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中国 发明 在审

一种靶材制备方法 【EN】A kind of target preparation method

申请(专利)号:CN201910254092.9国省代码:广西 45
申请(专利权)人:【中文】柳州呈奥科技有限公司【EN】Liuzhou Cheng Ao Technology Co., Ltd.
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摘要:
【中文】本发明公开了一种靶材制备方法,该靶材制备方法包括以下步骤:清洗原料,对清洗完成的靶材进行热处理,对具有一定形状的靶材进行冷等静压作业,对其常温升压,并且保持8‑15min后,并且采用顶电极不加持的方式进行退火处理去除靶材表面压力;将处理后的靶材放置在磁控溅射的样品台上,在靶材底部通入氩气,对其进行预溅射,再通入高纯氩气和氧气的混合气体,对其进行溅射,最终制得靶材;本发明所述的一种靶材制备方法,靶材质量得到提高,可以保证不同铝靶材之间晶粒大小的均一性,可以提高了生产效率,降低了生产成本,同时制得的靶材纯度高、致密性好、成膜均匀性好;操作工艺简单、能耗低、无污染且易于实现工业化,具有很好的应用前景。 【EN】Paragraph:The invention discloses a kind of target preparation methods, the target preparation method is the following steps are included: cleaning raw material, the target completed to cleaning is heat-treated, isostatic cool pressing operation is carried out to having effigurate target, it boosts to its room temperature, and after keeping 8-15min, and annealing removal target material surface pressure is carried out in such a way that top electrode does not accommodate;By treated, target is placed on the sample stage of magnetron sputtering, is passed through argon gas in target bottom, is carried out pre-sputtering to it, then be passed through the mixed gas of high-purity argon gas and oxygen, sputter to it, and target is finally made;A kind of target preparation method of the present invention, target quality is improved, it is ensured that production efficiency has can be improved in the homogeneity of grain size between different aluminum target, production cost is reduced, while target obtained purity is high, compactness are good, good at film uniformity;Operating procedure is simple, low energy consumption, pollution-free and be easily industrialized, and has a good application prospect.

主权项:
【中文】1.一种靶材制备方法,其特征在于,该靶材制备方法包括以下步骤: 步骤一、清洗原料,对靶材原料进行清洗,用喷枪除去靶材原料表面的灰尘和污垢; 步骤二、对清洗完成的靶材进行热处理,经过热处理后,将靶材放置冷藏密封容器中冷藏30-50min,保持靶材温度在160-180℃之间,随后取出降温后的靶材对其进行锻打形成靶材胚料,将靶材锻打形成靶材胚料靶材进行第二次热处理,热处理时间为1-2h,最终形成具有一定形状的靶材; 步骤三、对步骤二中具有一定形状的靶材进行冷等静压作业,对其常温升压,并且保持8-15min后,并且采用顶电极不加持的方式进行退火处理去除靶材表面压力; 步骤四、将处理后的靶材放置在磁控溅射的样品台上,在靶材底部通入氩气,对其进行预溅射,再通入高纯氩气和氧气的混合气体,对其进行溅射,最终制得靶材。 【EN】1. a kind of target preparation method, which is characterized in that the target preparation method the following steps are included: Step 1: cleaning raw material, cleans target raw material, the dust and dirt on target raw material surface are removed with spray gun; Step 2: the target completed to cleaning is heat-treated, after Overheating Treatment, target is placed cold in refrigeration sealing container 30-50min is hidden, keeps target temperature between 160-180 DEG C, the target after then taking out cooling forge forming target to it Material embryo material, target is forged to form second of heat treatment of target embryo material target progress, and heat treatment time 1-2h ultimately forms tool Effigurate target; Step 3: carrying out isostatic cool pressing operation to having effigurate target in step 2, boost to its room temperature, and keep After 8-15min, and annealing removal target material surface pressure is carried out in such a way that top electrode does not accommodate; Step 4: by treated, target is placed on the sample stage of magnetron sputtering, is passed through argon gas in target bottom, is carried out to it Pre-sputtering, then it is passed through the mixed gas of high-purity argon gas and oxygen, it is sputtered, target is finally made.


