CN103862049A - Ni-Ti porous material mini-sized part and sintering method thereof - Google Patents
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Abstract
The invention discloses a Ni-Ti porous material mini-sized part sintered in an activated mode and prepared on the basis of a multi-physics field and a sintering method thereof. According to the method, metallic nickel Ni powder and metallic titanium Ti powder are weighed, fixed and filled into a die; then the die filled with Ni-Ti mixed powder is energized with alternating currents for quick heating under the conditions that the vacuum degree is smaller than or equal to 0.01Pa and the two ends of the die are applied with action force of 50-150MPa, wherein the electric field constant temperature sintering method or the electric heating fluctuation sintering method can be used as the heating technology. After the mixed powder form a shape in the die, the part can be taken out after power off and air cooling. According to the Ni-Ti porous material mini-sized part and the sintering method thereof, technology processes are simplified, the forming process is easy to control, the sintering process is free of pollution, sintering time is shortened, sintering temperature is reduced, and production quality is improved.
Description
Technical field
The present invention relates to Ni-Ti porous material miniature parts and sintering method thereof that based on multiple physical field prepared by activated sintering, belong to the technical field that Fast Sintering is prepared porous material part.
Background technology
Ni-Ti porous material miniature parts relies on its excellent biocompatibility, unique shape memory characteristic, super-elasticity and decay resistance to receive much concern in biologic medical field in the last few years.Research shows, loose structure can promote the regeneration of organism skeletal tissue, nutriment exchange and medicament transmission.Meanwhile, by the control to hole relevant parameter, make porous marmem can, by adjusting hardness and intensity, adapt to better bone environment around when as embedded material.Be expected to be applied to hard tissue substituting material and Srgery grafting material.Microcellular structures a large amount of in Ni-Ti porous material miniature parts make it have the damping characteristic higher than common metal material with the crystal boundary (comprising twin-plane boundary etc.) of the interior enormous amount of tissue, can be used as high damping material and make damping device.Super-elasticity (being also the called visually rubber elasticity) characteristic of marmem also makes it have good damping action and energy absorption. simultaneously, as porous material, its loose structure also can provide intrinsic damping characteristic, the scattering power of raising shock wave.At present, the preparation method of Ni-Ti porous material miniature parts has multiple, mainly contains combustion synthesis method, element powders mixed-sintering method, pre-alloyed powder sintering process and hot isostatic pressing method etc.In several preparation methods, be all first by Ni, Ti element mixed-powder high-energy ball milling, then finally obtain porous marmem through certain processing.
The employing self propagating high temperature synthetic methods such as Wang Xuecheng are prepared Ni-Ti porous material miniature parts, the method technique is simple, and has large porosity and porosity, but due to its anisotropic distribution of pores, mechanical performance is poor, and the course of reaction of technique and properties of product are difficult to control.
HIP sintering is a kind of comparatively desirable technique of preparing at present Ni-Ti porous material miniature parts.In the container of a special construction, processing component is applied to high pressure and high temperature carries out sintering simultaneously, under such heat and pressure condition, the defect (such as crackle and hole) in parts can be eliminated substantially.
Several preparation methods easily make Powder Oxidation and absorption impurity in mechanical milling process above, and are vulnerable to the pollution of ball grinder and abrading-ball, cause the existence of some impurity phases, and SME and super-elasticity are affected, and recovery of shape rate declines.
Micro shaping technology is a kind of emerging technology that only has more than ten years history, is different from traditional manufacturing process because its accessory size is small.At present, prepare miniature parts both at home and abroad and mainly contain micro-precision casting process, micro injection molding technology, Plastic Microforming Technology and traditional vacuum sintering technique etc.But these process technology present stages are all mainly used in the production of single and mini-batch production, in most cases production cost not only high and cannot meet that miniature parts is in enormous quantities, high efficiency, free of contamination manufacture requirement.
Summary of the invention
For current preparation Ni-Ti porous material miniature parts problem and shortage, such as, complex procedures, manufacturing cycle is long, forming temperature is high, product percent of pass is low, the dependence of raw material to additive and cause product purity not high, causes certain pollution etc. to environment; And have no the research of porous material in micro shaping theory, technical problem solved by the invention is to provide a kind of method that multiple physical field activated sintering micro shaping technology is prepared porous Ni-Ti porous material miniature parts fast, and the method great advantage is exactly that preparation time is short.
