CN114086138B - alpha-CN x Preparation method of Fe nano composite coating - Google Patents
alpha-CN x Preparation method of Fe nano composite coating Download PDFInfo
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- CN114086138B CN114086138B CN202111375984.8A CN202111375984A CN114086138B CN 114086138 B CN114086138 B CN 114086138B CN 202111375984 A CN202111375984 A CN 202111375984A CN 114086138 B CN114086138 B CN 114086138B
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- 238000000576 coating method Methods 0.000 title claims abstract description 76
- 239000011248 coating agent Substances 0.000 title claims abstract description 75
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000151 deposition Methods 0.000 claims description 21
- 238000004544 sputter deposition Methods 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 20
- 230000008021 deposition Effects 0.000 claims description 19
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000013077 target material Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 62
- 239000000463 material Substances 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 241000234282 Allium Species 0.000 abstract description 5
- 235000002732 Allium cepa var. cepa Nutrition 0.000 abstract description 5
- 239000011247 coating layer Substances 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 239000002103 nanocoating Substances 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 34
- 238000000034 method Methods 0.000 description 11
- 238000005461 lubrication Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- 238000007373 indentation Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000005087 graphitization Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Catalysts (AREA)
Abstract
alpha-CN x A preparation method of a/Fe nano composite coating relates to a CN x A preparation method of a base nano composite coating. The invention aims to improve alpha-CN by catalyzing and generating a self-lubricating onion carbon friction film x Tribological properties of the base nanocoating. The invention provides a CN x A base nanocomposite coating material comprising elemental carbon, elemental iron, and elemental nitrogen. The invention forms the self-lubricating onion carbon friction film by introducing ductile Fe element with catalytic activity and self-assembling in situ, and realizes the CN x The microstructure of the base coating is regulated and controlled, the compactness of the coating is improved, the friction coefficient of the coating is greatly reduced, the friction and wear properties of the coating are improved, and the CN is improved x The strength and toughness of the base coating layer are realized to CN x Controllable growth of the Fe nanocomposite coating.
Description
Technical Field
The invention relates to a CN x A preparation method of a base nano composite coating.
Background
For most materials widely used in industry, such as in mechanical systems, friction and wear remain the primary means of inducing energy dissipation and component failure. Low friction plays a key role in improving energy efficiency and reducing machine wear, which has a profound impact on technical and economic development and the environment. Amorphous carbon nitride thinThe film is widely used as a solid lubricating film. The carbon-based coating material has excellent mechanical properties and excellent low-friction lubrication and corrosion resistance, and is widely applied to marine equipment. Although amorphous CN x Has a low coefficient of friction, excellent wear resistance and chemical stability, but it is limited by low nanoindentation hardness and limited graphitization during sliding. In recent years, it has been found that a-CN can be significantly improved by introducing a hard metal element x The hardness and wear resistance of the coating are not improved obviously, but the limited graphitization degree is still not improved obviously, and the lubrication degree is low. The preparation of a coating material of excellent mechanical strength with excellent lubricating function is CN x Hot spot in the research field of base nano composite system and simultaneously CN x Future development of base coatings and understanding of solid lubrication provide guidance.
Notably, however, onion Carbon Structures (OLCs) with high graphitization are considered to be very excellent tribofilms. It is desirable to excite the formation of a friction film having a low friction coefficient by introducing a metal element having a catalytic function. Noble metals (gold, silver, copper, etc.) are currently the most effective catalysts, but their expensive cost severely limits their large-scale application. Development of low cost, high catalytic activity non-noble metal catalysts for CN x Base nanocomposite systems have become a research hotspot in this area. Therefore, the preparation of the multifunctional nano composite coating with high hardness, high toughness, self-lubrication, wear resistance and other performances as a whole is an urgent need of current research.
