CN101280399A - Titanium carbide-reinforced nickel-titanium shape memory alloy composite material and preparation thereof - Google Patents
Titanium carbide-reinforced nickel-titanium shape memory alloy composite material and preparation thereof Download PDFInfo
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- CN101280399A CN101280399A CNA2007100962406A CN200710096240A CN101280399A CN 101280399 A CN101280399 A CN 101280399A CN A2007100962406 A CNA2007100962406 A CN A2007100962406A CN 200710096240 A CN200710096240 A CN 200710096240A CN 101280399 A CN101280399 A CN 101280399A
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Abstract
The invention discloses a manufacturing method of titanium carbide / nickel titanium shape memory alloy composite material. The manufacturing method comprises the major technical process that Ti, Ni, and C powder lot is taken according to stoichiometric quantity and is uniformly mixed, salt which occupies 40 to 90 percent of the total weight of the powder lot is added into the powder lot, and the powder lot is filled into the steel can of a ball mill, the steel can of the ball mill is vacuumized and filled with argon gas, the rotating speed of the ball mill is 200 R/m, the ball material ratio is 20:1, the ball milling is performed for 1 hour, the powder lot is compressed into a green body and is put into 600 to 1300 DEG C fused salt, and is thermally insulated for 10 to 120 minutes, after cooling, through the desalination process, the TiC/NiTi composite powder body can be obtained, the TiC/NiTi composite powder body is put into a die and then is put into a vacuum heating-press sintering furnace, the vacuum heating-press sintering furnace is vacuumized to 10-2 to 10-3 Pa, the warming is started, the temperature rises to 800 to 1600 DEG C, the pressure is increased to 20 to 100 Mpa, and the heat is preserved for 60 to 240 minutes, after being cooled and demoulded, the TiC/NiTi composite material can be obtained. The manufacturing method has the advantages that firstly, the process is simple, and the cost is low, secondly, TiC and NiTi are both formed in situ, the interface between the TiC and the NiTi is clean, and the bonding strength is good, and thirdly, the NiTi in the product has obvious reversible Mar's phase alternation characteristic.
Description
(1) technical field
The present invention relates to the Composite Preparation field, specifically be meant a kind of titanium carbide/niti-shaped memorial alloy matrix material and preparation method thereof.
(2) background technology
Matrix material is a kind of multiphase solid material that is formed by two or more physics combinations of substances different with chemical property.Though the constituent materials of matrix material keeps its relative independentability, performance of composites be not simply adding of constituent materials performance and, but important improvement is arranged.In matrix material, have one to be external phase mutually usually, become matrix.Another phase place disperse phase is called strongthener.Disperse phase is to be distributed in the whole external phase with form independently, exists phase interface between the two-phase.
The nearly NiTi alloy that waits atomic ratio is expressed thermoelastic martensitic transformation between high temperature B2 cube phase and low temperature B19 ' phase, this phase transformation makes this alloy have super-elasticity and shape memory effect.Compare with other shape memory alloy, the NiTi alloy has the shape memory effect excellence, and fatigue property is good, and corrosion-resistant and excellent biological compatibility has obtained to use widely in fields such as medical science, instrument, aerospace and daily lifes.NiTi alloy phase change temperature is adjusted in the body scale easily, thereby especially active in application on medical field.
Yet, closely wait the yield strength of atomic ratio NiTi alloy big inadequately, recovery stress is less, and is not ideal enough in some applications; In addition, to the wear resistance of NiTi shape memory alloy, many application scenarios have also proposed higher requirement.This all needs further to strengthen the NiTi shape memory alloy, improves its yield strength and hardness.This paper uses the principle of making metal-base composites, adopts TiC material to strengthen the NiTi shape memory alloy, forms the TiC/NiTi matrix material, can thoroughly improve the mechanical property of shape memory alloy.