The sintering method of Ni-Ti porous material miniature parts of the present invention comprises the following steps:
A, will metal nickel, Titanium Ti powder weighing fills in mould after mixing, wherein, Ni, Ti mass percent are that Ni45-55%, Ti55-45%(preferable range are Ni49-51%, Ti51-49%); Ni, Ti particle size range are 500nm～70 μ m;
B, at vacuum≤0.01Pa, impose under the condition of 50～150MPa active force in both mold ends simultaneously, the mould indirect current that Ni, Ti mixed-powder are housed is carried out to instant heating:
Wherein, heating process is two kinds:
The first is electric field constant temperature sintering: the first step is heated to 100～300 ℃ of insulation 0～120s with 10～50 ℃/s, second step with 10～125 ℃/be incubated 0～14 minute while being heated to 500～1200 ℃;
The second is electric heating fluctuating sintering: the first step is heated to 100～300 ℃ of insulation 0～120s with 10～50 ℃/s, and second step is warming up to 800～1200 ℃ with the speed of 10～125 ℃/s, rises and falls 1～15 time 1200～400 ℃ of scopes;
C, mixed-powder are after die for molding, and power-off air cooling takes out part.
Further preferably, Ni described in steps A, Ti particle size range are 50 μ m～70 μ m; Ni, Ti granularity be 50 μ m most preferably.
Further preferably, in the heating process in step B: the programming rate of the first step is 10～20 ℃/s, the programming rate of second step is 50～100 ℃/s.
Further preferably, in step B, in the first electric field constant temperature sintering process, the temperature retention time of second step is 3～8 minutes.
Further preferably, in step B, the fluctuating temperature range of the second electric heating fluctuating sintering process is 1200～400 ℃, and the stage programming rate that rises and falls is 30～100 ℃/s, and cooling rate is 10～50 ℃/s.
Further preferably, in step B, the temperature fluctuation scope of the second electric heating fluctuating sintering process is 1200～800 ℃, and fluctuating number of times is 5～10 times.
Further preferably, in step B, in the second electric heating fluctuating sintering process, the sintering temperature of second step is 900～1100 ℃.
Further preferably, step B applied external force is 75～100MPa.
Further preferably, the condition of AC electric-heating in step B: voltage is 3～10V, electric current is 3000～30000A.
The present invention adopts electric field constant temperature sintering and two kinds of techniques of electric heating fluctuating sintering, generates triangle and cylindrical two kinds of products, also can need to prepare according to practical application the shape of needs.
The Ni-Ti porous material miniature parts that adopts the method for the invention to obtain, has finished product crystal grain tiny, becomes porosity high, the advantage of porous nickel, and without anisotropic distribution of pores, overcome the poor defect of product mechanical performance in the past.
The inventive method compared with prior art, has the following advantages:
1, simplified technological process.The inventive method is in sintering process, and powder is without being pressed in advance base, and in sintering process, mould heats, pressurizes together with powder, reduces green compact pressing process.In addition,, under the condition of large electric current, low-voltage, only several seconds or tens of seconds can complete sintering, have greatly shortened manufacturing cycle.
2, shortened preparation time.While adopting the inventive method to prepare Ni-Ti porous miniature parts, powder systems is Fast Sintering moulding under the coupling in electric field, the field of force and temperature field, programming rate reaches as high as 125 ℃/s, be much higher than the conventional sintering programming rate of 5 ℃/min left and right, and later stage temperature retention time is short, so the inventive method can realize the sinter molding of Ni, Ti powder in 20 seconds～16 minutes, thereby the heating-up time of part and preparation time are all significantly shortened.
3, optimized product quality.Due to the present invention, to realize sintering velocity fast, complete sintering process, and electric field action is even within the utmost point short time, can reduce to greatest extent alloying component segregation, and finished product crystal grain is tiny, becomes porosity high, porous nickel, excellent performance.
4, forming process is easy to control.Because the inventive method can be by regulating the technological parameters such as electric current, programming rate, sintering temperature, active force and temperature retention time, control flexibly and easily the forming process of part, thereby solved existing correlation technique very difficult problem that multiple technological parameters are controlled constantly in the preparation process of titanium parts.
5, process is pollution-free.The present invention adopts direct-electrifying mode to carry out instant heating to metal dust, not only realizes the Fast Sintering in the utmost point short time, realizes high efficiency, low power consuming; And broken away from dependences such as additives, production process meets the requirement of " green production ".
