CN1239284C - Method for directly preparing TiNi shape memory alloy pipe joint from element powders - Google Patents
Method for directly preparing TiNi shape memory alloy pipe joint from element powders Download PDFInfo
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- CN1239284C CN1239284C CN 01140301 CN01140301A CN1239284C CN 1239284 C CN1239284 C CN 1239284C CN 01140301 CN01140301 CN 01140301 CN 01140301 A CN01140301 A CN 01140301A CN 1239284 C CN1239284 C CN 1239284C
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- 238000000034 method Methods 0.000 title claims abstract description 55
- 229910010380 TiNi Inorganic materials 0.000 title claims abstract description 51
- 239000000843 powder Substances 0.000 title claims abstract description 49
- 229910001285 shape-memory alloy Inorganic materials 0.000 title abstract 2
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 239000000956 alloy Substances 0.000 claims abstract description 41
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000011521 glass Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000007514 turning Methods 0.000 claims abstract description 8
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 6
- 239000012530 fluid Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 230000008439 repair process Effects 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 238000000280 densification Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 230000003064 anti-oxidating effect Effects 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000005056 compaction Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 230000008595 infiltration Effects 0.000 claims description 5
- 238000001764 infiltration Methods 0.000 claims description 5
- 238000012946 outsourcing Methods 0.000 claims description 5
- 239000011241 protective layer Substances 0.000 claims description 5
- 238000007731 hot pressing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 14
- 238000005245 sintering Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000006835 compression Effects 0.000 abstract 3
- 238000007906 compression Methods 0.000 abstract 3
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000003723 Smelting Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 229910000734 martensite Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 238000005275 alloying Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 206010034703 Perseveration Diseases 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000008828 contractile function Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The present invention relates to a method for directly preparing TiNi shape memory alloy tube joints by element powder, which comprises the following steps: (1), powder mixture: Ti powder whose weight percentage is from 43.94 to 45.92% and granularity is from 100 to 325 meshes and Ni powder whose weight percentage is from 56.06 to 54.08% and granularity is from 100 to 400 meshes are sufficiently mixed in a grinding body or a ball mill; (2), cold compression: the density of a compressed compact is controlled to be in 60 to 85%; (3), cover wrapping: the cold compressed compact is placed in a glass tube, the glass tube is sealed to prevent oxidation after being evacuated, and a fluid mold compounded by glass and ceramic materials is wrapped outside the glass tube for transmitting pressure in an ROC process; (4), heating reaction sintering and rapidly omnidirectional compression (ROC): materials are heated and sintered in a common electric furnace, temperature is from 950 to 1100 DEG C, and time is from 0.5 to 2 hours. Then, the materials are compacted by ROC hot compression, pressure is from 300 to 1000Mpa, and the time is from 5 to 30 seconds; (5), rough turning, hole repair and finish turning are carried out to compact ingots, and TiNi alloy tube joint finished products are prepared. The method has the advantages of simple process, high material utilization rate and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of marmem pipe joint, belong to a kind of method that directly prepares the TiNi marmem pipe joint by element powders.
Background technology
The TiNi marmem is the best marmems of various so far combination properties, has extensive and important purposes, at present Aeronautics and Astronautics, machinery, intellectual material technology, medical science, agricultural, etc. the field be widely used, become a kind of important new function material.
Marmem has temperature-sensitive and drives dual-use function, so can have the element of driving effectively concurrently as temperature-sensitive, also can only make driver.All be applied at aspects such as pipe joint, electronic dry case, automobile thermostat, locomotive flow divider, hot machine, temperature relays.
Pipe joint is one of the most successful application of marmem, and the method for attachment of marmem pipe joint is as follows: earlier the memorial alloy internal diameter of pipe joint is made littler by about 4% than being connected pipe.After the memory processing, under the situation more much lower than phase transition temperature, the taper stick harness is squeezed in the pipe joint, make internal diameter expansion 7-8%, when pipe joint is in low-temperature condition, will be connected pipe and inserts from two ends, when pipe joint at room temperature heats up gradually, through the martensite reverse transformation, be returned to the preceding size of hole enlargement, just tightly block being connected pipe.
It is reported that this pipe joint has used at present and never occurred oil accident more than 1,500,000, shows high reliability in the world.In addition,, can not cause the material around infringement, be convenient to the operation of narrow space because of not needing melting welding.
TiNi memorial alloy pipe joint utilizes the memory contractile function of memorial alloy to come connecting pipe, it have high reliability, easy and simple to handle, can significantly reduce and take up room, be mainly used in fields such as aircraft, naval vessel, offshore oil field and machinery, electronics, chemical industry.Up to now, extensively adopting in countries such as American and Britain, Russia and Sweden, is one of maximum memorial alloy application ware of at present total use amount.
