CN101270424A - Nickel titanium niobium negative thermal expansion alloy and method of producing the same - Google Patents
Nickel titanium niobium negative thermal expansion alloy and method of producing the same Download PDFInfo
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- CN101270424A CN101270424A CNA2008100708240A CN200810070824A CN101270424A CN 101270424 A CN101270424 A CN 101270424A CN A2008100708240 A CNA2008100708240 A CN A2008100708240A CN 200810070824 A CN200810070824 A CN 200810070824A CN 101270424 A CN101270424 A CN 101270424A
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- alloy
- thermal expansion
- nickel
- negative thermal
- niobium
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Abstract
The invention discloses a negative thermal expansion alloy of Nickel-Titanium-Niobium and a preparation method thereof, relates to an alloy in particular to a negative thermal expansion alloy of Nickel-Titanium-Niobium and a preparation method thereof. The invention provides a negative thermal expansion alloy of Nickel-Titanium-Niobium which has negative thermal expansion characteristics in a wider temperature range and a preparation method. The component and the content in atom percentage is 40 to 49 percent of Nickel, 42 to 50 percent of Titanium and 1 to 18 percent of Niobium. The raw material of Nickel, Titanium and Niobium are added in furnace, the furnace is vacuumed and filled with Argon, and the Nickel-Titanium-Niobium alloy ingot is obtained after melting in 2500 to 2900 DEG C; the Nickel-Titanium-Niobium alloy ingot is hot-rolled to bulk alloy in 800 to 950 DEG C; the bulk alloy obtained is packaged in a quartz tube for heat treatment in the temperature of 800 to 950 DEG C and cooled in air. The bulk alloy after cooling is cool-rolled in 3 to 15 percent of the rolling reduction along the same direction and consequently the negative thermal expansion alloy of Nickel-Titanium-Niobium is obtained.
Description
Technical field
The present invention relates to a kind of alloy, especially relate to a kind of nickel titanium niobium (NiTiNb) negative thermal expansion alloy material and preparation method thereof.
Background technology
The negative thermal expansion material of the comparative maturity of having developed at present mainly is a stupalith, as devitrified glass, oxide ceramics (tungstate, molybdate, chromic salt etc.) and polynary magnetic compound etc.Some metallic substance have very little thermal expansivity, as Invar alloy, but can't obtain negative expansion.Consider from the point of view of practicability of material, advantages such as metallic substance has good toughness, can process, shock-resistant load, therefore, the negative thermal expansion material of research and development metal species be highly significant (referring to document: 1, Kang Lijun, Liu Tong, Su Zhimei, the technology of preparing and the constitutional features of beta-eucryptite negative expansion devitrified glass, functional materials, 2005,36,825; 2, warm Yongchun, Wang Cong, Sun Ying, magneticsubstance, forward position progress, 2007,36 with negative expansion performance; 3, J.J.Wang, T.Omori, Y.Sutou, R.Kainuma, K.Ishida, Microstructure and thermal expansionproperties of Invar-type Cu-Zn-Al shape memory alloys, J. Electron.Mater.2004,33,1098; 4, MaryT A, Evans J S O, Vogt T, Negative thermal expansion from 0.3to 1050Kelvin in ZrW
2O
8, Science, 1996,272,90).
At present, the metal low-expansion material of research mainly is an Invar alloy, this alloy is below Curie temperature, when temperature raises, saturation magnetization can sharply descend and be attended by bigger volumetric shrinkage, thereby offset normal thermal expansion, (20～100 ℃) have very low thermal expansivity (CTE≤1.8 * 10 in certain temperature range
-6℃
-1).In addition, the volume change that martensitic transformation in the alloy material causes offsets also and can obtain low thermal expansivity with the effect of expanding with heat and contract with cold, and has showed that as R.Kainuma etc. the control that in the cold working of CuZnAl alloy counter stress brings out martensitic transformation can produce low thermal expansivity (100～40 ℃ CTE ≈ 0 ± 3 * 10
-6℃
-1) (referring to document: 5, Liu Jiang, the application of low expansion alloy and development, Metallic Functional Materials, 2007,14,33-37; 6, R.Kainuma, J.J.Wang, T. Omori et al.Invar-type effect induced bycold-rolling deformation in shape memory alloys, Appl.Phys.Lett., 2002,80,4348-4350).
