on the Hardening layer surface of the glassware of the present embodiment 1.As seen from Figure 3, the compactness of Hardening layer is better.
Embodiment 2
Prepare glassware
1, provide thickness to be the unorganic glass substrate of 20mm, after this glass substrate is used pure water and caustic dip successively, then carry out two fluid spray, pure water spray and high-pressure spraying successively, then cold wind and hot blast drying is used successively, inspection glass baseplate surface cleaning quality is qualified, for subsequent use;
2, clean, dry glass substrate are put on the specimen holder of magnetron sputtering plating room, magnetron sputtering plating room is evacuated to 3.5 × 10
-1pa, and in 720 seconds, glass substrate is heated to 120 DEG C, and the temperature maintaining glass substrate is 120 DEG C, passes into oxygen and argon gas, the flow of oxygen is 220ccm
2the total gas pressure of oxygen and argon gas is 0.3Pa, the speed of service of glass substrate is 30 mm/second, be 340V at voltage, power is under 1000W, using aluminium neodymium alloy target (mol ratio of aluminium and neodymium is for 27:144) material as sputtering target material, start magnetron sputtering plating, plated film 240 seconds, prepares Hardening layer on the glass substrate, obtains glassware.The material of Hardening layer comprises aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3), wherein, aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3) mass ratio be 95:5, the thickness of Hardening layer is
, light transmittance reaches 98%.
The hardness of testing this glassware is 10H.
Embodiment 3
Prepare glassware
1, provide thickness to be the unorganic glass substrate of 0.3mm, after this glass substrate is used pure water and caustic dip successively, then carry out two fluid spray, pure water spray and high-pressure spraying successively, then cold wind and hot blast drying is used successively, inspection glass baseplate surface cleaning quality is qualified, for subsequent use;
2, clean, dry glass substrate are put on the specimen holder of magnetron sputtering plating room, magnetron sputtering plating room is evacuated to 3.0 × 10
-1pa, and in 720 seconds, glass substrate is heated to 200 DEG C, and the temperature maintaining glass substrate is 200 DEG C, passes into oxygen and argon gas, the flow of oxygen is 220ccm
2the total gas pressure of oxygen and argon gas is 0.3Pa, the speed of service of glass substrate is 30 mm/second, be 350V at voltage, power is under 1100W, using aluminium neodymium alloy target (mol ratio of aluminium and neodymium is for 27:144) as sputtering target material, start magnetron sputtering plating, plated film 180 seconds, prepares Hardening layer on the glass substrate, obtains glassware.The material of Hardening layer comprises aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3), wherein, aluminium oxide (Al
2o
3) and neodymium oxide (Nd
2o
3) mass ratio be 99:1, the thickness of Hardening layer is
, light transmittance reaches 96%.
The hardness of testing this glassware is 10H.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (7)
1. a glassware, it is characterized in that, comprise glass substrate and be laminated in the Hardening layer on described glass substrate, the material of described Hardening layer is made up of aluminium oxide and neodymium oxide, the mass ratio of described aluminium oxide and neodymium oxide is 95:5 ~ 99:1, and the thickness of described Hardening layer is
the thickness of described glass substrate is 0.3 millimeter ~ 20 millimeters.
2. a preparation method for glassware, is characterized in that, comprises the steps:
Glass substrate is provided; And
Adopt magnetron sputtering to prepare Hardening layer on described glass substrate, obtain described glassware, the material of described Hardening layer is made up of aluminium oxide and neodymium oxide, and the mass ratio of described aluminium oxide and neodymium oxide is 95:5 ~ 99:1, and the thickness of described Hardening layer is
the thickness of described glass substrate is 0.3 millimeter ~ 20 millimeters.
3. the preparation method of glassware according to claim 2, it is characterized in that, before described employing magnetron sputtering prepares the step of Hardening layer on described glass substrate, also comprise the step that described glass substrate is cleaned, the step of described cleaning is: after described glass substrate is used pure water and caustic dip successively, then carries out two fluid spray, pure water spray and high-pressure spraying successively.
4. the preparation method of glassware according to claim 2, is characterized in that, described employing magnetron sputtering is prepared in the step of Hardening layer on described glass substrate, and the vacuum of described magnetron sputtering is 2.5 × 10
-1pa ~ 3.50 × 10
-1pa.
5. the preparation method of glassware according to claim 2, is characterized in that, described employing magnetron sputtering is prepared in the step of Hardening layer on described glass substrate, and the temperature of described glass substrate is 120 DEG C ~ 200 DEG C.
6. the preparation method of glassware according to claim 2, is characterized in that, the step that described employing magnetron sputtering prepares Hardening layer on described glass substrate adopts neodymium aluminium alloy target, and passes into oxygen and argon gas.
7. the preparation method of glassware according to claim 6, is characterized in that, the flow of described oxygen is 200sccm ~ 220sccm, and the total gas pressure of described oxygen and argon gas is 0.3Pa.
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|---|---|---|---|
| CN201310681148.1A CN103738007B (en) | 2013-12-13 | 2013-12-13 | Glassware and preparation method thereof |
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| CN102717548A (en) * | 2012-05-29 | 2012-10-10 | 江西沃格光电科技有限公司 | Glass protecting film, glass product and anti-scratching of glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101448637A (en) * | 2006-05-17 | 2009-06-03 | 3M创新有限公司 | Armor composites and methods of making same |
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2013
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|---|---|---|---|---|
| CN102351438A (en) * | 2011-07-15 | 2012-02-15 | 深圳市三鑫精美特玻璃有限公司 | Method for preparing membrane on glass substrate and glass substrate and membrane system structure |
| CN102717548A (en) * | 2012-05-29 | 2012-10-10 | 江西沃格光电科技有限公司 | Glass protecting film, glass product and anti-scratching of glass |
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