CN112251745A - Preparation method of antibacterial stainless steel cutter with nano titanium nitride coating - Google Patents
Preparation method of antibacterial stainless steel cutter with nano titanium nitride coating Download PDFInfo
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- CN112251745A CN112251745A CN202011122835.6A CN202011122835A CN112251745A CN 112251745 A CN112251745 A CN 112251745A CN 202011122835 A CN202011122835 A CN 202011122835A CN 112251745 A CN112251745 A CN 112251745A
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 121
- 239000010935 stainless steel Substances 0.000 title claims abstract description 121
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 111
- 238000000576 coating method Methods 0.000 title claims abstract description 77
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000011248 coating agent Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 49
- 239000002245 particle Substances 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims abstract description 46
- 239000000758 substrate Substances 0.000 claims abstract description 44
- 239000011159 matrix material Substances 0.000 claims abstract description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000006104 solid solution Substances 0.000 claims abstract description 27
- 238000010288 cold spraying Methods 0.000 claims abstract description 26
- 238000005516 engineering process Methods 0.000 claims abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- 230000009467 reduction Effects 0.000 claims abstract description 8
- 238000013329 compounding Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 42
- 239000002131 composite material Substances 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 238000005242 forging Methods 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 18
- 238000004321 preservation Methods 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 17
- 230000001681 protective effect Effects 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000003723 Smelting Methods 0.000 claims description 12
- 238000000713 high-energy ball milling Methods 0.000 claims description 12
- 238000005098 hot rolling Methods 0.000 claims description 12
- 238000003801 milling Methods 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002105 nanoparticle Substances 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 241000894006 Bacteria Species 0.000 abstract description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 3
- 230000035882 stress Effects 0.000 description 9
- 230000032683 aging Effects 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 6
- 239000010949 copper Substances 0.000 description 5
- 238000009966 trimming Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal nitride Chemical class 0.000 description 1
- 238000007514 turning Methods 0.000 description 1
- 230000005514 two-phase flow Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
-
- 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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys
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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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating, which comprises the following steps: firstly, preparing nano titanium nitride particles by using an ammonia reduction method; then adding metal elements with an antibacterial function into the stainless steel matrix, and carrying out solid solution treatment to obtain an antibacterial stainless steel matrix; and finally, compounding the nano titanium nitride particles on the antibacterial stainless steel cutter material substrate by utilizing a cold spraying technology to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating. The titanium nitride coating reinforced antibacterial stainless steel cutter material prepared by combining the titanium nitride coating and the antibacterial stainless steel has the good characteristics of high hardness, high strength, high wear resistance, bacteria resistance and rust resistance.
Description
Technical Field
The invention belongs to the technical field of stainless steel cutter preparation, and particularly relates to a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating.
Background
Titanium nitride coatings were one of the most widely used hard coatings and were the earliest binary transition metal nitride coatings developed. Because titanium nitride has the characteristics of high melting point, high hardness, inactive chemical property under high temperature and the like, the titanium nitride coating can be used as a wear-resistant and hard film and widely applied to various cutting tools and mechanical parts. The antibacterial stainless steel has low cost and excellent antibacterial performance and can be applied to a plurality of fields. For example, the ferrite antibacterial stainless steel can be used for kitchen ware, household appliances and the like, the austenite antibacterial stainless steel can be used for kitchen ware, household appliances, food industry, medical appliances and the like, and the martensite antibacterial stainless steel can be used for manufacturing kitchen knives and the like.
When a traditional stainless steel cutter is used for cutting tools and mechanical parts, the cutter is in a high-temperature processing environment due to heat and friction generated by high-speed moving and cutting of the front cutter face of the cutter, and the size of cutting force often fluctuates along with use, so that the abrasion degree of different positions of the cutter is different. Therefore, the cutter needs to be replaced regularly, and the cost for replacing the cutter simultaneously influences the industrial production progress. In general turning, cemented carbide is the preferred tool material of various machine manufacturers, but in some fine machining occasions, the wear resistance and the sharpness of the cutting edge of the traditional cemented carbide tool material are difficult to meet the requirements of small dimensional tolerance, high surface quality and high production efficiency of workpieces at the same time. With the continuous progress of society, the living standard of people is gradually improved, the health consciousness of bacteria prevention and antibiosis is gradually enhanced, and the demand of antibacterial products is continuously increased. Therefore, research and development of novel nano titanium nitride coating reinforced antibacterial stainless steel cutter materials are very necessary.
