CN104894498A - Nanometer crystal twinning ultrahigh-hardness surface forming method of nickel base alloy - Google Patents
Nanometer crystal twinning ultrahigh-hardness surface forming method of nickel base alloy Download PDFInfo
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Abstract
The invention discloses a nanometer crystal twinning ultrahigh-hardness surface forming method of a nickel base alloy, and belongs to the technical field of plastic forming of nickel base alloys. The method is characterized in that a sample is the nickel alloy base; a submicron curvature radius diamond needle point is manufactured by methods of ultraprecise grinding and low-carbon steel polishing; a curvature radius of the needle point is 200-900 nm; an projection angle is 90-150 degrees; the needle point takes the shape of a triangular pyramid or a rectangular pyramid; the diamond needle point is mounted on a nanometer indentation instrument or a microhardness tester for impressing; the load is 0.2-2 N; the surface hardness can be increased by 20-40 times compared with a traditional alloy, and reaches 100-120 GP; the surface consists of nanometer twin crystals; and the nanometer twin crystals consist of arrays formed by a twin crystal plate with a thickness not smaller than 15 nm and one or several twin crystal plates with the thickness smaller than 15 nm, can bear 100 times of circular loading, and have no cracks on the surfaces after being loaded. The nanometer crystal twinning ultrahigh-hardness surface forming method of the nickel base alloy is realized.
Description
Technical field
The invention belongs to nickel-base alloy plastic forming technology field, relate to the precision plastic forming method of nickel-base alloy, particularly a kind of nickel-base alloy nano twin crystal ultrahigh hardness table surface forming method.
Background technology
Nickel-base alloy is the indispensable key components and parts material in the fields such as Aeronautics and Astronautics, nuclear power, ocean, and being the whether advanced reflection of a national industry, is also one of important indicator of a National Industrial advanced person.Nickel-base alloy ultrahigh hardness surface is the great demand of country, as core main pump main shaft, bearing, aircraft engine main shaft, bearing, the stressed key components and parts surface of nickel-base alloy, and the movement pair surface of nickel-base alloy, all need the high performance surface of wear-resisting antifatigue, this just needs nickel-base alloy surface to have ultrahigh hardness, keeps plasticity simultaneously.
Current raising alloy surface hardness mainly contains three kinds of methods: (1) third party's atom indentation, different from the interatomic diameter of body owing to embedding atom, therefore can form stress, hinder the slippage of dislocation, thus improve the hardness of material; (2) increase crystal boundary, also can hinder the slippage of dislocation; (3) coherent grain boundary-twin is formed.It is all premised on the plasticity of expendable material that the hardness that first two method obtains improves, and is therefore difficult to apply in engineering.Twin both can improve the hardness of material, can keep plasticity again, had great future in engineering applications.Be embodied in technically, coating and the method such as laser impact intensified, can improve hardness, but be also generally be reduced to cost with plasticity.Coating easily comes off after being hit, and strictly prohibits the use in fields such as aircraft engine and core main pumps.Laser impact intensified general hardness improves can reach 4-6 doubly.According to " Science ", nano twin crystal copper can improve hardness 10 times, keeps plasticity and electroconductibility simultaneously.But current nano twin crystal technology mainly concentrates on elemental copper, and simple substance element is due to the restriction of mechanical property, seldom in engineering field application, engineering field is widely used is alloy.
The manufacturing technology of nano twin crystal mainly contains surperficial mechanical rolled-on method, surface mechanical attrition method and dynamic plasticity deformation method etc.This several method is according to " Science ", and hardness is the highest improves 10 times, and mainly concentrates on nano twin crystal copper.
Summary of the invention
The object of this invention is to provide a kind of nickel-base alloy nano twin crystal ultrahigh hardness table surface forming method, solve the low not wear-resistant difficult problem of nickel-base alloy surface hardness.
