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一种采用磁控溅射制备柔性稀土氧化物薄膜的方法 【EN】A method of flexible rare-earth sull is prepared using magnetron sputtering

申请(专利)号:CN201610400932.4国省代码:江苏 32
申请(专利权)人:【中文】扬州君禾薄膜科技有限公司【EN】Yangzhou Jun Ye Film Technology Co., Ltd.
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摘要:
【中文】本发明公开了一种采用磁控溅射制备柔性稀土氧化物薄膜的方法,包括如下步骤:a:选用4N稀土金属靶材;b:采用液态PDMS前体作为衬底;c:抽真空,通入氩气,预溅射清洗靶材表面;d:升温加热台到沉积薄膜所需要的温度并保温;e:通入混合气体,施加溅射功率,控制气体流量,开始向衬底表面镀膜1小时;f:恒温3小时,待温度降至室温时即制得柔性薄膜。本发明解决了现有常规刚性衬底上无法制备可剥离功能薄膜的技术问题,改变了之前稀土金属氧化物薄膜只能沉积在刚性衬底的现状,而且稀土金属氧化物薄膜膜厚可精确控制。 【EN】Paragraph:The invention discloses a kind of methods for preparing flexible rare-earth sull using magnetron sputtering, include the following steps: a: selecting 4N rare earth metal target;B: using liquid PDMS precursor as substrate;C: vacuumizing, and is passed through argon gas, pre-sputter cleaning target material surface;D: temperature required for heating warm table to deposition film is simultaneously kept the temperature;E: being passed through mixed gas, applies sputtering power, controls gas flow, starts to substrate surface plated film 1 hour;F: constant temperature 3 hours, fexible film is obtained when temperature is down to room temperature.The present invention solves the technical issues of can not preparing peelable function film on existing conventional rigid substrate, and rare-earth oxide film can only be deposited on the status of rigid substrate before changing, and rare-earth oxide film film thickness accurately controls.

主权项:
【中文】1.一种采用磁控溅射制备柔性稀土氧化物薄膜的方法,其特征在于:包括如下步骤: a:选用氧化铕靶材为溅射靶材并将其置于磁控溅射室; b:采用液态PDMS前体作为沉积基底,并将液态PDMS衬底旋涂置于磁控溅射室的旋转加热台上; c:对磁控溅射室实施抽真空处理,并通入氩气对溅射靶材进行清洗; d:将旋转加热台加热升温至120℃,并保温1h; e:向磁控溅射室内通入混合气体直至室内压强达到3 帕时启辉实施磁控溅射处理,所述混合气体为氢气、氧气和惰性气体的混合物,其中氢气在混合气体中的含量为5-20%; f:待衬底上沉积薄膜完成后,停止通气,将磁控溅射室内的温度自然冷却至室温,对薄膜进行固化处理即可制得柔性稀土氧化铕薄膜。 【EN】1. a kind of method for preparing flexible rare-earth sull using magnetron sputtering, characterized by the following steps: A: europium oxide target is selected to be sputtering target material and place it in magnetron sputtering chamber; B: added using liquid PDMS precursor as deposition substrate, and by the rotation that liquid PDMS substrate spin coating is placed in magnetron sputtering chamber In thermal station; C: vacuumize process is implemented to magnetron sputtering chamber, and is passed through argon gas and sputtering target material is cleaned; D: rotary heating platform is heated to 120 DEG C, and keeps the temperature 1h; E: being passed through mixed gas into magnetron sputtering room until starter implements magnetron sputtering processing, institute when indoor pressure reaches 3 pa The mixture that mixed gas is hydrogen, oxygen and inert gas is stated, wherein content of the hydrogen in mixed gas is 5-20%; F: after the completion of deposition film on substrate, stop ventilation, by the temperature cooled to room temperature in magnetron sputtering room, to thin Film, which carries out curing process, can be prepared by flexible rare-earth europium oxide film.