Disclosure of Invention
The invention aims to provide a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating, and solves the problems of low hardness and poor antibacterial effect of the existing stainless steel cutter.
The invention adopts the technical scheme that a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating is implemented according to the following steps:
step 1, preparing nano titanium nitride particles by using an ammonia reduction method;
step 2, adding metal elements with an antibacterial function into a stainless steel matrix, and carrying out solid solution treatment to obtain an antibacterial stainless steel matrix;
and 3, compounding the nano titanium nitride particles on the antibacterial stainless steel cutter material substrate by using a cold spraying technology to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
The present invention is also characterized in that,
in the step 1, the method specifically comprises the following steps: putting the anatase phase titanium dioxide nano particles with the particle size of 40nm into a vacuum tube furnace for heat treatment to obtain nano titanium nitride particles; the particle size of the nano titanium nitride particles is 50-100 nm.
During heat treatment, nitrogen is used as protective gas, the temperature is raised to 800 ℃ at the speed of 5 ℃/min, the temperature is kept for 5h, ammonia gas is introduced during the heat preservation process, the flow rate of the ammonia gas is 100ml/min, and the temperature is naturally reduced after the heat treatment is finished.
In the step 2, the method specifically comprises the following steps:
step 2.1, adding metal powder on the surface of a stainless steel substrate, then placing the stainless steel substrate in a vacuum smelting furnace for smelting, casting the stainless steel substrate into an ingot, then peeling the surface of the ingot, trimming off 2-3 mm, and forging into a forging blank of 25 x 160 x 180 mm;
the metal powder is copper powder, silver powder or cerium powder;
the mass ratio of the metal powder to the stainless steel matrix is 1.0-3.0: 100, respectively;
forging process conditions are as follows: the heat preservation time is 2h, and the finish forging temperature is more than 950 ℃;
step 2.2, hot rolling the forging stock into a hot rolled plate with the thickness of 4 mm;
the hot rolling process conditions are as follows: the heat preservation temperature is 1250 ℃, the time is 2 hours, and the finishing temperature is above 950 ℃;
step 2.3, putting the thick hot rolled plate into a box furnace, performing antibacterial heat treatment, heating to 750 ℃ along with the furnace, preserving heat for 7 hours, and air cooling;
step 2.4, carrying out solid solution treatment on the thick hot rolled plate in a box type furnace to obtain an antibacterial stainless steel cutter material substrate;
the solid solution temperature is 1050 ℃, and the solid solution treatment time is 1-5 min.
In step 3, the method specifically comprises the following steps:
step 3.1, mixing silver powder with the purity of 99.9 percent and the granularity of 75 +/-38 mu m with nano titanium nitride particles, and carrying out high-energy ball milling in a high-energy ball mill to obtain Ag/TiN composite powder; grinding the Ag/TiN composite powder, then annealing for 2 hours at the temperature of 400 ℃, and releasing the milling stress;
step 3.2, polishing the antibacterial stainless steel tool material substrate by using abrasive paper, and cleaning by using ethanol; preparing an Ag/TiN composite coating on the antibacterial stainless steel cutter material substrate by adopting a cold spraying system; the thickness of the Ag/TiN composite coating is 1-2 mm, then polishing is carried out step by step, and finally, a sample of the antibacterial stainless steel cutter material substrate with the Ag/TiN composite coating is cleaned by water and is cleaned by acetone through ultrasonic waves;
and 3.3, preserving the antibacterial stainless steel substrate sample with the Ag/TiN composite coating obtained in the step 3.2 in a vacuum furnace at 850 ℃ for 2h, and cooling along with the furnace to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
In step 3.1, during high-energy ball milling, the ball-material ratio is 20: 1; the rotation speed of the milling cutter is 450 rmp; the ore grinding medium is absolute ethyl alcohol; the grinding time is 1 h.
