CN103757598A - Linear ion implantation surface modification method of M50NiL material - Google Patents
Linear ion implantation surface modification method of M50NiL material Download PDFInfo
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- CN103757598A CN103757598A CN201410003343.3A CN201410003343A CN103757598A CN 103757598 A CN103757598 A CN 103757598A CN 201410003343 A CN201410003343 A CN 201410003343A CN 103757598 A CN103757598 A CN 103757598A
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Abstract
The invention discloses a linear ion implantation surface modification method of an M50NiL material. The method comprises the following steps: carrying out surface modification on M50NiL material by adopting a linear ion implantation mode, carrying out continuous overlapping injection by adopting nitrogen ions and metal ions for surface modification; firstly, injecting the nitrogen ions, then injecting the metal ions, and orderly circulating at least twice, so that the nitrogen ions and the metal ions are injected at least twice. By adopting the linear ion implantation surface modification method of the M50NiL material and the surface-modified M50NiL material disclosed by the invention, the surface of the modified M50NiL material has good contact fatigue resistance.
Description
Technical field
The present invention relates to the surface modification treatment field of metallic substance, particularly M50NiL steel is carried out the method for Ion Beam Surface Modification.
Background technology
M50NiL and M50 bearing steel material (M50NiL, the M50 bearing steel trade mark for representing according to the regulation in national standard < < indicatingmethod of steel product grade > > (GB221-79)) are a large amount of high temperature resistant bearing materialss that use on present stage Aero-engine Bearing, the wherein low and distribution of carbides disperse more of M50NiL material heart portion carbon content, has good anti-fracture toughness property.Therefore meanwhile, because M50NiL material surface has the high rigidity that is not less than M50 after carburizing treatment, compare on the bearing that M50 is more widely used in high DN value (internal diameter size X rotating speed).M50NiL material bearing is usually operated under high temperature heavy loading and high rotating speed working condition, and Working environment is very severe, inevitably comes in contact in this case fatigue failure, therefore the contacting fatigue resistance of bearing materials is had higher requirement.Because the ball track surface accuracy of aviation main shaft class is had relatively high expectations, and lost efficacy and mainly occurred in its working-surface and subsurface layer, the germinating of fatigue cracking and expansion also mostly concentrate on working-surface and subsurface layer, effects on surface Accuracy is large, therefore, requiring under the constant condition of part shape and geometrical dimension, how to adopt process for modifying surface to improve the comprehensive mechanical performance on bearing materials surface, especially contacting fatigue resistance, becomes current Aero-engine Bearing problem demanding prompt solution.
Existing M50NiL material surface modifying method has, Xi'an University of Technology adopts traditional high temperature carbonitriding (900 ℃～920 ℃) technique to carry out surface treatment to M50NiL steel, but traditional expansion is oozed technology or chemical vapour deposition etc. often because high temperature makes bearing size lose due precision and cannot use.And the ion implantation machining at low temperature that can realize can not exert an influence to the dimensional precision of bearing, be particularly suitable as the last process of high-precision bearing.Harbin Institute of Technology's using plasma immersion ion injects (PIII) technology, and high energy nitrogen is ion implantation to material modified nearly upper layer, has improved the anti-contact fatigue of material surface, wearing and tearing and corrosion resistance.But plasma immersion ion implantation technique exists that Implantation Energy is low, input horizon is shallow, complex region implantation homogeneity causes not injecting effect performance boost undesirable, that inject product and is subject to certain restrictions while injecting.Orthoscopic ion implantation technique has advantages of that the higher and injection zone of Implantation Energy, implantation dosage precision are controlled.Meanwhile, water-cooling system can keep injection member surface modification at normal temperatures, without problems such as size distortion, deterioration in accuracy.The ion implantation compound that can change time top layer and upper layer of high energy orthoscopic forms phase, produces a large amount of dislocations, forms the features such as dislocations strengthening of higher-strength, can improve material surface contacting fatigue resistance.But still there is certain problem in existing orthoscopic ion implantation technology.One, existing non-overlapped formula are injected, the equilibrium concentration that the injection of every kind of element and sputter reach is low, implantation concentration (dosage) can reach capacity (it is saturated that average every kind of injection element injection peak concentration reaches 20% left and right) very soon, is difficult to improve concentration again.Two, inject element kind, injection order, Implantation Energy and implantation dosage to the concentration of the contained injection element of base material, the degree of depth, even to front a kind of concentration of element, the depth profile injected in base material, have the property difference (as structure matching) because of sputter and different injection elements to have relatively big difference.The ion implantation injection element of orthoscopic has sputter impact each other, and rear a kind of injection element is larger to front a kind of injection element sputter volume, causes element to inject the degree of depth more shallow.In practice, often run into the element of front a kind of element almost by rear a kind of element sputter phenomenon totally, greatly affected the performance of body material after injecting.For another example, the combination of the dual element of carbon and carbide forming element is injected, and carbide forming element is to carbon concentration, degree of depth important.Equally, the combination of the dual element of nitrogen element is injected and is had similar rule.Three, existing single-element overdose injects, and the radiation injury of ion implantation element is far longer than the radiation injury that different elements intersect after injecting.And excessive bombardment damage, also has considerable influence to material mechanical performance.
Therefore, develop a kind of orthoscopic ion implantation technology that can apply on heavy duty engine main shaft bearing, promoting the anti-contact fatigue of aircraft engine main shaft M50NiL material, wear-resistant, corrosion resistant process for modifying surface, is Aero-engine Bearing problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide a kind of ion-implanted surface-modified method of M50NiL material orthoscopic and surface modification M50NiL material, make M50NiL material surface there is good contacting fatigue resistance.
