CN106198206A - A kind of thin film high temperature mechanical property measuring device and method - Google Patents
A kind of thin film high temperature mechanical property measuring device and method Download PDFInfo
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- CN106198206A CN106198206A CN201610817983.7A CN201610817983A CN106198206A CN 106198206 A CN106198206 A CN 106198206A CN 201610817983 A CN201610817983 A CN 201610817983A CN 106198206 A CN106198206 A CN 106198206A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
- G01N3/06—Special adaptations of indicating or recording means
- G01N3/068—Special adaptations of indicating or recording means with optical indicating or recording means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
- G01N3/18—Performing tests at high or low temperatures
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Abstract
The invention discloses a kind of thin film high temperature mechanical property measuring device and method, measurement apparatus includes: optical measurement components, data process and display module, power charging assembly, heating assembly and sample stage, wherein optical measurement components, heating assembly, sample stage and power charging assembly set gradually, the light source and the hot spot that send during measurement are constant, bulge effect makes thin film deform upon, the transmission light path being sent to thin film changes owing to thin film deformation makes angle of reflection produce, the optical measurement components receiving reflected light path remotely connects data process and display module, receiving light path is obtained by optical measurement components and is processed by data and display module visual display measurement process record the change of receiving light path.Firing equipment is combined with bulge equipment and jointly realizes the measurement of thin film mechanical performance, compact conformation under high temperature by the present invention, it is adaptable to the thin film under various elastoplastic systems, can realize real-time, the measurement of full field of the change of its mechanical property in heating process.
Description
Technical field
The present invention relates to thin film mechanics behavior measurement of full field device and method under a kind of high temperature, belong to optical measurement mechanics, structure
Deformation and Experiments of Machanics technical field.
Background technology
Thin film refers to that the yardstick of its thickness direction is far smaller than the material structure of other direction yardsticks, and thickness is usually no more than
10 μm, owing to it is different from matrix material and has certain strengthening, protection or specific function, therefore at micro-nano, microelectronics
And in the technical field such as material, the application of thin film is quite varied.Membrane science and technology are microelectronics, information, sensor, light
The basis of the technology such as, Solar use, it penetrates into the every field of contemporary science and technology the most widely.In order to adapt to high intensity,
The different commercial Application requirements such as wear-resisting, high temperature resistant, corrosion-resistant, generally use the various process for treating surface such as surface coating to material
Surface is processed so that it is be suitable for the working environment of various complexity.Thin film technique is also microelectronic component and micro-electro-optical device
Basis, recent thin film technique more promotes rise and the development of microelectron-mechanical group system (MEMS).
Along with the development of membrane science technology, people have appreciated that the mechanical property research of thin-film material is for thin-film material
Production and normal use have very important significance.The mechanical property of thin film is mainly concerned with the elastic modelling quantity of thin film, bends
Take intensity, residual stress and interface bond strength etc..The elastic modelling quantity of thin film not only can be used in the design of thin-film device, and
And be also the basis of yield strength, fracture toughness and residual stress measurement and evaluation；Thin film in preparation process due to thin film with
The coefficient of thermal expansion of matrix and the difference of physical characteristic and residual stress in the film that causes, and wrinkling, the cracking of thin film may be caused,
Serious meeting causes film base to separate；Film base interfacial combined function is the key factor determining membrane element device service life.Therefore,
The mechanical property of thin film is the foundation of thin-film device design, is one of the important topic of current thin film study.
At present the test method of film performance test and sign mainly there are bulge method, Nanoindentation, pulling method, stripping
Measurement method etc..In these existing method of testings, Bubbling method physical thought is simple, is a kind of springform that both can determine that thin film
Amount, residual stress, can really transport again the important experimental technique of interface bonding energy, bulge method is simple because of its principle, certainty of measurement simultaneously
Height, and the advantages such as the elastic modelling quantity to thin film, Poisson's ratio, residual stress, yield limit can be realized, sent out the most rapidly
Exhibition, it has also become a kind of important method measuring thin film mechanical performance.
Along with improving constantly of flexible electronic technology and large scale integrated circuit integrated level, some flexible electronic products are
Arise at the historic moment, such as flexible display, utilize the thin-film solar cell panel etc. that flexible electronic technology makes.For microelectronics and half
Multi-layer film structure in conductor industry, every layer film all has different mechanics, physically and thermally conductive properties.In these devices
Thin film under arms during not only by power load, suffer from the effect of thermal force, device heat dissipation design is unreasonable just
Device reliability can be caused poor, occur the probability of damage inactivation to increase, the ductility of device will reduce.So needing to send out
The mechanical property of thin film is characterized by exhibition at different temperatures.