In step 3.2, the spraying distance is 30 mm; the powder feeding rate is 2 rmp; the flow rate of the carrier gas was 4m3H; the pressure intensity in the cavity is 1.6 MPa; the temperature in the cavity is 400 ℃; the protective gas is nitrogen.
The beneficial effect of the invention is that,
titanium nitride particles prepared by an ammonia reduction method are used for preparing a titanium nitride coating on an antibacterial stainless steel tool material substrate by a cold spraying technology. The titanium nitride has the characteristics of high melting point, high hardness, inactive chemical property under high temperature and the like, and is a wear-resistant protective high-quality coating material on the surface of the cutting tool. The antibacterial stainless steel contains metal elements with antibacterial function, and a precipitated phase obtained after solid solution treatment has the antibacterial function. The antibacterial stainless steel cutter material with the titanium nitride coating has antibacterial property, and the service life of the cutter can be greatly prolonged. Experiments have shown that the service life of the tool with the titanium nitride coating is four times longer than that of the conventional tool. The titanium nitride coating reinforced antibacterial stainless steel cutter material prepared by combining the titanium nitride coating and the antibacterial stainless steel has the good characteristics of high hardness, high strength, high wear resistance, bacteria resistance and rust resistance.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating, which is implemented according to the following steps:
step 1, preparing nano titanium nitride particles by using an ammonia reduction method;
the method specifically comprises the following steps: putting the anatase phase titanium dioxide nano particles with the particle size of 40nm into a vacuum tube furnace for heat treatment to obtain nano titanium nitride particles; the particle size of the nano titanium nitride particles is 50-100 nm;
during heat treatment, taking nitrogen as protective gas, heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 5h, introducing ammonia gas in the heat preservation process, wherein the flow rate of the ammonia gas is 100ml/min, naturally cooling after the heat treatment is finished, and introducing the nitrogen as the protective gas in the cooling process; the pressure of the vacuum tube furnace is normal pressure.
Step 2, adding metal elements with an antibacterial function into a stainless steel matrix, and carrying out aging treatment after solid solution to obtain the antibacterial stainless steel matrix; the method specifically comprises the following steps:
step 2.1, adding metal powder on the surface of a stainless steel substrate, then placing the stainless steel substrate in a vacuum smelting furnace for smelting, casting the stainless steel substrate into an ingot, then peeling the surface of the ingot, trimming off 2-3 mm, and forging into a forging blank of 25 x 160 x 180 mm;
the metal powder is copper powder, silver powder or cerium powder;
the mass ratio of the metal powder to the stainless steel matrix is 1.0-3.0: 100, respectively;
forging process conditions are as follows: the heat preservation time is 2h, and the finish forging temperature is more than 950 ℃;
step 2.2, hot rolling the forging stock into a hot rolled plate with the thickness of 4 mm;
the hot rolling process conditions are as follows: the heat preservation temperature is 1250 ℃, the time is 2 hours, and the finishing temperature is above 950 ℃;
step 2.3, putting the hot rolled plate with the thickness of 4mm into a box furnace, carrying out antibacterial heat treatment, heating to 750 ℃ along with the furnace, preserving heat for 7 hours, and air cooling;
step 2.4, carrying out solid solution treatment on the hot rolled plate with the thickness of 4mm in a box type furnace to obtain an antibacterial stainless steel cutter material substrate;
the solid solution temperature is 1050 ℃, and the solid solution treatment time is 1-5 min;
step 3, compounding the nano titanium nitride particles on an antibacterial stainless steel cutter material substrate by using a cold spraying technology to obtain an antibacterial stainless steel cutter with a nano titanium nitride coating; the method specifically comprises the following steps:
step 3.1, mixing silver powder with the purity of 99.9 percent and the granularity of 75 +/-38 mu m with nano titanium nitride particles, and carrying out high-energy ball milling in a high-energy ball mill to obtain a cold spraying raw material, namely Ag/TiN composite powder; and (3) grinding the Ag/TiN composite powder, and then annealing for 2h at 400 ℃ to release the milling stress.