Up to the present, yet there are no metallic substance and have negative thermal expansion character.
Summary of the invention
The object of the present invention is to provide a kind of nickel titanium niobium negative thermal expansion alloy that has the negative expansion characteristic in the wide temperature interval and preparation method thereof.
The composition of nickel titanium niobium negative thermal expansion alloy of the present invention and be nickel 40%～49%, titanium 42%～50%, niobium 1%～18% by the content of atomic percent.
The preparation method of nickel titanium niobium negative thermal expansion alloy of the present invention may further comprise the steps:
1) nickel, titanium and niobium raw material are put into stove, vacuumize, charge into argon gas,, get nickel titanium niobium alloy ingot 2500～2900 ℃ of meltings;
2) with nickel titanium niobium alloy ingot 800～950 ℃ of hot rollings, nickel titanium niobium alloy ingot is rolled into bulk alloy;
3) bulk alloy that obtains is encapsulated in the silica tube interior heat and handles, thermal treatment temp is 800～950 ℃, cools off in air;
4) cooled bulk alloy is carried out the cold rolling of 3%～15% draught along same direction, promptly obtain nickel titanium niobium negative thermal expansion alloy.
The purity of nickel, titanium and niobium raw material preferably is not less than 99.5%.Described stove is preferably non-consumable arc furnace; The vacuum tightness at least 6 that vacuumizes * 10
-3Pa charges into argon gas preferably to 0.5～0.7 * 10
5Pa is the number of times of 2500～2900 ℃ of meltings preferably at least 5 times.The bulk alloy that obtains is encapsulated in the processing of silica tube interior heat preferably will vacuumizes in the silica tube, vacuum tightness is preferably 2 * 10
-3～5 * 10
-3Pa, heat treatment period is 24h at least.Bulk alloy preferably cuts into tabular alloy before being encapsulated in the processing of silica tube interior heat, and the thickness of tabular alloy is preferably 6～8mm.Described cold rolling temperature is preferably room temperature or below the room temperature.
The present invention carries out cold rolling under differing temps to nickel titanium niobium negative thermal expansion alloy, by controlled rolling temperature, rolling draught and rolling direction, obtain to have the nickel titanium niobium negative thermal expansion alloy of negative expansion in wide temperature range.After tested, this alloy shows tangible negative expansion in-100～40 ℃ wide temperature range.Shrink during intensification, its thermal expansivity is-1.3 * 10
-6℃
-1, thermal expansivity is-6.5 * 10 during cooling
-7℃
-1
Nickel titanium niobium negative thermal expansion alloy of the present invention can be used for making to temperature sensitive or to the precise part of dimensional requirement harshness, also can be compound with other material, obtain having the matrix material of required thermal expansivity, thereby acquisition good thermal shock resistance, avoid distortion, stress and the inefficacy of its product effectively, have wide practical use in fields such as instrument element, opticfiber communication, Electronic Packaging, aerospace, optics, cryogenic engineerings.
Description of drawings
Fig. 1 is Ti
46.3Ni
44.7Nb
9Alloy cube matherial at room temperature, draught be 9% cold rolling after the thermal expansion test curve.In Fig. 1, X-coordinate be temperature T emperature (℃), ordinate zou is relative length changes delta l/l (* 10
-4), (a) be heating curve, (b) be cooling curve.
Fig. 2 is Ti
44Ni
47Nb
9Alloy cube matherial under liquid nitrogen temperature, draught be 7% cold rolling after thermal expansion heating test curve.In Fig. 2, X-coordinate be temperature T emperature (℃), ordinate zou is relative length changes delta l/l (* 10
-4), arrow represents to heat direction.
Fig. 3 is Ti
42Ni
40Nb
18Alloy cube matherial at room temperature, draught be 3% cold rolling after thermal expansion heating test curve.In Fig. 3, X-coordinate be temperature T emperature (℃), ordinate zou is relative length changes delta l/l (* 10
-4), arrow represents to heat direction.