说明书

【中文】

一种靶材制备方法

技术领域

本发明属于新材料领域,特别涉及一种靶材制备方法。

背景技术

镀膜靶材是通过磁控溅射、多弧离子镀或其他类型的镀膜系统在适当工艺条件下溅射在基板上形成各种功能薄膜的溅射源。简单说的话,靶材就是高速荷能粒子轰击的目标材料,用于高能激光武器中,不同功率密度、不同输出波形、不同波长的激光与不同的靶材相互作用时,会产生不同的杀伤破坏效应。例如:蒸发磁控溅射镀膜是加热蒸发镀膜、铝膜等。更换不同的靶材(如铝、铜、不锈钢、钛、镍靶等),即可得到不同的膜系(如超硬、耐磨、防腐的合金膜等);

而现有靶材制备时原料价格高,不可以保证不同铝靶材之间晶粒大小的均一性,生产成本较高,同时制得的靶材纯度不高、致密性不好、成膜均匀性不佳;同时操作工艺复杂、能耗高、有污染且不易于实现工业化,为此,我们提出一种靶材制备方法。

发明内容

本发明的主要目的在于提供一种靶材制备方法,可以有效解决背景技术中的问题。

为实现上述目的,本发明采取的技术方案为:

一种靶材制备方法,该靶材制备方法包括以下步骤:

步骤一、清洗原料,对靶材原料进行清洗,用喷枪除去靶材原料表面的灰尘和污垢;

步骤二、对清洗完成的靶材进行热处理,经过热处理后,将靶材放置冷藏密封容器中冷藏30-50min,保持靶材温度在160-180℃之间,随后取出降温后的靶材对其进行锻打形成靶材胚料,将靶材锻打形成靶材胚料靶材进行第二次热处理,热处理时间为1-2h,最终形成具有一定形状的靶材;

步骤三、对步骤二中具有一定形状的靶材进行冷等静压作业,对其常温升压,并且保持8-15min后,并且采用顶电极不加持的方式进行退火处理去除靶材表面压力;

步骤四、将处理后的靶材放置在磁控溅射的样品台上,在靶材底部通入氩气,对其进行预溅射,再通入高纯氩气和氧气的混合气体,对其进行溅射,最终制得靶材。

优选的,靶材原料的电阻小于0.6Ω,其中靶材内银含量为30%,且靶材粉末体积电阻率小于2×10-3Ωcm。

优选的,所述靶材基距为60-100mm,工作气压0.3-0.9Pa

优选的,所述预溅射时间不少于6min,溅射时间为40-80min。

优选的,靶材溅射功率60-90W,靶材基底温度为120℃。

优选的,步骤三中退火处理时注入氮气,且其加热温度为500-750℃,保温时间为20-30。

与现有技术相比,本发明具有如下有益效果:该靶材制备方法,靶材质量得到提高,可以保证不同铝靶材之间晶粒大小的均一性,可以提高了生产效率,降低了生产成本,同时制得的靶材纯度高、致密性好、成膜均匀性好;操作工艺简单、能耗低、无污染且易于实现工业化,具有很好的应用前景。