Chinese patent CN101355046A discloses the on-line measurement of a kind of multi-layer film basal body structure high-temperature mechanical behavior
Device.Firing equipment and optical device, by being transformed by traditional heating furnace, are combined and jointly realize height by this device
The stress measurement of the lower multi-layer film basal body structure of temperature.This apparatus structure is compact, can realize multi-layer film basal body structure in heating
During mechanical property change online, monitor in real time, but it is disadvantageous in that: measures object single, and requires sample
Curvature obvious by variations in temperature, only change the change of curvature by changing temperature.
Chinese patent CN104677748A discloses a kind of tympanum device for measuring thin film mechanical performance.This device
Thin plate is fixedly positioned on the inner bag of furnace interior near body of heater upper edge, and lid is positioned at above thin plate, and cover inside has
Flange so that after lid and body of heater are by Screw assembly, thin plate is pressed together by the flange of cover inside with inner bag edge,
And having space between thin plate and lid, heater is placed in bottom of furnace body, pressue device passes through the first pipeline and furnace interior
Being connected, controller is exported to institute by the pressure and temperature data in the temperature in polygon control survey body of heater and the body of heater that will record
Stating controller, optical microscope is placed in above transparent observation window for observing the three dimensional topography of tympanum on thin plate.It is not
Being in place of foot, the parts in addition to controller, optical microscope are all in inside heating furnace, and film sample to be measured preparation is multiple
Miscellaneous, thin film need to be made to be grown in advance in the substrate of glass of a layer photoetching glue, add thin film photolithography plastic structure the most again and be stamped in thin
On plate, and its pressue device loading velocity cannot stability contorting.
Device disclosed in Chinese patent CN101788427A uses Digital Speckle Correlation Method to measure deformation of thin membrane, combining drum
Bubble method and improvement move layer method both mechanical measuring and calculation method, can convenient, fast and also accurately measure pressure-deformation curve or
Person's corrosion thickness-deformation curve, obtains the mechanical property with coating according to corresponding theory model extraction, it is adaptable to various elastoplasticity
The instrument film of system, decorating film, polymeric membrane and the mensuration of other film types mechanical properties.But, thin-film material is in processing
During becoming device and using, owing to thin film also exists difference, therefore at machinery with base material at aspects such as performance and sizes
The mismatch of stress, strain can be produced under the various complex environment such as load, thermal force, cause the inefficacy of thin-film material；And thin film
Working environment more complicated, usually can be affected by environmental factorss such as temperature.But all measurements of this device are all often
Carry out under temperature, it is impossible to meet the requirement that under hot conditions, thin film mechanical performance is measured.
Chinese patent CN102081140 discloses and tests metallic film inefficacy row under a kind of power/heat/electro magnetic multi-scenarios method
For device, the warm table of embedded resistance wire is placed in heat insulation top, and warm table connects power supply, and it is right that heat insulation two ends are provided with
Stream recirculated cooling water；Tested metallic film is placed in above warm table, and arranges thermocouple, nanometer press-in transmission dress at specimen surface
Putting connection driven rod, the driven rod both sides between nanometer press-in transporter and tested metallic film dispose thermal baffle respectively,
Every piece of thermal baffle both sides arrange recirculated cooling water, and magnetic pole is placed in heat insulation both sides.This device is the basis at nano-hardness tester
On reequip.The mode of heating that it uses is to arrange a warm table below film sample to be measured, by the temperature of warm table
Degree is delivered to sample surfaces, and the temperature sensitive property of measurement result of nano-hardness tester is the highest, it is therefore desirable to for this equipment configurations
Cooling system, and the temperature range of heating is the most limited.
To sum up, for existing problem and existing technology, it would be desirable to thin film mechanics under research power thermal coupling effect
The change of energy.Therefore, we have invented a kind of thin film high temperature mechanical property measuring device and method, available thin film is in not equality of temperature
Multiple thin film mechanical performance parameters such as elastic modelling quantity under Du, interface bonding energy, strain-stress relation, interface shear strength.
Summary of the invention
The problems referred to above existed for prior art, it is an object of the invention to provide one can be at uniform temperature or temperature model
Enclose thin film high temperature mechanical property measuring device and the method for the interior measurement of full field realizing thin film mechanics behavior.