The technology of existing preparation TiC/NiTi matrix material is generally TiC and NiTi powder technique, perhaps the mixed sintering of TiC, Ni and Ti powder.The main drawback of these two kinds of methods is that the TiC powder surface pollutes the TiC cause and the bonding strength problem of NiTi, and because the atomic diffusion between TiC and the NiTi at high temperature, cause NiTi to lose reversible martensite phase change effect easily, and reduce performance of composites.
(3) summary of the invention
Purpose of the present invention is exactly the defective that exists in the above-mentioned prior art in order to solve, a kind of TiC/NiTi matrix material and preparation method thereof is provided, this method is by to the optimization design of atomic ratio between Ti, the C among the TiC, reduce even suppress the negative impact that diffusion or reaction caused that TiC and NiTi at high temperature exist, and in preparation process, original position forms TiC and NiTi overcomes its shortcoming, thereby improves composite effect, further improves performance of composites.While is simple owing to the required technology of this method, thereby reduces the cost of TiC/NiTi matrix material greatly, helps applying.
The preparation method of a kind of TiC/NiTi matrix material of the present invention comprises the steps and processing condition:
(1) be raw material with titanium valve, nickel powder and carbon dust, the molar ratio range of titanium valve, nickel powder and carbon dust is 2: 1: 1～2.5: 1: 1;
(2) proportioning is good raw material titanium valve, nickel powder and carbon dust ball milling mix;
(3) add 40～90% the mixing salt account for titanium valve, nickel powder and carbon dust gross weight, ball milling is even, makes base substrate;
(4) above-mentioned base substrate is carried out fused salt and handle, obtain titanium carbide/NiTi composite granule;
(5) above-mentioned titanium carbide/NiTi composite granule pre-molding is carried out hot pressed sintering then under vacuum.
The preparation method of a kind of TiC/NiTi matrix material of the present invention, it is further characterized in that the body preparation method is: add weight ratio in the powder and be after 40～90% the mixing salt, in the ball mill ball grinder of packing into, ratio of grinding media to material is 20: 1, and ball grinder is evacuated to 1～10
-1Pa also charges into argon gas, and argon pressure is controlled at 0.9～1.2 * 10
5The scope of Pa, drum's speed of rotation are controlled at 200 rev/mins, and ball milling 1 hour is pressed into base substrate under 2～6MPa pressure; The fused salt treating processes is: base substrate is put into 600～1300 ℃ of fused salts, be incubated 10～120 minutes, chemical reaction takes place in powder in fused salt, through demineralising process, obtains titanium carbide/NiTi composite granule after the cooling; The desalting treatment process is: will react the mixing salt that is loaded with the TiC/NiTi composite granule after the cooling and put in the water of 5 times of salt weight and soaked 10-15 hour, and after mixing salt 100% is dissolved in the water, filter out the TiC/NiTi composite granule; The heat pressing process process is: the TiC/NiTi composite granule is put into mould, place the vacuum heating-press sintering stove, be evacuated to 10
-2～10
-3Pa begins to heat up, and is warming up to 800～1600 ℃, is forced into 20～100MPa, is incubated 60～240 minutes, and the cooling back demoulding obtains the TiC/NiTi matrix material.
Compared with prior art, major advantage of the present invention is:
(1) technology is simple, and cost is low.
(2) TiC and NiTi are original position formation, the interface cleaning between the two, and bonding strength is good.
(3) NiTi in the product has tangible reversible martensitic transformation feature mutually.
(4) embodiment
Below in conjunction with specific examples, further specify details of the present invention.