The high-energy ball milling parameters are as follows: the ball material ratio is 20: 1; the rotation speed of the milling cutter is 450 rmp; the ore grinding medium is absolute ethyl alcohol; the grinding time is 1 h.
Step 3.2, polishing the antibacterial stainless steel tool material substrate by using abrasive paper, and cleaning by using ethanol; preparing an Ag/TiN composite coating on the antibacterial stainless steel cutter material substrate by adopting a cold spraying system; the thickness of the Ag/TiN composite coating is 1-2 mm, then polishing is carried out step by step, and finally, a sample of the antibacterial stainless steel cutter material substrate with the Ag/TiN composite coating is cleaned by water and is cleaned by acetone through ultrasonic waves;
wherein the spraying distance is 30 mm; the powder feeding rate is 2 rmp; the flow rate of the carrier gas was controlled to 4m3H; the pressure intensity in the cavity is 1.6 MPa; the temperature in the cavity is 400 ℃; filling nitrogen as a protective gas;
3.3, preserving the antibacterial stainless steel substrate sample with the Ag/TiN composite coating obtained in the step 3.2 in a vacuum furnace at 850 ℃ for 2 hours; eliminating residual stress in the sample, and cooling along with the furnace to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
The novel nano titanium nitride coating reinforced antibacterial stainless steel cutter material obtained by the cold spraying technology has the good characteristics of high hardness, high strength, high wear resistance, bacteria resistance and rust resistance, and solves the problems in the prior art.
Antibacterial tests show that the antibacterial rate of the antibacterial stainless steel matrix material containing 2.0% of Cu to escherichia coli and staphylococcus aureus can reach 99.9% after annealing for 7 hours at 750 ℃. The copper-rich phase gradually changes from a spherical shape to a rod shape along with the increase of the antibacterial annealing temperature and the prolongation of the time. The rod-shaped copper-rich surface is parallel to the surface, has the largest exposed area and can improve the antibacterial function of the experimental steel. Because the antibacterial annealing temperature is higher, the Cu content of solid solution in the matrix is still supersaturated at room temperature, and then the aging annealing is carried out to improve the strength of the test steel. After aging annealing, many copper-rich phase particles with nanometer-scale sizes are separated out, and the hardness, yield strength and tensile strength of the material are improved.
The cold spraying technology is a process for forming a coating on the surface of a metal or insulating substrate by using supersonic (300-1200 m/s) gas-solid two-phase flow formed by accelerating tiny particles by high-pressure airflow. The technology has low requirements on surface preparation, and does not need to consider the mechanical or thermal characteristics of a plated part. Compared with the traditional thermal spraying, the technology has the advantages of low spraying temperature, small heat influence of the coating on a matrix, high powder feeding speed, low porosity of the coating, compact coating and the like, so that the high-pressure cold spraying technology has wider application range, the sprayed powder can be recycled, and the spraying cost is reduced.
With the continuous development of cold spraying technology, the excellent performance of cold spraying coatings is gradually accepted. The high-pressure cold spraying method can be used for preparing metal coatings with low melting point and good plasticity, so that the cold spraying technology and the cold spraying coatings have wide application prospects in various fields of aerospace, shipbuilding, electronics, machinery, chemical engineering, automobiles and the like.
Example 1
The invention relates to a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating, which is implemented according to the following steps:
step 1, preparing nano titanium nitride particles by using an ammonia reduction method;
the method specifically comprises the following steps: putting the anatase phase titanium dioxide nano particles with the particle size of 40nm into a vacuum tube furnace for heat treatment to obtain nano titanium nitride particles; the particle size of the nano titanium nitride particles is 50 nm;
during heat treatment, taking nitrogen as protective gas, heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 5h, introducing ammonia gas in the heat preservation process, wherein the flow rate of the ammonia gas is 100ml/min, naturally cooling after the heat treatment is finished, and introducing the nitrogen as the protective gas in the cooling process; the pressure of the vacuum tube furnace is normal pressure.