Usually processes such as machined such as vacuum melting, hot-working and follow-up boring, turning are mainly passed through in the preparation of TiNi memorial alloy pipe joint.The method of smelting stock utilization is lower, the difficulty of TiNi memorial alloy cold working simultaneously.Especially tubing processing, the processing thermal conductance causes the intensification of material, and then the sclerosis that causes, and the caliber that SME causes shrinks, and makes with the unusual difficulty of drill bit punching.Thereby memorial alloy pipe joint class part material utilization rate is very low, nearly has only 20%, machined cost height, and product cost is very high.
The difficulty of conventional relatively melting processing TiNi method, powder art metallurgical method seemingly solves the choose reasonable of many difficult problems.Use powder metallurgy process,,, also have considerable part and be resolved even the existing problem of smelting process is not all like this owing to be alloying under solid state.In addition, powder metallurgy method can made the most of the advantage aspect the pipe joint member that make the complicated shape except line or plate at least.Begin each state from early eighties and all attempting making the TiNi alloy with powder metallurgy process, common flour metallurgical method and SHS (synthetic from the climing combustion) technology that mainly concentrates on prepares TiNi alloy two aspects.
With Ti powder, Ni powder is raw material, is the basic line that powder method is produced the TiNi alloy through fully mixing the aftershaping sintering, obtains densification and the TiNi alloy of sufficient reacting is its final purpose.Studies show that if use thicker raw meal, oxygen content can be lower, but in resulting TiNi alloy, because Ti is different with the Ni diffusion velocity, can be at Ti and TiNi
3The interface on produce the space, depend merely on the prolongation sintering time, the density that expect the TiNi alloy of producing near smelting process is unusual difficulty.The porosity of the TiNi alloy that this method obtains is generally greater than 10%; Use very thin raw meal, it is approaching with smelting process that density can reach, but the problem of bringing oxygen content to increase simultaneously, the excess of oxygen in the promptly thin Ti powder can form Ti in the TiNi alloy
4Ni
2The O oxide not only causes the alloying component change, and mechanical performance is significantly worsened.
In order to address the above problem, adopted on thick Ti powder stock basis, add the fine and close method of HIP (high temperature insostatic pressing (HIP)).I.e. mixed-forming at first, through 1000 ℃, 10 hours sintering obtains single-phase TiNi alloy, jacket then, through 950 ℃, 1 hour high temperature insostatic pressing (HIP) is eliminated inherent space.The billet that this method obtains can through subsequently be processed into TiNi sheet material or wire rod.But this method operation is many, the time is long, to the requirement height of material powder, and uses expensive high temperature insostatic pressing (HIP), cost to be difficult to reduce.
Once studied the energy that is equipped with the TiNi alloy by Ti, the isostatic pressing of Ni powder direct heat, but since pressure restraining the diffusion process between Ti, Ni powder, cause prolong greatly the action time of the TiNi alloy that obtains even composition, at 200MPa, under 950 ℃ of conditions, reach 20 hours, make cost increase greatly.If Ti is arranged in synthetic product
2Ni even reach full densification in HIP (high temperature insostatic pressing (HIP)), also can ftracture in reheating process and forms defective.
With Ti powder Ni powder is raw material, after fully mixing, can prepare the TiNi alloy with the method for hot-forming sintering.This method is under the situation of using graphite jig, and pressurization can be restricted, if but suitably select the sintering temperature time, relative density can bring up to 98%.
Also can make raw material,,, sinter blank into by the HIP moulding they good mixing by two kinds of alloyed powders with different martensite transformation temperatures.Further be processed into TiNi alloy wire or sheet material again with this blank.Because the alloyed powder of two kinds of known martensite transformation temperatures is mixed, so can be arbitrarily and produce alloy exactly with desired transition temperature.This method is at first wanted melting TiNi alloy, again melt is made powder with spray-on process, and what advantage the TiNi alloy that obtains does not have on cost.
Utilizing SHS (synthetic from climing combustion) method to prepare the TiNi alloy is a certain proportion of titanium valve, nickel powder to be divided mix, with isostatic cool pressing (CIP) moulding, with the synthetic TiNi intermetallic compound of SHS.Use high temperature insostatic pressing (HIP) (HIP) fixed then, make billet.Under the prerequisite of control powder quality, the SHS method can obtain the lower billet of oxygen content.And since billet do not have chemical composition on segregation, the cold and hot working performance of gained material and end article performance are all good relatively, can produce in a large number.Although used expensive HIP technology, this method is compared with fusion casting aspect properties of product at cost has the power of striving unexpectedly.
Summary of the invention
What the purpose of this invention is to provide that a kind of process is simple, stock utilization is high, cost is low directly prepares the method for TiNi marmem pipe joint by element powders.
