CN106319464A - Method for preparing barium titanate film on tungsten alloy substrate - Google Patents

Method for preparing barium titanate film on tungsten alloy substrate Download PDF

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CN106319464A
CN106319464A CN201610690514.3A CN201610690514A CN106319464A CN 106319464 A CN106319464 A CN 106319464A CN 201610690514 A CN201610690514 A CN 201610690514A CN 106319464 A CN106319464 A CN 106319464A
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sputtering
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不公告发明人
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Suzhou Sichuang Yuanbo Electronic Technology Co Ltd
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    • 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
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a method for preparing a barium titanate film on a tungsten alloy substrate. By the adoption of the method, the organizational structure of the material is improved and controlled remarkably, the prepared tungsten alloy and the barium titanate film can be perfectly matched, and the internal pressure stress of the BaTiO3 film can be increased, so that the dielectric loss can be reduced, the permittivity can be increased, and the problems that an existing BaTiO3 film generates oxygen vacancies during preparation and service, and consequently current leakage is caused and the dielectric loss is increased, even the failure is caused are solved.

Description

A kind of method preparing barium titanate film in tungsten alloy substrate
Technical field
The present invention relates to dielectric substance and manufacture field, be specifically related to one and prepare barium titanate film in tungsten alloy substrate Method.
Background technology
The BaTiO3 thin film of high-k has important application prospect in the field such as embedded capacitance and high energy-storage travelling wave tube, Particularly Direct precipitation BaTiO3 thin film on the base metal substrate such as Ni, Cu, attracts wide attention in recent years, especially, because of lining Residual stress that between the end and thin film, mismatch causes and the leakage current that Lacking oxygen migration, redistribution etc. cause have attracted people especially Sight.
Fusing point is high, intensity is big, electrical and thermal conductivity performance good, etch resistant properties is strong and high-temperature mechanics owing to having for tungsten and alloy thereof Can well wait advantage, be widely used in the high-temperature fields such as high-temperature heating, glass melting, thermal structure support member.
Experimentation finds multilamellar BaTiO3The barrier height at the homogeneity interface that thin film is formed also is greater than crystal boundary and is formed Back-to-back pair of schottky barrier height.Additionally, 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 along with the increase of film thickness, residual compressive stress is on a declining curve.Therefore It is necessary to research and develop a kind of migration with obstruction Lacking oxygen, increases BaTiO3Pellicular front internal pressure stress, can play reduction simultaneously and be situated between Electrical loss and the multi-layer film structure of raising dielectric constant effect.
Summary of the invention
The present invention provides a kind of method preparing barium titanate film in tungsten alloy substrate, and the method significantly improves and controls Materials microstructure structure so that the tungsten alloy of preparation can reach perfectly to mate with barium titanate film, it is also possible to increase BaTiO3Pellicular front internal pressure stress, therefore can play and reduce dielectric loss and improve the effect of dielectric constant, solve existing BaTiO3Thin film produces Lacking oxygen because of preparation, military service and causes leakage current, dielectric loss to increase, the problem even lost efficacy.
To achieve these goals, the invention provides a kind of method preparing barium titanate film in tungsten alloy substrate, This tungsten alloy matrix is made up of following components by weight percent: Fisher particle size is WC powder 90-95 part of 1-1.5um, and Fisher particle size is 0.5- Co powder 8-12 part of 0.8um, B powder 1-2 part, graphite powder 0.5-1 part；
The method comprises the steps:
(1) tungsten alloy matrix is prepared
Each material component is chosen by above-mentioned material formula；
Select 1Kg agitating ball mill, be initially charged B powder, C powder and Co powder, add amylalcohol as grinding medium in the ratio of 500ml/kg Matter, adds mill ball by ratio of grinding media to material example 5:1, is stirred grinding, mill ball diameter D7, ball mill mixing speed 480rpm, fills out Filling coefficient is 0.85, grinds 1 hour；
Then add tungsten carbide to grind 5-7 hour, form slip, form slip；
Filtering, be dried, the mesh number of filtration is 40-50 mesh, and baking temperature is 70-85 DEG C, makes carbide alloy mixture grain；
By carbide alloy mixture grain by molding or extruding or injection mo(u)lding, make hard alloy blank；
Hard alloy blank entering sintering furnace and is sintered molding, sintering temperature during sinter molding is 1400-1425 DEG C, Ar Pressure is 8-10Mpa, sintering time is 30-100min, obtains tungsten alloy matrix；
(2) substrate pretreated
Described substrate pretreated, can be ground polishing, ultrasonic cleaning and ion source successively and clean；
(3) by nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；
By BaTiO3Target is respectively washed 5min with in dehydrated alcohol, deionized water successively, with by BaTiO3Target material surface miscellaneous Matter cleaning is clean, the most in an oven by BaTiO3Target is dried；
(4) once sputter