Step 2, adding metal elements with an antibacterial function into a stainless steel matrix, and carrying out aging treatment after solid solution to obtain the antibacterial stainless steel matrix; the method specifically comprises the following steps:
step 2.1, adding metal powder on the surface of a stainless steel matrix, then placing the stainless steel matrix in a vacuum smelting furnace for smelting, casting the stainless steel matrix into an ingot, then peeling the surface of the ingot, trimming off 2mm, and forging the ingot into a forging blank with the thickness of 25 x 160 x 180 mm;
the metal powder is copper powder;
the mass ratio of the metal powder to the stainless steel matrix is 1.0: 100, respectively;
forging process conditions are as follows: the heat preservation time is 2h, and the finish forging temperature is more than 950 ℃;
step 2.2, hot rolling the forging stock into a hot rolled plate with the thickness of 4 mm;
the hot rolling process conditions are as follows: the heat preservation temperature is 1250 ℃, the time is 2 hours, and the finishing temperature is above 950 ℃;
step 2.3, putting the hot rolled plate with the thickness of 4mm into a box furnace, carrying out antibacterial heat treatment, heating to 750 ℃ along with the furnace, preserving heat for 7 hours, and air cooling;
step 2.4, carrying out solid solution treatment on the hot rolled plate with the thickness of 4mm in a box type furnace to obtain an antibacterial stainless steel cutter material substrate;
the solid solution temperature is 1050 ℃, and the solid solution treatment time is 1 min;
step 3, compounding the nano titanium nitride particles on an antibacterial stainless steel cutter material substrate by using a cold spraying technology to obtain an antibacterial stainless steel cutter with a nano titanium nitride coating; the method specifically comprises the following steps:
step 3.1, mixing silver powder with the purity of 99.9 percent and the granularity of 75 +/-38 mu m with nano titanium nitride particles, and carrying out high-energy ball milling in a high-energy ball mill to obtain a cold spraying raw material, namely Ag/TiN composite powder; and (3) grinding the Ag/TiN composite powder, and then annealing for 2h at 400 ℃ to release the milling stress.
The high-energy ball milling parameters are as follows: the ball material ratio is 20: 1; the rotation speed of the milling cutter is 450 rmp; the ore grinding medium is absolute ethyl alcohol; the grinding time is 1 h.
Step 3.2, polishing the antibacterial stainless steel tool material substrate by using abrasive paper, and cleaning by using ethanol; preparing an Ag/TiN composite coating on the antibacterial stainless steel cutter material substrate by adopting a cold spraying system; the thickness of the Ag/TiN composite coating is 1mm, then the Ag/TiN composite coating is gradually polished, and finally, an antibacterial stainless steel cutter material substrate sample with the Ag/TiN composite coating is cleaned by water and is ultrasonically cleaned by acetone;
wherein the spraying distance is 30 mm; the powder feeding rate is 2 rmp; the flow rate of the carrier gas was controlled to 4m3H; the pressure intensity in the cavity is 1.6 MPa; the temperature in the cavity is 400 ℃; filling nitrogen as a protective gas;
3.3, preserving the antibacterial stainless steel substrate sample with the Ag/TiN composite coating obtained in the step 3.2 in a vacuum furnace at 850 ℃ for 2 hours; eliminating residual stress in the sample, and cooling along with the furnace to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
Example 2
The invention relates to a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating, which is implemented according to the following steps:
step 1, preparing nano titanium nitride particles by using an ammonia reduction method;
the method specifically comprises the following steps: putting the anatase phase titanium dioxide nano particles with the particle size of 40nm into a vacuum tube furnace for heat treatment to obtain nano titanium nitride particles; the particle size of the nano titanium nitride particles is 80 nm;
during heat treatment, taking nitrogen as protective gas, heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 5h, introducing ammonia gas in the heat preservation process, wherein the flow rate of the ammonia gas is 100ml/min, naturally cooling after the heat treatment is finished, and introducing the nitrogen as the protective gas in the cooling process; the pressure of the vacuum tube furnace is normal pressure.