具体实施方式

为使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施方式,进一步阐述本发明。

本发明的一种靶材制备方法,在制备时,首先对原材料进行清洗,该靶材原料的电阻小于0.6Ω,其中靶材内银含量为30%,且靶材粉末体积电阻率小于2×10-3Ωcm,对靶材用喷枪除去靶材原料表面的灰尘和污垢,以确保靶材原材料无杂质,避免对后续制备产生不利影响,随后对清洗完成的靶材进行热处理,经过热处理后,将靶材放置冷藏密封容器中冷藏30-50min,保持靶材温度在160-180℃之间,随后取出降温后的靶材对其进行锻打形成靶材胚料,将靶材锻打形成靶材胚料靶材进行第二次热处理,热处理时间为1-2h,最终形成具有一定形状的靶材;靶材坯料本身是金属材料,金属的导热性能优异,因此在第二热处理的保温过程中,能够使接触在一起靶材温度达到均匀,从而使热处理后的靶材晶粒大小控制在80um以下,且不同铝靶材之间的晶粒大小均一,同时提高了生产效率,降低了生产成本,随后对具有一定形状的靶材进行冷等静压作业,对其常温升压,并且保持8-15min后,并且采用顶电极不加持的方式进行退火处理去除靶材表面压力,退火处理时注入氮气,且其加热温度为500-750℃,保温时间为20-30min,靶材基距为60-100mm,工作气压0.3-0.9Pa,预溅射时间不少于6min,溅射时间为40-80min,靶材溅射功率60-90W,靶材基底温度为120℃;将处理后的靶材放置在磁控溅射的样品台上,在靶材底部通入氩气,对其进行预溅射,再通入高纯氩气和氧气的混合气体,对其进行溅射,最终制得靶材,通过该制备方法制得的靶材质量得到提高,可以保证不同铝靶材之间晶粒大小的均一性,可以提高了生产效率,降低了生产成本,同时制得的靶材纯度高、致密性好、成膜均匀性好。

实施例1

在靶材制备时,首先对靶材原料进行清洗,用喷枪除去靶材原料表面的灰尘和污垢;对清洗完成的靶材进行热处理,经过热处理后,将靶材放置冷藏密封容器中冷藏30min,保持靶材温度在160℃之间,随后取出降温后的靶材对其进行锻打形成靶材胚料,将靶材锻打形成靶材胚料靶材进行第二次热处理,热处理时间为1h,最终形成具有一定形状的靶材;对具有一定形状的靶材进行冷等静压作业,对其常温升压,并且保持8min后,并且采用顶电极不加持的方式进行退火处理去除靶材表面压力,退火处理时注入氮气,且其加热温度为500℃,保温时间为20min,靶材基距为60mm,工作气压0.3Pa,预溅射时间不少于6min,溅射时间为40min,靶材溅射功率60W,靶材基底温度为120℃;将处理后的靶材放置在磁控溅射的样品台上,在靶材底部通入氩气,对其进行预溅射,再通入高纯氩气和氧气的混合气体,对其进行溅射,最终制得的靶材晶粒大小的均一,粒径为0.6nm,纯度为98%。

实施例2

在靶材制备时,首先对靶材原料进行清洗,用喷枪除去靶材原料表面的灰尘和污垢;对清洗完成的靶材进行热处理,经过热处理后,将靶材放置冷藏密封容器中冷藏50min,保持靶材温度在180℃之间,随后取出降温后的靶材对其进行锻打形成靶材胚料,将靶材锻打形成靶材胚料靶材进行第二次热处理,热处理时间为2h,最终形成具有一定形状的靶材;对具有一定形状的靶材进行冷等静压作业,对其常温升压,并且保持15min后,并且采用顶电极不加持的方式进行退火处理去除靶材表面压力,退火处理时注入氮气,且其加热温度为750℃,保温时间为30min,靶材基距为100mm,工作气压0.9Pa,预溅射时间不少于6min,溅射时间为80min,靶材溅射功率90W,靶材基底温度为120℃;将处理后的靶材放置在磁控溅射的样品台上,在靶材底部通入氩气,对其进行预溅射,再通入高纯氩气和氧气的混合气体,对其进行溅射,最终制得的靶材晶粒大小的均一,粒径为0.8nm,纯度为99%。

以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

【EN】

A kind of target preparation method

Technical field

The invention belongs to field of new materials, in particular to a kind of target preparation method.