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, simultaneously in magnetron sputtering apparatus Inner cavity chamber fixes BaTiO3Target, then magnetron sputtering apparatus inner chamber is evacuated to vacuum is 10-4Pa；
It is passed through Ar and O in equipment2Until operating pressure reaches 1.2Pa, and set the sputtering power of sputtering equipment as 145W, lining The sputtering parameter that end temperature is 380-420 DEG C, matrix rotary speed is 10-20rpm carries out sputtering for the first time；
In first time sputter procedure, detect the sputtering thickness of thin film at any time, until it reaches set thickness, after having sputtered, fall Temperature is to taking out sample after room temperature and being placed in sample box；
(5) secondary sputtering
First time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until the air of the inside is caught up with Going out clean, then tube furnace is warmed up to 750 DEG C, programming rate is 10 DEG C/min, carries out heat 750 DEG C of heated at constant temperature 30min Processing, then drop to room temperature, cooling rate is 10 DEG C/min；
Sputtered samples after completing heat treatment carries out second time and sputters, and the substrate temperature in sputtering parameter is set to for the second time 420-450 DEG C, the sputtering power of sputtering equipment is 145W, matrix rotary speed is 10-20rpm,
Sputtered samples is placed in tube furnace after having sputtered by second time, is passed through protective gas N22min, until the inside Air is forced out totally, then tube furnace is warmed up to 770 DEG C, and programming rate is 10 DEG C/min, 770oC heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 DEG C/min.
Preferably, in described step (2), described grinding and polishing, can be by matrix first on the boart boart wheel disc of 600 mesh Carry out roughly grinding 10min, on the boart boart wheel disc of 1200 mesh, then carry out fine grinding 10min, then with the diamond polishing of W2.5 Powder is polished to specimen surface the brightest, described ultrasonic cleaning, can be cleaned in the following order by the matrix after grinding and polishing, Acetone ultrasonic cleaning 5min → dehydrated alcohol ultrasonic cleaning 5min → dry is stand-by, and described ion source cleans, can use Hall from Component is carried out 5min to matrix, and pressure is 2 × 10-2Pa, substrate temperature is 300 DEG C, and argon flux is 10sccm, bias For-100V, cathode current is 29.5A, and cathode voltage is 19V, and anode current is 7A, and anode voltage is 80V, to remove matrix table The adsorbed gas in face and impurity, improve deposition coating and the bond strength of matrix and quality of forming film.
The method significantly improves and controls materials microstructure structure so that the tungsten alloy of preparation can reach with barium titanate film To perfect coupling, it is also possible to increase BaTiO3Pellicular front internal pressure stress, therefore can play reduction dielectric loss and improve Jie The effect of electric constant, solves existing BaTiO3Thin film produces Lacking oxygen because of preparation, military service and causes leakage current, dielectric loss to increase Add, the problem even lost efficacy.
Detailed description of the invention
Embodiment one
The present embodiment tungsten alloy matrix is made up of following components by weight percent: Fisher particle size is 90 parts of the WC powder of 1-1.5um, Fisher particle size For 8 parts of the Co powder of 0.5-0.8um, 1 part of B powder, graphite powder 0.5 part.
Each material component is chosen by above-mentioned material formula.
Select 1Kg agitating ball mill, be initially charged B powder, C powder and Co powder, add amylalcohol as grinding in the ratio of 500ml/kg Grinding media, adds mill ball by ratio of grinding media to material example 5:1, is stirred grinding, mill ball diameter D7, ball mill mixing speed 480rpm, activity coefficient is 0.85, grinds 1 hour.
Then add tungsten carbide to grind 5 hours, form slip, form slip.
Filtering, be dried, the mesh number of filtration is 40 mesh, and baking temperature is 70 DEG C, makes carbide alloy mixture grain.
By carbide alloy mixture grain by molding or extruding or injection mo(u)lding, make hard alloy blank.
Hard alloy blank entering sintering furnace and is sintered molding, sintering temperature during sinter molding is 1400 DEG C, Ar Pressure is 8Mpa, sintering time is 30min, obtains tungsten alloy matrix.
Substrate pretreated, described substrate pretreated, polishing, ultrasonic cleaning and ion source can be ground successively and clean.Institute State grinding and polishing, can first carry out matrix roughly grinding 10min, then at the Buddha's warrior attendant of 1200 mesh on the boart boart wheel disc of 600 mesh Carry out fine grinding 10min on stone sand wheel disc, then be polished to specimen surface the brightest with the diamond polishing powder of W2.5, described Ultrasonic cleaning, can clean in the following order by the matrix after grinding and polishing, and acetone ultrasonic cleaning 5min → dehydrated alcohol is ultrasonic clearly Washing 5min → dry stand-by, described ion source cleans, and can use hall ion source that matrix is carried out 5min, and pressure is 2 × 10-2Pa, substrate temperature is 300 DEG C, and argon flux is 10sccm, biases as-100V, and cathode current is 29.5A, and cathode voltage is 19V, anode current is 7A, and anode voltage is 80V, to remove adsorbed gas and the impurity of matrix surface, improves deposition coating Bond strength and quality of forming film with matrix.
By nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；By BaTiO3Target depends on Secondary dehydrated alcohol, deionized water are respectively washed 5min, with by BaTiO3The impurity cleaning of target material surface is clean, exists the most again By BaTiO in baking oven3Target is dried.