For achieving the above object, the invention provides a kind of ion-implanted surface-modified method of M50NiL material orthoscopic, the method comprises the following steps:
Under vacuum condition, adopt the ion implantation mode of orthoscopic to carry out surface modification to M50NiL material, surface modification adopts nitrogen ion and the continuous overlapping injection of metal ion, first injecting nitrogen ion, metal ion reinjects, circulation is at least 2 times successively, makes nitrogen ion and metal ion all carry out at least 2 times injection process.
Wherein, before surface modification, remove the step of grease: first use this pending M50NiL material surface grease of metal grease removal removal of solvents, then put it in free of contamination zellon and soak after 20～30 minutes and take out, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping;
Wherein, before surface modification, remove the step of rust spot: with the metal cleaner soaking and washing M50NiL material 10～20 minutes with rust removing function, make its surface without micro-rust spot;
Wherein, before surface modification, also comprise deimpurity step: M50NiL material is put into acetone, and ultrasonic cleaning was taken out after 20～40 minutes, used clean silk to dry.While drying, on the smooth surface of material, carry out in the same direction wiping, guarantee that material surface does not have water stain and impurity is residual; The wiping of the privileged sites of material (working face) emphasis, other positions (non-working surface) of material guarantee that material surface does not have water stain and impurity is residual.Meanwhile, do not use silk contaminated, that soak to carry out wiping to material.
Wherein, before surface modification, also comprise the M50NiL material through above-mentioned pre-treatment is put into deionized water, ultrasonic cleaning was taken out after 20～40 minutes, used clean silk to clean, dry and dry (be positioned in vacuum drying oven and dry 2～4 hours).
Wherein, M50NiL material is put on vacuum chamber sample bench, it is 3.0 * 10 that vacuum chamber is evacuated to vacuum tightness
-5pa～1.8 * 10
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously, surface modification adopts gaseous ion and the continuous overlapping injection technology of metal ion, first injecting gas ion, and metal ion reinjects, gaseous ion reinjects, the metal ion that reinjects, circulation is at least 2 times successively, guarantees that gaseous ion and metal ion have all carried out at least 2 injections.
Wherein, source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 70keV～100keV, injects total dose 1.0 * 10
17ions/cm
2～4.5 * 10
17ions/cm
2;
Wherein, metal ion is zirconium ion, titanium ion, molybdenum ion, chromium ion;
Wherein, the source metal of metal ion adopts the metallic target that purity is 99.8%, and the Implantation Energy that injects for the first time metal ion is 80keV～20keV, and Implantation Energy is decremented to minimum 15keV successively thereafter, and ion implantation total dose is 1.2 * 10
17ions/cm
2～4 * 10
17ions/cm
2;
Wherein, also comprise that the M50NiL material after injecting is put into acetone to be cleaned after 20～40 minutes and dry, seals its vacuum-sealing up for safekeeping.
Wherein, the M50NiL material surface after injection along with the increase that element injects the degree of depth forms amorphous, crystallite and alloy phase, that is, inwardly forms amorphous, crystallite and alloy phase by material surface successively.
Wherein, AES (Auger) detection that M50NiL material after injecting is carried out injecting element in surface (detects the about 100nm of the degree of depth, detection elements is unified is iron, chromium, molybdenum, carbon, nickel, nitrogen, zirconium, titanium), result shows, injected with metallic elements and nitrogen concentration of element peak value place atomicity are not less than the 30at.% of total atom number separately, , in M50NiL material surface 100nm after injection, injected with metallic elements and nitrogen concentration of element peak value place atomicity are not less than the 30at.% of total atom number separately, and nitrogen atom concentration peak value place atomicity is higher than atoms metal peak concentration place atomicity.
It is a kind of via the made surface modification M50NiL material of aforesaid method that the present invention also provides.
Wherein, the increase that this surface modification M50NiL material surface injects the degree of depth along with element, forms amorphous, crystallite and alloy phase,, by material surface, inwardly forms successively amorphous, crystallite and alloy phase that is.
Wherein, AES (Auger) detection that M50NiL material after injecting is carried out injecting element in surface (detects the about 100nm of the degree of depth, detection elements is unified is iron, chromium, molybdenum, carbon, nickel, nitrogen, zirconium, titanium), result shows, injected with metallic elements and nitrogen concentration of element peak value place atomicity are not less than the 30at.% of total atom number separately, , in M50NiL material surface 100nm after injection, injected with metallic elements and nitrogen concentration of element peak value place atomicity are not less than the 30at.% of total atom number separately, and nitrogen atom concentration peak value place atomicity is higher than atoms metal peak concentration place atomicity.
Compared with prior art, beneficial effect of the present invention is as follows:
Disclosed by the inventionly a kind of M50NiL material is carried out to the ion-implanted surface-modified method of orthoscopic and the made surface modification M50NiL material of the method, at M50NiL material surface, carry out dual element ion alternation and repeatedly inject, can guarantee that the ion implanted layer of M50NiL material surface has good contacting fatigue resistance.Method of the present invention has unique advantage to component in the very strict high-accuracy bearing of anti-contact fatigue characteristic requirements, can be in the situation that not changing accessory size, improve the condition of surface, slip characteristic of material etc., can form the anti-contact fatigue characteristic that solution strengthening, precipitated phase dispersion-strengthened and residual compressive stress strengthen piece surface simultaneously.Therefore the present invention carries out surface treatment with ion implantation to M50NiL material, can make M50NiL material have better contacting fatigue resistance, meets the performance requriements of aircraft engine.
