CN110373519B - Preparation method of high-hardness wear-resistant stainless steel - Google Patents
Preparation method of high-hardness wear-resistant stainless steel Download PDFInfo
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 54
- 239000010935 stainless steel Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 62
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000000576 coating method Methods 0.000 claims abstract description 50
- 239000011248 coating agent Substances 0.000 claims abstract description 48
- 239000010936 titanium Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 41
- 238000005468 ion implantation Methods 0.000 claims abstract description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 30
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000151 deposition Methods 0.000 claims abstract description 19
- 238000005498 polishing Methods 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 229910010037 TiAlN Inorganic materials 0.000 claims abstract description 10
- 239000010409 thin film Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims description 92
- 239000010408 film Substances 0.000 claims description 34
- 238000002347 injection Methods 0.000 claims description 24
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- 238000010306 acid treatment Methods 0.000 claims description 6
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- 239000007788 liquid Substances 0.000 claims description 6
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
-
- 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
-
- 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
-
- 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
- C23C14/48—Ion implantation
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/088—Iron or steel solutions containing organic acids
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/19—Iron or steel
Abstract
The invention provides a preparation method of high-hardness wear-resistant stainless steel, which comprises the following steps: firstly, carrying out mechanical processing, heat treatment, grinding and polishing treatment on a substrate, then cleaning and airing, carrying out ion implantation of titanium and nitrogen double elements by adopting an ion implantation method, then depositing a TiAlN thin film layer in a multi-arc ion coating machine, and then depositing a VN thin film layer in the multi-arc ion coating machine. The stainless steel prepared by the method has the advantages of high hardness, good machinability, electrical conductivity, thermal conductivity and the like, and meanwhile, the method has the advantages of precise and controllable conditions, complete functionality of the stainless steel surface coating and high yield.
Description
Technical Field
The invention relates to the technical field of alloy steel, in particular to high-hardness wear-resistant stainless steel.
Background
Stainless steel refers to steel which resists corrosion by weak corrosive media such as air, steam, water and the like and chemical corrosive media such as acid, alkali, salt and the like, and is also called as stainless acid-resistant steel. In practice, steel resistant to corrosion by weakly corrosive media is often referred to as stainless steel, while steel resistant to corrosion by chemical media is referred to as acid-resistant steel. Due to the difference in chemical composition between the two, the former is not necessarily resistant to corrosion by chemical media, while the latter is generally non-corrosive. The corrosion resistance of stainless steel depends on the alloying elements contained in the steel.
In modern society, stainless steel has extremely wide applications, and can be applied to both household products and industrial production. With the wider application of stainless steel, various performances of stainless steel are gradually improved. However, in the prior art, there is still no disclosure of stainless steel used in high-temperature machinery represented by various high-performance aero-engines, and in high-technical equipment fields such as geological drilling fields where continuous operation from room temperature to high temperature is required, because the hardness and wear resistance of stainless steel do not meet the requirements of high-strength operation. Therefore, the preparation of the stainless steel with high hardness, high melting point, good stability and low friction coefficient is an important technical means in future industrial production.
As is known from patent application publication No. CN 104520472 a, TiAlN has extremely high hardness and high elastic modulus as a coating layer; it is known from application publication No. CN 103726014 a that VN as a coating has the effects of high wear resistance and low wear rate. However, the problems of great internal stress, low adhesion and the like exist between the TiAlN and VN combined coating and between the coating and the substrate, so that the problems of delamination, peeling and failure of the film are caused; therefore, a composite coating adopting the combination of TiAlN and VN is not disclosed at present, so that the surface of the stainless steel has the characteristics of high hardness and self-lubrication (namely high wear resistance).
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide a preparation method of high-hardness wear-resistant stainless steel, and the prepared stainless steel has the advantages of high hardness, high melting point, good stability and low friction coefficient, and can be suitable for high-strength fields such as aeroengines and geological drilling.