This law is used Ti, Ni element powders, by mixing powder, is pressed into pipe, and outer jacket carries out heat-agglomerating then, and to make density by hot pressing be 100% TiNi memorial alloy pipe, is marmem pipe joint through simply being machined to.Method technology is simple, the stock utilization height, and cost is low.
This method is with the reaction-sintered (Reactive Sintering) and densified being integrated of ROC (omnidirectional's compacting fast) of Ti, Ni, promptly carry out reacting between element powders synthetic in the ROC heating period, finish end reaction and densification process by ROC at last, one step obtained closely knit and TiNi alloy pipe joint billet sufficient reacting, made pipe joint through simple machined then.So both overcome shortcomings such as prior powder metallurgy method material is not fine and close,, thereby reduced production costs effectively, formed a kind of new method for preparing the TiNi marmem pipe joint simultaneously because ROC method cost is lower than methods such as HIP.
A kind ofly directly prepare the method for TiNi marmem pipe joint by element powders, it comprises the following steps:
(1), mix powder: by weight percentage with 43.94～45.92%, granularity 100～325 purpose Ti powder, 56.06～54.08%, granularity 100～400 purpose Ni powder fully mix in grinding body or ball mill;
(2), cold compaction: the control green density is in 60～85% scopes, and the center has a metal mandrel smaller than internal diameter of pipe joint during compacting;
(3), the outer cover of protecting: the base of will colding pressing places sealed after being vacuumized in the glass tube, and is anti-oxidation, and the compound fluid mould of outsourcing glass and ceramic material is used for the ROC process and transmits pressure again;
(4), heating reaction-sintered+omnidirectional's compacting (ROC) fast: heat-agglomerating in common electric furnace, 950～1100 ℃ of temperature, 0.5～2 hour time, ROC hot pressing densification then, pressure 300～1000Mpa, obtains the TiNi alloy pipe joint billet of sufficient reacting at 5～30 seconds time;
(5), billet is rough turn, repair the hole, finish turning is made TiNi alloy pipe joint finished product.
It is characterized in that: the infiltration of Ti, Ni when preventing ROC scribbles one deck carbon protective layer on the surface of metal mandrel.
This method is produced the memorial alloy pipe joint utilization rate of material is brought up to 60%, although use the powder cost than directly using Ti, Ni metal cost height, because stock utilization improves, work simplification reduces amount of machining, and its integrated cost significantly reduces.
The problem that powder method prepares the TiNi marmem is that oxygen content is high slightly, it is poor that the plasticity ratio of alloy is smelted method, but pipe joint class part shape is simple, mainly utilize a SME of TiNi alloy, generally need not perseveration, therefore do not have memory fatigue and longevity to close problem, this point is just meeting powder method, and to prepare TiNi alloy oxygen content high relatively, the characteristics that performance is poor slightly.
The specific embodiment
Embodiment 1:
A kind ofly directly prepare the method for TiNi marmem pipe joint by element powders, it comprises the following steps:
(1), mix powder: by weight percentage with 43.94%, granularity 100 purpose Ti powder, 56.06%, granularity 200 purpose Ni powder fully mix in grinding body or ball mill;
(2), cold compaction: the control green density is in 60～85% scopes, and the center has a metal mandrel smaller than internal diameter of pipe joint during compacting; The infiltration of Ti, Ni scribbles one deck carbon protective layer on the surface of metal mandrel when preventing ROC.
(3), the outer cover of protecting: the base of will colding pressing places sealed after being vacuumized in the glass tube, and is anti-oxidation, and the compound fluid mould of outsourcing glass and ceramic material is used for the ROC process and transmits pressure again;
(4), heating reaction-sintered+fast omnidirectional's compacting (ROC): heat-agglomerating in common electric furnace, 950 ℃ of temperature, 2 hours time, ROC densification then, pressure 300Mpa, obtains the TiNi alloy pipe joint billet of sufficient reacting at 30 seconds time;
(5), billet is rough turn, repair the hole, finish turning is made TiNi alloy pipe joint finished product.
Embodiment 2:
A kind ofly directly prepare the method for TiNi marmem pipe joint by element powders, it comprises the following steps:
(1), mix powder: by weight percentage with 45.92%, granularity 325 purpose Ti powder, 54.08%, granularity 400 purpose Ni powder fully mix in grinding body or ball mill.
(2), cold compaction: the control green density is in 60～85% scopes, and the center has a metal mandrel smaller than internal diameter of pipe joint during compacting; The infiltration of Ti, Ni scribbles one deck carbon protective layer on the surface of metal mandrel when preventing ROC.
(3), the outer cover of protecting: the base of will colding pressing places sealed after being vacuumized in the glass tube, and is anti-oxidation, and the compound fluid mould of outsourcing glass and ceramic material is used for the ROC process and transmits pressure again.