The present invention adopts overlapping ion implantation nitrogen element and metallic element, and the method that this dual element injects can improve the contact resistance fatigue property of material.With dual element, inject M50NiL material, the increase of injecting the degree of depth along with element can form amorphous, crystallite and alloy phase, and causes the disturbance of atom (group) arrangement in depths more.Its nano hardness injecting in range of influence is obviously promoted.In the performance test of high temperature rolling contact fatigue, the M50NiL bill of material that injects modification has revealed higher contacting fatigue resistance, and wherein the rated life time of anti-contact fatigue test is 3 times of injecting material not, and median life improves and approaches 5 times.Compare with injection face not, the average loading life-span of injection face is greatly improved.And under the effect of cyclic loading.Concentration width and the degree of depth that dual element injects N all increase, and change in concentration is more steady.Dual element alternately injects the concentration distribution span of the injection element that makes base material and changes broader and relax, and has reduced the sharp change of concentration.Wherein the injection degree of depth of N element is higher than metallic element.
The surface modifying material that the inventive method is produced, is by metal ion and gaseous ion injection bearing steel top layer, forms a new modified layer.Inject modified sample and exist the amorphous layer of several nano thickness except top layer, the rule of its inner certain depth position is arranged atom (group) structure and has been occurred certain disturbance, arranges and becomes no longer regular.Injecting the energy that particle has 10～100keV after high energy and high speed, there is repeatedly cascade collision transferring energy in high-octane particle and substrate surface atom, to being finally still in gap or the empty place of some lattice, even replaces the original atom in lattice.Heavy dose of or accept the top layer that high-energy particle bombardment is strong, there is the disordering of atom (group), and can form non-crystal structure.In addition, high energy projectile can form certain radiation damage in darker position because of thermal spike effect.
By selected diffraction, can find out on the monocrystalline martensite diffraction spot on base material and occur certain ring-type, show that injection causes the grain refining of monocrystalline martensite and has polycrystalline trend.Simultaneously outside martensite single crystal diffraction spot, can also additionally observe the diffraction spot of another monocrystalline material, diffraction spot intensity relatively a little less than.By with base material same position on the comparing of diffraction spot, can determine that the M50NiL material surface that injects N+Zr has formed new monocrystalline phase material.
Fatigue damage district from injection sample and the fatigue point dense distribution degree in region thereof, the fatigue cracking that starts from top layer to produce has obtained suppressing significantly at injection sample.The surface strengthening that the amorphous layer that this mainly forms with material surface in injection process and the alloy phase of formation cause is relevant.Amorphous layer has reduced cosmetic bug, thereby reduces the germinating point quantity of fatigue cracking.Within the scope of the 200nm of base material top layer, front especially 100nm, the ratio that injection element accounts for total atom number is not less than 30at.%, and this just causes the alloy phase position distributing in high density to form solution strengthening, and forms clearance type lattice distortion at lower concentration distributing position.This is all conducive to produce certain stress on the surface of base material, and this stress can affect time top layer, and suppresses the expansion of crackle in this region.Above two kinds of modes, one side has reduced the germinating point of top layer fatigue cracking, has suppressed on the other hand the fatigue crack growth on inferior top layer, and its net effect is the contacting fatigue resistance that improves base material.The strengthening mechanism of injecting is mainly reflected in the germinating point quantity that reduces top layer fatigue cracking, and suppresses time top layer crack propagation and slow down the aspects such as grain hardening speed.
Below in conjunction with the drawings and specific embodiments, describe the present invention, but not as a limitation of the invention.
Accompanying drawing explanation
Fig. 1 is method steps schema of the present invention;
Fig. 2 is for adopting method of the present invention to carry out high temperature contact fatigue life test-results figure (contact fatigue life P-N graphic representation) to M50NiL material;
Fig. 3 A is for adopting the high resolution transmission electron microscope figure after method of the present invention is injected M50NiL material;
Fig. 3 B is a-quadrant diffractogram in Fig. 3 A;
Fig. 3 C is the diffractogram of a-quadrant when injecting in Fig. 3 A.
Wherein, Reference numeral:
S1～S4: step
Embodiment
The method that M50NiL material orthoscopic of the present invention is ion-implanted surface-modified and surface modification M50NiL material, can make M50NiL material surface have good contacting fatigue resistance.Please refer to Fig. 1, the method comprises the following steps:
1) get a pending M50NiL material ready, remove its surperficial grease, rust spot, impurity;
2) the M50NiL material of processing through step 1) is washed and dried, obtain the M50NiL material of a processing;
3) under vacuum condition, adopt the ion implantation mode of orthoscopic to carry out surface modification to the M50NiL material of this processing, surface modification adopts nitrogen ion and the continuous overlapping injection technology of metal ion, first injecting nitrogen ion, the metal ion that reinjects, the nitrogen ion that reinjects, metal ion reinjects, circulation is at least 2 times successively, makes nitrogen ion and metal ion all carry out obtaining the M50NiL material after an injection after at least 2 injections;
4) clean and dry the M50NiL material after this injection, vacuum-sealing is sealed up for safekeeping.
Of the present invention M50NiL material is carried out to the ion-implanted surface-modified method of orthoscopic, particularly, can adopt following embodiment:
Step 1) is got a pending M50NiL material ready,
Remove its surperficial grease: the grease of first using this pending M50NiL material surface of metal grease removal removal of solvents, then put it in free of contamination zellon and soak after 20～30 minutes and take out, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping; It is that commercially available plain metal removes fatsolvent that described metal removes fatsolvent, and composition comprises sodium hydroxide, sodium carbonate, ten water sodium phosphates, water glass, washing composition, inhibiter, aqueous solvent etc.; Clean also available other organic solvents replacements of zellon of use.
