CN113463023A - Preparation method of silicon nitride composite film for surface abrasion resistance of medical instrument die - Google Patents

Preparation method of silicon nitride composite film for surface abrasion resistance of medical instrument die Download PDF

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CN113463023A
CN113463023A CN202110470649.XA CN202110470649A CN113463023A CN 113463023 A CN113463023 A CN 113463023A CN 202110470649 A CN202110470649 A CN 202110470649A CN 113463023 A CN113463023 A CN 113463023A
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composite film
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argon
tin
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杜刚
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East China Normal University
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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
    • C23C14/46—Sputtering by ion beam produced by an external ion source
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • 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
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
    • C23C14/0641—Nitrides
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation

Abstract

The invention discloses a preparation method of a silicon nitride composite film for surface abrasion resistance of a medical instrument die, which is characterized in that Si is doped on the basis of a TiN film to form nc-TiN/a-Si by adopting a method of magnetic filtration cathodic arc and ion beam sputtering codeposition3N4The preparation method of the ternary nano composite film specifically comprises the following steps: substrate pretreatment, ICP cleaning, deposition of a transition layer, preparation of a ternary composite film and the like. Compared with the prior art, the method has the advantages of simple process, environmental protection and environmental protection, and Si is doped on the basis of TiN film to form Si3N4The composite film greatly reduces the roughness, has good abrasion resistance and antifriction effectThe method is obvious in separation, is particularly suitable for surface films of molds for large-scale production of medical instrument parts, and is a preparation method with a good application prospect and a good practical value.