(4), heating reaction-sintered+fast omnidirectional's compacting (ROC): heat-agglomerating in common electric furnace, 1100 ℃ of temperature, 0.5 hour time, ROC densification then, pressure 1000Mpa, obtains the TiNi alloy pipe joint billet of sufficient reacting at 5 seconds time.
(5), billet is rough turn, repair the hole, finish turning is made TiNi alloy pipe joint finished product.
Embodiment 3:
1, a kind ofly directly prepare the method for TiNi marmem pipe joint by element powders, it comprises the following steps:
(1), mix powder: by weight percentage with 44.93%, granularity 230 purpose Ti powder, 55.07%, granularity 230 purpose Ni powder fully mix in grinding body or ball mill;
(2), cold compaction: the control green density is in 60～85% scopes, and the center has a metal mandrel smaller than internal diameter of pipe joint during compacting; The infiltration of Ti, Ni scribbles one deck carbon protective layer on the surface of metal mandrel when preventing ROC.
(3), the outer cover of protecting: the base of will colding pressing places sealed after being vacuumized in the glass tube, and is anti-oxidation, and the compound fluid mould of outsourcing glass and ceramic material is used for the ROC process and transmits pressure again;
(4), heating reaction-sintered+fast omnidirectional's compacting (ROC): heat-agglomerating in common electric furnace, 1025 ℃ of temperature, 1.25 hours time, ROC densification then, pressure 650Mpa, obtains the TiNi alloy pipe joint billet of sufficient reacting at 17.5 seconds time;
(5), billet is rough turn, repair the hole, finish turning is made TiNi alloy pipe joint finished product.
Claims (1)
1, a kind ofly directly prepare the method for TiNi marmem pipe joint by element powders, it comprises the following steps:
(1), mix powder: by weight percentage with 43.94～45.92%, granularity 100～325 purpose Ti powder, 56.06～54.08%, granularity 100～400 purpose Ni powder fully mix in grinding body or ball mill;
(2), cold compaction: the control green density is in 60～85% scopes, and the center has a metal mandrel smaller than internal diameter of pipe joint during compacting;
(3), the outer cover of protecting: the base of will colding pressing places sealed after being vacuumized in the glass tube, and is anti-oxidation, and the compound fluid mould of outsourcing glass and ceramic material is used for the ROC process and transmits pressure again;
(4), the heating reaction-sintered+omnidirectional suppresses ROC fast: heat-agglomerating in common electric furnace, 950～1100 ℃ of temperature, 0.5～2 hour time, ROC hot pressing densification then, pressure 300～1000MPa, obtains the TiNi alloy pipe joint billet of sufficient reacting at 5～30 seconds time;
(5), billet is rough turn, repair the hole, finish turning is made TiNi alloy pipe joint finished product.
It is characterized in that: during the omnidirectional's compacting ROC of heating reaction-sintered+fast, remain with metal mandrel in the pipe joint, the infiltration of Ti, Ni scribbles one deck carbon protective layer on the surface of metal mandrel when preventing ROC.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01140301 CN1239284C (en) | 2001-12-03 | 2001-12-03 | Method for directly preparing TiNi shape memory alloy pipe joint from element powders |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01140301 CN1239284C (en) | 2001-12-03 | 2001-12-03 | Method for directly preparing TiNi shape memory alloy pipe joint from element powders |
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| CN1422717A CN1422717A (en) | 2003-06-11 |
| CN1239284C true CN1239284C (en) | 2006-02-01 |
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| CN 01140301 Expired - Lifetime CN1239284C (en) | 2001-12-03 | 2001-12-03 | Method for directly preparing TiNi shape memory alloy pipe joint from element powders |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100337764C (en) * | 2005-04-27 | 2007-09-19 | 中国科学院金属研究所 | High speed-ratio hot pressing method for NiTi alloy piping billet and its special mould |
| CN101450870B (en) * | 2007-12-07 | 2011-02-09 | 中国科学院金属研究所 | Preparation device of graphite metal sheath for hot isostatic pressing |
| CN102366836B (en) * | 2011-10-25 | 2013-08-14 | 航天材料及工艺研究所 | Production method of high-performance titanium alloy blind pipe |
| CN103909386B (en) * | 2014-03-31 | 2016-08-17 | 攀钢集团成都钢钒有限公司 | A kind of processing method of titanium alloy oil connection |
| CN110814352B (en) * | 2019-11-15 | 2022-04-01 | 武汉理工大学 | Hot-pressing sintering method of hollow gradient pipe fitting |
| CN115386755B (en) * | 2022-06-21 | 2023-07-18 | 中南大学 | A preparation method of low-cost element-mixed NiTi shape memory alloy by high-temperature homogenization treatment |
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2001
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