说明书

【中文】

一种采用磁控溅射制备柔性稀土氧化物薄膜的方法

技术领域

本发明涉及柔性薄膜的制备方法技术领域,尤其是涉及了一种采用磁控溅射制备柔性稀土氧化物薄膜的方法。

背景技术

现有的薄膜制备技术中的磁控溅射薄膜制备装置, 可以实现金属、非金属单质及化合物等镀膜, 但是在现有的平面反应磁控溅射装置所应用的几乎都是刚性衬底,如硅片,玻璃,云母等。这类衬底无法应用于柔性器件,严重影响了该类薄膜进一步的加工与使用。其次,对于存在变价的金属,如氧化铕薄膜等,当其暴露与空气中后,将被进一步氧化进而影响功能,最终造成器件功能丧失或损坏。

因此,为了解决上述存在的问题,本发明特提供了一种新的技术方案。

发明内容

本发明的目的是提供了一种采用磁控溅射制备柔性稀土氧化物薄膜的方法,能够解决现有技术中刚性衬底无法应用于柔性器件、磁控溅射氧化物薄膜难以加工以及薄膜易氧化变价等问题。

本发明针对上述技术缺陷所采用的技术方案是:

一种采用磁控溅射制备柔性稀土氧化物薄膜的方法,包括如下步骤:

a:选用4N稀土金属靶材为溅射靶材并将其置于磁控溅射室;

b:采用液态PDMS前体作为沉积基底,并将液态PDMS衬底旋涂置于磁控溅射室的旋转加热台上;

c:对磁控溅射室实施抽真空处理,并通入氩气对溅射靶材进行清洗;

d:将旋转加热台加热升温至120℃,并保温1h;

e:向磁控溅射室内通入混合气体直至室内压强达到3 帕时启辉实施磁控溅射处理;

f:待衬底上沉积薄膜完成后,停止通气,将磁控溅射室内的温度自然冷却至室温,对薄膜进行固化处理即可制得柔性稀土氧化物薄膜。

进一步地,步骤a中所述溅射靶材可为氧化铕靶、氧化铬靶、氧化镍靶、氧化铝靶、氧化钛靶。

进一步地,步骤c中所述抽真空处理后的真空度为1.0×10-4 帕。

进一步地,步骤c中通入氩气调整磁控溅射室内的真空度至3 帕,启辉对靶材表面进行清洗, 时间为5-8min。

进一步地,步骤d中在加热旋转台对衬底升温前,需要对衬底进行清洗,清洗方法可为电离清洗或超声清洗中的任意一种。

进一步地,步骤e中所述混合气体为氢气、氧气和惰性气体的混合物,其中氢气在混合气体中的含量为5-20%。

进一步地,所述惰性气体为氩气、氦气和氖气中的至少一种,其中氩气在混合气体中的含量大于50%。

进一步地,步骤e中所述磁控溅射处理的溅射功率为0.5-1.2千瓦,预溅射2-3min后移开挡板,再溅射沉积1h。

进一步地,步骤f中所述磁控溅射室内的温度在自然降温前需要恒温3h。

本发明的有益效果是:

1、本发明制备的柔性稀土氧化物薄膜,能够解决现有溅射薄膜难以加工的缺点,方便薄膜的加工切割;

2、本发明采用PDMS前体作为液体衬底,在120℃下溅射1h,使得氧化物薄膜沉积并固化在PDMS中,即使具有变价特征的氧化铕薄膜也能得到有效保护,避免氧化铕薄膜因暴露而被氧化变价的现象,提高器件的使用寿命和功能性;

3、本发明整个制备工艺简单,稀土金属氧化物薄膜的厚度可精确控制,成本投入低,便于实现产业化生产,提高企业的经济效益。

具体实施方式

一种采用磁控溅射制备柔性稀土氧化物薄膜的方法,包括如下步骤:

a:选用4N稀土金属靶材为溅射靶材并将其置于磁控溅射室,其中溅射靶材可为氧化铕靶、氧化铬靶、氧化镍靶、氧化铝靶、氧化钛靶;

b:采用液态PDMS前体作为沉积基底,并将液态PDMS衬底旋涂置于磁控溅射室的旋转加热台上;