Remove the rust spot of M50NiL material surface: metal cleaner (Deruster for metal) the soaking and washing M50NiL material 10～20 minutes with having rust removing function, makes its surface without micro-rust spot; Described Deruster for metal is commercially available plain metal rust remover, and composition comprises: tensio-active agent, organic acid, promotor, inhibiter, deionized water etc.
Remove the water stain and impurity of M50NiL material surface: M50NiL material is put into acetone, ultrasonic cleaning was taken out after 20～40 minutes, use clean silk to dry (in the process of the water stain and impurity of removal M50NiL material surface, using silk to clean or dry should be noted: on the smooth surface of material, carry out in the same direction wiping, guarantee that material surface does not have water stain and impurity is residual; The wiping of the privileged sites of material (working face) emphasis, other positions (non-working surface) of material guarantee that material surface does not have water stain and impurity is residual; Meanwhile, do not use silk contaminated, that soak to carry out wiping to material); Clean also available other organic solvents replacements of acetone of use.
Step 2) the M50NiL material of processing through step 1) is put into deionized water, ultrasonic cleaning was taken out after 20～40 minutes, use clean silk to clean, dry and dry (be positioned in vacuum drying oven and dry 2～4 hours), obtain the M50NiL material of a processing;
Step 3) is by through step 2) the M50NiL material processed is put on vacuum chamber sample bench, and it is 3.0 * 10 that vacuum chamber is evacuated to vacuum tightness
-5pa～1.8 * 10
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, use ion implanter (SYZ-100 implanter) to carry out surface modification to M50NiL material simultaneously, surface modification adopts nitrogen ion and the continuous overlapping injection technology of metal ion, first injecting nitrogen ion, and metal ion reinjects, nitrogen ion reinjects, the metal ion that reinjects, circulation is at least 2 times successively, guarantees that nitrogen ion and metal ion have all carried out obtaining the M50NiL material after an injection after at least 2 injections; Wherein, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 70keV～100keV, injects total dose 1.0 * 10
17ions/cm
2～4.5 * 10
17ions/cm
2; Metal ion be in zirconium ion, titanium ion, molybdenum ion, chromium ion any one, the source metal of metal ion adopts the metallic target that purity is 99.8%, the ion implantation parameter of injecting for the first time metal ion is Implantation Energy 80keV～20keV, thereafter Implantation Energy is decremented to minimum 15keV successively, and ion implantation total dose is 1.2 * 10
17ions/cm
2～4 * 10
17ions/cm
2;
Step 4) is put into acetone by the M50NiL material after injecting and is cleaned after 20～40 minutes and dry, and its vacuum-sealing is sealed up for safekeeping.
It is a kind of via the made surface modification M50NiL material of aforesaid method that the present invention also provides, the increase that this surface modification M50NiL material surface injects the degree of depth along with element, by material surface, inwardly form successively amorphous, crystallite and alloy phase, and, AES (Auger) detection that this surface modification M50NiL material is carried out injecting element in surface (detects the about 100nm of the degree of depth, detection elements is unified is iron, chromium, molybdenum, carbon, nickel, nitrogen, zirconium, titanium) result shows: injected with metallic elements and nitrogen concentration of element peak value place atomicity are not less than the 30at.% of total atom number separately, wherein nitrogen atom concentration peak value place atomicity is higher than atoms metal peak concentration place atomicity.
Below in conjunction with specific embodiment so that embodiments of the present invention are described in detail:
In the present embodiment, adopt nitrogen ion and zirconium ion to carry out surface modification to M50NiL material, go through 3 injections.Zirconium ion wherein can replace with titanium ion, molybdenum ion, chromium ion on an equal basis, and parameters (as Implantation Energy, implantation dosage etc.) is constant.
Step 1) is got a pending M50NiL material ready, first use the grease of this pending M50NiL material surface of metal grease removal removal of solvents, then put it in free of contamination zellon and take out after 20 minutes, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping; With the metal cleaner soaking and washing M50NiL material 10 minutes with rust removing function, make its surface without micro-rust spot; M50NiL material is put into acetone, and ultrasonic cleaning was taken out after 20 minutes, used clean silk to dry.
Step 2) the M50NiL material of processing through step 1) is put into deionized water, ultrasonic cleaning was taken out after 20 minutes, used clean silk to clean, dry and dry, and obtained the M50NiL material of a processing;
Step 3) is by through step 2) the M50NiL material processed is put on vacuum chamber sample bench, and it is 3.0 * 10 that vacuum chamber is evacuated to vacuum tightness
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously, surface modification adopts nitrogen ion and the continuous overlapping injection technology of zirconium ion, first injecting nitrogen ion, the zirconium ion that reinjects, circulates 3 times successively, guarantees that nitrogen ion and zirconium ion have all carried out obtaining the M50NiL material after an injection after 3 injections; Wherein, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 70keV, and each implantation dosage is 0.5 * 10
17ions/cm
2, inject total dose 1.5 * 10
17ions/cm
2; Zirconium ion source adopts the zirconium target that purity is 99.8%, and the Implantation Energy that injects for the first time zirconium ion is 20keV, and implantation dosage is 1 * 10
17ions/cm
2, the Implantation Energy that injects for the second time zirconium ion is 18keV, implantation dosage is 1 * 10
17ions/cm
2, the Implantation Energy that injects for the third time zirconium ion is 15keV, implantation dosage is 1 * 10
17ions/cm
2, that is, it is 3 * 10 that zirconium ion injects total dose
17ions/cm
2;
Step 4) is put into acetone by the M50NiL material after injecting and is cleaned after 20 minutes and dry, and its vacuum-sealing is sealed up for safekeeping.