Step 2, adding metal elements with an antibacterial function into a stainless steel matrix, and carrying out aging treatment after solid solution to obtain the antibacterial stainless steel matrix; the method specifically comprises the following steps:
step 2.1, adding metal powder on the surface of a stainless steel matrix, then placing the stainless steel matrix in a vacuum smelting furnace for smelting, casting the stainless steel matrix into an ingot, then peeling the surface of the ingot, trimming off 3mm, and forging into a forging blank of 25 x 160 x 180 mm;
the metal powder is silver powder;
the mass ratio of the metal powder to the stainless steel matrix is 2.0: 100, respectively;
forging process conditions are as follows: the heat preservation time is 2h, and the finish forging temperature is more than 950 ℃;
step 2.2, hot rolling the forging stock into a hot rolled plate with the thickness of 4 mm;
the hot rolling process conditions are as follows: the heat preservation temperature is 1250 ℃, the time is 2 hours, and the finishing temperature is above 950 ℃;
step 2.3, putting the hot rolled plate with the thickness of 4mm into a box furnace, carrying out antibacterial heat treatment, heating to 750 ℃ along with the furnace, preserving heat for 7 hours, and air cooling;
step 2.4, carrying out solid solution treatment on the hot rolled plate with the thickness of 4mm in a box type furnace to obtain an antibacterial stainless steel cutter material substrate;
the solid solution temperature is 1050 ℃, and the solid solution treatment time is 5 min;
step 3, compounding the nano titanium nitride particles on an antibacterial stainless steel cutter material substrate by using a cold spraying technology to obtain an antibacterial stainless steel cutter with a nano titanium nitride coating; the method specifically comprises the following steps:
step 3.1, mixing silver powder with the purity of 99.9 percent and the granularity of 75 +/-38 mu m with nano titanium nitride particles, and carrying out high-energy ball milling in a high-energy ball mill to obtain a cold spraying raw material, namely Ag/TiN composite powder; and (3) grinding the Ag/TiN composite powder, and then annealing for 2h at 400 ℃ to release the milling stress.
The high-energy ball milling parameters are as follows: the ball material ratio is 20: 1; the rotation speed of the milling cutter is 450 rmp; the ore grinding medium is absolute ethyl alcohol; the grinding time is 1 h.
Step 3.2, polishing the antibacterial stainless steel tool material substrate by using abrasive paper, and cleaning by using ethanol; preparing an Ag/TiN composite coating on the antibacterial stainless steel cutter material substrate by adopting a cold spraying system; the thickness of the Ag/TiN composite coating is 2mm, then the Ag/TiN composite coating is gradually polished, and finally, an antibacterial stainless steel cutter material substrate sample with the Ag/TiN composite coating is cleaned by water and is ultrasonically cleaned by acetone;
wherein the spraying distance is 30 mm; the powder feeding rate is 2 rmp; the flow rate of the carrier gas was controlled to 4m3H; the pressure intensity in the cavity is 1.6 MPa; the temperature in the cavity is 400 ℃; filling nitrogen as a protective gas;
3.3, preserving the antibacterial stainless steel substrate sample with the Ag/TiN composite coating obtained in the step 3.2 in a vacuum furnace at 850 ℃ for 2 hours; eliminating residual stress in the sample, and cooling along with the furnace to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
Example 3
The invention relates to a preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating, which is implemented according to the following steps:
step 1, preparing nano titanium nitride particles by using an ammonia reduction method;
the method specifically comprises the following steps: putting the anatase phase titanium dioxide nano particles with the particle size of 40nm into a vacuum tube furnace for heat treatment to obtain nano titanium nitride particles; the particle size of the nano titanium nitride particles is 100 nm;
during heat treatment, taking nitrogen as protective gas, heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 5h, introducing ammonia gas in the heat preservation process, wherein the flow rate of the ammonia gas is 100ml/min, naturally cooling after the heat treatment is finished, and introducing the nitrogen as the protective gas in the cooling process; the pressure of the vacuum tube furnace is normal pressure.