Embodiment 1:
By the atom proportioning get at 2: 1: 1 200 purposes and Ti, Ni and C powder each 4.6022,2.8206 and 0.5772 gram, prepare burden altogether 8 the gram, the NaCl and the KCl mixing salt of mol ratios such as adding 5.3333 grams, put into ball mill stainless steel cylinder of steel after the mixing, with cylinder of steel with seal with elastometic washer after, be evacuated to 1Pa and charge into argon gas, pressure is 0.9 * 10
5Pa, ratio of grinding media to material is 20: 1, the control drum's speed of rotation is 200 rev/mins, behind the ball milling 1 hour, the base substrate of 30mm in being pressed under the axle pressure with 3MPa in mould, base substrate was put into the NaCl of mol ratios such as 750 ℃ and the insulation of KCl mixed melting salt 30 minutes, the mixing salt that is loaded with the TiC/NiTi powder after the reaction cooling is put in the water of 5 times of salt weight and soaked 15 hours, after mixing salt 100% is dissolved in the water, filter out the TiC/NiTi powder, the TiC/NiTi powder is washed the back oven dry repeatedly with deionized water, the TiC/NiTi composite granule after the oven dry is added in the mould, put into the vacuum heating-press sintering stove, be evacuated to 10
-2Pa, heat temperature raising to 1200 ℃ is incubated 60 minutes, and the cooling back demoulding obtains the TiC/NiTi matrix material, measure this matrix material by TiC and NiTi two phase composites through X-ray diffractometer, the NiTi that measures in this matrix material through differential scanning calorimeter has tangible reversible martensitic transformation feature mutually.
Embodiment 2:
By the atom proportioning get at 2.5: 1: 1 200 purposes and Ti, Ni and C powder each 5.0294,2.4660 and 0.5046 gram, prepare burden altogether 8 the gram, the NaCl and the KCl mixing salt of mol ratios such as adding 5.3333 grams, put into ball mill stainless steel cylinder of steel after the mixing, with cylinder of steel with seal with elastometic washer after, be evacuated to 1Pa and charge into argon gas, pressure is 1.1 * 10
5Pa, ratio of grinding media to material is 20: 1, the control drum's speed of rotation is 200 rev/mins, behind the ball milling 1 hour, the base substrate of 30mm in being pressed under the axle pressure with 3MPa in mould, base substrate was put into the NaCl of mol ratios such as 850 ℃ and the insulation of KCl mixed melting salt 60 minutes, the mixing salt that is loaded with the TiC/NiTi powder after the reaction cooling is put in the water of 5 times of salt weight and soaked 15 hours, after mixing salt 100% is dissolved in the water, filter out the TiC/NiTi powder, the TiC/NiTi powder is washed the back oven dry repeatedly with deionized water, the TiC/NiTi composite granule after the oven dry is added in the mould, put into the vacuum heating-press sintering stove, be evacuated to 10
-2Pa, heat temperature raising to 1300 ℃, be incubated 120 minutes, the cooling back demoulding obtains the TiC/NiTi matrix material, measure this matrix material by TiC and NiTi two phase composites through X-ray diffractometer, the NiTi that measures in this matrix material through differential scanning calorimeter has tangible reversible martensitic transformation feature mutually.
Claims (7)
1. titanium carbide-reinforced nickel-titanium shape memory alloy matrix material is characterized in that this material is is matrix with the niti-shaped memorial alloy, adds the matrix material that a certain amount of titanium carbide forms.
2. according to the described titanium carbide-reinforced nickel-titanium shape memory alloy material of claim 1, it is characterized in that described titanium carbide weight percent is 10～50%, the niti-shaped memorial alloy weight percent is 50～90%.
3. a method for preparing titanium carbide-reinforced nickel-titanium shape memory alloy matrix material is characterized in that, the step of preparation is:
(1) be raw material with titanium valve, nickel powder and carbon dust, the molar ratio range of titanium valve, nickel powder and carbon dust is 2: 1: 1～2.5: 1: 1;
(2) proportioning is good raw material titanium valve, nickel powder and carbon dust ball milling mix;
(3) add 40～90% the mixing salt account for titanium valve, nickel powder and carbon dust gross weight, ball milling is even, makes base substrate;
(4) above-mentioned base substrate is carried out fused salt handle after again through desalting treatment, obtain titanium carbide/NiTi composite granule;
(5) above-mentioned titanium carbide/NiTi composite granule pre-molding is carried out hot pressed sintering then under vacuum.