c:对磁控溅射室实施抽真空处理直至真空度为1.0×10-4 帕,并通入氩气调整磁控溅射室内的真空度至3 帕,启辉对靶材表面进行清洗, 时间为5-8min;

d:在加热旋转台对衬底升温前,需要对衬底进行清洗,其后将旋转加热台加热升温至120℃,并保温1h,其中清洗方法可为电离清洗或超声清洗中的任意一种;

e:向磁控溅射室内通入混合气体直至室内压强达到3 帕时启辉实施磁控溅射处理,溅射功率为0.5-1.2千瓦,预溅射2-3min后移开挡板,再溅射沉积1h,其中,混合气体为氢气、氧气和惰性气体的混合物,氢气在混合气体中的含量为5-20%,其次,惰性气体为氩气、氦气和氖气中的至少一种,其中氩气在混合气体中的含量大于50%;

f:待衬底上沉积薄膜完成后,停止通气,恒温3h后,将磁控溅射室内的温度自然冷却至室温,对薄膜进行固化处理即可制得柔性稀土氧化物薄膜。

为了加深对本发明的理解,下面将结合实施例对本发明作进一步详述,该实施例仅用于解释本发明,并不构成对本发明的保护范围的限定。

实施例1

以制备柔性稀土氧化铕薄膜为例对本发明的实施过程做具体阐述。

一种采用磁控溅射制备柔性稀土氧化铕薄膜的方法,包括如下步骤:

a:选用氧化铕靶材为溅射靶材并将其置于磁控溅射室;

b:采用液态PDMS前体作为沉积基底,并将液态PDMS衬底旋涂置于磁控溅射室的旋转加热台上;

c:对磁控溅射室实施抽真空处理直至真空度为1.0×10-4 帕,并通入氩气调整磁控溅射室内的真空度至3 帕,启辉对氧化铕靶材表面进行清洗, 时间为5min;

d:在加热旋转台对衬底升温前,需要对衬底进行超声清洗,清洗时间为5min,其后将旋转加热台加热升温至120℃,并保温1h;

e:向磁控溅射室内通入混合气体直至室内压强达到3 帕时启辉实施磁控溅射处理,溅射功率为1.2千瓦,预溅射2min后移开挡板,再溅射沉积1h,其中,混合气体为氢气、氧气和氩气的混合物,氢气在混合气体中的含量为15%,氩气在混合气体中的含量为80%,其余为氧气。

f:待衬底上沉积薄膜完成后,停止通气,恒温3h后,将磁控溅射室内的温度自然冷却至室温,对薄膜进行固化处理即可制得柔性稀土氧化铕薄膜。

特别强调,氧化铕薄膜具有变价特征的特点,当氧化铕薄膜被暴露在空气中后,很容易被进一步氧化而发生变价影响功能,针对氧化铕薄膜的这一局限性,本发明采用PDMS前体作为液体衬底,在120℃下溅射1h,使得氧化铕薄膜沉积并固化在PDMS中,即使氧化铕薄膜被暴露在空气中,也能保证氧化铕薄膜得到有效保护,避免氧化铕薄膜被氧化变价的现象,提高器件的使用寿命和功能性。

本发明的有益效果是:本发明制备的柔性稀土氧化物薄膜,能够解决现有溅射薄膜难以加工的缺点,方便薄膜的加工切割;而且本发明整个制备工艺简单,稀土金属氧化物薄膜的厚度可精确控制,成本投入低,便于实现产业化生产,提高企业的经济效益。

以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。

【EN】

A method of flexible rare-earth sull is prepared using magnetron sputtering

Technical field

The present invention relates to the preparation method technical fields of fexible film, are prepared more particularly, to a kind of using magnetron sputtering

The method of flexible rare-earth sull.

Background technique

Magnetron Sputtering Thin Film preparation facilities in existing film preparing technology, may be implemented metal, non-metal simple-substance and

The plated films such as compound, but be nearly all rigid substrate applied by the existing planar reaction magnetic control sputtering device, such as silicon

Piece, glass, mica etc..This kind of substrate can not be applied to flexible device, seriously affected such film and further processed and make

With.Secondly, for there is the metal that appraises at the current rate, such as europium oxide film, after its exposure is with air, will be further oxided into

And function is influenced, it ultimately causes device function and loses or damage.

