CN1399005A - Prepn of shape memory alloy film with very small heat stagnation - Google Patents
Prepn of shape memory alloy film with very small heat stagnation Download PDFInfo
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Abstract
The present invention invention belongs to the field of film material and film technology. The invented very small thermo-lag shape memory alloy film consists of two-element NiTi alloy with Ni 51.9-52.6 wt% and Ti 47.4-48.1 wt% and has a thickness of 5-8 microns. It is prepared through magnetically controlled sputtering and post-crystallizing process including the step of: selecting cast NiTi alloy as sputtering target; sputtering NiTi film and post-crystallizing treatment of the NiTi film. The present invention has typical R phase change characteristic at room temperature, and can take complete R phase change and inverse phase change. NiTi/Si driving film has characteristic frequency up to 400 Hz and obvious raised dynamic characteristic. The present invention raises the response frequency of the shape memory alloy.
Description
Technical field
That the present invention relates to is a kind of preparation method's of shape memory alloy film, particularly a kind of shape memory alloy film with very small heat stagnation preparation method, belongs to the micro-processing technology field.
Background technology
Shape memory alloy is used as the detection and the controlling elements of temperature and power owing to its unique mechanical characteristic, is used widely.Its Application Areas relates to Industry Control, various fields such as electronic technology, health care, aerospace, military and national defense.The NiTi shape memory alloy is to use one of maximum shape memory alloy material at present.Through the research of decades accumulation, its body material forms as, the utilisation technology of piece, plate, strip, silk is very ripe.From the eighties in last century, fast development along with micro electro mechanical system (MEMS) technology, the research of the important and key part-mini drive in this technology has been caused the extensive attention of countries in the world research institutions, and the gordian technique of research comprises little technology of preparing of functional materials preparation, drives structure design and driving mechanism etc.At present the main drive principle of microdrive have that piezoelectricity, static, electromagnetism, hot gas are moving, bimetallic effect and shape memory effect driving etc.In above-mentioned various type of drive, the merit density maximum that shape memory alloy drives reaches 5 * 10
7J/m
3, drive big nearly two orders of magnitude of merit density than other, be acknowledged as a kind of comparatively ideal type of drive.The shape memory alloy material of form of film is because preparation technology and other micro fabrication compatibility are good, and has bigger surface-area and volume ratio, can improve rate of heat exchange, compares response speed with shape memory alloy body material and increases.Therefore, in the research of microdrive and transmitter, the research of the shape memory alloy film of excellent performance there is very important meaning.In existing relevant NiTi base marmem film microdrive research report, majority is based on martensitic transformation in the NiTi material and realizes shape memory effect.The patentee is: Shanghai Communications University, the patent No. is: 99113953.4, this patent has proposed a kind of Micropump that adopts shape-memory alloy/silicon double-layer film drives structure, Micropump is made up of microdrive, pump housing and little valve, core technology is the top direct deposition shape memorial alloy film at the pump housing of silicon formation, but forms the NiTi/Si drive membrane of bidirectional-movement.In above-mentioned shape-memory alloy/silicon Micropump, shape memory alloy film is the NiTi material, and material phase transformation mainly changes between the austenite of the martensitic phase of monocline and high temperature body-centered cubic structure mutually.Follow martensitic transformation, gathering and relaxing of thermal stresses takes place, thereby cause change in displacement.Though the dependent variable of martensitic transformation is bigger, needed temperature province from the martensitic transformation to the austenite phase transformation (being the phase transformation heat stagnation) broad is generally 20-30 ℃.This means when phase transformation needs the more heating and cooling time to overcome heat stagnation, has therefore limited the raising of driving frequency.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of shape memory alloy film with very small heat stagnation is provided.On the basis of existing technology, the R phase transformation shape memory alloy that has minimum heat stagnation by employing has obviously improved the kinetic characteristic of microdrive as main driving material.The present invention realizes according to following technical scheme: R becomes diamond structure mutually, also is a kind of thermoelastic martensitic transformation, and its outstanding feature is to have minimum phase transformation heat stagnation, and the heat stagnation width only is about 0-2 ℃.In addition, transformation temperature influences all more stable to thermal cycling, stress, composition.Though the recoverable strain or the displacement of R phase transformation are little than martensitic transformation, but because the decline significantly of heat stagnation, cold-hot descends cycling time when causing changing mutually, makes in the upper frequency section, help the raising of phase transformation generation and degree of transformation, thereby improve displacement and Frequency Response comprehensively.In driving mechanism with the shape memory alloy film preparation, the general applying pulse electric current that adopts heats shape memory alloy film, when temperature in the film when phase change region changes, the phase transformation of film generating period, stress gathers thereupon and relaxes, and makes driving mechanism produce the reciprocating machine vibration.Because the phase transformation heat stagnation has directly influenced the time of complete phase transformation, the just size of phase variable period.So, reduce the cycle that heat stagnation can shorten vibration, improve vibrational frequency.From the material angle, utilize the minimum heat stagnation characteristic of R phase transformation to improve the Frequency Response of shape memory alloy film driving mechanism, be a kind of effective and easy row method.
