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一种超耐磨高透过率氧化锆薄膜的制备方法 【EN】A kind of preparation method of super abrasive high transmittance zirconia film

申请(专利)号:CN201711415344.9国省代码:安徽 34
申请(专利权)人:【中文】中建材蚌埠玻璃工业设计研究院有限公司【EN】China building materials Bengbu Glass Industry Design & Research Institute Co., Ltd.
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摘要:
【中文】本发明公开一种超耐磨高透过率氧化锆薄膜的制备方法,包括以下步骤:S1、清洗衬底,去除衬底表面污渍并吹干;S2、将清洗后的衬底置入磁控溅射镀膜设备,当溅射腔体真空度符合要求时,对溅射腔体进行烘烤,排出溅射腔体内的杂质分子;S3、烘烤结束后,以锆为靶材,采用射频电源,氩气与氧气为溅射气体,通过磁控溅射在衬底沉积氧化锆薄膜;在过氧的情况下,采用大功率射频溅射,保证锆原子在沉积过程中能与反应气体充分反应得到氧化锆;大功率溅射可以保证锆原子初始能量较高,沉积在衬底时可以使氧化锆薄膜更致密,耐磨性好,且可以保证膜基结合力更好;工艺过程可以精确控制,保证氧化锆薄膜的厚度可控,满足透过率要求。 【EN】Paragraph:The present invention discloses a kind of preparation method of super abrasive high transmittance zirconia film, includes the following steps:S1, cleaning substrate, remove substrate surface spot and dry up;S2, the substrate after cleaning is placed in magnetic-controlled sputtering coating equipment, when sputter chamber vacuum degree meets the requirements, sputter chamber is toasted, discharge the impurity molecule in sputter chamber;After S3, baking, using zirconium as target, using radio-frequency power supply, argon gas is sputter gas with oxygen, by magnetron sputtering in substrate deposition zirconia film;It in the case of peroxide, is sputtered using high-power RF, ensures that in deposition process zirconium oxide can be fully obtained by the reaction with reaction gas in zirconium atom;High-power sputtering can ensure that zirconium atom primary power is higher, can make zirconia film finer and close when being deposited on substrate, and wearability is good, and can ensure that film-substrate cohesion is more preferable;Technical process can be controlled accurately, ensure that the thickness of zirconia film is controllable, meet transmitance requirement.Image:

主权项:
【中文】1.一种超耐磨高透过率氧化锆薄膜的制备方法,其特征在于,包括以下步骤: S1、清洗衬底,去除衬底表面污渍并吹干; S2、将清洗后的衬底置入磁控溅射镀膜设备,当溅射腔体真空度符合要求时,对溅射腔体进行烘烤,排出溅射腔体内的杂质分子; S3、烘烤结束后,以锆为靶材,采用射频电源,氩气与氧气为溅射气体,通过磁控溅射在衬底沉积氧化锆薄膜。 【EN】1. a kind of preparation method of super abrasive high transmittance zirconia film, which is characterized in that include the following steps: S1, cleaning substrate, remove substrate surface spot and dry up; S2, the substrate after cleaning is placed in magnetic-controlled sputtering coating equipment, when sputter chamber vacuum degree meets the requirements, to sputtering chamber Body is toasted, and discharges the impurity molecule in sputter chamber; After S3, baking, using zirconium as target, using radio-frequency power supply, argon gas is sputter gas with oxygen, is existed by magnetron sputtering Substrate deposition zirconia film.


说明书

【中文】

一种超耐磨高透过率氧化锆薄膜的制备方法

技术领域

本发明涉及玻璃薄膜制造技术领域,具体是一种超耐磨高透过率氧化锆薄膜的制备方法。

背景技术

玻璃因其优异的光学、力学性能成为我们日常生活中广泛使用的一种建筑、装饰材料,而在长时间的使用过程中,玻璃的耐磨性会遭到极大的考验。我们用磁控溅射技术在玻璃表面镀上一层高致密性薄膜,会大大提高玻璃的耐磨性,改善玻璃品质。

氧化锆是锆的主要氧化物,化学性质不活泼,难溶于水、盐酸和稀硫酸,且具有高熔点,高电阻率和低热膨胀系数的性质,线胀系数较高,高温下形变较小,接近金属基质。弹性模量高,缓解应力能力强,弹性极限内受到形变之后回复能力强,应力向周围发散快。其本身密度高,且非常致密。作为薄膜时其具有高透过率,高致密性,耐酸、碱、盐。这些优良的性能为其作为最外层保护型硬质膜打下了良好的基础。

但是目前氧化锆薄膜的制备工艺存在缺陷,制备出来的氧化锆薄膜耐磨性不高,透过率不好。

发明内容

本发明的目的在于提供一种超耐磨高透过率氧化锆薄膜的制备方法,该方法制备得到的氧化锆薄膜均匀致密、耐磨性好、透过率高,且工艺简单。

本发明解决其技术问题所采用的技术方案是:

一种超耐磨高透过率氧化锆薄膜的制备方法,包括以下步骤:

S1、清洗衬底,去除衬底表面污渍并吹干;