Step 2, adding metal elements with an antibacterial function into a stainless steel matrix, and carrying out aging treatment after solid solution to obtain the antibacterial stainless steel matrix; the method specifically comprises the following steps:
step 2.1, adding metal powder on the surface of a stainless steel matrix, then placing the stainless steel matrix in a vacuum smelting furnace for smelting, casting the stainless steel matrix into an ingot, then peeling the surface of the ingot, trimming off 3mm, and forging into a forging blank of 25 x 160 x 180 mm;
the metal powder is cerium powder;
the mass ratio of the metal powder to the stainless steel matrix is 3.0: 100, respectively;
forging process conditions are as follows: the heat preservation time is 2h, and the finish forging temperature is more than 950 ℃;
step 2.2, hot rolling the forging stock into a hot rolled plate with the thickness of 4 mm;
the hot rolling process conditions are as follows: the heat preservation temperature is 1250 ℃, the time is 2 hours, and the finishing temperature is above 950 ℃;
step 2.3, putting the hot rolled plate with the thickness of 4mm into a box furnace, carrying out antibacterial heat treatment, heating to 750 ℃ along with the furnace, preserving heat for 7 hours, and air cooling;
step 2.4, carrying out solid solution treatment on the hot rolled plate with the thickness of 4mm in a box type furnace to obtain an antibacterial stainless steel cutter material substrate;
the solid solution temperature is 1050 ℃, and the solid solution treatment time is 3 min;
step 3, compounding the nano titanium nitride particles on an antibacterial stainless steel cutter material substrate by using a cold spraying technology to obtain an antibacterial stainless steel cutter with a nano titanium nitride coating; the method specifically comprises the following steps:
step 3.1, mixing silver powder with the purity of 99.9 percent and the granularity of 75 +/-38 mu m with nano titanium nitride particles, and carrying out high-energy ball milling in a high-energy ball mill to obtain a cold spraying raw material, namely Ag/TiN composite powder; and (3) grinding the Ag/TiN composite powder, and then annealing for 2h at 400 ℃ to release the milling stress.
The high-energy ball milling parameters are as follows: the ball material ratio is 20: 1; the rotation speed of the milling cutter is 450 rmp; the ore grinding medium is absolute ethyl alcohol; the grinding time is 1 h.
Step 3.2, polishing the antibacterial stainless steel tool material substrate by using abrasive paper, and cleaning by using ethanol; preparing an Ag/TiN composite coating on the antibacterial stainless steel cutter material substrate by adopting a cold spraying system; the thickness of the Ag/TiN composite coating is 1mm, then the Ag/TiN composite coating is gradually polished, and finally, an antibacterial stainless steel cutter material substrate sample with the Ag/TiN composite coating is cleaned by water and is ultrasonically cleaned by acetone;
wherein the spraying distance is 30mm; the powder feeding rate is 2 rmp; the flow rate of the carrier gas was controlled to 4m3H; the pressure intensity in the cavity is 1.6 MPa; the temperature in the cavity is 400 ℃; filling nitrogen as a protective gas;
3.3, preserving the antibacterial stainless steel substrate sample with the Ag/TiN composite coating obtained in the step 3.2 in a vacuum furnace at 850 ℃ for 2 hours; eliminating residual stress in the sample, and cooling along with the furnace to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
Claims (7)
1. A preparation method of an antibacterial stainless steel cutter with a nano titanium nitride coating is characterized by comprising the following steps:
step 1, preparing nano titanium nitride particles by using an ammonia reduction method;
step 2, adding metal elements with an antibacterial function into a stainless steel matrix, and carrying out solid solution treatment to obtain an antibacterial stainless steel matrix;
and 3, compounding the nano titanium nitride particles on the antibacterial stainless steel cutter material substrate by using a cold spraying technology to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
2. The method for preparing the antibacterial stainless steel cutter with the nano titanium nitride coating according to claim 1, wherein in the step 1, the method specifically comprises the following steps: putting the anatase phase titanium dioxide nano particles with the particle size of 40nm into a vacuum tube furnace for heat treatment to obtain nano titanium nitride particles; the particle size of the nano titanium nitride particles is 50-100 nm.
