CN108239717A - A kind of preparation method of tungsten nickel dielectric substance for having barium titanate film - Google Patents

A kind of preparation method of tungsten nickel dielectric substance for having barium titanate film Download PDF

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CN108239717A
CN108239717A CN201611213309.4A CN201611213309A CN108239717A CN 108239717 A CN108239717 A CN 108239717A CN 201611213309 A CN201611213309 A CN 201611213309A CN 108239717 A CN108239717 A CN 108239717A
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sputtering
matrix
batio
powder
temperature
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不公告发明人
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Qingdao Xiangzhi Electronic Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/088—Oxides of the type ABO3 with A representing alkali, alkaline earth metal or Pb and B representing a refractory or rare earth metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Semiconductor Memories (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of preparation methods of tungsten nickel dielectric substance for having barium titanate film, dielectric substance prepared by this method, solve the problems, such as often occur " nickel pond " and hole in traditional fine grained cemented carbide preparation process, multi-layer film structure can not only hinder the migration of Lacking oxygen, can also increase BaTiO3Pellicular front internal pressure stress, therefore can play the role of reducing dielectric loss and improve dielectric constant, solve existing BaTiO3Film causes leakage current, dielectric loss to increase or even fail when generating Lacking oxygen because preparing, being on active service the problem of.

Description

A kind of preparation method of tungsten nickel dielectric substance for having barium titanate film
Technical field
The present invention relates to dielectric substance manufacturing fields, and in particular to a kind of tungsten nickel electricity for having barium titanate film is situated between The preparation method of material.
Background technology
The BaTiO3 films of high-k have important application prospect in the fields such as embedded capacitance and high energy-storage travelling wave tube, Particularly Direct precipitation BaTiO3 films on the base metals substrate such as Ni, Cu, attract wide attention in recent years, especially, because of lining Leakage current caused by residual stress caused by mismatch and Lacking oxygen migration, redistribution etc. is even more to have attracted people between bottom and film Sight.
WC-Ni hard alloy has high intensity, high rigidity, excellent wearability, heat resistance and good corrosion resistance The features such as, therefore it is widely used in the working environments such as high pressure, high rotating speed, high temperature, Korrosionsmedium.Since Ni belongs to face-centered cubic (F.c.c) crystallographic system, plasticity is fine, is easily plastically deformed during wet-milling, forms the Ni powder balls of sheet.Industrial production with Ni will be grown as the Ball-milling Time of the hard alloy of binding agent, even in this way, cannot guarantee that the uniform refinement of Ni powder, this is Based on Ni powder, there is the Refining Mechanisms completely different with Co powder.
Mainly WC grain is refined, by stringent technology controlling and process, reduces hole by adding alloying element in the prior art And the methods of defect, improves the performance of WC-Ni hard alloy.The WC-Ni mixtures prepared using conventional method are in vacuum-sintering Under the conditions of often there is " nickel pond " and hole." nickel pond " and hole can seriously affect the comprehensive performance of alloy, such as intensity, wear-resisting Property, corrosion resistance etc..
Multilayer BaTiO is found in experimentation3The barrier height at the homogeneity interface that film is formed also is greater than crystal boundary and is formed Back-to-back double schottky barrier heights.In addition, research shows that face internal pressure stress can improve BaTiO3Base-multi-layer ceramics electricity The dielectric constant (being parallel to substrate surface) of container.And with the increase of film thickness, residual compressive stress is on a declining curve.Therefore It is a kind of to hinder the migration of Lacking oxygen it is necessary to research and develop, increase BaTiO3Pellicular front internal pressure stress, while reduction can be played and be situated between Electrical loss and the multi-layer film structure for improving dielectric constant effect.