Description

Preparation method of silicon nitride composite film for surface abrasion resistance of medical instrument die
Technical Field
The invention relates to the technical field of preparation of inorganic composite films, in particular to Si for resisting abrasion on the surface of a medical instrument die3N4A method for preparing a composite film.
Background
In recent years, nc-TiN/a-Si formed by doping Si on the basis of TiN thin film3N4Nanocomposite films are of interest because of their ultra-high hardness, which approaches that of diamond. Method for producing the same, and superhard machineAnd other mechanical properties such as tribological properties and fracture toughness have attracted a great deal of research. Since chemical vapor deposition involves toxic gases and the substrate temperature is high, it is currently used for preparing nc-TiN/a-Si3 N 4The method of the ternary nano composite film mainly adopts physical methods such as magnetron sputtering and the like. However, magnetron sputtering is prone to generate more pores and spherical crystals due to high air pressure and low ionization rate, and the prepared thin film is not ideal in the aspects of film-substrate bonding strength, tribology and the like, and the crystallization property of TiN and the a-Si can be improved by increasing the substrate temperature3N4The phases are separated to achieve a superhard result. Whereby several methods are followed to increase the ionization rate and ion energy. Such as magnetron sputtering deposition with an auxiliary ion source, ion beam sputtering with an auxiliary ion source, or magnetron sputtering co-deposition of a Si target and Ti cathode arc. Of these, cathodic arc is of great interest due to its high ionization rate and high ion energy. But micron-sized particles generated by the cathodic arc also reduce the mechanical properties and chemical stability of the film.
Disclosure of Invention
The invention aims to provide Si for resisting the abrasion of the surface of a medical instrument die aiming at the defects of the prior art3N4A composite film preparing method, adopting a magnetic filtration cathodic arc and ion beam sputtering codeposition method, doping Si on the basis of TiN film to form nc-TiN/a-Si3N4 ternary nano composite film, thereby obtaining the composite film with good tribological performance, being used for surface abrasion resistance of medical appliance molds, having simple process, the self-assembled composite film has good antifriction performance, not only retaining the characteristics of high ionization rate, high ion energy and high film-substrate bonding strength of cathodic arc ion plating, but also eliminating micron-sized large particles, obtaining a smoother, compact and uniform film, effectively solving the tribological problem on the surface of the medical appliance, and having the advantages of simple operation, good quality stability, high preparation efficiency and high finished product quality.
The purpose of the invention is realized as follows: si for surface abrasion resistance of medical instrument die3N4Method for preparing composite film, its characteristicsAdopts a method of magnetic filtration cathodic arc and ion beam sputtering codeposition to dope Si on the basis of TiN film to form nc-TiN/a-Si3N4The preparation method of the ternary nano composite film specifically comprises the following steps:
step a: substrate pretreatment
The substrate material is a 550 mu m thick Si (400) monocrystalline silicon wafer, which is ultrasonically cleaned for 20min by absolute ethyl alcohol, acetone and deionized water in sequence, taken out, dried by nitrogen and placed in a vacuum chamber.
Step b: ICP cleaning
Adopting FDJ high vacuum multifunctional film deposition equipment, firstly pumping the vacuum chamber to 5.0 x 10 -4 Pa, before depositing the film, cleaning the surface of the monocrystalline silicon by using argon ions generated by an ICP (inductively coupled plasma) ion source, wherein the vacuum degree is 0.1Pa, the argon flow is 30.0sccm, the output power is 400W, the screen electrode voltage is 400V, the acceleration voltage is 60V, and the ion energy is 400 ev. Preheating for 15min at the temperature of 70-80 ℃, and opening a baffle to start bombardment cleaning. After 20min, closing the voltage of the shield and the accelerating voltage, slowly closing the flow of argon gas, and returning the vacuum degree in the vacuum chamber to 5 × 10 -4 Pa。
In the cleaning process, ions generated by the ion source can probably etch the surface of the silicon wafer by about 20nm, and the process mainly removes various impurities (mainly oxides) on the surface of the silicon substrate so as to improve the migration energy of atoms on the surface of the substrate, further enhance the activity of the surface of the substrate and improve the bonding strength of the film and the substrate material.
Step c: deposition of transition layer
Cleaning a substrate, depositing a transition layer, and in order to further increase the bonding strength of the film and the substrate, depositing a Ti transition layer by using ion beam sputtering, wherein the purity of a Ti target material is 99.99%; the voltage of the screen electrode is 1600V; the accelerating voltage is 120V; the cathode discharge current was 10A; the beam current is 50 mA; the argon flow is 7-9 sccm; the deposition pressure is 2.5X 10 -2 Pa, pre-sputtering for 15min to remove oxides and other impurities on the surface of the target.
Opening the baffle plate to deposit a Ti transition layer of 5 min-10 nm, and keeping the substrate temperature at 25 +/-2 ℃ in the deposition process. And (4) closing the baffle after the deposition is finished, closing the screen electrode voltage, the accelerating voltage, the anode voltage and the cathode voltage, slowly closing the argon flow, and returning the vacuum degree in the vacuum chamber to 5 multiplied by 10 < -4 > Pa again.
Step d: preparation of ternary composite film
After the deposition of the transition layer is finished, argon ion beam sputtering is adopted to deposit Si3N4Method for preparing nc-TiN/a-Si by simultaneous magnetic filtration cathodic arc deposition of TiN3N4Ternary nanocomposite films. Wherein the ion beam sputtering target is alpha-Si3N4(the purity is 99.99%), argon (the purity is 99.999%), the flow is controlled to be 7-9 sccm, and the beam current of a sputtering ion gun is controlled to be 50 mA; the magnetic filtration cathode target material is a Ti target (the purity is 99.96%); the reaction gas adopts a mixed gas of nitrogen and argon (the purity is 99.999 percent). Wherein the argon flow is 7.0 sccm; the nitrogen flow rate is 21.0 sccm; the outlet coil current is 1.5A; the current of a source coil is 0.25A; the current of the magnetic filtering coil is controlled to be 5.0A, 3.5A and 3.0A respectively; the cathode current was maintained at 70A. Preparing a series of Si with different Si contents by adjusting beam current of ion beam sputtering and current of magnetic filter coil3N4A nanocomposite film.