The purpose of the invention is realized by the following technical scheme:
a preparation method of high-hardness wear-resistant stainless steel selects stainless steel as a base material, and is characterized by comprising the following steps of: firstly, carrying out mechanical processing, heat treatment, grinding and polishing treatment on a substrate, then cleaning and airing, carrying out ion implantation of titanium and nitrogen double elements by adopting an ion implantation method, then depositing a TiAlN thin film layer in a multi-arc ion coating machine, and then depositing a VN thin film layer in the multi-arc ion coating machine.
The high-hardness wear-resistant stainless steel prepared by the steps effectively reduces the internal stress of the film and the substrate, improves the binding force between the film and the substrate, avoids the problems of delamination, peeling, failure and the like of the film, and ensures the yield of the high-hardness wear-resistant stainless steel.
Further, the heat treatment needs 1240 ℃ high-temperature quenching and three times of 560 ℃ high-temperature tempering; the grinding is carried out on a grinding machine, and 800#, 1000#, 1500# water sand paper are used for grinding in sequence; the polishing treatment was performed on a polishing machine using diamond having a particle size of 0.1 μm as a polishing agent.
Further, the above cleaning is carried out by using an acid-alkali treatment solution, and the alkali treatment is carried out first and then the acid treatment is carried out.
In the pretreatment process before ion implantation, if scratches exist on the surface of the substrate or the hardness of the substrate is low, the acid-alkali treatment liquid reacts with the surface of the substrate during acid-alkali treatment, so that subsequent ion implantation and film deposition are influenced. By adopting the step combination and the treatment process, the smoothness of the surface of the substrate is ensured under the condition of ensuring the hardness of the substrate, and the smooth proceeding of the ion implantation and the film deposition after the pretreatment is ensured, so that the conditions for preparing the film are accurate and controllable, and the film function is complete.
Further, the ion implantation method adopts a Metal Vapor Vacuum Arc (MEVVA) ion implanter; the ion implantation method adopts high-purity titanium as a target material and introduces nitrogen gas to carry out the ion implantation of titanium and nitrogen double elements.
Further, the energy of the Ti ions in the ion implantation method is: 45-50keV, the projection range Rp and range divergence of Ti ions are 45.1 and 16.5nm, and the implantation dose of the Ti ions is fixed as follows: 1.0X1017-1.5×1017ions/cm2(ii) a The N ion implantation parameters are: background vacuum degree of vacuum chamber 1.0x10-3Pa，N2The partial pressure is 0.6-0.9Pa, a bias voltage of-2.5 to-2.0 kV is applied on the substrate, the frequency is 16-20kHz, and the N ion injection time is 2.5-3.5 h; in the process of injecting Ti ions, the incident ions and the surface of the stainless steel substrate keep an included angle of 90 degrees, and the beam intensity is controlled to be 4.0-4.5A/cm2To avoid the temperature increase effect caused by the ion implantation process; in the process of injecting the N ions, the N ions are vertically incident.
When the ion implantation method is adopted, the technical problem of agglomeration of the ion implantation substrate is caused due to the instability of the motion track of the ions and the impact generated when the ions are incident on the surface of the substrate, so that the subsequent steps of preparing the multilayer film are invalid or uneven, the preparation yield is not high, and the bonding force between the substrate and each layer of film is also influenced; by adopting the treatment process and the step combination, the dispersibility and the uniformity of the ion implantation are ensured, the smooth proceeding of the subsequent steps is ensured, and the uniformity, the yield and the bonding strength between the matrix and the film are ensured.
Further, the multi-arc ion coating machine adopts a WH-800 type multi-arc ion coating machine, and the main coating process parameters are deposition temperature: 450 ℃ and 500 ℃, nitrogen partial pressure: 0.8-1.0Pa, flow rate: 80sccm, arc current: 80-90A, negative voltage: -220 to-180V, vacuum: 4X 10-3Pa, coating time: 60-80 min.
Further, the TiAlN thin film layer is deposited in the multi-arc ion coating machine, high-purity titanium and high-purity aluminum are used as target materials, and nitrogen is introduced; depositing a VN film layer in a multi-arc ion coating machine, taking high-purity vanadium as a target material, and introducing nitrogen.
Further, the TiAlN thin film layer is 110nm-130 nm; the VN film layer is 120nm-140 nm.