4. by the described preparation method of claim 3, it is characterized in that the preparation method of base substrate is: add weight ratio in the powder and be after 40～90% the mixing salt, in the ball mill ball grinder of packing into, ratio of grinding media to material is 20: 1, and ball grinder is evacuated to 1～10
-1Pa also charges into argon gas, and argon pressure is controlled at 0.9～1.2 * 10
5The scope of Pa, drum's speed of rotation are controlled at 200 rev/mins, and ball milling 1 hour is pressed into base substrate under 2～6MPa pressure.
5. by the described preparation method of claim 3, it is characterized in that the fused salt treating processes is: base substrate is put into 600～1300 ℃ of fused salts, be incubated 10～120 minutes, chemical reaction takes place in powder in fused salt, through demineralising process, obtain titanium carbide/NiTi composite granule after the cooling;
6. by the described preparation method of claim 3, it is characterized in that, the desalting treatment process is: will react the mixing salt that is loaded with titanium carbide/NiTi composite granule after the cooling and put in the water of 5 times of salt weight and soaked 10-15 hour, after mixing salt 100% is dissolved in the water, filter out titanium carbide/NiTi composite granule;
7. by the described preparation method of claim 3, it is characterized in that the heat pressing process process is: titanium carbide/NiTi composite granule is put into graphite jig, is evacuated to 10
-2～10
-3Pa begins to heat up, and is warming up to 800～1600 ℃, is forced into 20～100MPa, is incubated 60～240 minutes, and the cooling back demoulding obtains titanium carbide/NiTi matrix material.
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| CNA2007100962406A CN101280399A (en) | 2007-04-03 | 2007-04-03 | Titanium carbide-reinforced nickel-titanium shape memory alloy composite material and preparation thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104801704A (en) * | 2015-03-26 | 2015-07-29 | 成都新柯力化工科技有限公司 | Shape memory alloy material for three-dimensional printing and preparation method of shape memory alloy material |
| CN110997194A (en) * | 2017-07-13 | 2020-04-10 | 于利奇研究中心有限公司 | Method for sintering metals, non-oxide ceramics and other easily oxidized materials |
| CN115475947A (en) * | 2022-10-17 | 2022-12-16 | 吉林大学 | Preparation method and application of transition metal carbide particles with {100} crystal face cube surfaces |
| CN116024449A (en) * | 2022-12-14 | 2023-04-28 | 中国石油大学(北京) | Preparation method of functionally graded shape memory alloy |
-
2007
- 2007-04-03 CN CNA2007100962406A patent/CN101280399A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104801704A (en) * | 2015-03-26 | 2015-07-29 | 成都新柯力化工科技有限公司 | Shape memory alloy material for three-dimensional printing and preparation method of shape memory alloy material |
| CN104801704B (en) * | 2015-03-26 | 2017-01-25 | 成都新柯力化工科技有限公司 | Shape memory alloy material for three-dimensional printing and preparation method of shape memory alloy material |
| CN110997194A (en) * | 2017-07-13 | 2020-04-10 | 于利奇研究中心有限公司 | Method for sintering metals, non-oxide ceramics and other easily oxidized materials |
| CN115475947A (en) * | 2022-10-17 | 2022-12-16 | 吉林大学 | Preparation method and application of transition metal carbide particles with {100} crystal face cube surfaces |
| CN115475947B (en) * | 2022-10-17 | 2024-01-12 | 吉林大学 | Preparation method and application of surface {100} crystal face cube transition metal carbide particles |
| CN116024449A (en) * | 2022-12-14 | 2023-04-28 | 中国石油大学(北京) | Preparation method of functionally graded shape memory alloy |
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Open date: 20081008 |