CN103447530A - Method for preparing pure titanium miniature parts on basis of multi-physical-field activated sintering - Google Patents
Method for preparing pure titanium miniature parts on basis of multi-physical-field activated sintering Download PDFInfo
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Abstract
The invention discloses a method for preparing pure titanium miniature parts on the basis of multi-physical-field activated sintering. According to the method, pure titanium powder is weighed and is then filled into a mold, then, alternating current is introduced into the mold containing the titanium powder for carrying out fast heating under the sintering conditions that the temperature rise speed is 25 to 125 DEG C/s, and the vacuum degree is smaller than or equal to 0.01Pa, meanwhile, the acting force being 10 to 200MPa is exerted to the two ends of the mold, under the continuous effect of an electric field and a force field, the heat insulation is carried out for 0 to 10 minutes when the mold is heated to 800 to 1200 DEG C so that the titanium powder is formed in the mold, finally, the power is cut off, and the parts are cooled in the air and are then taken out. The method has the advantages that the technical flow process is simplified, the forming process can be easily controlled, no pollution is caused in the sintering process, the sintering time is shortened, the sintering temperature is lowered, and the product quality is improved.
Description
Technical field
The present invention relates to the method that based on multiple physical field activated sintering prepares pure titanium miniature parts, belong to the technical field that Fast Sintering prepares pure titanium miniature parts.
Background technology
In the later stage eighties 20th century, machinery manufacturing industry has started a technological revolution in the world, and product is towards microminiaturized future development.Swift and violent the increasing of the demand of microminiaturized product makes micro-forming technique have broad application prospects in bioscience, information, Aero-Space, national defence, industry, agricultural, traffic, new forms of energy and family etc.Titanium have specific strength high, corrosion-resistant, without advantages such as magnetic, superconduction, shape memory, good biocompatibilities, be described as " space metal ", " marine metal " and " wisdom metal ", be particularly suitable as structural material and special material and use.In modern military application field, the maximum of application are miniplane, microsensor, wireless communication signal processor etc., and wherein the titanium miniature parts is these miniature standby vital parts of preparation.Learn field at modern biologic medical, requisite medical device when mini Titanium plate for treatment, minitype titanium screw and Miniscrew etc. become the skeleton treatment.But with materials such as stainless steel, copper, nickel, compare, the price of titanium products is obviously higher.At present numerous for the preparation method of titanium or titanium alloy, but preparing the method for minitype titanium product, processing rarely has report, this has greatly affected the promotion and application of minitype titanium part at modern industry.
The people such as Li Baogan provide a kind of titanium or titanium alloy powder metallurgy special-shaped pieces preparation method in Chinese patent CN102407337A, the method has solved profiled piece goods internal porosity and density problem on the low side, has improved physical property and the chemical property of profiled piece goods.But technical process comprises: choose raw material-hydrogenation-ball milling-making rubber soft mold-by the powder rubber soft mold-steps such as isostatic cool pressing die cast-vacuum-sintering of packing into.Due to complex technical process, the precision of product is controlled to difficulty and strengthen.
The real titanium new material development in science and technology Co., Ltd in Harbin method by hot investment casting in Chinese patent CN102294436A prepares titanium alloy and titanium-aluminium alloy.The method has solved cast(ing) surface and the poor technical problem of internal soundness of the method for existing employing fused alumina, Ludox reduction titanium alloy and titanium-aluminium alloy precision-investment casting cost.But need to use the chemical reagent such as zirconium colloidal sol, Ludox, wetting agent jfc, n-octyl alcohol while in technical process, preparing investment precoat.Also need to obtain shell after dewaxing, sintering, so the method has been polluted titanium products itself to a certain extent, environment is also had to negative impact.
The people such as Weiqiang have prepared the titanium filter core material by microwave sintering in Chinese patent CN102808102A, and the porosity of prepared porous titanium material is up to 60%.Although the method has reduced sintering temperature to a certain extent, has shortened sintering time, has reduced production cost.But the productivity ratio concerning the product mass of the sintering time about 1 hour is still lower, and the compacting link that technical process comprises green compact, can idiosome by good sintering, depend on to a great extent the initial density of pressed compact, initial density is lower, the final densified sintering product of sample is poorer, and its corresponding physical and chemical performance and mechanical property also will be greatly affected.
At present, numerous for the preparation method of titanium or titanium alloy, but the preparation method of minitype titanium part is rarely had to report.