The high-hardness wear-resistant stainless steel and the preparation method thereof are characterized by comprising the following steps of:
a. selecting stainless steel as a base material, and carrying out proper machining on the base material to enable the base material to be in a tool or die shape which meets the industrial use standard; then, carrying out 1240 ℃ high-temperature quenching and three times of 560 ℃ high-temperature tempering heat treatment on the substrate, sequentially grinding the substrate on a grinding machine by using 800#, 1000# and 1500# water sand paper, and polishing the substrate on a polishing machine by using diamond with the grain diameter of 0.1 mu m as a polishing agent;
b. sequentially cleaning and pretreating a tool or a mold matrix by using a mixed solvent such as tap water and alcohol, an acid-alkali treatment solution, high-purity water-ultrasonic waves, acetone-ultrasonic waves and the like, and then airing for later use; wherein the acid and alkali treatment liquid is HF + HNO3+ HAC (molar ratio 1: 1) mixed acid and K3(Fe(CN)6) + KOH (mass ratio 1: 1) mixed alkali solution, firstly carrying out alkali treatment to roughen the surface of the substrate material, and then carrying out acid treatment to remove impurities on the surface of the substrate;
c. placing the pretreated and cleaned substrate into an injection chamber of an ion implanter, pumping the injection chamber to a vacuum state, cleaning the required injection element target material for 3-10 min by using argon gas, and injecting nitrogen gas into a titanium target to perform ion injection treatment of titanium and nitrogen double elements; wherein, the energy of Ti ions is: 45-50keV, the projection range Rp and range divergence of Ti ions are 45.1 and 16.5nm, and the implantation dose of the Ti ions is fixed as follows: 1.0X1017-1.5×1017ions/cm2(ii) a The N ion implantation parameters are: background vacuum degree of vacuum chamber 1.0x10-3Pa，N2The partial pressure is 0.6-0.9Pa, a bias voltage of-2.5 to-2.0 kV is applied on the substrate, the frequency is 16-20kHz, and the N ion injection time is 2.5-3.5 h; in the process of injecting Ti ions, the incident ions and the surface of the stainless steel substrate keep an included angle of 90 degrees, and the beam intensity is controlled to be 4.0-4.5A/cm2To avoid the temperature increase effect caused by the ion implantation process; in the process of injecting N ions, the N ions vertically enter;
d. putting the substrate into a multi-arc ion plating machine, bombarding and cleaning impurities adsorbed on the surface by using nitrogen ions, then using titanium and aluminum as target materials, and generating N by arc ablation3-、Al3+、Ti2+Ions which are deposited under the action of negative bias to obtain a film with a certain thickness as a high-hardness surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating process parameters are depositionVolume temperature: 450 ℃ and 500 ℃, nitrogen partial pressure: 0.8-1.0Pa, flow rate: 80sccm, arc current: 80-90A, negative voltage: -220 to-180V, vacuum: 4X 10-3Pa, coating time: 60-80 min;
e. putting the substrate with the high-hardness surface layer into a multi-arc ion coating machine, introducing nitrogen, using vanadium as a target material, and generating N by arc ablation3-、V3+The ions are deposited under the action of negative bias to obtain a film with a certain thickness as a self-lubricating surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating technological parameters are deposition temperature: 450 ℃ and 500 ℃, nitrogen partial pressure: 0.8-1.0Pa, flow rate: 80sccm, arc current: 80-90A, negative voltage: -220 to-180V, vacuum: 4X 10-3Pa, coating time: 60-80 min.
The invention has the following technical effects:
the invention provides a preparation method of high-hardness wear-resistant stainless steel, which enables the prepared stainless steel to have higher hardness, good machinability, electrical conductivity, thermal conductivity and the like; meanwhile, the ceramic material has ceramic characteristics such as higher elastic modulus, good corrosion resistance, high-temperature oxidation resistance and the like. Meanwhile, the method for preparing the high-hardness wear-resistant stainless steel has the advantages of precise and controllable conditions, complete functionality of the stainless steel surface coating and high yield, and solves the problems of reduction of hardness and elastic modulus and lubrication of friction pairs under different conditions caused by film coating treatment; the problem of ion agglomeration during ion implantation is solved, and the uniformity of the film and the bonding strength between the substrate and the film are ensured.