Therefore, to solve the above problems, the present invention provides a kind of new technical solutions.

Summary of the invention

The object of the present invention is to provide a kind of methods for preparing flexible rare-earth sull using magnetron sputtering, can

Solve in the prior art rigid substrate can not be applied to flexible device, magnetron sputtering sull is difficult to and film is easy

The problems such as oxidation is appraised at the current rate.

Used technical solution is the present invention in view of the above technical defects:

A method of flexible rare-earth sull is prepared using magnetron sputtering, is included the following steps:

A: 4N rare earth metal target is selected to be sputtering target material and place it in magnetron sputtering chamber;

B: using liquid PDMS precursor as deposition substrate, and liquid PDMS substrate spin coating is placed in the rotation of magnetron sputtering chamber

Turn on warm table;

C: vacuumize process is implemented to magnetron sputtering chamber, and is passed through argon gas and sputtering target material is cleaned;

D: rotary heating platform is heated to 120 DEG C, and keeps the temperature 1h;

E: being passed through mixed gas into magnetron sputtering room until starter is implemented at magnetron sputtering when indoor pressure reaches 3 pa

Reason;

F: after the completion of deposition film on substrate, stopping ventilation, by the temperature cooled to room temperature in magnetron sputtering room,

Carrying out curing process to film can be prepared by flexible rare-earth sull.

Further, sputtering target material described in step a can for europium oxide target, chromium oxide target, nickel oxide target, aluminium oxide target,

Titanium oxide target.

Further, the vacuum degree after vacuumize process described in step c is 1.0 × 10-4Pa.

Further, the vacuum degree in argon gas adjustment magnetron sputtering room is passed through in step c to 3 pas, starter is to target material surface

It is cleaned, time 5-8min.

Further, it needs to clean substrate, cleaning method before heating turntable is to substrate heating in step d

It can be any one in ionization cleaning or ultrasonic cleaning.

Further, mixed gas described in step e is the mixture of hydrogen, oxygen and inert gas, and wherein hydrogen exists

Content in mixed gas is 5-20%.

Further, the inert gas is at least one of argon gas, helium and neon, and wherein argon gas is in mixed gas

In content be greater than 50%.

Further, the sputtering power of the processing of magnetron sputtering described in step e is 0.5-1.2 kilowatts, pre-sputtering 2-3min

After remove baffle, then sputtering sedimentation 1h.

Further, the temperature in magnetron sputtering room described in step f needs constant temperature 3h before Temperature fall.

The beneficial effects of the present invention are:

1, flexible rare-earth sull prepared by the present invention, is able to solve the shortcomings that existing sputtered film is difficult to,

The processing of film is facilitated to cut;

2, the present invention sputters 1h at 120 DEG C using PDMS precursor as liquid substrate, so that sull deposition is simultaneously

It is solidificated in PDMS, can be effectively protected there is the europium oxide film for feature of appraising at the current rate, avoid europium oxide film because sudden and violent

Reveal and be oxidized the phenomenon that appraising at the current rate, improves the service life and functionality of device;

3, the entire preparation process of the present invention is simple, and the thickness of rare-earth oxide film accurately controls, cost input

It is low, it is easy to implement industrialization production, improves the economic benefit of enterprise.