Disclosure of Invention
The invention aims to solve the problem of the prior alpha-CN x The technical problem of high cost of introducing noble metal as a catalyst into the base nano coating is solved, and an alpha-CN is provided x A preparation method of Fe nano composite coating.
alpha-CN of the invention x The preparation method of the Fe nano composite coating comprises the following steps:
1. sequentially cleaning and drying the substrate; the substrate is made of titanium-based materials;
2. cleaning and drying in the first stepPlacing the substrate into a vacuum cavity of a magnetron sputtering device, and adding graphite target and Fe 3 The C target is arranged on the target position of the magnetron sputtering device, the distance between the target and the substrate is 12 cm-13 cm, and the cavity is vacuumized until the vacuum degree is 1 multiplied by 10 -4 Pa～1.1×10 -4 Pa；
3. Ar and N are introduced into the cavity 2 The mixed gas of the chamber is used as sputtering gas, and the working pressure in the chamber is regulated to be 0.8 Pa-0.9 Pa; the graphite target adopts direct current, and the sputtering current of the graphite target is set to be 0.5A-0.6A; fe (Fe) 3 The C target adopts radio frequency current, fe 3 C, setting the deposition temperature to be 500-800 ℃ at the radio frequency power of 40-45W; sputtering is started simultaneously by the two targets, and the sputtering thickness of the two targets is equal and is 0.9-1.1 mu m;
the flow rate of Ar is 60 sccm-65 sccm;
said N 2 The flow rate of the water is 20 sccm-25 sccm;
4. after sputtering, cooling the cavity to room temperature to obtain alpha-CN x and/Fe coating.
The invention aims to improve alpha-CN by catalyzing and generating a self-lubricating onion carbon friction film x Tribological properties of the base nanocoating.
The invention provides a CN x A base nanocomposite coating material comprising elemental carbon, elemental iron, and elemental nitrogen. The invention forms the self-lubricating onion carbon friction film by introducing ductile Fe element with catalytic activity and self-assembling in situ, and realizes the CN x The microstructure of the base coating is regulated and controlled, the compactness of the coating is improved, the friction coefficient of the coating is greatly reduced, the friction and wear properties of the coating are improved, and the CN is improved x The strength and toughness of the base coating layer are realized to CN x Controllable growth of the Fe nanocomposite coating. The key metal kinematic pair of the marine equipment is exposed to the seawater environment with high salt, high humidity, erosion and abrasion interaction for a long time, the service life of the marine equipment is seriously threatened, and the carbon-based coating material is an ideal friction-resistant material. The invention provides a method for constructing CN which integrates high hardness, high toughness, self lubrication, wear resistance and the like by utilizing a magnetron sputtering method x Fe nanoNovel method for rice composite coating, CN prepared by the method x The Fe nano composite coating material has good development and application prospect on the surface of the marine equipment titanium-based moving part.
A series of α -CNs prepared in the present invention x Fe coating and pure alpha-CN x The addition of a small amount of Fe element has a great influence on the hardness of the coating compared with the coating, and the alpha-CN x The hardness variation of the Fe coating has a great relationship with the deposition temperature, which may be related to Fe 4 The presence of an N-crystalline phase is associated with high surface density. alpha-CN at 600 DEG C x The Fe coating has the highest hardness value, about pure alpha-CN x 2.13 times the coating. Series of alpha-CNs x The friction coefficient in the Fe coating increases and decreases with increasing temperature, and decreases to a minimum of 0.18 when the deposition temperature increases to 600 ℃, about pure alpha-CN x 46% of the coating. Fe when the coating is deposited at 700 ℃ and 800 DEG C 4 The N phase disappears, the surface is hollow, the density of the coating is reduced, the friction coefficient is obviously increased, and the friction coefficient is kept at 0.23 and 0.25. And depositing alpha-CN at a temperature of 600 DEG C x The formation of highly graphitized OLC tribofilms was found in the wear debris of the Fe coating (FIG. 3), which is also one of the important reasons for its excellent tribological properties. The invention proves that the addition of Fe element in the coating can be used for improving the catalytic activity and promoting the formation of an in-situ friction film under friction conditions. To realize CN x The coating is tough, and the self-lubricating and wear-resistant integrated regulation and control provides a new method.