Accompanying drawing explanation
Fig. 1 the inventive method sintering Preparation equipment is to being arranged in the metal dust energising heating of mould sintering and the schematic diagram of the mode of exerting pressure
Fig. 2 the inventive method mould is in the simplified schematic diagram of the continuous action in electric field and the field of force
Wherein, 1 is die, and 2 is sintered powder, and 3 is punch.
The specific embodiment
The specific embodiment of form by the following examples, is described in further detail foregoing of the present invention again, illustrates but does not limit the present invention.
The sintering Preparation equipment that following examples adopt is the Gleeble-1500D thermal simulation machine of U.S. DSI science and technology association development.The granularity of Ni and Ti and addition parameter are as follows:
| ? | (μ m) for order number | Fusing point (℃) | Density (g/cm 3） | Mixed weight percentage (%) |
| Ni | 50 | 1452 | 8.902 | 49.2 |
| Ti | 50 | 1688 | 4.450 | 50.8 |
Embodiment 1
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 50MPa, be warming up to 200 ℃ with the speed of 10 ℃/s, after insulation 30s, be warming up to 800 ℃ with the speed of 50 ℃/s subsequently, sintering 3 times rises and falls within the scope of 800 ℃-400 ℃; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 2
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 150MPa, be warming up to 300 ℃ with the speed of 20 ℃/s, after insulation 120s, be warming up to 1200 ℃ with the speed of 100 ℃/s subsequently, sintering 15 times rises and falls within the scope of 1200 ℃-800 ℃; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 3
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 150MPa, be warming up to 200 ℃ with the speed of 20 ℃/s, after insulation 60s, be warming up to 1000 ℃ with the speed of 50 ℃/s subsequently, sintering 5 times rises and falls within the scope of 1000 ℃-600 ℃; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 4
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 96MPa, be warming up to 150 ℃ with the speed of 10 ℃/s, after insulation 60s, be warming up to 1200 ℃ with the speed of 100 ℃/s subsequently, 1200 ℃ of insulations 14 minutes; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 5
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 100MPa, be warming up to 200 ℃ with the speed of 10 ℃/s, after insulation 120s, be warming up to 800 ℃ with the speed of 100 ℃/s subsequently, 800 ℃ of insulations 5 minutes; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 6
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 100MPa, be warming up to 200 ℃ with the speed of 10 ℃/s, after insulation 30s, be warming up to 1000 ℃ with the speed of 50 ℃/s subsequently, 1000 ℃ of insulations 10 minutes; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 7
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 125MPa, be warming up to 300 ℃ with the speed of 10 ℃/s, after insulation 120s, be warming up to 1100 ℃ with the speed of 50 ℃/s subsequently, sintering 15 times rises and falls within the scope of 1100 ℃-700 ℃; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 8
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 150MPa, be warming up to 200 ℃ with the speed of 10 ℃/s, after insulation 30s, be warming up to 1100 ℃ with the speed of 100 ℃/s subsequently, sintering 5 times rises and falls within the scope of 1100 ℃-700 ℃; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Embodiment 9
After Ni shown in upper table, Ti powder are weighed by precasting process parameter, packing mould chuck into fixes, the vacuum of≤0.01Pa and simultaneously two ends apply under the pressure condition of 85MPa, be warming up to 200 ℃ with the speed of 10 ℃/s, after insulation 30s, be warming up to 1200 ℃ with the speed of 150 ℃/s subsequently, sintering 15 times rises and falls within the scope of 1200 ℃-800 ℃; Powder is in die for molding and complete sintering, and last power-off air cooling takes out part.
Through observing, the crystal grain that embodiment 1-9 prepares gained Ni-Ti porous material miniature parts finished product is tiny, becomes porosity high, porous nickel.Gained Ni-Ti porous material miniature parts of the present invention, without anisotropic distribution of pores, has overcome the poor defect of product mechanical performance in the past.
To sum up, due to increasing substantially of the inventive method programming rate, aggravate interatomic diffusion, make metal dust more easily be molten state, in addition be applied with pressure in both mold ends again, not only make pressed compact moulding and compactness sintering carry out simultaneously, also suppressed growing up of crystal grain, can obtain ultra-fine grain structure, guarantee the performance after part microminiaturization.The present invention has simplified technological process, and forming process is easy to control, sintering process is pollution-free, shortened sintering time, reduced sintering temperature, improved product quality.The inventive method is simple, and site technique workflow reengineering is convenient, and feasibility is strong, and application prospect is wide.