For achieving the above object, the technical solution used in the present invention is as follows:
One goal of the invention of the present invention is to provide a kind of thin film high temperature mechanical property measuring device, its measurement apparatus bag
Include: optical measurement components, data process and display module, power charging assembly, heating assembly and sample stage, wherein optical measurement
Assembly, heating assembly, sample stage and power charging assembly set gradually, in other words, and optical measurement components, heating assembly, sample
Platform and power charging assembly from top to bottom set gradually, and during measurement in the case of transmission light path is constant, bulge effect makes thin
Film deforms upon, and optical measurement components remotely connects data and processes and display module, and data process and display module is visual
Show measurement process and record the change of receiving light path.
Preferably, heating assembly is vertical heater, including: heating furnace body, resistance wire, temperature sensor and control
Device, carries out the bulge experiment of film sample to be measured in heating-furnace body, resistance wire is uniformly arranged along the inwall of heating furnace body, heating
The top of furnace body is provided with an observation window, and controller can control the temperature of heating.
It is furthermore preferred that the heating-up temperature of measurement apparatus is 0～400 DEG C.
It is furthermore preferred that inboard wall of furnace body is additionally provided with temperature sensor, for monitoring feedback temperature in real time, preferred as one
Embodiment, temperature sensor is electroheat pair temperature sensor.
It is furthermore preferred that heating furnace body is heat-insulating heat-preserving material.
It is furthermore preferred that optical measurement components is observed by the observation window at heating furnace top.
It is further preferred that optical measurement components includes light source, speckle parts processed, lens assembly and photographic head parts, light source,
Speckle parts processed, telecentric lens are sequentially connected to send in light path, and photographic head parts are connected in receiving light path.
As one preferred embodiment, lens assembly includes telecentric lens, launches white light, for being arrived by dot projection
Film sample surface to be measured, photographic head parts are CCD camera, for capturing the change of light path and situation of change being transferred to number
According to processing and display module.
Preferably, power charging assembly includes motor, piston, oil pocket and pressure transducer.
It is furthermore preferred that oil pocket is connected with piston built with high temperature resistant silicone oil, oil pocket side, opposite side and film sample to be measured
Connect.
Preferably, measurement apparatus also includes a base, and base is placed in bottom power charging assembly.
It is furthermore preferred that base bottom is provided with a displacement governor motion, it is used for regulating film sample position to be measured and is positioned at shooting
The center of head member visual field.
It is furthermore preferred that sample stage is lifting structure, need to carry out lift adjustment according to the focusing of photographic head parts.
A kind of use is according to the measuring method of thin film high temperature mechanical property measuring device, and measuring method comprises the steps:
A. thin film is fixed in sample stage, unlatching light source and data handling component；
B. being enclosed within sample stage by heating furnace, regulate film sample to be measured and be positioned at the center of optical lens visual field, speckle becomes
As clear；
C. start controller, film sample to be measured is heated；
D. power charging assembly applies uniform pressure to film sample to be measured, and data process and display module is used for controlling
Loading velocity；
E. pressure transducer Real-time Collection pressure data, corresponding deformation of thin membrane amount of deflection is surveyed by Digital Speckle Correlation Method
, thus obtain pressure (p)-central point amount of deflection (w) curve；
F. processed by data and image and data are analyzed by display module, obtain the mechanical property of film sample to be measured
Can parameter；
G. change heating-up temperature, repeat step a～f, obtain the mechanical property of film sample to be measured under different temperatures.
Preferably, step c particularly as follows:
Start controller, heat film sample to be measured and keep constant temperature to design temperature.
Preferably, step c particularly as follows:
Starting controller, heat film sample to be measured in the range of design temperature, in temperature range, pointwise is surveyed
Amount.
Preferably, step d particularly as follows:
By step motor drive piston, the oil plant in plunger forces fuel tank moves, and applies uniform to film sample to be measured
Pressure, data process and the loading velocity of display module control motor.
Preferably, mechanical property parameters includes: elastic modelling quantity, interface bonding energy, yield strength and stress-strain relation.
Compared with prior art, the present invention uses vertical heater to heat measurement apparatus and thin film to be measured, vertical
Heating furnace is placed in above sample stage, can load and unload easily, and vertical heater is column structure, and heater is distributed in
Body of heater surrounding, furnace temperature is uniform, and heating is fast, has that temperature measurement accuracy is high, temperature control is accurate, furnace temperature is uniform, thermal conductivity is low, energy-efficient etc.