In the present embodiment, adopt nitrogen ion and zirconium ion to carry out surface modification to M50NiL material, go through 4 injections.Zirconium ion wherein can replace with titanium ion, molybdenum ion, chromium ion on an equal basis, and parameters (as Implantation Energy, implantation dosage etc.) is constant.
Step 1) is got a pending M50NiL material ready, first use the grease of this pending M50NiL material surface of metal grease removal removal of solvents, then put it in free of contamination zellon and take out after 30 minutes, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping; With the metal cleaner soaking and washing M50NiL material 20 minutes with rust removing function, make its surface without micro-rust spot; M50NiL material is put into acetone, and ultrasonic cleaning was taken out after 40 minutes, used clean silk to dry.
Step 2) the M50NiL material of processing through step 1) is put into deionized water, ultrasonic cleaning was taken out after 40 minutes, used clean silk to clean, dry and dry, and obtained the M50NiL material of a processing;
Step 3) is by through step 2) the M50NiL material processed is put on vacuum chamber sample bench, and it is 1.8 * 10 that vacuum chamber is evacuated to vacuum tightness
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously, surface modification adopts nitrogen ion and the continuous overlapping injection technology of zirconium ion, first injecting nitrogen ion, the zirconium ion that reinjects, circulates 4 times successively, guarantees that nitrogen ion and zirconium ion have all carried out obtaining the M50NiL material after an injection after 4 injections; Wherein, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 83keV, each implantation dosage 0.5 * 10
17ions/cm
2, total implantation dosage is 2 * 10
17ions/cm
2; Zirconium ion source adopts the zirconium target that purity is 99.8%, and the Implantation Energy that injects for the first time zirconium ion is 45keV, and implantation dosage is 0.5 * 10
17ions/cm
2, the Implantation Energy that injects for the second time zirconium ion is 40keV, implantation dosage is 0.5 * 10
17ions/cm
2, the Implantation Energy that injects for the third time zirconium ion is 30keV, implantation dosage is 0.5 * 10
17ions/cm
2, the Implantation Energy that injects zirconium ion for the 4th time is 20keV, implantation dosage is 0.5 * 10
17ions/cm
2, that is, it is 2 * 10 that zirconium ion injects total dose
17ions/cm
2;
Step 4) is put into acetone by the M50NiL material after injecting and is cleaned after 40 minutes and dry, and its vacuum-sealing is sealed up for safekeeping.
Embodiment 3
In the present embodiment, adopt nitrogen ion and titanium ion to carry out surface modification to M50NiL material, go through 5 injections.Titanium ion wherein can replace with zirconium ion, molybdenum ion, chromium ion on an equal basis, and parameters (as Implantation Energy, implantation dosage etc.) is constant.
Step 1) is got a pending M50NiL material ready, first use the grease of this pending M50NiL material surface of metal grease removal removal of solvents, then put it in free of contamination zellon and take out after 25 minutes, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping; With the metal cleaner soaking and washing M50NiL material 15 minutes with rust removing function, make its surface without micro-rust spot; M50NiL material is put into acetone, and ultrasonic cleaning was taken out after 30 minutes, used clean silk to dry.
Step 2) the M50NiL material of processing through step 1) is put into deionized water, ultrasonic cleaning was taken out after 30 minutes, used clean silk to clean, dry and dry, and obtained the M50NiL material of a processing;
Step 3) is by through step 2) the M50NiL material processed is put on vacuum chamber sample bench, and it is 1.8 * 10 that vacuum chamber is evacuated to vacuum tightness
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously, surface modification adopts nitrogen ion and the continuous overlapping injection technology of titanium ion, first injecting nitrogen ion, the titanium ion that reinjects, circulates 5 times successively, guarantees that nitrogen ion and titanium ion have all carried out obtaining the M50NiL material after an injection after 5 injections; Wherein, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 83keV, each implantation dosage 0.5 * 10
17ions/cm
2, total implantation dosage is 2.5 * 10
17ions/cm
2; Titanium ion source adopts the titanium target that purity is 99.8%, and the Implantation Energy of Implanted Titanium ion is 48keV for the first time, and implantation dosage is 0.7 * 10
17ions/cm
2, the Implantation Energy of Implanted Titanium ion is 43keV for the second time, implantation dosage is 0.7 * 10
17ions/cm
2, the Implantation Energy of Implanted Titanium ion is 38keV for the third time, implantation dosage is 0.7 * 10
17ions/cm
2, the Implantation Energy of the 4th Implanted Titanium ion is 33keV, implantation dosage is 0.7 * 10
17ions/cm
2, the Implantation Energy of the 5th Implanted Titanium ion is 23keV, implantation dosage is 0.7 * 10
17ions/cm
2, that is, Ti ion implantation total dose is 3.5 * 10
17ions/cm
2;
Step 4) is put into acetone by the M50NiL material after injecting and is cleaned after 30 minutes and dry, and its vacuum-sealing is sealed up for safekeeping.
Embodiment 4
In the present embodiment, adopt nitrogen ion and molybdenum ion to carry out surface modification to M50NiL material, go through 3 injections.Molybdenum ion wherein can replace with zirconium ion, titanium ion, chromium ion on an equal basis, and parameters (as Implantation Energy, implantation dosage etc.) is constant.