Specific embodiment

A method of flexible rare-earth sull is prepared using magnetron sputtering, is included the following steps:

A: 4N rare earth metal target is selected as sputtering target material and places it in magnetron sputtering chamber, wherein sputtering target material can be oxygen

Change europium target, chromium oxide target, nickel oxide target, aluminium oxide target, titanium oxide target;

B: using liquid PDMS precursor as deposition substrate, and liquid PDMS substrate spin coating is placed in the rotation of magnetron sputtering chamber

Turn on warm table;

C: vacuumize process is implemented to magnetron sputtering chamber until vacuum degree is 1.0 × 10-4Pa, and it is passed through argon gas adjustment magnetic

Control sputters indoor vacuum degree to 3 pas, and starter cleans target material surface, time 5-8min;

D: it before heating turntable is to substrate heating, needs to clean substrate, rotary heating platform is heated rise thereafter

Temperature keeps the temperature 1h to 120 DEG C, and wherein cleaning method can be any one in ionization cleaning or ultrasonic cleaning;

E: being passed through mixed gas into magnetron sputtering room until starter is implemented at magnetron sputtering when indoor pressure reaches 3 pa

Reason, sputtering power are 0.5-1.2 kilowatts, remove baffle, then sputtering sedimentation 1h after pre-sputtering 2-3min, wherein mixed gas is

The mixture of hydrogen, oxygen and inert gas, content of the hydrogen in mixed gas is 5-20%, secondly, inert gas is argon

At least one of gas, helium and neon, wherein content of the argon gas in mixed gas is greater than 50%;

F: after the completion of deposition film on substrate, stopping ventilating, after constant temperature 3h, the temperature in magnetron sputtering room is naturally cold

But to room temperature, carrying out curing process to film can be prepared by flexible rare-earth sull.

In order to deepen the understanding of the present invention, the present invention will be described in further detail with reference to the examples below, the embodiment

For explaining only the invention, it does not restrict the protection scope of the present invention.

Embodiment 1

Implementation process of the invention is specifically described for preparing flexible rare-earth europium oxide film.

A method of flexible rare-earth europium oxide film is prepared using magnetron sputtering, is included the following steps:

A: europium oxide target is selected to be sputtering target material and place it in magnetron sputtering chamber;

B: using liquid PDMS precursor as deposition substrate, and liquid PDMS substrate spin coating is placed in the rotation of magnetron sputtering chamber

Turn on warm table;

C: vacuumize process is implemented to magnetron sputtering chamber until vacuum degree is 1.0 × 10-4Pa, and it is passed through argon gas adjustment magnetic

Control sputters indoor vacuum degree to 3 pas, and starter cleans europium oxide target material surface, time 5min;

D: it before heating turntable is to substrate heating, needs to be cleaned by ultrasonic substrate, scavenging period 5min, thereafter

Rotary heating platform is heated to 120 DEG C, and keeps the temperature 1h;

E: being passed through mixed gas into magnetron sputtering room until starter is implemented at magnetron sputtering when indoor pressure reaches 3 pa

Reason, sputtering power are 1.2 kilowatts, remove baffle, then sputtering sedimentation 1h after pre-sputtering 2min, wherein mixed gas is hydrogen, oxygen

The mixture of gas and argon gas, content of the hydrogen in mixed gas are 15%, and content of the argon gas in mixed gas is 80%, remaining

For oxygen.

F: after the completion of deposition film on substrate, stopping ventilating, after constant temperature 3h, the temperature in magnetron sputtering room is naturally cold

But to room temperature, carrying out curing process to film can be prepared by flexible rare-earth europium oxide film.

It especially emphasizes, europium oxide film has the characteristics that feature of appraising at the current rate, after europium oxide film is exposed in air, very

It is easy to be further oxided and appraising at the current rate influences function, for this limitation of europium oxide film, the present invention uses PDMS

Precursor sputters 1h at 120 DEG C as liquid substrate, so that europium oxide film is deposited and is solidificated in PDMS, even if europium oxide

Film is exposed in air, also can guarantee that europium oxide film is effectively protected, and avoids europium oxide film from being oxidized and appraises at the current rate

Phenomenon improves the service life and functionality of device.

The beneficial effects of the present invention are: flexible rare-earth sull prepared by the present invention, it is thin to be able to solve existing sputtering

The shortcomings that film is difficult to facilitates the processing of film to cut;And the entire preparation process of the present invention is simple, rare-earth oxide

The thickness of film accurately controls, and cost input is low, is easy to implement industrialization production, improves the economic benefit of enterprise.

The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field

For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair

Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

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