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, sets at magnetron sputtering simultaneously Standby middle inner cavity chamber fixes BaTiO3Target, then magnetron sputtering apparatus inner chamber is evacuated to vacuum is 10-4Pa；Lead in equipment Enter Ar and O2Until operating pressure reaches 1.2Pa, and set the sputtering power of sputtering equipment as 145W, underlayer temperature as 380 DEG C, Matrix rotary speed is that the sputtering parameter of 10rpm carries out sputtering for the first time.
In first time sputter procedure, detect the sputtering thickness of thin film at any time, until it reaches setting thickness, sputtering completes After, take out sample after cooling to room temperature and be placed in sample box.
First time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until the air of the inside Being forced out clean, then tube furnace is warmed up to 750 DEG C, programming rate is 10 DEG C/min, enters 750 DEG C of heated at constant temperature 30min Row heat treatment, then drops to room temperature, and cooling rate is 10 DEG C/min；Sputtered samples after completing heat treatment carries out second time and spatters Penetrating, the substrate temperature in sputtering parameter is set to 420 DEG C for the second time, and the sputtering power of sputtering equipment is 145W, matrix rotates speed Degree is 10rpm.
Sputtered samples is placed in tube furnace after having sputtered by second time, is passed through protective gas N22min, until in The air in face is forced out totally, then tube furnace is warmed up to 770 DEG C, and programming rate is 10 DEG C/min, 770oC heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 DEG C/min.
Embodiment two
The tungsten alloy material matrix of the present embodiment is made up of following components by weight percent: Fisher particle size is 95 parts of the WC powder of 1-1.5um, takes Family name's granularity is 12 parts of the Co powder of 0.5-0.8um, 2 parts of B powder, graphite powder 1 part.
Each material component is chosen by above-mentioned material formula.
Select 1Kg agitating ball mill, be initially charged B powder, C powder and Co powder, add amylalcohol as grinding in the ratio of 500ml/kg Grinding media, adds mill ball by ratio of grinding media to material example 5:1, is stirred grinding, mill ball diameter D7, ball mill mixing speed 480rpm, activity coefficient is 0.85, grinds 1 hour.
Then add tungsten carbide to grind 7 hours, form slip, form slip.
Filtering, be dried, the mesh number of filtration is 50 mesh, and baking temperature is 85 DEG C, makes carbide alloy mixture grain.
By carbide alloy mixture grain by molding or extruding or injection mo(u)lding, make hard alloy blank.
Hard alloy blank entering sintering furnace and is sintered molding, sintering temperature during sinter molding is 1425 DEG C, Ar Pressure is 10Mpa, sintering time is 100min, obtains tungsten alloy matrix.
Substrate pretreated, described substrate pretreated, polishing, ultrasonic cleaning and ion source can be ground successively and clean.Institute State grinding and polishing, can first carry out matrix roughly grinding 10min, then at the Buddha's warrior attendant of 1200 mesh on the boart boart wheel disc of 600 mesh Carry out fine grinding 10min on stone sand wheel disc, then be polished to specimen surface the brightest with the diamond polishing powder of W2.5, described Ultrasonic cleaning, can clean in the following order by the matrix after grinding and polishing, and acetone ultrasonic cleaning 5min → dehydrated alcohol is ultrasonic clearly Washing 5min → dry stand-by, described ion source cleans, and can use hall ion source that matrix is carried out 5min, and pressure is 2 × 10-2Pa, substrate temperature is 300 DEG C, and argon flux is 10sccm, biases as-100V, and cathode current is 29.5A, and cathode voltage is 19V, anode current is 7A, and anode voltage is 80V, to remove adsorbed gas and the impurity of matrix surface, improves deposition coating Bond strength and quality of forming film with matrix.
By nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；By BaTiO3Target depends on Secondary dehydrated alcohol, deionized water are respectively washed 5min, with by BaTiO3The impurity cleaning of target material surface is clean, exists the most again By BaTiO in baking oven3Target is dried.
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, sets at magnetron sputtering simultaneously Standby middle inner cavity chamber fixes BaTiO3Target, then magnetron sputtering apparatus inner chamber is evacuated to vacuum is 10-4Pa；Lead in equipment Enter Ar and O2Until operating pressure reaches 1.2Pa, and set the sputtering power of sputtering equipment as 145W, underlayer temperature as 420 DEG C, Matrix rotary speed is that the sputtering parameter of 20rpm carries out sputtering for the first time.
In first time sputter procedure, detect the sputtering thickness of thin film at any time, until it reaches setting thickness, sputtering completes After, take out sample after cooling to room temperature and be placed in sample box.
First time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until the air of the inside Being forced out clean, then tube furnace is warmed up to 750 DEG C, programming rate is 10 DEG C/min, enters 750 DEG C of heated at constant temperature 30min Row heat treatment, then drops to room temperature, and cooling rate is 10 DEG C/min；Sputtered samples after completing heat treatment carries out second time and spatters Penetrating, the substrate temperature in sputtering parameter is set to 450 DEG C for the second time, and the sputtering power of sputtering equipment is 145W, matrix rotates speed Degree is 20rpm.
Sputtered samples is placed in tube furnace after having sputtered by second time, is passed through protective gas N22min, until in The air in face is forced out totally, then tube furnace is warmed up to 770 DEG C, and programming rate is 10 DEG C/min, 770oC heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 DEG C/min.