Technical scheme of the present invention is sample is nickel-base alloy, the method of superfine grinding and soft steel polishing is adopted to manufacture submicron radius-of-curvature Diamond tip, the radius-of-curvature of needle point is 100nm-900nm, projection angle is 90-150 °, shape is triprismo or rectangular pyramid, Diamond tip is installed on nano-hardness tester or microhardness tester, carry out nano impression, load is 0.1-2N, the more former alloy of hardness on surface can improve 20-40 doubly, reach the hardness of natural diamond, form nickel-base alloy ultrahigh hardness surface, surface is made up of nano twin crystal, nano twin crystal forms array by the twin sheet of a thickness >=15nm with the twin sheet of one or several <15nm and forms, 100 CYCLIC LOADING can be born simultaneously, load rear surface flawless, as excellent as before, maintain plasticity.
Sample is nickel-base alloy.Nickel-base alloy is widely used in Aeronautics and Astronautics, ocean, nuclear power, chemical line transport, the field such as superalloy, corrosion-resisting alloy, it is the high material of a kind of added value, also be widely used engineering materials, plate, line, tubing can be made, except the demand of the high leading-edge field of satisfied country, the product for civilian use also there is demand widely.Therefore, select nickel-base alloy as starting material, there is great future in engineering applications.
The raw material of Diamond tip is natural diamond, the method for the fixing employing hight frequency welding of Diamond tip and the body of rod, with Ni-based and Co-based alloy powder as melting material.The extreme hardness of natural diamond, the impurity that the inside is contained is considerably less, and purity is high, is therefore elected to be the starting material of nano impression needle point.Due to circulation impression load many times will be born, therefore select the natural diamond of 1mm size.According to the texture of natural diamond, select the hardest (111) face as impression face, and mark of marking.45# steel pole body is got out a duck eye, is of a size of adamantine twice, fill with nickel-base alloy or Co-based alloy powder in gap, graphite rod gets out an aperture more bigger than diamond, pushes down diamond.Adopt the method melting of hight frequency welding to fill powder, diamond is fixed on the body of rod.
Adopt the method for superfine grinding and soft steel polishing to manufacture submicron radius-of-curvature Diamond tip, the radius-of-curvature of needle point is 200-900nm, and projection angle is 90-150 °, and shape is triprismo or rectangular pyramid.Adopt the method processing submicron radius-of-curvature Diamond tip of superfine grinding.Natural diamond is fixed in dividing apparatus, the grinding rotating speed of emery wheel is 3000-5000rpm, and grit size is followed successively by 40,20,5 μm, is resin anchoring agent diamond grinding wheel, final superfine grinding wheel is Technique of Vitrified Diamond Wheels, and the grit size of emery wheel is 2 μm.The grinding depth of emery wheel is 1-10 μm/min.After superfine grinding completes, 15# steel is adopted to carry out polishing.15# steel is soft steel, and diamond cutter can not be used for machined steel iron material, especially at high temperature.This programme utilizes the unfavorable character of diamond at high temperature easily carbonization to carry out polishing just.The rotating speed of emery wheel is 5000rpm, and grinding and feeding amount is 200-500nm/min.The grinding heat utilizing emery wheel and Diamond tip to produce, makes the carbon atom of Diamond tip permeate to soft steel, realizes the polishing on Diamond tip surface, thus make Diamond tip sharp, smooth surface.Adopt the combined method of superfine grinding and soft steel polishing can obtain submicron radius-of-curvature Diamond tip.Consider the wear resistance of needle point, the projection angle of needle point is 90-150 °, and the radius-of-curvature of needle point is 200-900nm.Because leg-of-mutton shape is very firm, therefore impression is preferably the pattern of trilateral composition, therefore elects needlepoint form as triprismo or rectangular pyramid.