The invention has the beneficial effects that:
1. the magnetron sputtering deposition technology adopted by the invention is used for preparing the coating material, the process is simple, the cost is low, the yield is high, and the mass industrial production can be realized;
2. the invention provides a method for constructing CN which integrates high hardness, high toughness, self lubrication, wear resistance and the like by utilizing a magnetron sputtering method x Novel method of Fe nanocomposite coating.
Drawings
FIG. 1 is an XRD pattern;
FIG. 2 is a graph of coefficient of friction;
fig. 3 is a HRTEM image.
Detailed Description
The first embodiment is as follows: the present embodiment is an alpha-CN x The preparation method of the Fe nano composite coating comprises the following steps:
1. sequentially cleaning and drying the substrate; the substrate is made of titanium-based materials;
2. placing the substrate cleaned and dried in the first step into a vacuum cavity of a magnetron sputtering device, and mixing graphite target material and Fe 3 The C target is arranged on the target position of the magnetron sputtering device, the distance between the target and the substrate is 12 cm-13 cm, and the cavity is vacuumized until the vacuum degree is 1 multiplied by 10 -4 Pa～1.1×10 -4 Pa；
3. Ar and N are introduced into the cavity 2 The mixed gas of the chamber is used as sputtering gas, and the working pressure in the chamber is regulated to be 0.8 Pa-0.9 Pa; the graphite target adopts direct current, and the sputtering current of the graphite target is set to be 0.5A-0.6A; fe (Fe) 3 The C target adopts radio frequency current, fe 3 C, setting the deposition temperature to be 500-800 ℃ at the radio frequency power of 40-45W; sputtering is started simultaneously by the two targets, and the sputtering thickness of the two targets is equal and is 0.9-1.1 mu m;
the flow rate of Ar is 60 sccm-65 sccm;
said N 2 The flow rate of the water is 20 sccm-25 sccm;
4. after sputtering, cooling the cavity to room temperature to obtain alpha-CN x and/Fe coating.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the titanium-based material in the first step is alloy Ti-6Al-4V. The other is the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: sequentially selecting absolute ethyl alcohol, acetone and deionized water to ultrasonically clean the substrate, cleaning for 20-25 min each, and finally drying the substrate in a drying oven at 60 ℃. The other embodiments are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: this embodiment modeThe differences from the first to third embodiments are that: in the second step, the vacuum degree of the cavity is pumped to 1 multiplied by 10 by a mechanical pump and a turbomolecular pump -4 Pa. The other is the same as in one of the first to third embodiments.
Fifth embodiment: the fourth difference between this embodiment and the third embodiment is that: setting the sputtering current of the graphite target to be 0.5A; fe (Fe) 3 The C target adopts radio frequency current, fe 3 C has a radio frequency power of 40W. The other is the same as in the fourth embodiment.
Specific embodiment six: the first difference between this embodiment and the specific embodiment is that: the flow rate of Ar in the third step is 60sccm; said N 2 The flow rate of (2) was 20sccm. The other is the same as in the first embodiment.
Seventh embodiment: the first difference between this embodiment and the specific embodiment is that: in the third step, the deposition temperature was set at 600 ℃. The other is the same as in the first embodiment.