Claims (2)

1. the method preparing barium titanate film in tungsten alloy substrate, this tungsten alloy matrix is made up of following components by weight percent: Fisher particle size is WC powder 90-95 part of 1-1.5um, and Fisher particle size is Co powder 8-12 part of 0.5-0.8um, B powder 1-2 part, graphite Powder 0.5-1 part；
The method comprises the steps:
(1) tungsten alloy matrix is prepared
Each material component is chosen by above-mentioned material formula；
Select 1Kg agitating ball mill, be initially charged B powder, C powder and Co powder, add amylalcohol as grinding medium in the ratio of 500ml/kg Matter, adds mill ball by ratio of grinding media to material example 5:1, is stirred grinding, mill ball diameter D7, ball mill mixing speed 480rpm, fills out Filling coefficient is 0.85, grinds 1 hour；
Then add tungsten carbide to grind 5-7 hour, form slip, form slip；
Filtering, be dried, the mesh number of filtration is 40-50 mesh, and baking temperature is 70-85 DEG C, makes carbide alloy mixture grain；
By carbide alloy mixture grain by molding or extruding or injection mo(u)lding, make hard alloy blank；
Hard alloy blank entering sintering furnace and is sintered molding, sintering temperature during sinter molding is 1400-1425 DEG C, Ar Pressure is 8-10Mpa, sintering time is 30-100min, obtains tungsten alloy matrix；
(2) substrate pretreated
Described substrate pretreated, can be ground polishing, ultrasonic cleaning and ion source successively and clean；
(3) by nanometer BaTiO3Powder is pressed into the BaTiO of a diameter of 75mm at 1000 DEG C3Target；
By BaTiO3Target is respectively washed 5min with in dehydrated alcohol, deionized water successively, with by BaTiO3The impurity of target material surface Cleaning is clean, the most in an oven by BaTiO3Target is dried；
(4) once sputter
Pretreated matrix is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, simultaneously in magnetron sputtering apparatus Inner cavity chamber fixes BaTiO3Target, then magnetron sputtering apparatus inner chamber is evacuated to vacuum is 10-4Pa；
It is passed through Ar and O in equipment2Until operating pressure reaches 1.2Pa, and set the sputtering power of sputtering equipment as 145W, lining The sputtering parameter that end temperature is 380-420 DEG C, matrix rotary speed is 10-20rpm carries out sputtering for the first time；
In first time sputter procedure, detect the sputtering thickness of thin film at any time, until it reaches set thickness, after having sputtered, fall Temperature is to taking out sample after room temperature and being placed in sample box；
(5) secondary sputtering
First time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until the air of the inside is forced out Totally, then tube furnace being warmed up to 750 DEG C, programming rate is 10 DEG C/min, carries out at heat 750 DEG C of heated at constant temperature 30min Reason, then drops to room temperature, and cooling rate is 10 DEG C/min；
Sputtered samples after completing heat treatment carries out second time and sputters, and the substrate temperature in sputtering parameter is set to for the second time 420-450 DEG C, the sputtering power of sputtering equipment is 145W, matrix rotary speed is 10-20rpm,
Sputtered samples is placed in tube furnace after having sputtered by second time, is passed through protective gas N22min, until the inside Air is forced out totally, then tube furnace is warmed up to 770 DEG C, and programming rate is 10 DEG C/min, 770oC heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 DEG C/min.
2. the method for claim 1, it is characterised in that in described step (2), described grinding and polishing, can be by matrix First carry out roughly grinding 10min on the boart boart wheel disc of 600 mesh, on the boart boart wheel disc of 1200 mesh, then carry out fine grinding 10min, then it is polished to specimen surface the brightest with the diamond polishing powder of W2.5, described ultrasonic cleaning, can will grind Matrix after polishing cleans in the following order, and acetone ultrasonic cleaning 5min → dehydrated alcohol ultrasonic cleaning 5min → dry is stand-by, Described ion source cleans, and can use hall ion source that matrix is carried out 5min, and pressure is 2 × 10-2Pa, substrate temperature is 300 DEG C, argon flux is 10sccm, biases as-100V, and cathode current is 29.5A, and cathode voltage is 19V, and anode current is 7A, anode voltage is 80V, to remove adsorbed gas and the impurity of matrix surface, improves deposition coating strong with the combination of matrix Degree and quality of forming film.
CN201610690514.3A 2016-08-20 2016-08-20 Method for preparing barium titanate film on tungsten alloy substrate Pending CN106319464A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106835045A (en) * 2017-02-15 2017-06-13 苏州思创源博电子科技有限公司 A kind of preparation method of barium titanate film
CN108213446A (en) * 2018-03-07 2018-06-29 戴爱娟 A kind of preparation method for the tungsten alloy for having silicon coating
CN108251814A (en) * 2018-03-07 2018-07-06 瞿凌飞 A kind of preparation method for the tungsten alloy for having memory alloy layer