Be installed on by Diamond tip on nano-hardness tester or microhardness tester, impress, load is 0.2-2N, and the loading time is 1-10s, and hold time is 1-5s, and discharge time is 1-5s.The body of rod of Diamond tip is processed into the shape of the needle point needed for nano-hardness tester or microhardness tester, then the body of rod of Diamond tip is installed on nano-hardness tester or microhardness tester, impresses.Because the formation of nano twin crystal needs critical stress, therefore only nano twin crystal could be produced under certain load, and load is excessive, also unfavorable to formation nano twin crystal, hardness is caused to reduce, by experiment, the nickel-base alloy surface hardness that load is formed within the scope of 0.2-2N is the highest, therefore selects 0.2-2N to be loaded load.Also there is important impact loading time on the formation of nano twin crystal, and consider imprint time and effect, the selection loading time is 1-10s, and hold time is 1-5s, and discharge time is 1-5s.
The miles of relative movement in the horizontal and vertical direction of setting Diamond tip is impression size, impress nickel-base alloy surface successively, behind the full surface of triprismo needle point pressure, by rotary sample 180 °, the miles of relative movement in needle point horizontal and vertical direction is similarly impression size, impress in gap, the full nickel-base alloy surface of pressure.Select suitable load to impress, watch the size of impression under an optical microscope, according to the impression miles of relative movement in this size setting needle point horizontal and vertical direction, impress, observe stamping surface after impression more whether to meet the requirements, then slightly adjust, until select suitable distance.Then Lookup protocol impression is carried out, the full nickel-base alloy surface of impression.After using the needle point of triprismo to carry out single impression, there is the space of a needle point in every two needle points, behind the full surface of pressure, by rotary sample 180 degree, then arranges the same miles of relative movement of horizontal and vertical, impress in gap, can press completely whole surface.
After having impressed, by same load in embossed locations tested for hardness, the more former alloy of hardness on surface can improve 20-40 doubly, reaches 100-120GPa.After having impressed, same needle point is adopted to carry out hardness test in impression, find that loading and unloading curve can significantly move to left, this is because sub-surface defines nano-twin crystal structure, hardness can reach 100-120GPa, more former alloy can improve hardness 20-40 doubly, reaches the hardness of natural diamond, forms nickel-base alloy ultrahigh hardness surface.
Nickel-base alloy ultrahigh hardness surface is made up of nano twin crystal, and nano twin crystal forms array by the twin sheet of a thickness >=15nm with the twin sheet of one or several <15nm and forms, and nano twin crystal has the unidirectional continuous feature without crystal boundary.Play hardening effect during twin size >=15nm, and play bating effect during twin size <15nm.The twin with sclerosis and bating effect can produce synergy, thus hardness is increased substantially.Nano twin crystal forms array by the twin sheet of a thickness >=15nm with the twin sheet of one or several <15nm, it is a kind of novel nano-twin crystal structure, and there is the unidirectional continuous feature without crystal boundary, can hardness fast lifting be made.
100 CYCLIC LOADING can be born in nickel-base alloy ultrahigh hardness surface, load rear surface flawless.Nickel-base alloy nano twin crystal is made up of the twin array with sclerosis and bating effect, when being subject to loading stress, can form new twin to reduce stress, resistance to deformation, improve hardness, when unloaded, twin can occur to separate twinning, thus make the volume of twin and the quantity overall stability of twin, therefore, this novel nano twin structure can bear the cyclic loading of 100 times, and surface does not have crackle, as excellent as before, maintain plasticity.
Effect of the present invention and benefit achieve nickel-base alloy nano twin crystal ultrahigh hardness table surface forming method, with Diamond tip as instrument, adopts the method for nano impression to form nickel-base alloy nano twin crystal ultrahigh hardness surface.
Embodiment
The specific embodiment of the present invention is described in detail below in conjunction with technical scheme.
Select nickel ternary chrome molybdenum, main component is (wt.%) Ni56-Cr23-Mo16.The hardness of alloy is 2.6-3.0GPa.Alloy is of a size of 10 × 10 × 1mm
3, grinding and chemically machinery polished after, through acetone and sherwood oil ultrasonic cleaning, after spontaneous evaporation, the surface roughness Ra of the nickel-base alloy that U.S. Zygo noncontact contourgraph Newview5022 records is 1.2nm.Nickel-base alloy sheet to be gluingly connected on the round steel sheet of nano-hardness tester TI950 with 502, to be placed in the sample table of nano-hardness tester, to be fixed in sample table by the mode of magnetic-adsorption.