Fig. 4 is Ti
50Ni
49Nb
1Alloy cube matherial at room temperature, draught be 15% cold rolling after thermal expansion heating test curve.In Fig. 4, X-coordinate be temperature T emperature (℃), ordinate zou is relative length changes delta l/l (* 10
-4), arrow represents to heat direction.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1: the preparation room temperature amount of pressing down down is 9% Ti
46.3Ni
44.7Nb
9Cold rolling bulk
Take by weighing 46.3% purity and be 99.9% titanium, 44.7% purity and be 99.5% nickel and 9% purity and be 99.9% niobium.Above-mentioned titanium, nickel and niobium raw material are put into non-consumable arc furnace, be evacuated to 6 * 10
-3Pa charges into high-purity argon gas to 0.7 * 10
5Pa 2800 ℃ of melt backs 5 times, obtains the nickel titanium niobium negative thermal expansion alloy ingot then.The above-mentioned nickel titanium niobium negative thermal expansion alloy ingot that makes is rolled into bulk under 850 ℃ of temperature.The above-mentioned NiTiNb bulk alloy that makes is cut into tabular with wire cutting method, puts into vacuum heat treatment furnace and heat-treat, vacuum tightness is 5 * 10
-3Pa behind 850 ℃ of following insulation 24h of thermal treatment temp, cools off in air.Alloy cube matherial is at room temperature carried out same rolling direction, draught be 9% cold rolling.Above-mentioned sample after cold rolling is cut sample with the method for line cutting along rolling direction, promptly obtain requirement of the present invention the thermal expansivity test sample.
Adopt NETZSCH DIL 402C thermal dilatometer to carry out the test of thermal expansivity, sample length is greater than 10mm, resulting specimen length relative variation curve as shown in Figure 1, shrinking when nickel titanium niobium negative thermal expansion alloy heats up as can see from Figure 1, is-1.3 * 10 at-100～40 ℃ averages coefficient of linear expansion
-6℃
-1Shrinking during cooling, is-6.5 * 10 at 40～-100 ℃ averages coefficient of linear expansion
-7℃
-1
Embodiment 2: draught is 7% Ti under the preparation liquid nitrogen temperature
44Ni
47Nb
9Cold rolling bulk
Take by weighing 44% purity and be 99.9% titanium, 47% purity and be 99.5% nickel and 9% purity and be 99.9% niobium.Above-mentioned titanium, nickel and niobium raw material are put into non-consumable arc furnace, be evacuated to 3 * 10
-3Pa charges into high-purity argon gas to 0.6 * 10
5Pa 2500 ℃ of melt backs 6 times, obtains the nickel titanium niobium negative thermal expansion alloy ingot then.The above-mentioned nickel titanium niobium negative thermal expansion alloy ingot that makes is rolled into bulk under 950 ℃ of temperature.The above-mentioned NiTiNb bulk alloy that makes is cut into tabular with wire cutting method, puts into vacuum heat treatment furnace and heat-treat, vacuum tightness is 4 * 10
-3Pa behind 950 ℃ of following insulation 24h of thermal treatment temp, cools off in air.Alloy cube matherial is carried out same rolling direction under liquid nitrogen temperature, draught be 7% cold rolling.Above-mentioned sample after cold rolling is cut sample with the method for line cutting along rolling direction, promptly obtain requirement of the present invention the thermal expansivity test sample.
Adopt NETZSCH DIL 402C thermal dilatometer to carry out the test of thermal expansivity, sample length is greater than 10mm, resulting specimen length relative variation curve as shown in Figure 2, shrinking when nickel titanium niobium negative thermal expansion alloy heats up as can see from Figure 2, is-2.0 * 10 at-40～50 ℃ averages coefficient of linear expansion
-6℃
-1
Embodiment 3: the preparation room temperature amount of pressing down down is 3% Ti
42Ni
40Nb
18Cold rolling bulk
Take by weighing 42% purity and be 99.9% titanium, 40% purity and be 99.5% nickel and 18% purity and be 99.9% niobium.Above-mentioned titanium, nickel and niobium raw material are put into non-consumable arc furnace, be evacuated to 5 * 10
-3Pa charges into high-purity argon gas to 0.6 * 10
5Pa 2700 ℃ of melt backs 6 times, obtains the nickel titanium niobium negative thermal expansion alloy ingot then.The above-mentioned nickel titanium niobium negative thermal expansion alloy ingot that makes is rolled into bulk under 900 ℃ of temperature.The above-mentioned NiTiNb bulk alloy that makes is cut into tabular with wire cutting method, puts into vacuum heat treatment furnace and heat-treat, vacuum tightness is 2 * 10
-3Pa behind 900 ℃ of following insulation 48h of thermal treatment temp, cools off in air.Alloy cube matherial is at room temperature carried out same rolling direction, draught be 3% cold rolling.Above-mentioned sample after cold rolling is cut sample with the method for line cutting along rolling direction, promptly obtain requirement of the present invention the thermal expansivity test sample.