Summary of the invention
The objective of the invention is to rarely have for current titanium miniature parts preparation method the present situation of report; And the preparation present situation of titanium or titanium alloy product, such as complex procedures, manufacturing cycle is long, forming temperature is high, product percent of pass is low, raw material to the dependence of additive and cause product purity not high, cause certain defects such as pollution to environment.And provide, a kind of based on multiple physical field, activated sintering prepares the method for pure titanium miniature parts.
Purpose of the present invention is realized by following technical measures:
It is a kind of that based on multiple physical field, activated sintering prepares the method for pure titanium miniature parts, the method is to fill in mould after pure titanium powder is weighed, then at programming rate, be 25～125 ℃/s, under the sintering condition of vacuum≤0.01Pa, the mould indirect current that titanium powder is housed is carried out to instant heating, impose the active force of 10～200MPa in both mold ends simultaneously, under the continuous action in electric field and the field of force, when being heated to 800～1200 ℃, insulation makes titanium powder in die for molding in 0～10 minute, and the air cooling that finally cuts off the power supply takes out part and gets final product.
Described method, the programming rate of the method is 25～125 ℃/s.
Described method, the sintering temperature of the method is 900～1000 ℃.
Described method, the applied force of the method is 50～100MPa.
Described method, it is after sintering temperature reaches preset temperature, sintered body to be carried out to insulation in 4～6 minutes to process that the method is carried out the insulation of sintering later stage.
Described method, the method adopts AC electric-heating, and wherein voltage is 3～10V, and electric current is 3000～30000A.
Performance test
1, relative density preparation method.At first adopt the TP-214 assay balance that precision is 0.0001g to be measured, utilize formula
calculate the actual density of titanium sintered specimen, recycling
calculate the relative density of titanium sintering sample.
2, hardness detects and carries out according to GB/T4340.1-1999, adopts the HV-1000 Vickers to be detected, and setting load is 100g, and the load time is 15s, at 5 diverse locations of sample, surveys hardness, gets its mean value.
The present invention compared with prior art, has the following advantages:
1, simplified technological process.Because the inventive method is that load weighted pure titanium powder is filled in mould, direct sintering moulding under the coupling in electric field, the field of force and temperature field, reduced the operation of making green compact.The inventive method has solved when prior powder metallurgy prepares the titanium or titanium alloy part, and the product quality height depends on the problem of green density.Titanium miniature parts prepared by the inventive method has not only improved product quality, has also greatly shortened manufacturing cycle.
2, 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 a plurality of technological parameters are controlled constantly in the preparation process of titanium parts.
3, sintering process is pollution-free.Due to the inventive method without add the additives such as rubber or paraffin in the titanium powder system, without as investment casting method, in the sintering process of titanium valve, powder being carried out to the degreasing degraded.The inventive method has shortened manufacturing cycle greatly, pollution-free, and the utilization rate of material is high.Meet the requirement of " green production ".
4, shortened sintering time.While adopting the inventive method to prepare the titanium 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 200 ℃/s, the conventional sintering programming rate that is much higher than 5 ℃/min left and right, due to powder systems be in temperature-rise period fast, realize densified, the later stage temperature retention time is short, so the inventive method can realize the sinter molding of titanium powder in 20 seconds～10 minutes, thereby the heating-up time of part and preparation time are all significantly shortened.
5, reduced sintering temperature.Because the inventive method adopts the alternating current of large electric current, low-voltage (Ampere currents up to ten thousand, 10 volts of left and right voltages), the titanium powder system is heated, utilize joule heating effect evenly to be rapidly heated, so 1600～1700 ℃ used are reduced to 800～1200 ℃ by original powder metallurgy process, greatly reduce sintering temperature, improved production efficiency and saved the energy.
6, improved product quality.Due to increasing substantially of the inventive method programming rate, aggravated the diffusion that atom is asked, make metal dust more easily be molten state, be applied with pressure in both mold ends again in addition, not only make pressed compact moulding and sintering carry out simultaneously, also make powder can realize at a lower temperature the sintering of compactness within the very fast time, thereby suppressed growing up of crystal grain, can obtain ultra-fine grain structure, thereby solved the problem that the grain growth of micro-element is difficult to achieve effective control, guaranteed the performance after the part microminiaturization.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
The Gleeble-1500D thermal simulation machine that the sintering Preparation equipment that following examples adopt is the development of U.S. DSI science and technology association.
Embodiment 1
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 25 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 97.90%, and Vickers hardness is 189HV.
Embodiment 2
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 98.60%, and Vickers hardness is 196HV.