Natural diamond selected by the starting material of Diamond tip, is of a size of 1mm.According to the texture of natural diamond, select the hardest (111) face as impression face, and use marked.On the body of rod top of 45# steel, the aperture of a drilling diameter 2mm, puts into diamond wherein, and hole place nickel-base alloy fills up.By the aperture of a graphite rod drilling 1.2mm, push down the index face of natural diamond.The method of hight frequency welding is adopted to be fixed on the body of rod of 45# steel by Diamond tip.With dividing apparatus according to 120 ° of calibration, Diamond tip is ground to triangular pyramid shape.Select grit size to be 40,20 successively, the resin bond wheel grinding Diamond tip of 5 μm, grinding wheel speed is 5000rpm, and the amount of feed is followed successively by 10,5,2 μm/min.Final utilization grit size is the Technique of Vitrified Diamond Wheels grinding Diamond tip of 2 μm, and grinding wheel speed is 5000rpm, and the amount of feed is 1 μm/min.Then 15# soft steel is adopted to carry out polishing.Grinding wheel speed is 5000rpm, and the amount of feed is 400nm/min.Diamond tip radius-of-curvature after grinding and soft steel polishing is 395nm, and projection angle is 139 °, is similar to the shape and size of Berkovich needle point, therefore carries out hardness test according to Berkovich needle point.45# steel pole body is processed into the business needle point body of rod size of TI950, is installed on TI950 nano-hardness tester and carries out nano impression.Loading time is 2s, and hold time is 1s, and discharge time is 2s, and load selects 1N, by pressure testing, impression is of a size of 31 μm, considers the nano twin crystal of indentation edge, the distance of horizontal and vertical is set as 35 μm, after TI950 programmes, is impressed by nano-hardness tester.After once having impressed, by rotary sample 180 °, carry out secondary impression in the gap of impression, the distance of horizontal and vertical is still set as 35 μm, after performing secondary impression, the surface of the full nickel-base alloy of pressure, the surface being covered with impression of the final nickel-base alloy obtained is 2.6 square millimeters.Measure hardness at impression place, the loading time is 5s, and hold time is 2s, and discharge time is 5s, and hardness value is 105GPa, is 35 times (former alloy rigidity is 2.6-3.0GPa) of former alloy, reaches the hardness of natural diamond.Carry out 100 CYCLIC LOADING at impression position, each loading time is 2s, and hold time is 1s, and discharge time is 2s.After 100 times CYCLIC LOADING completes, sweep in Electronic Speculum FEI Quanta 200 at Flied emission ring and characterize, surperficial flawless, as excellent as before, maintain good plasticity.
Nickel-base alloy ultrahigh hardness surface sample is placed in FEI Helios600i Focused Ion Beam instrument, ionic fluid cutting is carried out in indentation edge, after having cut, be welded on the special small copper ring of transmission electron microscope with gripper of manipulator sample thief, copper ring external diameter is 3mm, internal diameter is 1mm, then cuts, and forms sample for use in transmitted electron microscope.Carry out ion milling subsequently, in order to drop to minimum by the damage of ion milling, the voltage and current value adopted successively is 30kV, 2.5nA; 30kV, 83pA; 16kV, 0.13nA; 8kV, 61pA; 5kV, 43pA; 2kV, 25pA.When sample is reduced to enough thin, sample is taken out from focused ion beam vacuum chamber, be put in transmission electron microscope and carry out testing and characterizing.First be put in FEI F20 transmission electron microscope, acceleration voltage is 200kV.In transmission electron microscope, adopting selected area electron diffraction method, found the spot of two point array, is the characteristic feature of nano twin crystal.Nickel-base alloy ultrahigh hardness surface is made up of nano twin crystal, the twin of a 22nm is close to the little twin of a 3nm, opposite side is the twin of a 3.5nm, the twin of adjacent an is 3.5nm, then being the twin of 4nm, is the twin of a 5nm, by the twin of a 16nm subsequently, by the twin of a 3nm, by the twin of a 8nm.Form a twin by thickness >=15nm, twin array by one or several < 15nm forms, forming the twin array with sclerosis and softening synergy, and have the unidirectional continuous feature without crystal boundary, is a kind of novel nickel-base alloy nano-twin crystal structure.In order to obtain atomic response more clearly, sample being put in JOEL ARM200F transmission electron microscope and characterizing, found that the thickness of high-resolution is the atomic lattice picture of the nano twin crystal of 5nm.