Adopt NETZSCH DIL 402C thermal dilatometer to carry out the test of thermal expansivity, sample length is greater than 10mm, resulting specimen length relative variation curve as shown in Figure 3, when nickel titanium niobium negative thermal expansion alloy heats up as can see from Figure 3 is negative expansion, is-2.2 * 10 at-140～60 ℃ averages coefficient of linear expansion
-6℃
-1
Embodiment 4: the preparation room temperature amount of pressing down down is 15% Ti
50Ni
49Nb
1Cold rolling bulk
Take by weighing 50% purity and be 99.9% titanium, 49% purity and be 99.5% nickel and 1% purity and be 99.9% niobium.Above-mentioned titanium, nickel and niobium raw material are put into non-consumable arc furnace, be evacuated to 4 * 10
-3Pa charges into high-purity argon gas to 0.5 * 10
5Pa 2900 ℃ of melt backs 5 times, obtains the nickel titanium niobium negative thermal expansion alloy ingot then.The above-mentioned nickel titanium niobium negative thermal expansion alloy ingot that makes is rolled into bulk under 800 ℃ of temperature.The above-mentioned NiTiNb bulk alloy that makes is cut into tabular with wire cutting method, puts into vacuum heat treatment furnace and heat-treat, vacuum tightness is 3 * 10
-3Pa behind 800 ℃ of following insulation 36h of thermal treatment temp, cools off in air.Alloy cube matherial is at room temperature carried out same rolling direction, draught be 15% cold rolling.Above-mentioned sample after cold rolling is cut sample with the method for line cutting along rolling direction, promptly obtain requirement of the present invention the thermal expansivity test sample.
Adopt NETZSCH DIL 402C thermal dilatometer to carry out the test of thermal expansivity, sample length is greater than 10mm, resulting specimen length relative variation curve as shown in Figure 4, shrinking when nickel titanium niobium negative thermal expansion alloy heats up as can see from Figure 4, is-2.1 * 10 at-140～60 ℃ averages coefficient of linear expansion
-6℃
-1
Claims (10)
1. nickel titanium niobium negative thermal expansion alloy is characterized in that its composition and is nickel 40%～49%, titanium 42%～50%, niobium 1%～18% by the content of atomic percent.
2. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 1 is characterized in that may further comprise the steps:
1) nickel, titanium and niobium raw material are put into stove, vacuumize, charge into argon gas,, get nickel titanium niobium alloy ingot 2500～2900 ℃ of meltings;
2) with nickel titanium niobium alloy ingot 800～950 ℃ of hot rollings, nickel titanium niobium alloy ingot is rolled into bulk alloy;
3) bulk alloy that obtains is encapsulated in the silica tube interior heat and handles, thermal treatment temp is 800～950 ℃, cools off in air;
4) cooled bulk alloy is carried out the cold rolling of 3%～15% draught along same direction, promptly obtain nickel titanium niobium negative thermal expansion alloy.
3. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that the purity of nickel, titanium and niobium raw material is not less than 99.5%.
4. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that described stove is a non-consumable arc furnace.
5. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that vacuum tightness at least 6 * 10 that vacuumize
-3Pa; Charge into argon gas to 0.5～0.7 * 10
5Pa.
6. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that the number of times of 2500～2900 ℃ of meltings 5 times at least.
7. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that the bulk alloy that will obtain is encapsulated in the silica tube interior heat and handles and will vacuumize in the silica tube, and vacuum tightness is 2 * 10
-3～5 * 10
-3Pa.
8. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that heat treatment period 24h at least.
9. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that bulk alloy cuts into tabular alloy before being encapsulated in the processing of silica tube interior heat, and the thickness of tabular alloy is 6～8mm.
10. the preparation method of nickel titanium niobium negative thermal expansion alloy as claimed in claim 2 is characterized in that described cold rolling temperature is a room temperature or below the room temperature.