S2、将清洗后的衬底置入磁控溅射镀膜设备,当溅射腔体真空度符合要求时,对溅射腔体进行烘烤,排出溅射腔体内的杂质分子;

S3、烘烤结束后,以锆为靶材,采用射频电源,氩气与氧气为溅射气体,通过磁控溅射在衬底沉积氧化锆薄膜。

进一步的,步骤S3磁控溅射前还包括预溅射步骤,使靶材起辉,去除靶材表面杂质。

进一步的,步骤S3磁控溅射射频电源功率150w,氩气为30sccm,氧气12~15sccm。

进一步的,预溅射射频电源功率250W,先以200sccm氩气使靶材起辉,然后以30sccm氩气预溅射1h。

进一步的,步骤S2真空度为2.5*10-3Pa,烘烤温度60~65℃,烘烤时间20~30min。

本发明的有益效果是:

一、在磁控溅射前对溅射腔体进行烘烤,排出溅射腔体内的杂质分子,降低分子自由程,使溅射得到的薄膜更致密;

二、在过氧的情况下,采用大功率射频溅射,保证锆原子在沉积过程中能与反应气体充分反应得到氧化锆;

三、大功率溅射可以保证锆原子初始能量较高,沉积在衬底时可以使氧化锆薄膜更致密,耐磨性好,且可以保证膜基结合力更好;

四、采用射频溅射,保证锆靶不会氧中毒;

五、工艺过程可以精确控制,保证氧化锆薄膜的厚度可控,满足透过率要求。

具体实施方式

实施例一

本发明提供一种超耐磨高透过率氧化锆薄膜的制备方法,包括以下步骤:

S1、选用1.1mm普通白玻璃作为衬底,清洗衬底,去除衬底表面污渍并吹干;

S2、将清洗后的衬底置入磁控溅射镀膜设备,对溅射腔体抽真空,当真空度2.5*10-3Pa时,对溅射腔体进行烘烤,烘烤温度60℃,烘烤时间20min,排出溅射腔体内的杂质分子;

S3、烘烤结束后,以锆为靶材,采用射频电源,当真空度为1*10-4Pa时先进行预溅射,预溅射射频电源功率250W,先以200sccm氩气使靶材起辉,然后以30 sccm氩气预溅射1h;

预溅射结束后,在真空度为9.4*10-4Pa时,通入氧气12sccm,再调节真空度到达0.5Pa,射频电源功率150w,溅射15min,在衬底沉积得到透过率83.1%、折射率1.832、厚度39.4nm的氧化锆薄膜。

实施例二

本发明提供一种超耐磨高透过率氧化锆薄膜的制备方法,包括以下步骤:

S1、选用1.1mm普通白玻璃作为衬底,清洗衬底,去除衬底表面污渍并吹干;

S2、将清洗后的衬底置入磁控溅射镀膜设备,对溅射腔体抽真空,当真空度2.5*10-3Pa时,对溅射腔体进行烘烤,烘烤温度65℃,烘烤时间30min,排出溅射腔体内的杂质分子;

S3、烘烤结束后,以锆为靶材,采用射频电源,当真空度为1*10-4Pa时先进行预溅射,预溅射射频电源功率250W,先以200sccm氩气使靶材起辉,然后以30 sccm氩气预溅射1h;

预溅射结束后,在真空度为7.9*10-4Pa时,通入氧气15sccm,再调节真空度到达0.5Pa,射频电源功率150w,溅射15min,在衬底沉积得到透过率82.5%、折射率1.81、厚度26.7nm的氧化锆薄膜。

以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制;任何熟悉本领域的技术人员,在不脱离本发明技术方案范围情况下,都可利用上述揭示的方法和技术内容对本发明技术方案做出许多可能的变动和修饰,或修改为等同变化的等效实施例。因此,凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所做的任何简单修改、等同替换、等效变化及修饰,均仍属于本发明技术方案保护的范围内。

【EN】

A kind of preparation method of super abrasive high transmittance zirconia film

Technical field

The present invention relates to glass film manufacturing technology field, the system of specifically a kind of super abrasive high transmittance zirconia film

Preparation Method.

Background technology

Glass becomes a kind of widely used building, decoration in our daily lifes because of its excellent optics, mechanical property

Material, and during much time using, the wearability of glass can be tested greatly.We are existed with magnetron sputtering technique

Glass surface plates a floor height compactness film, can greatly improve the wearability of glass, improves glass quality.

Zirconium oxide is the main oxides of zirconium, and chemical property torpescence is insoluble in water, hydrochloric acid and dilute sulfuric acid, and with height

The property of fusing point, high resistivity and low thermal coefficient of expansion, linear expansion coefficient is higher, and deformation is smaller under high temperature, close to metal matrix.Bullet

Property modulus it is high, alleviate that stress ability is strong, and strong by recovery capacity after deformation in elastic limit, stress dissipates fast to surrounding.Its

Density itself is high, and very fine and close.It is with high transmittance, high compactness, acid and alkali resistance, salt during as film.These are excellent

Performance is laid a good foundation for it as outermost layer protection type hard films.

But the preparation process existing defects of current zirconia film, the zirconia film wearability prepared is not high,

Transmitance is bad.