Embodiment 3
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 75 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 98.80%, and Vickers hardness is 198HV.
Embodiment 4
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 100 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 98.90%, and Vickers hardness is 200HV.
Embodiment 5
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 125 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 99.20%, and Vickers hardness is 211HV.
Embodiment 6
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 800 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 90.10%, and Vickers hardness is 159HV.
Embodiment 7
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 900 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 92.30%, and Vickers hardness is 162HV.
Embodiment 8
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1000 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 94.70%, and Vickers hardness is 178HV.
Embodiment 9
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1100 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 96.30%, and Vickers hardness is 186HV.
Embodiment 10
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 50MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 96.90%, and Vickers hardness is 190HV.
Embodiment 11
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 75MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 97.50%, and Vickers hardness is 194HV.
Embodiment 12
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 125MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 99.00%, and Vickers hardness is 199HV.
Embodiment 13
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 150MPa in both mold ends simultaneously.Be incubated 0min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 99.30%, and Vickers hardness is 213HV.
Embodiment 14
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 2min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 98.70%, and Vickers hardness is 197HV.
Embodiment 15
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 4min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 99.10%, and Vickers hardness is 209HV.
Embodiment 16
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 6min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 99.40%, and Vickers hardness is 214HV.
Embodiment 17
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 8min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 99.70%, and Vickers hardness is 221HV.
Embodiment 18
Solid density by titanium miniature gears size (pitch diameter is 1.6mm, and the number of teeth is 8, and thickness is 3mm) and corresponding powder calculates powder quality.The mould of packing into after the titanium valve weighing is good fixes with chuck, and under the vacuum condition of≤0.01Pa, controlling programming rate is 50 ℃/s, loads active force 100MPa in both mold ends simultaneously.Be incubated 10min after temperature reaches 1200 ℃, powder is in die for molding and complete densification, and the air cooling that finally cuts off the power supply takes out part and gets final product.The relative density of prepared part is 99.80%, and Vickers hardness is 224HV.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (6)
- One kind based on multiple physical field, activated sintering prepares the method for pure titanium miniature parts, it is characterized in that, after being weighed, pure titanium powder fills in mould, then at programming rate, be 25～125 ℃/s, under the sintering condition of vacuum≤0.01Pa, the mould indirect current that titanium powder is housed is carried out to instant heating, impose the active force of 10～200MPa in both mold ends simultaneously, under the continuous action in electric field and the field of force, when being heated to 800～1200 ℃, insulation makes titanium powder in die for molding in 0～10 minute, and the air cooling that finally cuts off the power supply takes out part and gets final product.
- 2. method according to claim 1, is characterized in that, described programming rate is 50～100 ℃/s.
- 3. method according to claim 1, is characterized in that, described sintering temperature is 900～1000 ℃.
- 4. method according to claim 1, is characterized in that, described applied external force is 50～100MPa.
- 5. method according to claim 1, is characterized in that, described insulation is after sintering temperature reaches preset temperature, sintered body to be carried out to insulation in 4～6 minutes to process.
- 6. method according to claim 1, is characterized in that, the method adopts AC electric-heating, and wherein voltage is 3～10V, and electric current is 3000～30000A.
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Cited By (6)
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| CN103862049A (en) * | 2014-04-02 | 2014-06-18 | 四川大学 | Ni-Ti porous material mini-sized part and sintering method thereof |
| CN103864436A (en) * | 2014-04-02 | 2014-06-18 | 四川大学 | Aluminum oxide miniature part prepared by active sintering based on multiple physical fields and sintering method of miniature part |
| 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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| CN102941343A (en) * | 2012-11-16 | 2013-02-27 | 西北有色金属研究院 | Quick manufacturing method of titanium-aluminum alloy composite part |
| CN102994852A (en) * | 2012-11-26 | 2013-03-27 | 四川大学 | Method for preparing WC-Co hard alloy by rapid sintering under multi-physics coupling action |
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| CN103862049A (en) * | 2014-04-02 | 2014-06-18 | 四川大学 | Ni-Ti porous material mini-sized part and sintering method thereof |
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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 |
| CN109079135B (en) * | 2018-08-09 | 2021-01-26 | 四川大学 | Method for preparing miniature ultrasonic motor stator based on multi-physical-field activated sintering |
| CN108941536B (en) * | 2018-08-09 | 2021-05-28 | 四川大学 | Near-net manufacturing method of titanium alloy micro part and micro ultrasonic motor rotor |
| 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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Application publication date: 20131218 |