Background technique

Plated film target be by magnetron sputtering, multi-arc ion coating or other kinds of coating system under appropriate process conditions

It sputters on substrate and forms the sputtering source of various function films.Briefly, target is exactly the mesh of high speed lotus energy particle bombardment

Mark material, in high energy laser weapon, different capacity density, different output waveforms, different wave length laser and different targets

When material interacts, different killing damage effects can be generated.Such as: magnetron evaporation sputter coating is heating evaporation plated film, aluminium

Film etc..Replace different targets (such as aluminium, copper, stainless steel, titanium, nickel target), can be obtained different membrane systems (it is such as superhard, wear-resisting,

Corrosion-resistant alloy film etc.);

And cost of material is high when the preparation of existing target, it is not possible to guarantee the homogeneity of grain size between different aluminum target, produce

Higher cost, while target purity obtained is not high, compactness is bad, bad at film uniformity;Operating procedure complexity, energy simultaneously

Consumption is high, has pollution and is not easy to realize industrialization, for this purpose, it is proposed that a kind of target preparation method.

Summary of the invention

The main purpose of the present invention is to provide a kind of target preparation methods, can effectively solve asking in background technique

Topic.

To achieve the above object, the technical scheme adopted by the invention is as follows:

A kind of target preparation method, the target preparation method the following steps are included:

Step 1: cleaning raw material, cleans target raw material, the dust and dirt on target raw material surface are removed with spray gun;

Step 2: the target completed to cleaning is heat-treated, after Overheating Treatment, target is placed cold in refrigeration sealing container

30-50min is hidden, keeps target temperature between 160-180 DEG C, the target after then taking out cooling forge forming target to it

Material embryo material, target is forged to form second of heat treatment of target embryo material target progress, and heat treatment time 1-2h ultimately forms tool

Effigurate target;

Step 3: carrying out isostatic cool pressing operation to having effigurate target in step 2, boost to its room temperature, and keep

After 8-15min, and annealing removal target material surface pressure is carried out in such a way that top electrode does not accommodate;

Step 4: by treated, target is placed on the sample stage of magnetron sputtering, is passed through argon gas in target bottom, is carried out to it

Pre-sputtering, then it is passed through the mixed gas of high-purity argon gas and oxygen, it is sputtered, target is finally made.

Preferably, the resistance of target raw material is less than 0.6 Ω, and wherein silver content is 30% in target, and target powder volume electricity

Resistance rate is less than 2 × 10-3 Ω cm.

Preferably, the target cardinal distance is 60-100mm, operating air pressure 0.3-0.9Pa

Preferably, the pre-sputtering time is no less than 6min, sputtering time 40-80min.

Preferably, target as sputter power 60-90W, target base reservoir temperature are 120 DEG C.

Preferably, nitrogen is injected when making annealing treatment in step 3, and its heating temperature is 500-750 DEG C, soaking time is

20-30。

Compared with prior art, the invention has the following beneficial effects: the target preparation method, target quality is mentioned

It is high, it is ensured that the homogeneity of grain size between different aluminum target can be improved production efficiency, reduce production cost,

Target purity is high obtained, compactness are good, good at film uniformity simultaneously;Operating procedure is simple, low energy consumption, pollution-free and be easy to real

It now industrializes, has a good application prospect.

Specific embodiment

To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, below with reference to

Specific embodiment, the present invention is further explained.

A kind of target preparation method of the invention in the preparation first cleans raw material, the electricity of the target raw material

Resistance is less than 0.6 Ω, and wherein silver content is 30% in target, and target powder volume resistivity is less than 2 × 10-3 Ω cm, to target

The dust and dirt on target raw material surface are removed with spray gun, to ensure target source material free from admixture, avoid generating subsequent preparation

Adverse effect, the target then completed to cleaning is heat-treated, and after Overheating Treatment, target is placed in refrigeration sealing container

30-50min is refrigerated, keeps target temperature between 160-180 DEG C, the target after then taking out cooling forge being formed to it

Target embryo material, target is forged to form second of heat treatment of target embryo material target progress, and heat treatment time 1-2h is ultimately formed

Has effigurate target;Target blank itself is metal material, the excellent thermal conductivity of metal, therefore in the second heat treatment