Invention content
The present invention provides a kind of preparation method of tungsten nickel dielectric substance for having barium titanate film, prepared by this method Dielectric substance, solve the problems, such as in traditional fine grained cemented carbide preparation process " nickel pond " and hole, multi-layer thin often occur Membrane structure can not only hinder the migration of Lacking oxygen, can also increase BaTiO3Pellicular front internal pressure stress, therefore drop can be played Low-dielectric loss and the effect for improving dielectric constant, solve existing BaTiO3Film is led when generating Lacking oxygen because preparing, being on active service The problem of leakage current, dielectric loss is caused to increase or even fail.
To achieve these goals, the present invention provides a kind of tungsten nickel dielectric substances for having barium titanate film Preparation method, this method comprises the following steps：
(1) matrix is prepared
Mixed powder is prepared by following composition by weight
Tungsten carbide, 90.1%-92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%-6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus；
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive Chromium carbide adds in ball grinding cylinder wet-milling 12-16 hours, adds nickel powder wet-milling 14-18 hours；
The mixture slurry that ball milling is finished is dried；
Dry pack is pressed into the compacting product of required shape；
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450-1470 DEG C, soaking time 70-90min, Sintering pressure is 4.5-5.0Mpa, obtains tungsten nickel matrix；
(2) substrate pretreated
Described matrix pre-processes, and can be ground polishing, ultrasonic cleaning and ion source cleaning successively；
(3) by nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；
By BaTiO3Target is respectively washed 5min in absolute ethyl alcohol, deionized water successively, by BaTiO3Target material surface Impurity is clean, then again in an oven by BaTiO3Target is dried；
(4) primary sputtering
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, while is set in magnetron sputtering BaTiO is fixed in standby middle inner cavity chamber3Target, then it is 10 that magnetron sputtering apparatus inner cavity is evacuated to vacuum degree-4Pa；
Ar and O are passed through in equipment2Until operating pressure reaches 1.2Pa, and set the sputtering power of sputtering equipment as
The sputtering parameter that 145W, underlayer temperature are 380-420 DEG C, matrix rotary speed is 10-20rpm carries out first time sputtering；
In first time sputtering process, the sputtering thickness of film is detected at any time, until reaching setting thickness, sputtering is completed Afterwards, it takes out sample after cooling to room temperature and is placed in sample box；
(5) secondary sputtering
First time sputtered samples are placed in tube furnace, are passed through protective gas N2About 2min, until the air of the inside Be forced out clean, tube furnace be then warming up to 750 DEG C, heating rate is 10 DEG C/min, 750 DEG C of heated at constant temperature 30min into Row heat treatment, then drops to room temperature, and cooling rate is 10 DEG C/min；
It will complete the sputtered samples after being heat-treated sputter for the second time, the substrate temperature setting in second of sputtering parameter It is 420-450 DEG C, the sputtering power of sputtering equipment is 145W, matrix rotary speed is 10-20rpm,
Sputtered samples are placed in tube furnace after the completion of second of sputtering, are passed through protective gas N22min, until inner The air in face is forced out totally, tube furnace then is warming up to 770 DEG C, heating rate is 10 DEG C/min, in 770 DEG C of heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 DEG C/min, must have the tungsten nickel dielectric substance of barium titanate film into Product.
Preferably, in the step (2), the grinding and polishing can be first on the boart boart wheel disc of 600 mesh by matrix Corase grinding 10min is carried out, fine grinding 10min, then the diamond polishing with W2.5 are then carried out on the boart boart wheel disc of 1200 mesh Powder is polished, the ultrasonic cleaning uniformly bright to specimen surface, can clean the matrix after grinding and polishing in the following order, Acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol for use, the ion source cleaning that is cleaned by ultrasonic 5min → drying, can be used Hall from Component carries out matrix cleaning 5min, and pressure is 2 × 10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, is biased For -100V, cathode current 29.5A, cathode voltage 19V, anode current 7A, anode voltage 80V, to remove matrix table The adsorbed gas in face and impurity improve depositing coating and the bond strength and quality of forming film of matrix.