Shape memory alloy film with very small heat stagnation of the present invention is the NiTi binary alloy, and its weight percent is: Ni:52.6-51.9%, Ti:47.4-48.1%, thickness are the 5-8 micron, and be soft and yielding.The above phase transition process of room temperature is that R phase transformation and reverse transformation are austenite phase transformation, has complete phase change characteristics.R phase transformation medial temperature is 50 ℃-70 ℃, and phase transformation heat stagnation width is almost 0-2 ℃, and membrane structure is R phase and a spot of Ti during room temperature
2The Ni precipitated phase.
By selecting the component and the thin film deposition of NiTi material, can obtain the shape memory alloy film of the above complete R phase structure of room temperature, key is: the strictness of (1) NiTi component control, because phase change structure and transformation temperature have the intensive dependency to the ratio of component; The selection of (2) thin film deposition parameter, depositing of thin film process can influence film forming component and film internal stress situation.(3) the crystallization process parameter is determined.By the back crystallization after the thin film deposition is handled, can effectively control precipitated phase, the R phase transformation is separated with martensitic transformation, and transformation temperature is controlled at more than the room temperature.The present invention adopts magnetically controlled sputter method and back crystallization and thermal treatment, selects appropriate parameters to prepare shape memory alloy film with very small heat stagnation, and the preparation method is specific as follows:
(1) select for use NiTi cast alloy material as sputtering target material, strict control NiTi component, the Ti that determines to take an examination when considering sputter of target composition consumes more, guarantees that post-depositional film has certain Ti content, weight percent is: Ni:52.6-51.9%, Ti:47.4-48.1%.
(2) sputtering sedimentation of NiTi film, the parameters when sputter initial vacuum environment and deposition has the certain influence rule to film composition and stress, need select and optimize.Common thin film sputtering parameter is: the base vacuum degree before the sputter: 4-8 * 10
-5Pa; Argon gas is as working gas during sputter, and pressure is 0.1-0.8Pa; Sputtering power is 150W-250W; Sputtering time 100-180 minute; Substrate does not heat during sputter, and resulting film is a non-crystalline state after the sputter, and film need carry out the back crystallization to be handled.
(3) the back crystallization of NiTi film is handled, and adopts the photo-thermal rapid heating furnace, carries out under argon shield atmosphere, and the crystallization processing parameter is: temperature is 500-550 ℃, and the time is 20-30 minute.The certain NiTi alloy of Ti content precipitated phase can occur when crystallization, utilize the effect of precipitation hardened inhibition martensitic transformation, and the R phase transformation is separated from martensitic transformation, and can independent appearance more than room temperature.The temperature and time may command amount of separating out of crystallization, crystallization temperature are crossed the low crystallization degree that can influence film, and too high meeting weakens the restraining effect to martensitic transformation.Therefore, phase transformation is very crucial to control R in the selection of suitable crystallization temperature.
The present invention has substantive distinguishing features and marked improvement, the film of the inventive method preparation, has the typical R phase change characteristics during room temperature, it is carried out heating-refrigeration cycle more than the room temperature, can produce heat stagnation and be approximately zero complete phase transition process, compare with 20-30 ℃ of heat stagnation of martensitic transformation, greatly improve the Frequency Response of drive membrane.When shape memory alloy film is applied the pulse heating electric current, R phase transformation completely and reverse transformation can take place, the characteristic frequency of NiTi/Si drive membrane can reach 400Hz, and kinetic characteristic obviously improves.From the material angle, preferably resolve the not high built-in problem of shape memory alloy response frequency, widened the range of application of shape memory alloy film in MEMS (micro electro mechanical system).
Embodiment
Embodiment 1:
Adopt glass substrate, the base vacuum degree before the sputter: 8 * 10
-5Pa; Sputtering Ar operating air pressure: 0.8Pa; Sputtering power is 250W; Sputtering time 100 minutes; Crystallization temperature is 500 ℃, and the time is 30 minutes.The weight percent of the film composition that deposition obtains is: Ni:52.6%, Ti:47.4%, thickness are 5 microns.After film peeled off from substrate, soft and yielding, satisfactory mechanical property.Resistance-temperature test curve shows that the above phase transition process of room temperature is that R phase transformation and reverse transformation are austenite phase transformation, has complete phase change characteristics.R phase transformation medial temperature is 58 ℃, and phase transformation heat stagnation width is almost 0 ℃.X diffraction analysis result shows that membrane structure is R phase and a spot of Ti during room temperature
2The Ni precipitated phase.
Embodiment 2:
Ni:51.9%, Ti:48.1%, thickness are 8 microns.But with thin film deposition in Micropump silicon cavity top deformation region, as the driving mechanism of Micropump.Sputtering condition is: base vacuum degree: 6 * 10
-5Pa; Argon gas operating air pressure: 0.4Pa; Sputtering power is 200W; Sputtering time 110 minutes; Crystallization temperature is 530 ℃, and the time is about 30 minutes.