Feature.
In a word, the thin film high temperature mechanical property measuring device of present invention offer and method, by firing equipment and bulge equipment
Combining and jointly realize the measurement of thin film mechanical performance under high temperature, vertical heater is placed in above sample stage, and small volume can
Conveniently load and unload, and height can be regulated along with sample stage, carry out the focusing of optical measurement；Use programming heating and cooling, add
Hot temperature range be room temperature to 400 DEG C, and have special program to realize the control of temperature, attainable function is at certain
Test at a temperature of Gu Ding, or in certain temperature range, realize thermal cycle, and the change of viewing film mechanical property,
Standing heater is to provide a temperature field sealed around thin film, and does not affect the light of thin film mechanical property at high temperature
Learn and measure；Controller passes through the temperature in polygon control survey environmental cabinet and the temperature data output extremely described controller that will record,
Optical features device is positioned at detection deformation of thin membrane situation above observation window.Measurement apparatus compact conformation of the present invention, it is not necessary to other are auxiliary
Helping equipment, temperature controls precisely, it is adaptable to the thin film under various elastoplastic systems, can realize its mechanical property in heating process
Real-time, the measurement of full field that can change.
Accompanying drawing explanation
Fig. 1 is the constructive embodiment schematic diagram of the measurement apparatus that the present invention provides.
Fig. 2 is the electrical schematics of the controller that the present invention provides.
Reference
1-optical measurement components, 11-light source, 12-speckle parts, 13-telecentric lens, 14-photographic head,
2-heats assembly, 21-controller, 22-body of heater, 23-resistance wire, 24-observation window, 25-temperature sensor
3-power charging assembly, 31-motor, 32-piston, 33-oil pocket, 34-pressure transducer,
4-data process and display module, 5-sample stage, 6-base, 7-film sample to be measured,
FU-insures, K-relay, T-thermocouple, A-ammeter, KP-controllable silicon, TA-stop button, QA-start button,
RL-loads, D-display lamp, TC-temperature controller.
Detailed description of the invention
The present invention is made the most in detail below in conjunction with embodiment and comparative example, intactly illustrates.
The embodiment schematic diagram of the thin film high temperature mechanical property measuring device of the present invention as shown in Figure 1.This device includes
Optical measurement components 1, heating assembly 2, power charging assembly 3 and data process and display module 4.Wherein optical measurement components 1,
Heating assembly 2, sample stage 5 and power charging assembly 3 set gradually, in other words, and optical measurement components 1, heating assembly 2, sample
Platform 3 and power charging assembly 3 from top to bottom set gradually, and during measurement in the case of transmission light path is constant, bulge effect makes
Thin film deforms upon, and optical measurement components 1 remotely connects data and processes and display module 4, and data process and display module 4 is visual
The display measurement process changed the change recording receiving light path.
Optical measurement components 1 includes light source 11, speckle parts 12 processed, telecentric lens 13 and photographic head 14.Light source 11, speckle portion processed
Part 12, telecentric lens 13 are sequentially connected to send in light path, and photographic head 14 is connected in receiving light path.Light source 11 sends light, excellent
Elect white light as, enter speckle parts 12 processed by optical fiber, after light is by the optical glass of speckle parts 12 processed, is the formation of speckle processed
Figure, projects the surface of film sample 7 to be measured by telecentric lens 13, dissipating after film sample surface topography to be measured is modulated
Speckle figure is received by photographic head 14 through telecentric lens 13 and is transferred to data and processes and display module 4.Photographic head 14 is preferably CCD
Photographic head, for capturing the change of light path and situation of change being transferred to data process and display module.
Above-mentioned white light source is only the preferred implementation in the present embodiment, and any can being connected in transmission light path is played
The monochromatic light of light source effect or polychromatic light all should fall into protection scope of the present invention.
Heating assembly 2 includes controller 21, body of heater 22, resistance wire 23, observation window 24 and temperature sensor 25.Controller 21
Controlling in-furnace temperature, in heating-furnace body, 22 carry out the bulge experiment of film sample to be measured, and resistance wire 23 is along heating furnace body 22
Inwall is uniformly arranged, and the top of heating furnace body 22 is provided with an observation window 24, and optical measurement components 1 is seen by observation window 24
Surveying, send light path and receiving light path enters to film sample 7 to be measured by observation window and reflects, heating furnace body temperature is
0～400 DEG C, body of heater uses heat-insulating heat-preserving material so that the temperature in body of heater keeps effect more preferable.Preferred temperature in the present embodiment
Degree sensor is T-shaped thermocouple temperature sensor, for Real-time Feedback in-furnace temperature.