Claims (10)
- The sintering method of 1.Ni-Ti porous material miniature parts, is characterized in that: step is as follows:A, will metal nickel, Titanium Ti powder weighing fills in mould after mixing, wherein, Ni, Ti mass percent are Ni45-55%, Ti55-45%; Ni, Ti particle size range are 500nm～70 μ m;Wherein, Ni, the preferred Ni49-51% of Ti mass percent, Ti49-51% described in steps A;B, at vacuum≤0.01Pa, impose under the condition of 50～150MPa active force in both mold ends simultaneously, the mould indirect current that Ni, Ti mixed-powder are housed is carried out to instant heating:Wherein, heating process is two kinds:To be the first step be heated to 100～300 ℃ of insulation 0～120s with 10～50 ℃/s to the first, second step with 10～125 ℃/be incubated 0～14 minute while being heated to 500～1200 ℃;The second is that the first step is heated to 100～300 ℃ of insulation 0～120s with 10～50 ℃/s, and second step is warming up to 800～1200 ℃ with the speed of 10～125 ℃/s, rises and falls 1～15 time 1200～400 ℃ of scopes;C, mixed-powder are after die for molding, and power-off air cooling takes out part.
- 2. method according to claim 1, is characterized in that: described in steps A, Ni, Ti particle size range are 50 μ m～70 μ m; Preferably, described in steps A, Ni, Ti granularity are 50 μ m.
- 3. the sintering method of Ni-Ti porous material miniature parts according to claim 1, is characterized in that: in the heating process in described step B: the programming rate of the first step is 10～20 ℃/s, and the programming rate of second step is 50～100 ℃/s.
- 4. the sintering method of Ni-Ti porous material miniature parts according to claim 1, is characterized in that: described in step B, in the first electric field constant temperature sintering process, the temperature retention time of second step is 3～8 minutes.
- 5. the sintering method of Ni-Ti porous material miniature parts according to claim 1, it is characterized in that: in step B, the second electric heating fluctuating technique mesorelief temperature range is 1200～400 ℃, and the stage programming rate that rises and falls is 30～100 ℃/s, and cooling rate is 10～50 ℃/s.
- 6. the sintering method of Ni-Ti porous material miniature parts according to claim 1 or 5, is characterized in that: in step B, the temperature fluctuation scope of the second electric heating fluctuating sintering process is 1200～800 ℃, and fluctuating number of times is 5～10 times.
- 7. according to the sintering method of the Ni-Ti porous material miniature parts described in claim 1 or 6, it is characterized in that: in step B, in the second electric heating fluctuating technique, the sintering temperature of second step is 900～1100 ℃.
- 8. the sintering method of Ni-Ti porous material miniature parts according to claim 1, is characterized in that: the additional active force of step B is 75～100MPa.
- 9. the sintering method of Ni-Ti porous material miniature parts according to claim 1, is characterized in that: the condition of AC electric-heating in step B: voltage is 3～10V, and electric current is 3000～30000A.
- 10. the Ni-Ti porous material miniature parts of being prepared by the sintering method described in claim 1-9 any one.
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| CN104874796A (en) * | 2015-05-21 | 2015-09-02 | 四川大学 | WC-Ni mini-type component prepared based on multi-physics field activated sintering and preparing method of WC-Ni mini-type component |
| CN108941536A (en) * | 2018-08-09 | 2018-12-07 | 四川大学 | The near net manufacturing method and Miniature ultrasonic motor rotor of Ti alloy miniature part |
| CN109079135A (en) * | 2018-08-09 | 2018-12-25 | 四川大学 | Method based on multiple physical field activated sintering preparation Miniature ultrasonic motor stator |
| CN113588390A (en) * | 2021-07-16 | 2021-11-02 | 四川大学 | Method for in-situ TiC generation in titanium-based micro part |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104874796A (en) * | 2015-05-21 | 2015-09-02 | 四川大学 | WC-Ni mini-type component prepared based on multi-physics field activated sintering and preparing method of WC-Ni mini-type component |
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| CN108941536A (en) * | 2018-08-09 | 2018-12-07 | 四川大学 | The near net manufacturing method and Miniature ultrasonic motor rotor of Ti alloy miniature part |
| CN109079135A (en) * | 2018-08-09 | 2018-12-25 | 四川大学 | Method based on multiple physical field activated sintering preparation Miniature ultrasonic motor stator |
| CN113588390A (en) * | 2021-07-16 | 2021-11-02 | 四川大学 | Method for in-situ TiC generation in titanium-based micro part |
| CN113588390B (en) * | 2021-07-16 | 2022-11-15 | 四川大学 | Method for in-situ TiC generation in titanium-based micro part |
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