Insulating process in, the target temperature that can make to contact reaches uniformly, to make the target crystalline grains size control after heat treatment

Make in 80um hereinafter, and grain size between different aluminum target it is uniform, while improving production efficiency, reduce and be produced into

This, then carries out isostatic cool pressing operation to having effigurate target, boosts to its room temperature, and after keeping 8-15min, and

And annealing removal target material surface pressure is carried out in such a way that top electrode does not accommodate, when annealing, injects nitrogen, and its

Heating temperature be 500-750 DEG C, soaking time 20-30min, target cardinal distance be 60-100mm, operating air pressure 0.3-0.9Pa,

The pre-sputtering time is no less than 6min, sputtering time 40-80min, target as sputter power 60-90W, and target base reservoir temperature is 120

℃;By treated, target is placed on the sample stage of magnetron sputtering, is passed through argon gas in target bottom, is carried out pre-sputtering to it,

It is passed through the mixed gas of high-purity argon gas and oxygen again, it is sputtered, target is finally made, as made from the preparation method

Target quality is improved, it is ensured that production efficiency has can be improved in the homogeneity of grain size between different aluminum target, drop

Low production cost, while target obtained purity is high, compactness are good, good at film uniformity.

Embodiment 1

In target preparation, target raw material is cleaned first, the dust and dirt on target raw material surface are removed with spray gun;It is right

The target that cleaning is completed is heat-treated, and after Overheating Treatment, target is placed in refrigeration sealing container and refrigerates 30min, is kept

Between 160 DEG C, the target after then taking out cooling forge forming target embryo material target temperature to it, and target is forged shape

Second is carried out at target embryo material target to be heat-treated, heat treatment time 1h, ultimately form the effigurate target of tool;To tool

Effigurate target carries out isostatic cool pressing operation, boosts to its room temperature, and after keeping 8min, and not using top electrode

The mode of aid carries out annealing removal target material surface pressure, and when annealing injects nitrogen, and its heating temperature is 500

DEG C, soaking time 20min, target cardinal distance is 60mm, operating air pressure 0.3Pa, and the pre-sputtering time is no less than 6min, sputtering time

For 40min, target as sputter power 60W, target base reservoir temperature is 120 DEG C;By the sample of treated target is placed on magnetron sputtering

In sample platform, it is passed through argon gas in target bottom, pre-sputtering is carried out to it, then be passed through the mixed gas of high-purity argon gas and oxygen, to it

It is sputtered, uniform, the partial size 0.6nm of final target crystalline grains size obtained, purity 98%.

Embodiment 2

In target preparation, target raw material is cleaned first, the dust and dirt on target raw material surface are removed with spray gun;It is right

The target that cleaning is completed is heat-treated, and after Overheating Treatment, target is placed in refrigeration sealing container and refrigerates 50min, is kept

Between 180 DEG C, the target after then taking out cooling forge forming target embryo material target temperature to it, and target is forged shape

Second is carried out at target embryo material target to be heat-treated, heat treatment time 2h, ultimately form the effigurate target of tool;To tool

Effigurate target carries out isostatic cool pressing operation, boosts to its room temperature, and after keeping 15min, and uses top electrode

The mode not accommodated carries out annealing removal target material surface pressure, and when annealing injects nitrogen, and its heating temperature is 750

DEG C, soaking time 30min, target cardinal distance is 100mm, operating air pressure 0.9Pa, and the pre-sputtering time is no less than 6min, when sputtering

Between be 80min, target as sputter power 90W, target base reservoir temperature be 120 DEG C;By treated, target is placed on magnetron sputtering

On sample stage, it is passed through argon gas in target bottom, pre-sputtering is carried out to it, then be passed through the mixed gas of high-purity argon gas and oxygen, it is right

It is sputtered, uniform, the partial size 0.8nm of final target crystalline grains size obtained, purity 99%.

The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry

Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this

The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes

Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its

Equivalent thereof.

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