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CN101921982A (en) * 2010-09-06 2010-12-22 厦门大学 Method for preparing nano-structured nitrogen silicon zirconium coating on surface of hard alloy substrate
CN105671400A (en) * 2014-11-21 2016-06-15 河南省大地合金股份有限公司 Preparation method for high-abrasion-resistance hard alloy
CN105803395A (en) * 2016-03-31 2016-07-27 长江大学 Preparation method for multi-layer Ni/BaTiO3 thin film capable of reducing dielectric losses

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Publication number Priority date Publication date Assignee Title
CN101921982A (en) * 2010-09-06 2010-12-22 厦门大学 Method for preparing nano-structured nitrogen silicon zirconium coating on surface of hard alloy substrate
CN105671400A (en) * 2014-11-21 2016-06-15 河南省大地合金股份有限公司 Preparation method for high-abrasion-resistance hard alloy
CN105803395A (en) * 2016-03-31 2016-07-27 长江大学 Preparation method for multi-layer Ni/BaTiO3 thin film capable of reducing dielectric losses

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CN106835045A (en) * 2017-02-15 2017-06-13 苏州思创源博电子科技有限公司 A kind of preparation method of barium titanate film
CN108213446A (en) * 2018-03-07 2018-06-29 戴爱娟 A kind of preparation method for the tungsten alloy for having silicon coating
CN108251814A (en) * 2018-03-07 2018-07-06 瞿凌飞 A kind of preparation method for the tungsten alloy for having memory alloy layer

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