Compared with the prior art, the method has the advantages of simple process, environmental protection and environmental protection, and Si is doped on the basis of TiN film to form Si3N4The composite film greatly reduces the roughness, has good abrasion resistance and obvious antifriction effect, is particularly suitable for surface films of dies for large-scale production of medical appliance parts, and is a preparation method with good application prospect and practical value.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
The substrate material is a 550 mu m thick Si (400) monocrystalline silicon wafer, which is ultrasonically cleaned for 20min by absolute ethyl alcohol, acetone and deionized water in sequence, taken out, dried by nitrogen and placed in a vacuum chamber. Then, ICP cleaning and transition are carried outLayer deposition, namely sputtering and depositing a Ti transition layer by using ion beams, wherein the target is a high-purity Ti target with the purity of 99.99 percent, the voltage of a screen electrode is 1600V, the accelerating voltage is 120V, the cathode discharge current is 10A, the beam current is 50mA, the argon flow is 8.0sccm, and the deposition pressure is 2.5 multiplied by 10-2Pa, pre-sputtering for 15min to remove oxides and other impurities on the surface of the target.
Opening the baffle plate to start deposition, depositing the Ti transition layer for 5min, wherein the temperature of the substrate is kept at 25 +/-2 ℃ during the deposition process, and the thickness of the Ti transition layer is about 10 nm. After the deposition of the transition layer is finished, argon ion beam sputtering is adopted to deposit Si3N4Preparing the nc-TiN/a-Si3N4 ternary nano composite film by a method simultaneously performing magnetic filtration cathodic arc deposition of TiN, wherein: the ion beam sputtering target is alpha-Si3N4(purity 99.99%); argon (99.999% pure); the flow rate is controlled to be about 8.0 sccm; controlling the beam current of the sputtering ion gun to be 50 mA; the magnetic filtration cathode target material is a Ti target (the purity is 99.96%). The reaction gas adopts a nitrogen and argon mixed gas (the purity is 99.999%), wherein: the argon flow is 7.0 sccm; the nitrogen flow rate is 21.0 sccm; the outlet coil current is 1.5A; the current of a source coil is 0.25A; controlling the current of the magnetic filtering coil to be 5.0A; cathode current is maintained at 70A, and nc-TiN/a-Si is prepared3N4The thickness of the ternary nano composite film is 210nm, and the content of Si is 3.20%.
The tribological performance of the film in the air environment is inspected by adopting UMT-2 multifunctional friction produced by American CETR, and the prepared nc-TiN/a-Si is measured3N4The surface roughness of the ternary nano composite film is 1.01nm, which shows that the film has better anti-wear effect.
Example 2
The substrate material is a 550 mu m thick Si (400) monocrystalline silicon wafer, which is ultrasonically cleaned for 20min by absolute ethyl alcohol, acetone and deionized water in sequence, taken out, dried by nitrogen and placed in a vacuum chamber. Then, ICP cleaning and transition layer deposition are carried out, a Ti transition layer is deposited by ion beam sputtering, the target material is a high-purity Ti target with the purity of 99.99 percent, the voltage of a screen electrode is 1600V, the accelerating voltage is 120V, the discharge current of a cathode is 10A, the beam current is 50mA, the argon flow is 8.0sccm, and deposition is carried outThe air pressure is 2.5 multiplied by 10 -2Pa, pre-sputtering for 15min to remove oxides and other impurities on the surface of the target.
Opening the baffle plate to start deposition, depositing the Ti transition layer for 5min, wherein the temperature of the substrate is kept at 25 +/-2 ℃ during the deposition process, and the thickness of the Ti transition layer is about 10 nm. After the deposition of the transition layer is finished, argon ion beam sputtering is adopted to deposit Si3N4Preparing the nc-TiN/a-Si3N4 ternary nano composite film by a method simultaneously performing magnetic filtration cathodic arc deposition of TiN, wherein: the ion beam sputtering target is alpha-Si3N4(purity 99.99%); argon (99.999% pure); the flow rate is controlled to be about 8.0 sccm; controlling the beam current of the sputtering ion gun to be 50 mA; the magnetic filtration cathode target material is a Ti target (the purity is 99.96%). The reaction gas adopts a nitrogen and argon mixed gas (the purity is 99.999%), wherein: the argon flow is 7.0 sccm; the nitrogen flow rate is 21.0 sccm; the outlet coil current is 1.5A; the current of a source coil is 0.25A; controlling the current of the magnetic filtering coil to be 3.5A; cathode current is maintained at 70A, and nc-TiN/a-Si is prepared3N4The thickness of the ternary nano composite film is 200nm, and the content of Si is 8.12%.
Si prepared by evaluating the quality of the film by the characterization means in example 13N4The ternary nano composite film can reduce the roughness to 0.35nm and has obvious anti-wear effect.
Example 3
The substrate material is a 550 mu m thick Si (400) monocrystalline silicon wafer, which is ultrasonically cleaned for 20min by absolute ethyl alcohol, acetone and deionized water in sequence, taken out, dried by nitrogen and placed in a vacuum chamber. Then, ICP cleaning and transition layer deposition are carried out, ion beam sputtering is used for depositing a Ti transition layer, the target material is a high-purity Ti target with the purity of 99.99 percent, the voltage of a screen electrode is 1600V, the acceleration voltage is 120V, the discharge current of a cathode is 10A, the beam current is 50mA, the argon flow is 8.0sccm, and the deposition pressure is 2.5 multiplied by 10 -2Pa, pre-sputtering for 15min to remove oxides and other impurities on the surface of the target.
Opening the baffle plate to start deposition, depositing the Ti transition layer for 5min, wherein the temperature of the substrate is kept at 25 +/-2 ℃ during the deposition process, and the thickness of the Ti transition layer is about 10 nm. Mining after the deposition of the transition layer is finishedSputter deposition of Si with argon ion beam3N4Preparing the nc-TiN/a-Si3N4 ternary nano composite film by a method simultaneously performing magnetic filtration cathodic arc deposition of TiN, wherein: the ion beam sputtering target was α -Si3N4 (purity 99.99%), argon (purity 99.999%); the flow rate is controlled to be about 8.0 sccm; controlling the beam current of the sputtering ion gun to be 50 mA; the magnetic filtration cathode target material is a Ti target (the purity is 99.96%). The reaction gas adopts a nitrogen and argon mixed gas (the purity is 99.999%), wherein: the argon flow is 7.0 sccm; the nitrogen flow rate is 21.0 sccm; the outlet coil current is 1.5A; the current of a source coil is 0.25A; controlling the current of the magnetic filtering coil to be 3.0A; cathode current is maintained at 70A, and nc-TiN/a-Si is prepared3N4The thickness of the ternary nano composite film is 210nm, and the content of Si is 10.9%.
The film quality was evaluated by the characterization procedure in example 1. Prepared Si3N4The ternary nano composite film can reduce the roughness to 0.31nm and has very obvious anti-wear effect.
The invention has been described in further detail in order to avoid limiting the scope of the invention, and it is intended that all such equivalent embodiments be included within the scope of the following claims.