According to dielectric substance prepared by the above method, solve and often occur in traditional fine grained cemented carbide preparation process The problem of " nickel pond " and hole, multi-layer film structure can not only hinder the migration of Lacking oxygen, can also increase BaTiO3Film Face internal pressure stress, therefore can play the role of reducing dielectric loss and improve dielectric constant, solve existing BaTiO3Film The problem of leakage current, dielectric loss is caused to increase or even fail when generating Lacking oxygen because preparing, being on active service.
Specific embodiment
Embodiment one
Mixed powder is prepared by following composition by weight：
Tungsten carbide, 90.1%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus.
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive Chromium carbide adds in ball grinding cylinder wet-milling 12 hours, adds nickel powder wet-milling 14 hours.
The mixture slurry that ball milling is finished is dried.
Dry pack is pressed into the compacting product of required shape.
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450 DEG C, soaking time 70-90min, sintering pressure Power is 4.5Mpa, obtains tungsten nickel matrix.
Substrate pretreated, described matrix pretreatment can be ground polishing, ultrasonic cleaning and ion source cleaning successively.Institute Grinding and polishing is stated, can matrix be first subjected to corase grinding 10min on the boart boart wheel disc of 600 mesh, then in the Buddha's warrior attendant of 1200 mesh Fine grinding 10min is carried out on stone sand wheel disc, then be polished with the diamond polishing powder of W2.5 it is uniformly bright to specimen surface, it is described It is cleaned by ultrasonic, the matrix after grinding and polishing can be cleaned in the following order, it is clear that acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol ultrasound It is for use to wash 5min → drying, ion source cleaning can be used hall ion source and carry out cleaning 5min to matrix, pressure for 2 × 10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, is biased as -100V, cathode current 29.5A, and cathode voltage is 19V, anode current 7A, anode voltage 80V to remove the adsorbed gas of matrix surface and impurity, improve depositing coating With the bond strength and quality of forming film of matrix.
By nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；By BaTiO3Target according to It is secondary to be respectively washed 5min in absolute ethyl alcohol, deionized water, by BaTiO3The impurity of target material surface is clean, then exists again By BaTiO in baking oven3Target is dried.
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, while is set in magnetron sputtering BaTiO is fixed in standby middle inner cavity chamber3Target, then it is 10 that magnetron sputtering apparatus inner cavity is evacuated to vacuum degree-4Pa；Lead in equipment Enter Ar and O2Until operating pressure reaches 1.2Pa, and set the sputtering power of sputtering equipment as 145W, underlayer temperature be 380 DEG C, The sputtering parameter that matrix rotary speed is 10rpm carries out first time sputtering.
In first time sputtering process, the sputtering thickness of film is detected at any time, until reaching setting thickness, sputtering is completed Afterwards, it takes out sample after cooling to room temperature and is placed in sample box.
First time sputtered samples are placed in tube furnace, are passed through protective gas N2About 2min, until the air of the inside Be forced out clean, tube furnace be then warming up to 750 DEG C, heating rate is 10 DEG C/min, 750 DEG C of heated at constant temperature 30min into Row heat treatment, then drops to room temperature, and cooling rate is 10 DEG C/min；The sputtered samples after being heat-treated will be completed to be splashed for the second time It penetrates, the substrate temperature in second of sputtering parameter is set as 420 DEG C, and the sputtering power of sputtering equipment is 145W, matrix rotates speed It spends for 10rpm.
Sputtered samples are placed in tube furnace after the completion of second of sputtering, are passed through protective gas N22min, until inner The air in face is forced out totally, tube furnace then is warming up to 770 DEG C, heating rate is 10 DEG C/min, in 770 DEG C of heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 DEG C/min, must have the tungsten nickel dielectric substance of barium titanate film into Product.
Embodiment two
Mixed powder is prepared by following composition by weight：
Tungsten carbide, 92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus.