Drawings
FIG. 1 is a cross-sectional view of the surface of a stainless steel prepared in example 1 of the present invention.
FIG. 2 is a diagram showing the shape of the stainless steel and SiC ball counter-grinding produced in example 2 of the present invention.
FIG. 3 is an indentation chart of the stainless steel bonding force test prepared in example 3 of the present invention.
FIG. 4 is a scratch pattern of the stainless steel bonding force test prepared in example 3 of the present invention.
In the figure, (a) is a scratch surface image, and (b) is an electron micrograph.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments, but not all embodiments, of the present invention.
Example 1
A method for preparing high-hardness wear-resistant stainless steel with Cr steel grade25Mo3Ti and stainless steel with the size of 60x60mm are taken as base materials, and the method is characterized in that:
a. for steel number Cr25Mo3Ti, stainless steel base material with the size of 60x60mm is properly machined to form a tool or a die shape which meets the standard of industrial use; then, carrying out 1240 ℃ high-temperature quenching and three times of 560 ℃ high-temperature tempering heat treatment on the substrate, sequentially grinding the substrate on a grinding machine by using 800#, 1000# and 1500# water sand paper, and polishing the substrate on a polishing machine by using diamond with the grain diameter of 0.1 mu m as a polishing agent;
b. sequentially cleaning and pretreating a tool or a mold matrix by using a mixed solvent such as tap water and alcohol, an acid-alkali treatment solution, high-purity water-ultrasonic waves, acetone-ultrasonic waves and the like, and then airing for later use; wherein the acid and alkali treatment liquid is HF + HNO3+ HAC (molar ratio 1: 1) mixed acid and K3(Fe(CN)6) + KOH (mass ratio 1: 1) mixed alkali solution, firstly carrying out alkali treatment to roughen the surface of the substrate material, and then carrying out acid treatment to remove impurities on the surface of the substrate;
c. placing the pretreated and cleaned substrate into an injection chamber of an ion implanter, pumping the injection chamber to a vacuum state, cleaning the required injection element target material for 3-10 min by using argon gas, and injecting nitrogen gas into a titanium target to perform ion injection treatment of titanium and nitrogen double elements; wherein, the energy of Ti ions is: 45ke V, the projection range Rp and range divergence of Ti ions are 45.1 nm and 16.5nm, and the injection dose of the Ti ions is fixed as follows: 1.0X1017ions/cm2(ii) a The N ion implantation parameters are: trueBackground vacuum degree of empty chamber 1.0x10-3Pa，N2The partial pressure is 0.6Pa, a bias voltage of-2.0 kV is applied to the substrate, the frequency is 16kHz, and the N ion injection time is 2.5 h; in the process of injecting Ti ions, the incident ions and the surface of the stainless steel substrate keep an included angle of 90 degrees, and the beam intensity is controlled to be 4.0A/cm2To avoid the temperature increase effect caused by the ion implantation process; in the process of injecting N ions, the N ions vertically enter;
d. putting the substrate into a multi-arc ion plating machine, bombarding and cleaning impurities adsorbed on the surface by using nitrogen ions, then using titanium and aluminum as target materials, and generating N by arc ablation3-、Al3+、Ti2+Ions which are deposited under the action of negative bias to obtain a film with the thickness of 110nm as a high-hardness surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating technological parameters are deposition temperature: 450 ℃, nitrogen partial pressure: 0.8Pa, flow rate: 80sccm, arc current: 80A, negative voltage: -180V, vacuum: 4X 10-3Pa, coating time: 60 min;
e. putting the substrate with the high-hardness surface layer into a multi-arc ion coating machine, introducing nitrogen, using vanadium as a target material, and generating N by arc ablation3-、V3+The ions are deposited under the action of negative bias to obtain a film with the thickness of 120nm as a self-lubricating surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating technological parameters are deposition temperature: 450 ℃, nitrogen partial pressure: 0.8Pa, flow rate: 80sccm, arc current: 80A, negative voltage: -180V, vacuum: 4X 10-3Pa, coating time: and (5) 60 min.