Claims (4)

1. A process for preparing the antiwear composite silicon nitride film used for the surface of medical apparatus or die features that the magnetically filtered cathode arc and ion beam sputtering are used to co-deposit, and Si is doped in the TiN film to form nc-TiN/a-Si3N4The preparation method of the ternary nano composite film specifically comprises the following steps:
step a: substrate pretreatment
Selecting a 550-micrometer-thick monocrystalline silicon wafer as a substrate, ultrasonically cleaning the monocrystalline silicon wafer with absolute ethyl alcohol, acetone and deionized water in sequence, blow-drying the monocrystalline silicon wafer with nitrogen, and placing the monocrystalline silicon wafer into a vacuum chamber for later use;
step b: ICP cleaning
The vacuum chamber is pumped to 5.0X 10-4Pa, preheating for 15min at the temperature of 70-80 ℃, and then feeding the monocrystalline silicon wafer by using argon ions generated by a radio frequency induction coupling ion source under the vacuum of 0.1PaLine bombardment cleaning is carried out, and the cleaning time is 20 min;
step c: deposition of transition layer
Depositing a Ti transition layer with the thickness of 5 min-10 nm on a substrate by using ion beam sputtering, wherein the purity of a Ti target material sputtered by the ion beam is 99.99%, and the deposition pressure is 2.5 multiplied by 10-2 Pa, screen electrode voltage is 1600V, accelerating voltage is 120V, cathode discharge current is 10A, beam current is 50mA, and argon flow is 8.0 sccm; pre-sputtering the Ti target for 15 min; the deposition temperature of the substrate is 25 +/-2 ℃;
step d: preparation of ternary composite film
Sputtering deposition of Si using argon ion beam3N4The method for simultaneously depositing TiN with the magnetic filtering cathodic arc prepares nc-TiN/a-Si with different Si contents on the Ti transition layer by adjusting the beam current of ion beam sputtering and the current of the magnetic filtering coil3N4The thickness of the ternary nano composite film is 25-50 nm.
2. The method for preparing the silicon nitride composite film for the surface abrasion resistance of the medical instrument die according to claim 1, wherein the flow rate of argon gas generated by the radio frequency induction coupling ion source is 30.0 sccm; the output power is 400W; the voltage of the screen electrode is 400V; the accelerating voltage is 60V; the ion energy was 400 eV.
3. The method for preparing the silicon nitride composite film for abrasion resistance of the surface of the medical instrument die as claimed in claim 1, wherein the argon ion beam sputtering target is α -Si3N4The purity is 99.99%; the purity of argon is 99.999 percent; the flow rate is 7-9 sccm; the beam current of the sputtering ion gun is 50 mA.
4. The method for preparing the silicon nitride composite film for the surface abrasion resistance of the medical instrument die according to claim 1, wherein the target material of the magnetic filtration cathode is a Ti target with the purity of 99.96%, and the reaction adopts a mixed gas of nitrogen and argon with the purity of 99.999%, wherein the flow of the argon gas is 7.0sccm, and the flow of the nitrogen gas is 21.0 sccm; the outlet coil current is 1.5A; the current of a source coil is 0.25A; the current of the magnetic filter coil is controlled to be 5.0A, 3.5A and 3.0A respectively; the cathode current was 70A.
CN202110470649.XA 2021-04-29 2021-04-29 Preparation method of silicon nitride composite film for surface abrasion resistance of medical instrument die Pending CN113463023A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102277556A (en) * 2011-08-18 2011-12-14 河南大学 Method for preparing nano composite ultra-hard thin film

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102277556A (en) * 2011-08-18 2011-12-14 河南大学 Method for preparing nano composite ultra-hard thin film

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
杨友志等: "磁控溅射TiN/Si_3N_4纳米复合膜的制备及其环境摩擦学特性", 《材料科学与工程学报》 *
杨莹泽: "nc-TiN/a-Si3N4纳米复合薄膜的制备与性能研究", 《工程科技Ⅰ辑》 *
杨莹泽等: "Ti-Si-N纳米复合薄膜的制备及其力学性能", 《中国有色金属学报》 *

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