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First by carbide powder and additive Chromium carbide adds in ball grinding cylinder wet-milling 16 hours, adds nickel powder wet-milling 18 hours.
The mixture slurry that ball milling is finished is dried.
Dry pack is pressed into the compacting product of required shape.
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1470 DEG C, soaking time 90min, sintering pressure For 5.0Mpa, tungsten nickel matrix is obtained.
Substrate pretreated, described matrix pretreatment can be ground polishing, ultrasonic cleaning and ion source cleaning successively.Institute Grinding and polishing is stated, can matrix be first subjected to corase grinding 10min on the boart boart wheel disc of 600 mesh, then in the Buddha's warrior attendant of 1200 mesh Fine grinding 10min is carried out on stone sand wheel disc, then be polished with the diamond polishing powder of W2.5 it is uniformly bright to specimen surface, it is described It is cleaned by ultrasonic, the matrix after grinding and polishing can be cleaned in the following order, it is clear that acetone is cleaned by ultrasonic 5min → absolute ethyl alcohol ultrasound It is for use to wash 5min → drying, ion source cleaning can be used hall ion source and carry out cleaning 5min to matrix, pressure for 2 × 10-2Pa, substrate temperature are 300 DEG C, and argon gas flux is 10sccm, is biased as -100V, cathode current 29.5A, and cathode voltage is 19V, anode current 7A, anode voltage 80V to remove the adsorbed gas of matrix surface and impurity, improve depositing coating With the bond strength and quality of forming film of matrix.
By nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；By BaTiO3Target according to It is secondary to be respectively washed 5min in absolute ethyl alcohol, deionized water, by BaTiO3The impurity of target material surface is clean, then exists again By BaTiO in baking oven3Target is dried.
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, while is set in magnetron sputtering BaTiO is fixed in standby middle inner cavity chamber3Target, then it is 10 that magnetron sputtering apparatus inner cavity is evacuated to vacuum degree-4Pa；Lead in equipment Enter Ar and O2Until operating pressure reaches 1.2Pa, and set the sputtering power of sputtering equipment as 145W, underlayer temperature be 420 DEG C, The sputtering parameter that matrix rotary speed is 20rpm carries out first time sputtering.
In first time sputtering process, the sputtering thickness of film is detected at any time, until reaching setting thickness, sputtering is completed Afterwards, it takes out sample after cooling to room temperature and is placed in sample box.
First time sputtered samples are placed in tube furnace, are passed through protective gas N2About 2min, until the air of the inside Be forced out clean, tube furnace be then warming up to 750 DEG C, heating rate is 10 DEG C/min, 750 DEG C of heated at constant temperature 30min into Row heat treatment, then drops to room temperature, and cooling rate is 10 DEG C/min；The sputtered samples after being heat-treated will be completed to be splashed for the second time It penetrates, the substrate temperature in second of sputtering parameter is set as 450 DEG C, and the sputtering power of sputtering equipment is 145W, matrix rotates speed It spends for 20rpm.
Sputtered samples are placed in tube furnace after the completion of second of sputtering, are passed through protective gas N22min, until inner The air in face is forced out totally, tube furnace then is warming up to 770 DEG C, heating rate is 10 DEG C/min, in 770 DEG C of heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 DEG C/min, must have the tungsten nickel dielectric substance of barium titanate film into Product.