Invention content

The purpose of the present invention is to provide a kind of preparation method of super abrasive high transmittance zirconia film, prepared by this method

Obtained zirconia film even compact, wearability is good, transmitance is high, and simple for process.

The technical solution adopted by the present invention to solve the technical problems is:

A kind of preparation method of super abrasive high transmittance zirconia film, includes the following steps:

S1, cleaning substrate, remove substrate surface spot and dry up;

S2, the substrate after cleaning is placed in magnetic-controlled sputtering coating equipment, when sputter chamber vacuum degree meets the requirements, to sputtering chamber

Body is toasted, and discharges the impurity molecule in sputter chamber;

After S3, baking, using zirconium as target, using radio-frequency power supply, argon gas is sputter gas with oxygen, is existed by magnetron sputtering

Substrate deposition zirconia film.

Further, pre-sputtering step is further included before step S3 magnetron sputterings, makes target build-up of luminance, removal target material surface is miscellaneous

Matter.

Further, step S3 magnetron sputterings radio-frequency power supply power 150w, argon gas 30sccm, 12~15sccm of oxygen.

Further, pre-sputtering radio-frequency power supply power 250W first makes target build-up of luminance, then with 30 with 200sccm argon gas

Sccm argon gas pre-sputterings 1h.

Further, step S2 vacuum degrees are 2.5*10-3Pa, 60~65 DEG C of baking temperature, 20~30min of baking time.

The beneficial effects of the invention are as follows:

First, sputter chamber is toasted before magnetron sputtering, discharges the impurity molecule in sputter chamber, it is free to reduce molecule

Journey makes the film that sputtering obtains finer and close;

2nd, it in the case of peroxide, is sputtered using high-power RF, ensures that zirconium atom can fill in deposition process with reaction gas

Divide and zirconium oxide is obtained by the reaction;

3rd, high-power sputtering can ensure that zirconium atom primary power is higher, zirconia film can be made more to cause when being deposited on substrate

Close, wearability is good, and can ensure that film-substrate cohesion is more preferable;

4th, using radio-frequency sputtering, ensure that zirconium target will not oxygen poisoning;

5th, technical process can be controlled accurately, ensure that the thickness of zirconia film is controllable, meet transmitance requirement.

Specific embodiment

Embodiment one

The present invention provides a kind of preparation method of super abrasive high transmittance zirconia film, includes the following steps:

S1, the common white glass of 1.1mm is selected to clean substrate as substrate, remove substrate surface spot and dry up;

S2, the substrate after cleaning is placed in magnetic-controlled sputtering coating equipment, sputter chamber is vacuumized, as vacuum degree 2.5*10-3Pa

When, sputter chamber is toasted, 60 DEG C, baking time 20min of baking temperature, discharge the impurity molecule in sputter chamber;

After S3, baking, using zirconium as target, using radio-frequency power supply, when vacuum degree is 1*10-4Pre-sputtering is first carried out during Pa, in advance

Radio-frequency power supply power 250W is sputtered, target build-up of luminance is first made with 200sccm argon gas, then with 30 sccm argon gas pre-sputterings 1h;

It is 9.4*10 in vacuum degree after pre-sputtering-4During Pa, oxygen 12sccm is passed through, then adjusts vacuum degree and reaches 0.5Pa,

Radio-frequency power supply power 150w sputters 15min, and transmitance 83.1%, refractive index 1.832, thickness 39.4nm are obtained in substrate deposition

Zirconia film.

Embodiment two

The present invention provides a kind of preparation method of super abrasive high transmittance zirconia film, includes the following steps:

S1, the common white glass of 1.1mm is selected to clean substrate as substrate, remove substrate surface spot and dry up;

S2, the substrate after cleaning is placed in magnetic-controlled sputtering coating equipment, sputter chamber is vacuumized, as vacuum degree 2.5*10-3Pa

When, sputter chamber is toasted, 65 DEG C, baking time 30min of baking temperature, discharge the impurity molecule in sputter chamber;

After S3, baking, using zirconium as target, using radio-frequency power supply, when vacuum degree is 1*10-4Pre-sputtering is first carried out during Pa, in advance

Radio-frequency power supply power 250W is sputtered, target build-up of luminance is first made with 200sccm argon gas, then with 30 sccm argon gas pre-sputterings 1h;

It is 7.9*10 in vacuum degree after pre-sputtering-4During Pa, oxygen 15sccm is passed through, then adjusts vacuum degree and reaches 0.5Pa,

Radio-frequency power supply power 150w sputters 15min, and transmitance 82.5%, refractive index 1.81, thickness 26.7nm are obtained in substrate deposition

Zirconia film.

The above described is only a preferred embodiment of the present invention, not make limitation in any form to the present invention;Appoint

What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above

Method and technology contents make technical solution of the present invention many possible changes and modifications or are revised as the equivalent reality of equivalent variations

Apply example.Therefore, every content without departing from technical solution of the present invention, technical spirit according to the present invention do above example

Any simple modification, equivalent replacement, equivalence changes and modification, still fall within technical solution of the present invention protection in the range of.

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