Example 2
A method for preparing high-hardness wear-resistant stainless steel with Cr steel grade17Mo2Ti and stainless steel with the size of 80x80mm are taken as base materials, and the method is characterized in that:
a. to the matrix number Cr17Mo2A stainless steel material of Ti and 80x80mm size is properly machined into a tool or die shape meeting the industry standard; then the substrate is subjected to heat treatment of 1240 ℃ high-temperature quenching and three times of 560 ℃ high-temperature tempering, and the substrate is sequentially used on a grinding machinePolishing with 800#, 1000# and 1500# water sand paper, and polishing with diamond with particle size of 0.1 μm as polishing agent on a polishing machine;
b. sequentially cleaning and pretreating a tool or a mold matrix by using a mixed solvent such as tap water and alcohol, an acid-alkali treatment solution, high-purity water-ultrasonic waves, acetone-ultrasonic waves and the like, and then airing for later use; wherein the acid and alkali treatment liquid is HF + HNO3+ HAC (molar ratio 1: 1) mixed acid and K3(Fe(CN)6) + KOH (mass ratio 1: 1) mixed alkali solution, firstly carrying out alkali treatment to roughen the surface of the substrate material, and then carrying out acid treatment to remove impurities on the surface of the substrate;
c. placing the pretreated and cleaned substrate into an injection chamber of an ion implanter, pumping the injection chamber to a vacuum state, cleaning the required injection element target material for 3-10 min by using argon gas, and injecting nitrogen gas into a titanium target to perform ion injection treatment of titanium and nitrogen double elements; wherein, the energy of Ti ions is: 47ke V, the projection range Rp and range divergence of Ti ions are 45.1 and 16.5nm, and the implantation dose of the Ti ions is fixed as follows: 1.2X 1017ions/cm2(ii) a The N ion implantation parameters are: background vacuum degree of vacuum chamber 1.0x10-3Pa，N2The partial pressure is 0.75Pa, a bias voltage of-2.2 kV is applied to the substrate, the frequency is 18kHz, and the N ion injection time is 3.0 h; in the process of injecting Ti ions, the incident ions and the surface of the stainless steel substrate keep an included angle of 90 degrees, and the beam intensity is controlled to be 4.2A/cm2To avoid the temperature increase effect caused by the ion implantation process; in the process of injecting N ions, the N ions vertically enter;
d. putting the substrate into a multi-arc ion plating machine, bombarding and cleaning impurities adsorbed on the surface by using nitrogen ions, then using titanium and aluminum as target materials, and generating N by arc ablation3-、Al3+、Ti2+Ions which are deposited under the action of negative bias to obtain a film with the thickness of 120nm as a high-hardness surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating technological parameters are deposition temperature: 475 ℃, nitrogen partial pressure: 0.9Pa, flow rate: 80sccm, arc current: 85A, negative voltage: -200V, vacuum: 4X 10-3Pa, plating filmTime: 70 min;
e. putting the substrate with the high-hardness surface layer into a multi-arc ion coating machine, introducing nitrogen, using vanadium as a target material, and generating N by arc ablation3-、V3+The ions are deposited under the action of negative bias to obtain a film with the thickness of 130nm as a self-lubricating surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating technological parameters are deposition temperature: 475 ℃, nitrogen partial pressure: 0.9Pa, flow rate: 80sccm, arc current: 85A, negative voltage: -200V, vacuum: 4X 10-3Pa, coating time: and (4) 70 min.