Claims (2)

1. a kind of preparation method of tungsten nickel dielectric substance for having barium titanate film, this method comprises the following steps：
(1) matrix is prepared
Mixed powder is prepared by following composition by weight
Tungsten carbide, 90.1%-92.8%, 0.8-1 μm of Fisher particle size；
Nickel powder, 5%-6%, 0.5-1.0 μm of Fisher particle size；
Chromium carbide, surplus；
The mixed powder of said ratio is subjected to wet-milling；Wherein Ball-milling Time Discrete control；First carbide powder and additive are carbonized Chromium adds in ball grinding cylinder wet-milling 12-16 hours, adds nickel powder wet-milling 14-18 hours；
The mixture slurry that ball milling is finished is dried；
Dry pack is pressed into the compacting product of required shape；
Compacting product are placed on high temperature sintering in sintering furnace, sintering temperature is 1450-1470 DEG C, soaking time 70-90min, sintering Pressure is 4.5-5.0Mpa, obtains tungsten nickel matrix；
(2) substrate pretreated
Described matrix pre-processes, and can be ground polishing, ultrasonic cleaning and ion source cleaning successively；
(3) by nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；
By BaTiO3Target is respectively washed 5min in absolute ethyl alcohol, deionized water successively, by BaTiO3The impurity of target material surface It is clean, then again in an oven by BaTiO3Target is dried；
(4) primary sputtering
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, while in magnetron sputtering apparatus BaTiO is fixed in inner cavity chamber3Target, then it is 10 that magnetron sputtering apparatus inner cavity is evacuated to vacuum degree-4Pa；
Ar and O are passed through in equipment2Until operating pressure reaches 1.2Pa, and the sputtering power of sputtering equipment is set as 145W, lining The sputtering parameter that bottom temperature is 380-420 DEG C, matrix rotary speed is 10-20rpm carries out first time sputtering；
In first time sputtering process, the sputtering thickness of film is detected at any time, until reach setting thickness, after the completion of sputtering, drop Sample is taken out after temperature to room temperature and is placed in sample box；
(5) secondary sputtering
First time sputtered samples are placed in tube furnace, are passed through protective gas N2About 2min, until the air of the inside is forced out Totally, tube furnace is then warming up to 750 DEG C, heating rate is 10 DEG C/min, and hot place is carried out in 750 DEG C of heated at constant temperature 30min Reason, then drops to room temperature, and cooling rate is 10 DEG C/min；
It will complete the sputtered samples after being heat-treated sputter for the second time, the substrate temperature in second of sputtering parameter is set as 420-450 DEG C, the sputtering power of sputtering equipment is 145W, matrix rotary speed is 10-20rpm,
Sputtered samples are placed in tube furnace after the completion of second of sputtering, are passed through protective gas N22min, until the sky of the inside Gas is forced out totally, and tube furnace then is warming up to 770 DEG C, and heating rate is 10 DEG C/min, in 770 DEG C of heated at constant temperature 30min, Then room temperature is dropped to, cooling rate is 10 DEG C/min, the tungsten nickel dielectric substance finished product that must have barium titanate film.
2. the method as described in claim 1, which is characterized in that in the step (2), the grinding and polishing can be by matrix Corase grinding 10min first is carried out on the boart boart wheel disc of 600 mesh, then carries out fine grinding on the boart boart wheel disc of 1200 mesh 10min, then, the ultrasonic cleaning uniformly bright to specimen surface is polished with the diamond polishing powder of W2.5, it can will grind Matrix after polishing cleans in the following order, and acetone ultrasonic cleaning 5min → absolute ethyl alcohol ultrasonic cleaning 5min → drying is for use, The ion source cleaning can be used hall ion source and cleaning 5min carried out to matrix, and pressure is 2 × 10-2Pa, substrate temperature are 300 DEG C, argon gas flux is 10sccm, is biased as -100V, cathode current 29.5A, cathode voltage 19V, and anode current is 7A, anode voltage 80V, to remove the adsorbed gas of matrix surface and impurity, the combination for improving depositing coating and matrix is strong Degree and quality of forming film.
CN201611213309.4A 2016-12-25 2016-12-25 A kind of preparation method of tungsten nickel dielectric substance for having barium titanate film Pending CN108239717A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114602877A (en) * 2022-03-21 2022-06-10 宁波江丰电子材料股份有限公司 Cleaning method for target material containing pores

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114602877A (en) * 2022-03-21 2022-06-10 宁波江丰电子材料股份有限公司 Cleaning method for target material containing pores

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Application publication date: 20180703