Step 1) is got a pending M50NiL material ready, first use the grease of this pending M50NiL material surface of metal grease removal removal of solvents, then put it in free of contamination zellon and take out after 25 minutes, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping; With the metal cleaner soaking and washing M50NiL material 15 minutes with rust removing function, make its surface without micro-rust spot; M50NiL material is put into acetone, and ultrasonic cleaning was taken out after 30 minutes, used clean silk to dry.
Step 2) the M50NiL material of processing through step 1) is put into deionized water, ultrasonic cleaning was taken out after 30 minutes, used clean silk to clean, dry and dry, and obtained the M50NiL material of a processing;
Step 3) is by through step 2) the M50NiL material processed is put on vacuum chamber sample bench, and it is 1.8 * 10 that vacuum chamber is evacuated to vacuum tightness
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously, surface modification adopts nitrogen ion and the continuous overlapping injection technology of molybdenum ion, first injecting nitrogen ion, the molybdenum ion that reinjects, circulates 3 times successively, guarantees that nitrogen ion and molybdenum ion have all carried out obtaining the M50NiL material after an injection after 3 injections; Wherein, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 83keV, each implantation dosage 0.5 * 10
17ions/cm
2, total implantation dosage is 1.5 * 10
17ions/cm
2; Sources of molybdenum ions adopts the molybdenum target that purity is 99.8%, and the Implantation Energy that injects for the first time molybdenum ion is 40keV, and implantation dosage is 0.5 * 10
17ions/cm
2, the Implantation Energy that injects for the second time molybdenum ion is 33keV, implantation dosage is 1.2 * 10
17ions/cm
2, the Implantation Energy that injects for the third time molybdenum ion is 25keV, implantation dosage is 1.8 * 10
17ions/cm
2, that is, it is 3.5 * 10 that molybdenum ion injects total dose
17ions/cm
2;
Step 4) is put into acetone by the M50NiL material after injecting and is cleaned after 30 minutes and dry, and its vacuum-sealing is sealed up for safekeeping.
In the present embodiment, adopt nitrogen ion and chromium ion to carry out surface modification to M50NiL material, go through 4 injections.Chromium ion wherein can replace with zirconium ion, titanium ion, molybdenum ion on an equal basis, and parameters (as Implantation Energy, implantation dosage etc.) is constant.
Step 1) is got a pending M50NiL material ready, first use the grease of this pending M50NiL material surface of metal grease removal removal of solvents, then put it in free of contamination zellon and take out after 25 minutes, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping; With the metal cleaner soaking and washing M50NiL material 15 minutes with rust removing function, make its surface without micro-rust spot; M50NiL material is put into acetone, and ultrasonic cleaning was taken out after 30 minutes, used clean silk to dry.
Step 2) the M50NiL material of processing through step 1) is put into deionized water, ultrasonic cleaning was taken out after 30 minutes, used clean silk to clean, dry and dry, and obtained the M50NiL material of a processing;
Step 3) is by through step 2) the M50NiL material processed is put on vacuum chamber sample bench, and it is 1.8 * 10 that vacuum chamber is evacuated to vacuum tightness
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously, surface modification adopts nitrogen ion and the continuous overlapping injection technology of chromium ion, first injecting nitrogen ion, the chromium ion that reinjects, circulates 4 times successively, guarantees that nitrogen ion and chromium ion have all carried out obtaining the M50NiL material after an injection after 4 injections; Wherein, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 70keV, and each implantation dosage is respectively 0.5 * 10
17ions/cm
2, 1.0 * 10
17ions/cm
2, 1.5 * 10
17ions/cm
2, 1.5 * 10
17ions/cm
2, total implantation dosage is 4.5 * 10
17ions/cm
2; Chromium ion source adopts the chromium target that purity is 99.8%, and the Implantation Energy that injects for the first time chromium ion is 80keV, and implantation dosage is 0.4 * 10
17ions/cm
2, the Implantation Energy that injects for the second time chromium ion is 70keV, implantation dosage is 0.8 * 10
17ions/cm
2, the Implantation Energy that injects for the third time chromium ion is 46keV, implantation dosage is 1.2 * 10
17ions/cm
2, the Implantation Energy that injects chromium ion for the 4th time is 30keV, implantation dosage is 1.6 * 10
17ions/cm
2, that is, it is 4.0 * 10 that chromium ion injects total dose
17ions/cm
2;
Step 4) is put into acetone by the M50NiL material after injecting and is cleaned after 30 minutes and dry, and its vacuum-sealing is sealed up for safekeeping.
In the present embodiment, adopt nitrogen ion and titanium ion to carry out surface modification to M50NiL material, go through 2 injections.Titanium ion wherein can replace with zirconium ion, molybdenum ion, chromium ion on an equal basis, and parameters (as Implantation Energy, implantation dosage etc.) is constant.
Step 1) is got a pending M50NiL material ready, first use the grease of this pending M50NiL material surface of metal grease removal removal of solvents, then put it in free of contamination zellon and take out after 25 minutes, with the rice paper residual solvent that exhausts, use again absorbent cotton Wiping material surface, finally with clean silk, carry out wiping; With the metal cleaner soaking and washing M50NiL material 15 minutes with rust removing function, make its surface without micro-rust spot; M50NiL material is put into acetone, and ultrasonic cleaning was taken out after 30 minutes, used clean silk to dry.