Obtain film thickness through above-mentioned sputtering parameter deposition and be about 5 microns, room temperature is above to be the R phase transformation.Film to its pulsed current heating that applies certain frequency, produces periodically phase transformation after the resistance bar shapedization.Measure the change in displacement of NiTi/Si film respectively with R phase transformation and martensitic transformation with interference of light micro displacement meter.During less than 20Hz, the drive membrane displacement with R phase transformation is littler than the drive membrane with certain martensitic transformation in frequency.But when frequency was higher than 20Hz, wanting of the displacement inverse ratio martensitic transformation of R phase transformation was big, and displacement still can reach 0.5 micron when 400Hz, and characteristic frequency is 4 times of martensitic transformation feature.
Embodiment 3:
Ni:52.25%, Ti:47.75%, but thickness be 6.5 microns with thin film deposition in Micropump silicon cavity top deformation region, as the driving mechanism of Micropump.Sputtering condition is: base vacuum degree: 4 * 10
-5Pa; Argon gas operating air pressure: 0.1Pa; Sputtering power is 150W; Sputtering time 120 minutes; Crystallization temperature is 550 ℃, and the time is about 20 minutes.
Above-mentioned condition deposit has obtained to have R phase character shape-memory alloy/silicon drive membrane, and is assembled in the Micropump.Driving under the identical condition of area, shape, relatively the working condition of R phase transformation and martensitic transformation.Characteristic frequency during R phase transformation Micropump water ballast can reach 167Hz (flow is 7um/min), and characteristic frequency is to have 6 times of martensitic transformation.In addition, the high reliability of original martensitic transformation feature Micropump and the advantage of long service live have still been kept.
Claims (3)
1, a kind of preparation method of shape memory alloy film with very small heat stagnation is characterized in that film is made of the NiTi binary alloy, and its weight percent is: Ni:52.6-51.9%, Ti:47.4-48.1%, thickness are the 5-8 micron.
2, the preparation method of this shape memory alloy film with very small heat stagnation according to claim 1 is characterized in that the preparation method is specific as follows: (1) selects for use NiTi cast alloy material as sputtering target material; (2) the sputtering sedimentation parameter of NiTi film is: the base vacuum degree before the sputter: 4-8 * 10
-5Pa, argon gas is as working gas during sputter, and pressure is 0.1-0.8Pa, and sputtering power is 150W-250W; (3) the back crystallization of NiTi film is handled, and adopts the photo-thermal rapid heating furnace, carries out under argon shield atmosphere, and the crystallization treatment process is: temperature is 500-550 ℃, and the time is 20-30 minute.
3, the preparation method of this shape memory alloy film with very small heat stagnation according to claim 1, it is characterized in that the above phase transition process of film room temperature is R phase transformation and reverse transformation, R phase transformation medial temperature is 50 ℃-70 ℃, phase transformation heat stagnation width is 0-2 ℃, and membrane structure is R phase and a spot of Ti during room temperature
2The Ni precipitated phase.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317419C (en) * | 2004-12-02 | 2007-05-23 | 上海交通大学 | Process for preparing TiNiPd shape memory alloy free film |
| CN100431157C (en) * | 2006-01-24 | 2008-11-05 | 河北大学 | Oxide ferroelectric memory cell and prepn process |
| CN100462473C (en) * | 2007-04-11 | 2009-02-18 | 北京航空航天大学 | Medical TiNi shape memory alloy sputtered by TiTaCo composite film on surface and its production |
| CN105840701A (en) * | 2016-05-31 | 2016-08-10 | 尔智机器人（上海）有限公司 | Bidirectional power output shape memory alloy and preparing method thereof |
| CN107242911A (en) * | 2017-05-09 | 2017-10-13 | 深圳市速航科技发展有限公司 | Flexible root canal file of a kind of Nitinol gradient and preparation method thereof |
-
2002
- 2002-08-29 CN CN 02136712 patent/CN1399005A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317419C (en) * | 2004-12-02 | 2007-05-23 | 上海交通大学 | Process for preparing TiNiPd shape memory alloy free film |
| CN100431157C (en) * | 2006-01-24 | 2008-11-05 | 河北大学 | Oxide ferroelectric memory cell and prepn process |
| CN100462473C (en) * | 2007-04-11 | 2009-02-18 | 北京航空航天大学 | Medical TiNi shape memory alloy sputtered by TiTaCo composite film on surface and its production |
| CN105840701A (en) * | 2016-05-31 | 2016-08-10 | 尔智机器人（上海）有限公司 | Bidirectional power output shape memory alloy and preparing method thereof |
| CN107242911A (en) * | 2017-05-09 | 2017-10-13 | 深圳市速航科技发展有限公司 | Flexible root canal file of a kind of Nitinol gradient and preparation method thereof |
| CN107242911B (en) * | 2017-05-09 | 2019-10-01 | 深圳市速航科技发展有限公司 | A kind of Nitinol gradient flexibility root canal file and preparation method thereof |
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