The invention was verified with the following test:
test one: the test is an alpha-CN x The preparation method of the Fe nano composite coating comprises the following steps:
1. sequentially selecting absolute ethyl alcohol, acetone and deionized water to ultrasonically clean the substrate for 25min, and finally drying the substrate in a drying oven at 60 ℃; the substrate is alloy Ti-6Al-4V;
2. placing the substrate cleaned and dried in the first step into a vacuum cavity of a magnetron sputtering device, and mixing graphite target material and Fe 3 The C target is arranged on the target position of the magnetron sputtering device, the distance between the target and the substrate is 12cm, and the cavity is vacuumized by a mechanical pump and a turbomolecular pump until the vacuum degree is 1 multiplied by 10 -4 Pa；
3. Ar and N are introduced into the cavity 2 As sputtering gas, adjusting the working pressure in the cavity to 0.8Pa; the graphite target adopts direct current, and the sputtering current of the graphite target is set to be 0.5A; fe (Fe) 3 The C target adopts radio frequency current, fe 3 C, setting the deposition temperature to be 500 ℃ with the radio frequency power of 40W; two targetsSputtering is started simultaneously, and the sputtering thickness of the two targets is equal and is 1 mu m;
the flow rate of Ar is 60sccm; said N 2 The flow rate of (2) was 20sccm;
4. after sputtering, cooling the cavity to room temperature to obtain alpha-CN x and/Fe coating.
Test with nanoindenter test one prepared alpha-CN x The hardness of the/Fe coating was 20.5Gpa.
Test one prepared alpha-CN was measured by a ball-and-disc tribometer under dry friction conditions x The friction coefficient of the/Fe coating was 0.24 (FIG. 2, temperature on the curve corresponds to the deposition temperature of step three).
Determination of the alpha-CN prepared by XPS x The content of carbon element in the Fe coating was 90.38at.%, the content of iron element was 3.55at.%, and the content of nitrogen element was 6.08at.%.
And (2) testing II: the first difference between this test and the test is: in the third step, the deposition temperature was set at 600 ℃. The others are the same as in test one.
alpha-CN prepared by using nano indentation instrument to test II x The hardness of the/Fe coating was 27Gpa.
Measurement of alpha-CN prepared in test II by ball-and-disc frictional wear instrument under dry friction condition x The friction coefficient of the/Fe coating was 0.18 (FIG. 2, temperature on the curve corresponds to the deposition temperature of step three).
alpha-CN prepared by the second test x HRTEM observation of Fe coated wear debris it is seen in fig. 3 that most of the wear debris consisted of graphitized OLCs reels, the low friction performance of this nano-reel structure was due to insufficient contact of the highly graphitized nano-reels with the friction surface during friction, which was effective in reducing friction during friction, so that the highly graphitized OLCs friction film had excellent lubrication function, which was a good solid lubrication friction film.
And (3) test III: the first difference between this test and the test is: setting the deposition temperature to 700 ℃. The others are the same as in test one.
Test three with nanometer indentation instrumentPrepared alpha-CN x The hardness of the/Fe coating was 10.1Gpa.
Measurement of alpha-CN prepared in test three by ball-and-disc frictional wear instrument under dry friction condition x The friction coefficient of the/Fe coating was 0.24 (see FIG. 2, temperature on the curve corresponds to the deposition temperature of step three).
And (3) testing four: the test is a comparative test, no iron element is added, and the specific process is different from the test one in that: in the second step, fe is not installed 3 And C, target material. The others are the same as in test one.
Determination of the alpha-CN prepared by test four by XPS x The carbon content in the coating was 93.46at.%, the iron content was 0at.%, and the nitrogen content was 6.54at.%.
alpha-CN prepared by nano indentation instrument test four x The hardness of the coating was 12.7GPa.
Measurement of test four prepared alpha-CN by ball and disc tribo-abrader under dry Friction conditions x The coefficient of friction of the coating was 0.39 (see fig. 2, temperature on the curve corresponds to the deposition temperature of step three).
Test five: the first difference between this test and the test is: setting the deposition temperature to 800 ℃. The others are the same as in test one.
alpha-CN prepared by nano indentation instrument test four x The hardness of the coating was 9.8GPa.
Measurement of test five prepared alpha-CN by ball and disc tribo-wear instrument under dry Friction conditions x The friction coefficient of the/Fe coating was 0.25 (see FIG. 2, temperature on the curve corresponds to the deposition temperature of step three).