3. The method for preparing the antibacterial stainless steel cutter with the nano titanium nitride coating according to claim 2, wherein during heat treatment, nitrogen is used as protective gas, the temperature is raised to 800 ℃ at the speed of 5 ℃/min, the temperature is kept for 5h, ammonia gas is introduced during the heat preservation process, and the flow rate of the ammonia gas is 100 ml/min.
4. The method for preparing the antibacterial stainless steel cutter with the nano titanium nitride coating according to claim 1, wherein in the step 2, the method specifically comprises the following steps:
step 2.1, adding metal powder on the surface of a stainless steel matrix, then placing the stainless steel matrix in a vacuum smelting furnace for smelting, casting the stainless steel matrix into an ingot, then peeling the surface of the ingot, and forging the ingot into a forging blank with the thickness of 25 x 160 x 180 mm;
the metal powder is copper powder, silver powder or cerium powder;
the mass ratio of the metal powder to the stainless steel matrix is 1.0-3.0: 100, respectively;
forging process conditions are as follows: the heat preservation time is 2h, and the finish forging temperature is more than 950 ℃;
step 2.2, hot rolling the forging stock into a hot rolled plate with the thickness of 4 mm;
the hot rolling process conditions are as follows: the heat preservation temperature is 1250 ℃, the time is 2 hours, and the finishing temperature is above 950 ℃;
step 2.3, putting the thick hot rolled plate into a box furnace, performing antibacterial heat treatment, heating to 750 ℃ along with the furnace, preserving heat for 7 hours, and air cooling;
step 2.4, carrying out solid solution treatment on the thick hot rolled plate in a box type furnace to obtain an antibacterial stainless steel cutter material substrate;
the solid solution temperature is 1050 ℃, and the solid solution treatment time is 1-5 min.
5. The method for preparing the antibacterial stainless steel cutter with the nano titanium nitride coating according to claim 1, wherein in the step 3, the specific steps are as follows:
step 3.1, mixing silver powder and nano titanium nitride particles, and performing high-energy ball milling in a high-energy ball mill to obtain Ag/TiN composite powder; grinding the Ag/TiN composite powder, then annealing for 2 hours at the temperature of 400 ℃, and releasing the milling stress;
step 3.2, polishing the antibacterial stainless steel tool material substrate by using abrasive paper, and cleaning by using ethanol; preparing an Ag/TiN composite coating on the antibacterial stainless steel cutter material substrate by adopting a cold spraying system; the thickness of the Ag/TiN composite coating is 1-2 mm, then polishing is carried out step by step, and finally water cleaning and acetone ultrasonic cleaning are carried out;
and 3.3, preserving the antibacterial stainless steel substrate sample with the Ag/TiN composite coating obtained in the step 3.2 in a vacuum furnace at 850 ℃ for 2h, and cooling along with the furnace to obtain the antibacterial stainless steel cutter with the nano titanium nitride coating.
6. The method for preparing the antibacterial stainless steel cutter with the nano titanium nitride coating according to claim 5, wherein in the step 3.1, the ball-to-material ratio in the high-energy ball milling is 20: 1; the rotation speed of the milling cutter is 450 rmp; the ore grinding medium is absolute ethyl alcohol; the grinding time is 1 h.
7. The method for preparing the antibacterial stainless steel cutter with the nano titanium nitride coating according to the claim 1, wherein in the step 3.2, the spraying distance is 30 mm; the powder feeding rate is 2 rmp; the flow rate of the carrier gas was 4m3H; the pressure intensity in the cavity is 1.6 MPa; the temperature in the cavity is 400 ℃; the protective gas is nitrogen.
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