Step 2) the M50NiL material of processing through step 1) is put into deionized water, ultrasonic cleaning was taken out after 30 minutes, used clean silk to clean, dry and dry, and obtained the M50NiL material of a processing;
Step 3) is by through step 2) the M50NiL material processed is put on vacuum chamber sample bench, and it is 1.8 * 10 that vacuum chamber is evacuated to vacuum tightness
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously, surface modification adopts nitrogen ion and the continuous overlapping injection technology of titanium ion, first injecting nitrogen ion, the titanium ion that reinjects, circulates 2 times successively, guarantees that nitrogen ion and titanium ion have all carried out obtaining the M50NiL material after an injection after 2 injections; Wherein, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 100keV, each implantation dosage 0.5 * 10
17ions/cm
2, total implantation dosage is 1.0 * 10
17ions/cm
2; Titanium ion source adopts the titanium target that purity is 99.8%, and the Implantation Energy of Implanted Titanium ion is 60keV for the first time, and implantation dosage is 0.5 * 10
17ions/cm
2, the Implantation Energy of Implanted Titanium ion is 40keV for the second time, implantation dosage is 0.7 * 10
17ions/cm
2, that is, Ti ion implantation total dose is 1.2 * 10
17ions/cm
2;
Step 4) is put into acetone by the M50NiL material after injecting and is cleaned after 30 minutes and dry, and its vacuum-sealing is sealed up for safekeeping.
Compared with prior art, beneficial effect of the present invention is as follows:
The present invention adopts overlapping ion implantation nitrogen element and metallic element, and the method that this dual element injects improves the contact resistance fatigue property of material.Please refer to Fig. 2, the result that M50NiL material is carried out after the test of high temperature contact fatigue life shows, dual element injects M50NiL material (injections N+Zr is example), and the increase of injecting the degree of depth along with element forms amorphous, crystallite and alloy phase, and causes the disturbance of atom (group) arrangement in depths more.Its nano hardness injecting in range of influence is obviously promoted.In the performance test of high temperature rolling contact fatigue, the M50NiL bill of material that injects modification has revealed higher contacting fatigue resistance, and wherein the rated life time of anti-contact fatigue test is 3 times of injecting material not, and median life improves and approaches 5 times.Compare with injection face not, the average loading life-span of injection face is greatly improved.And under the effect of cyclic loading.Concentration width and the degree of depth that dual element injects N all increase, and change in concentration is more steady.Dual element alternately injects the concentration distribution span of the injection element that makes base material and changes broader and relax, and has reduced the sharp change of concentration.Wherein the injection degree of depth of N element is higher than metallic element.
The surface modifying material that the inventive method is produced, is by metal ion and gaseous ion injection bearing steel top layer, forms a new modified layer.Refer again to Fig. 3 A to Fig. 3 C, inject the shape characteristic of modified sample (injection N+Zr is example) under high resolution transmission electron microscopy and constituency (a-quadrant) diffraction result as shown in the figure, provided diffractogram when a-quadrant is injected simultaneously.By high resolution photo, can be found out and be existed the amorphous layer of several nano thickness except top layer, the rule of its inner certain depth position is arranged atom (group) structure and has been occurred certain disturbance, arranges and becomes no longer regular.Injecting the energy that particle has 10～100keV after high energy and high speed, there is repeatedly cascade collision transferring energy in high-octane particle and substrate surface atom, to being finally still in gap or the empty place of some lattice, even replaces the original atom in lattice.Heavy dose of or accept the top layer that high-energy particle bombardment is strong, there is the disordering of atom (group), and can form non-crystal structure.In addition, high energy projectile can form certain radiation damage in darker position because of thermal spike effect.
By selected diffraction, can find out on the monocrystalline martensite diffraction spot on base material and occur certain ring-type, show that injection causes the grain refining of monocrystalline martensite and has polycrystalline trend.Simultaneously outside martensite single crystal diffraction spot, can also additionally observe the diffraction spot of another monocrystalline material, diffraction spot intensity relatively a little less than.By with base material same position on the comparing of diffraction spot, can determine that the M50NiL material surface that injects N+Zr has formed new monocrystalline phase material.
Fatigue damage district from injection sample and the fatigue point dense distribution degree in region thereof, the fatigue cracking that starts from top layer to produce has obtained suppressing significantly at injection sample.The surface strengthening that the amorphous layer that this mainly forms with material surface in injection process and the alloy phase of formation cause is relevant.Amorphous layer has reduced cosmetic bug, thereby reduces the germinating point quantity of fatigue cracking.Within the scope of the 200nm of base material top layer, front especially 100nm, the ratio that injection element accounts for total atom number is not less than 30at.%, and this just causes the alloy phase position distributing in high density to form solution strengthening, and forms clearance type lattice distortion at lower concentration distributing position.This is all conducive to produce certain stress on the surface of base material, and this stress can affect time top layer, and suppresses the expansion of crackle in this region.Above two kinds of modes, one side has reduced the germinating point of top layer fatigue cracking, has suppressed on the other hand the fatigue crack growth on inferior top layer, and its net effect is the contacting fatigue resistance that improves base material.The strengthening mechanism of injecting is mainly reflected in the germinating point quantity that reduces top layer fatigue cracking, and suppresses time top layer crack propagation and slow down the aspects such as grain hardening speed.
Certainly; the present invention also can have other various embodiments; in the situation that not deviating from spirit of the present invention and essence thereof; those of ordinary skill in the art can make according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the claims in the present invention.
Claims (10)
1. the ion-implanted surface-modified method of M50NiL material orthoscopic, is characterized in that:
Under vacuum condition, adopt the ion implantation mode of orthoscopic to carry out surface modification to M50NiL material, surface modification adopts nitrogen ion and the continuous overlapping injection of metal ion, first injecting nitrogen ion, metal ion reinjects, circulation is at least 2 times successively, makes nitrogen ion and metal ion all carry out at least 2 times and injects.