Example 3
A preparation method of high-hardness wear-resistant stainless steel selects a grade of 0Cr19Ni9The stainless steel with the size of 60x70mm is used as a base material, and is characterized in that:
a. the number of the registration is 0Cr19Ni9Stainless steel base material 60x70mm in size is machined appropriately into a tool or die shape that meets industry standards; then, carrying out 1240 ℃ high-temperature quenching and three times of 560 ℃ high-temperature tempering heat treatment on the substrate, sequentially grinding the substrate on a grinding machine by using 800#, 1000# and 1500# water sand paper, and polishing the substrate on a polishing machine by using diamond with the grain diameter of 0.1 mu m as a polishing agent;
b. sequentially cleaning and pretreating a tool or a mold matrix by using a mixed solvent such as tap water and alcohol, an acid-alkali treatment solution, high-purity water-ultrasonic waves, acetone-ultrasonic waves and the like, and then airing for later use; wherein the acid and alkali treatment liquid is HF + HNO3+ HAC (molar ratio 1: 1) mixed acid and K3(Fe(CN)6) + KOH (mass ratio 1: 1) mixed alkali solution, firstly carrying out alkali treatment to roughen the surface of the substrate material, and then carrying out acid treatment to remove impurities on the surface of the substrate;
c. placing the pretreated and cleaned substrate into an injection chamber of an ion implanter, pumping the injection chamber to a vacuum state, cleaning the required injection element target material for 3-10 min by using argon gas, and injecting nitrogen gas into a titanium target to perform ion injection treatment of titanium and nitrogen double elements; wherein, the energy of Ti ions is: 50ke V, Ti ionThe projection range Rp and range straggle of the ions are 45.1 and 16.5nm, and the injection dosage of Ti ions is fixed as follows: 1.5X 1017ions/cm2(ii) a The N ion implantation parameters are: background vacuum degree of vacuum chamber 1.0x10-3Pa，N2The partial pressure is 0.9Pa, a bias voltage of-2.5 kV is applied to the substrate, the frequency is 20kHz, and the N ion injection time is 3.5 h; in the process of injecting Ti ions, the incident ions and the surface of the stainless steel substrate keep an included angle of 90 degrees, and the beam intensity is controlled to be 4.5A/cm2To avoid the temperature increase effect caused by the ion implantation process; in the process of injecting N ions, the N ions vertically enter;
d. putting the substrate into a multi-arc ion plating machine, bombarding and cleaning impurities adsorbed on the surface by using nitrogen ions, then using titanium and aluminum as target materials, and generating N by arc ablation3-、Al3+、Ti2+Ions, which are deposited under the action of negative bias to obtain a film with the thickness of 130nm as a high-hardness surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating technological parameters are deposition temperature: 500 ℃, nitrogen partial pressure: 1.0Pa, flow rate: 80sccm, arc current: 90A, negative voltage: -220V, vacuum degree: 4X 10-3Pa, coating time: 80 min;
e. putting the substrate with the high-hardness surface layer into a multi-arc ion coating machine, introducing nitrogen, using vanadium as a target material, and generating N by arc ablation3-、V3+The ions are deposited under the action of negative bias to obtain a film with the thickness of 140nm as a self-lubricating surface layer; wherein, a WH-800 type multi-arc ion coating machine is adopted, and the coating technological parameters are deposition temperature: 500 ℃, nitrogen partial pressure: 1.0Pa, flow rate: 80sccm, arc current: 90A, negative voltage: -220V, vacuum degree: 4X 10-3Pa, coating time: and 80 min.
The stainless steels obtained in examples 1 to 3 were subjected to microhardness testing using a DUH-211S Shimadzu dynamic ultramicrohardness tester with a diamond micro Vickers indenter with an experimental load of 10mN and a maximum load holding time of 5 sec. The test result shows that the microhardness value of the stainless steel is 38-42 GPa.
Fig. 1 is a cross-sectional view of the high-performance high-speed steel manufactured in example 1, and it can be seen from fig. 1 that the hard and wear-resistant high-speed steel manufactured by the present invention has clear and uniform layers on the surface, and each layer has complete functions.
FIG. 2 is a diagram of the high-performance high-speed steel and SiC ball-on-ball grinding profile obtained in example 2, wherein the load is 3N, the rotation angular velocity is 95.49rmp, the wear radius is 3.00mm, and the wear is 5 ten thousand cycles; the surface of the high-speed steel after the experiment has no obvious change, the specific appearance of the high-speed steel is observed under a microscope, as can be seen from figure 2, the surface of the high-speed steel has small friction area and shallow friction depth, and the high-hardness wear-resistant high-speed steel shows good wear resistance and wear resistance in the experiment, so that the self-lubricating effect of the high-speed steel is good.