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| CN101805843A (en) * | 2010-04-16 | 2010-08-18 | 中国石油大学(北京) | NbTi/TiNi memory alloy composite material and preparation method thereof |
| CN101886188A (en) * | 2010-04-08 | 2010-11-17 | 厦门大学 | Beta titanium alloy and preparation method thereof |
| CN102357622A (en) * | 2011-07-08 | 2012-02-22 | 宝鸡三线有色金属制造有限公司 | Technology for preparing titanium-nickel-niobium memory alloy pipes or rings |
| CN104237280A (en) * | 2014-09-05 | 2014-12-24 | 北京科技大学 | Method for detecting solid-phase reaction between inclusions and alloy matrix in thermal treatment process |
| CN105821246A (en) * | 2016-05-06 | 2016-08-03 | 中国科学院理化技术研究所 | Preparation method for titanium alloy with nearly-zero thermal expansion characteristic |
| CN105886981A (en) * | 2016-05-06 | 2016-08-24 | 中国科学院理化技术研究所 | Alloy sealing element with negative thermal expansion property |
| CN107164653A (en) * | 2017-04-13 | 2017-09-15 | 华南理工大学 | A kind of rich Ti content Ti-Ni alloy with negative expansion performance and preparation method thereof |
| CN109554578A (en) * | 2018-12-21 | 2019-04-02 | 中国工程物理研究院机械制造工艺研究所 | A kind of negative expansion memorial alloy and preparation method thereof |
| CN110646461A (en) * | 2018-06-27 | 2020-01-03 | 上海梅山钢铁股份有限公司 | Method for measuring continuous cooling phase transition temperature of ultrathin gauge thickness steel plate |
| CN112680681A (en) * | 2020-11-27 | 2021-04-20 | 东南大学 | Preparation method of titanium-niobium alloy with adjustable negative thermal expansion coefficient |
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|---|---|---|---|---|
| CN101886188A (en) * | 2010-04-08 | 2010-11-17 | 厦门大学 | Beta titanium alloy and preparation method thereof |
| CN101805843A (en) * | 2010-04-16 | 2010-08-18 | 中国石油大学(北京) | NbTi/TiNi memory alloy composite material and preparation method thereof |
| CN101805843B (en) * | 2010-04-16 | 2011-11-16 | 中国石油大学(北京) | NbTi/TiNi memory alloy composite material and preparation method thereof |
| CN102357622A (en) * | 2011-07-08 | 2012-02-22 | 宝鸡三线有色金属制造有限公司 | Technology for preparing titanium-nickel-niobium memory alloy pipes or rings |
| CN104237280A (en) * | 2014-09-05 | 2014-12-24 | 北京科技大学 | Method for detecting solid-phase reaction between inclusions and alloy matrix in thermal treatment process |
| CN105886981A (en) * | 2016-05-06 | 2016-08-24 | 中国科学院理化技术研究所 | Alloy sealing element with negative thermal expansion property |
| CN105821246A (en) * | 2016-05-06 | 2016-08-03 | 中国科学院理化技术研究所 | Preparation method for titanium alloy with nearly-zero thermal expansion characteristic |
| CN105886981B (en) * | 2016-05-06 | 2017-07-11 | 中国科学院理化技术研究所 | A kind of alloy seal part with negative expansion property |
| CN107164653A (en) * | 2017-04-13 | 2017-09-15 | 华南理工大学 | A kind of rich Ti content Ti-Ni alloy with negative expansion performance and preparation method thereof |
| CN107164653B (en) * | 2017-04-13 | 2019-05-14 | 华南理工大学 | A kind of rich Ti content Ti-Ni alloy and preparation method thereof with negative expansion performance |
| CN110646461A (en) * | 2018-06-27 | 2020-01-03 | 上海梅山钢铁股份有限公司 | Method for measuring continuous cooling phase transition temperature of ultrathin gauge thickness steel plate |
| CN110646461B (en) * | 2018-06-27 | 2022-05-10 | 上海梅山钢铁股份有限公司 | Method for measuring continuous cooling phase transition temperature of ultrathin gauge thickness steel plate |
| CN109554578A (en) * | 2018-12-21 | 2019-04-02 | 中国工程物理研究院机械制造工艺研究所 | A kind of negative expansion memorial alloy and preparation method thereof |
| CN112680681A (en) * | 2020-11-27 | 2021-04-20 | 东南大学 | Preparation method of titanium-niobium alloy with adjustable negative thermal expansion coefficient |
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| CN100545283C (en) | 2009-09-30 |
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