2. the ion-implanted surface-modified method of M50NiL material orthoscopic according to claim 1, is characterized in that, M50NiL material is put on vacuum chamber sample bench, and it is 3.0 * 10 that vacuum chamber is evacuated to vacuum tightness
-5pa～1.8 * 10
-5after Pa, make vacuum chamber sample bench along self axis uniform speed slow rotation, with ion implanter, M50NiL material is carried out to surface modification simultaneously.
3. the ion-implanted surface-modified method of M50NiL material orthoscopic according to claim 1, is characterized in that, nitrogen ion source of the gas adopts the nitrogen that purity is 99.99%, and each Implantation Energy is 70keV～100keV, and injecting total dose is 1.0 * 10
17ions/cm
2～4.5 * 10
17ions/cm
2.
4. the ion-implanted surface-modified method of M50NiL material orthoscopic according to claim 1, is characterized in that, metal ion be in zirconium ion, titanium ion, molybdenum ion, chromium ion any.
5. the ion-implanted surface-modified method of M50NiL material orthoscopic according to claim 1, it is characterized in that, metal ion source metal adopts the metallic target that purity is 99.8%, the Implantation Energy that injects for the first time metal ion is 80keV～20keV, thereafter Implantation Energy is decremented to minimum 15keV successively, and ion implantation total dose is 1.2 * 10
17ions/cm
2～4 * 10
17ions/cm
2.
6. the ion-implanted surface-modified method of M50NiL material orthoscopic according to claim 1, is characterized in that, the M50NiL material surface after injection, along with the increase that element injects the degree of depth, inwardly forms amorphous, crystallite and alloy phase successively by material surface.
7. the ion-implanted surface-modified method of M50NiL material orthoscopic according to claim 1, it is characterized in that, in M50NiL material surface 100nm after injection, injected with metallic elements and nitrogen concentration of element peak value place atomicity are not less than the 30at.% of total atom number separately, and nitrogen atom concentration peak value place atomicity is higher than atoms metal peak concentration place atomicity.
8. a surface modification M50NiL material, is characterized in that, it is made via method claimed in claim 1.
9. surface modification M50NiL material according to claim 8, is characterized in that, this surface modification M50NiL material surface, along with the increase that element injects the degree of depth, inwardly forms amorphous, crystallite and alloy phase successively by material surface.
10. surface modification M50NiL material according to claim 8, it is characterized in that, in M50NiL material surface 100nm after injection, injected with metallic elements and nitrogen concentration of element peak value place atomicity are not less than the 30at.% of total atom number separately, and nitrogen atom concentration peak value place atomicity is higher than atoms metal peak concentration place atomicity.
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| CN106521444A (en) * | 2016-10-21 | 2017-03-22 | 清华大学 | Method for treating M50NiL bearing steel, strengthened M50NiL bearing steel and bearing |
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| CN107164737A (en) * | 2017-05-08 | 2017-09-15 | 清华大学 | A kind of ultralow temperature Ion Implantation Strengthening system and method for bearing steel |
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| CN115637414A (en) * | 2022-10-31 | 2023-01-24 | 江苏省特种设备安全监督检验研究院 | Ultrasonic-assisted ion implantation device and processing method |
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| CN104195521A (en) * | 2014-09-16 | 2014-12-10 | 朱忠良 | Method for modifying metal surface by mixed implantation of plasma source ion beams |
| CN104195521B (en) * | 2014-09-16 | 2017-07-14 | 曹炜 | Plasma source Ion Mixing injects the method to metal surface modification |
| CN106521407A (en) * | 2016-08-23 | 2017-03-22 | 清华大学 | Treatment method for cronidur30 bearing steel, reinforced cronidur30 bearing steel and bearing |
| CN106521444A (en) * | 2016-10-21 | 2017-03-22 | 清华大学 | Method for treating M50NiL bearing steel, strengthened M50NiL bearing steel and bearing |
| CN106521406A (en) * | 2016-10-21 | 2017-03-22 | 清华大学 | Method for treating M50 bearing steel, strengthened M50 bearing steel and bearing |
| CN106521444B (en) * | 2016-10-21 | 2018-10-02 | 清华大学 | It handles the method for M50NiL bearing steels, strengthen M50NiL bearing steels and bearing |
| CN107164737A (en) * | 2017-05-08 | 2017-09-15 | 清华大学 | A kind of ultralow temperature Ion Implantation Strengthening system and method for bearing steel |
| CN111733395A (en) * | 2020-07-30 | 2020-10-02 | 山东增材工业技术研究院有限公司 | Special steel surface treatment method |
| CN111893431A (en) * | 2020-08-17 | 2020-11-06 | 中国人民解放军陆军装甲兵学院 | 20Cr2Ni4A carburizing steel with high contact fatigue resistance and preparation method thereof |
| CN111893431B (en) * | 2020-08-17 | 2022-12-20 | 中国人民解放军陆军装甲兵学院 | 20Cr2Ni4A carburizing steel with high contact fatigue resistance and preparation method thereof |
| CN114457317A (en) * | 2021-12-22 | 2022-05-10 | 北京机械工业自动化研究所有限公司 | Preparation method of ion implantation nano-reinforcing layer |
| CN115637414A (en) * | 2022-10-31 | 2023-01-24 | 江苏省特种设备安全监督检验研究院 | Ultrasonic-assisted ion implantation device and processing method |
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