The film-based bond strength can be evaluated qualitatively or semi-quantitatively by indentation morphology. The experiment was conducted on the high-performance high-speed steel produced in example 3 using a diamond cone indenter having a vickers indentation method with an apex angle of 136, and the indentation experiment was conducted using a 3N load. As can be seen from FIG. 3, the tested high-speed steel has almost no cracks in the whole observation, only has very slight cracks at the indentation edge, does not have any film peeling phenomenon, and shows better film-substrate bonding force.
The scratch test method is a test method widely applied to measuring the bonding strength of a hard film-substrate interface. In the experiment, for the high-performance high-speed steel prepared in the embodiment 3, a phi 2(mm) ball with a pressure head made of GCr15 is adopted, the load is gradually increased from 0N to 100N, and the scratch is continuously loaded. As seen from fig. 4(a), at the 100N end of the load, no peeling occurred during the whole loading and sliding process, and only scratches occurred due to a small amount of plastic deformation, the film still remained extremely intact, which indicates that the film has good toughness and plastic deformation resistance, and the multilayer film has good intrinsic bond strength and film-based bond strength.
Fig. 4(b) is the obtained HRTEM image, and it can be seen from the high resolution electron micrograph that there is a mixed region between the two regions with different contrast, the brightness distinction is not obvious, and is very blurred, forming an obvious transition region. The existence of the transition zone can effectively enhance the bonding property between the film layers.
The combination state of the film and the substrate is improved to a certain extent by combining the results of Vickers indentation and scratch experiments. The composite structure formed by a plurality of layers with different elastic modulus can prevent the section microcracks from growing, thereby playing the role of improving the film-substrate binding force and the integral toughness of the multilayer film.
Claims (4)
1. A preparation method of high-hardness wear-resistant stainless steel selects stainless steel as a base material, and is characterized by comprising the following steps of: firstly, carrying out mechanical processing, heat treatment, grinding and polishing treatment on a substrate, then cleaning and airing, carrying out ion implantation of titanium and nitrogen double elements by adopting an ion implantation method, then depositing a TiAlN thin film layer in a multi-arc ion coating machine, and then depositing a VN thin film layer in the multi-arc ion coating machine;
the cleaning adopts acid-alkali treatment liquid, and the alkali treatment is firstly carried out, and then the acid treatment is carried out;
the energy of the Ti ions in the ion implantation method is as follows: 45-50keV, the projection range Rp and range divergence of Ti ions are 45.1 and 16.5nm, and the implantation dose of the Ti ions is fixed as follows: 1.0X1017-1.5×1017 ions/cm2(ii) a The N ion implantation parameters are: background vacuum degree of vacuum chamber 1.0x10-3Pa，N2The partial pressure is 0.6-0.9Pa, a bias voltage of-2.5 to-2.0 kV is applied on the substrate, the frequency is 16-20kHz, and the N ion injection time is 2.5-3.5 h; in the process of injecting Ti ions, the incident ions and the surface of the stainless steel substrate keep an included angle of 90 degrees, and the beam intensity is controlled to be 4.0-4.5A/cm2To avoid the temperature increase effect caused by the ion implantation process; in the process of injecting the N ions, the N ions are vertically incident.
2. The method for preparing a high hardness wear resistant stainless steel according to claim 1, wherein: the multi-arc ion coating machine adopts a WH-800 type multi-arc ion coating machine, and the main coating technological parameters are deposition temperature: 450 ℃ and 500 ℃, nitrogen partial pressure: 0.8-1.0Pa, flow rate: 80sccm, arc current: 80-90A, negative voltage: -220 to-180V, vacuum: 4X 10-3Pa, coating time: 60-80 min.
3. The method for preparing a high hardness wear resistant stainless steel according to claim 2, wherein: the TiAlN thin film layer is deposited in the multi-arc ion plating machine, high-purity titanium and high-purity aluminum are used as targets, and nitrogen is introduced; depositing a VN film layer in a multi-arc ion coating machine, taking high-purity vanadium as a target material, and introducing nitrogen.
4. The method for preparing a high hardness wear resistant stainless steel according to claim 3, wherein: the TiAlN thin film layer is 110nm-130 nm; the VN film layer is 120nm-140 nm.
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