FIG. 1 is an XRD pattern of a sputtered product, the temperature on the pattern corresponding to the deposition temperature in step three, from which it can be seen that alpha-CN is deposited at 500℃and 600℃due to the introduction of Fe element x Fe coating exhibiting weak diffraction peak Fe 4 N, while Fe was not observed at 700℃and 800 ℃C 4 The presence of an N diffraction peak; for pure alpha-CN x The coating (run four) had no distinct peaks and exhibited a typical amorphous structure.
Summary of the inventionin one of the preparations of the inventionSeries alpha-CN x Fe coating and pure alpha-CN x The addition of a small amount of Fe element has a great influence on the hardness of the coating layer compared with the coating layer (test four), and the alpha-CN x The hardness variation of the Fe coating has a great relationship with the deposition temperature, which may be related to Fe 4 The presence of an N-crystalline phase is associated with high surface density. alpha-CN at 600 DEG C x The Fe coating has the highest hardness value, about pure alpha-CN x 2.13 times the coating. Series of alpha-CNs x The friction coefficient in the Fe coating increases and decreases with increasing temperature, and decreases to a minimum of 0.18 when the deposition temperature increases to 600 ℃, about pure alpha-CN x 46% of the coating. Fe when the coating is deposited at 700 ℃ and 800 DEG C 4 The N phase disappears, the surface is hollow, the density of the coating is reduced, the friction coefficient is obviously increased, and the friction coefficient is kept at 0.23 and 0.25. And depositing alpha-CN at a temperature of 600 DEG C x The formation of highly graphitized OLC tribofilms was found in the wear debris of the Fe coating (FIG. 3), which is also one of the important reasons for its excellent tribological properties. The invention proves that the addition of Fe element in the coating can be used for improving the catalytic activity and promoting the formation of an in-situ friction film under friction conditions. To realize CN x The coating is tough, and the self-lubricating and wear-resistant integrated regulation and control provides a new method.
Claims (1)
1. alpha-CN x A process for preparing the nano Fe-composite coating features that alpha-CN x The preparation method of the Fe nano composite coating comprises the following steps:
1. sequentially selecting absolute ethyl alcohol, acetone and deionized water to ultrasonically clean the substrate for 25min, and finally drying the substrate in a drying oven at 60 ℃; the substrate is alloy Ti-6Al-4V;
2. placing the substrate cleaned and dried in the first step into a vacuum cavity of a magnetron sputtering device, and mixing graphite target material and Fe 3 The C target is arranged on the target position of the magnetron sputtering device, the distance between the target and the substrate is 12cm, and the cavity is vacuumized by a mechanical pump and a turbomolecular pump until the vacuum degree is 1 multiplied by 10 -4 Pa；
3. Into the cavityAr and N are introduced 2 As sputtering gas, adjusting the working pressure in the cavity to 0.8Pa; the graphite target adopts direct current, and the sputtering current of the graphite target is set to be 0.5A; fe (Fe) 3 The C target adopts radio frequency current, fe 3 C, setting the deposition temperature to be 600 ℃ with the radio frequency power of 40W; sputtering is started simultaneously by the two targets, and the sputtering thickness of the two targets is equal and is 1 mu m;
the flow rate of Ar is 60sccm; said N 2 The flow rate of (2) was 20sccm;
4. after sputtering, cooling the cavity to room temperature to obtain alpha-CN x a/Fe coating;
the alpha-CN x The coefficient of friction of the/Fe coating was 0.18.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111375984.8A CN114086138B (en) | 2021-11-19 | 2021-11-19 | alpha-CN x Preparation method of Fe nano composite coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111375984.8A CN114086138B (en) | 2021-11-19 | 2021-11-19 | alpha-CN x Preparation method of Fe nano composite coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114086138A CN114086138A (en) | 2022-02-25 |
| CN114086138B true CN114086138B (en) | 2024-03-15 |
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