Thus this experiment completes a kind of nickel-base alloy nano twin crystal ultrahigh hardness table surface forming method.
Claims (1)
1. a nickel-base alloy nano twin crystal ultrahigh hardness table surface forming method, with Diamond tip as instrument, adopts the method for nano impression to form nickel-base alloy nano twin crystal ultrahigh hardness surface, it is characterized in that:
(1) sample is nickel-base alloy;
(2) raw material of Diamond tip is natural diamond, the method for the fixing employing hight frequency welding of Diamond tip and the body of rod, with Ni-based and Co-based alloy powder as melting material;
(3) adopt the method for superfine grinding and soft steel polishing to manufacture submicron radius-of-curvature Diamond tip, the radius-of-curvature of needle point is 200-900nm, and projection angle is 90-150 °, and shape is triprismo or rectangular pyramid;
(4) be installed on nano-hardness tester or microhardness tester by Diamond tip, impress, load is 0.2-2N, and the loading time is 1-10s, and hold time is 1-5s, and discharge time is 1-5s;
(5) miles of relative movement setting the horizontal and vertical direction of Diamond tip is impression size, impress nickel-base alloy surface successively, behind the full surface of triprismo needle point pressure, by rotary sample 180 °, the miles of relative movement in needle point horizontal and vertical direction is similarly impression size, impress in gap, the full nickel-base alloy surface of pressure;
(6) after having impressed, by same load in embossed locations tested for hardness, the more former alloy of hardness on surface can improve 20-40 doubly, reaches 100-120GPa;
(7) nickel-base alloy ultrahigh hardness surface is made up of nano twin crystal, nano twin crystal forms array by the twin sheet of a thickness >=15nm with the twin sheet of one or several <15nm and forms, and nano twin crystal has the unidirectional continuous feature without crystal boundary;
(8) 100 CYCLIC LOADING can be born in nickel-base alloy ultrahigh hardness surface, load rear surface flawless.
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Cited By (6)
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| CN105463402A (en) * | 2015-11-18 | 2016-04-06 | 大连理工大学 | Nanometer twin crystallization surface manufacturing method for diamond needle tip array template coining |
| CN105823659A (en) * | 2016-03-15 | 2016-08-03 | 南昌航空大学 | Manufacturing technology of test block for comparison of micro cracks in thermal barrier coating of engine blade |
| CN107621471A (en) * | 2017-08-28 | 2018-01-23 | 大连理工大学 | Micron alloy contains the transmission electron microscope in-situ nano creasing method of isometric single nano twin crystal |
| CN110373708A (en) * | 2019-07-31 | 2019-10-25 | 东南大学 | Adjustable concentration realizes that the nanometer pinpoint of needle point cone angle control prepares platform and method |
| CN111850624A (en) * | 2019-04-24 | 2020-10-30 | 中国科学院金属研究所 | Nano twin crystal nickel with extremely small twin crystal lamella thickness and ultrahigh strength and preparation thereof |
| CN113308627A (en) * | 2020-02-27 | 2021-08-27 | 南京理工大学 | Nickel-based alloy containing carbide and nano twin crystal composite structure and preparation method thereof |
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| CN105463402A (en) * | 2015-11-18 | 2016-04-06 | 大连理工大学 | Nanometer twin crystallization surface manufacturing method for diamond needle tip array template coining |
| CN105823659A (en) * | 2016-03-15 | 2016-08-03 | 南昌航空大学 | Manufacturing technology of test block for comparison of micro cracks in thermal barrier coating of engine blade |
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