Power charging assembly 3 includes motor 31, piston 32, oil pocket 33 and pressure transducer 34.It is resistance in oil pocket 33
High-temperature silicon oil, motor 31 drives lives, and applies uniform pressure to film sample to be measured, and the pressure in pressure process is by pressure
Sensor 34 Real-time Collection, corresponding deformation of thin membrane is recorded by optical measurement components 1.
The speckle pattern that optical measurement components 1 collects gives the meter that data handling component 4 carries out Digital Speckle Correlation Method
Calculate and analyze, obtain the three-dimensional appearance of deformation of thin membrane, speckle image is analyzed, calculate various under corresponding temperature of thin film
Mechanical property parameters, such as elastic modelling quantity, interface bonding energy, yield strength and stress-strain relation etc..
Sample stage 5 is used for fixing and support film sample 7 to be measured, and heating furnace is positioned at the top of sample stage, and sample stage 5 sets
There is steel cover plate (not shown), for spacing film sample to be measured.After used time sets film sample to be measured, bonnet will be heated
Being located at outside sample stage, sample stage both sides are slightly above table top, can play position-limiting action, and sample stage 5 is lifting structure, can be according to taking the photograph
As the focusing of head member needs to carry out lift adjustment.
Measurement apparatus also includes a base 6, and base 6 is placed in bottom power charging assembly 3.Base 6 is provided with a displacement regulation
Mechanism's (not shown), is used for regulating film sample position to be measured so that it is be positioned at the center of photographic head 14 visual field.
Utilize the present invention to realize the measurement of thin film high temperature mechanical behavior, comprise the steps:
A. film sample 7 to be measured is placed on sample stage 5, sample is tightened fixing with steel cover plate, open light source 11, and open
Dynamic data process and display module 4；
B. heating furnace is enclosed within sample stage 5, by the displacement governor motion regulation sample position of regulation substrate 6, is allowed to
It is positioned at the center of optical lens visual field, and speckle imaging clearly；
C. start controller 21 program and the temperature that experiment is to be reached is set, the film sample to be measured 7 in heating furnace is entered
Row heating, is read current heating-up temperature by the instrumental panel on controller 21 panel, and is recorded by this temperature value, stable temperature
Angle value is tested；
D. motor 31 drives piston 32, applies uniform pressure to film sample to be measured, and data process and display group
Part 4 can control motor loading velocity；
E. the pressure in pressure process is by pressure transducer 34 Real-time Collection, and corresponding deformation of thin membrane amount of deflection is by digital speckle
Correlation technique records, thus obtains pressure (p)-central point amount of deflection (w) curve；
F. processed by data and display module 4 processes testing the speckle pattern obtained, obtain relevant experimental data；
G. change heating-up temperature by controller, repeat step a～f can obtain the mechanics at different heating temperature thin-film
Performance, elastic modelling quantity, interface bonding energy, yield strength and stress-strain relation etc..
When needs carry out thin film mechanics detection in temperature range, step c is:
Starting controller 21, follow procedure arranges the temperature range that experiment is to be reached, to the thin film sample to be measured in heating furnace
Product 7 heat, and change temperature value, again test after having tested, and pointwise changes until testing whole temperature range.
Finally it is necessary described herein: above example is served only for making technical scheme the most in detail
Ground explanation, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the foregoing of the present invention
The nonessential improvement of some made and adjustment belong to protection scope of the present invention.
Claims (10)
1. a thin film high temperature mechanical property measuring device, it is characterised in that measurement apparatus includes: optical measurement components, data
Process and display module, power charging assembly, heating assembly and sample stage, wherein optical measurement components, heating assembly, sample stage
And power charging assembly sets gradually, the light source and the hot spot that send during measurement are constant, and bulge effect makes thin film deform upon, and send out
The transmission light path delivering to thin film changes owing to thin film deformation makes angle of reflection produce, and the optical measurement components receiving reflected light path is remote
Journey connects data and processes and display module, and receiving light path is obtained by optical measurement components and processed by data and display module is visual
The display measurement process changed the change recording receiving light path.
Thin film high temperature mechanical property measuring device the most according to claim 1, it is characterised in that heating assembly is vertical adding
Hot stove, including: heating furnace body, resistance wire, temperature sensor and controller, carry out film sample to be measured in heating-furnace body
Bulge is tested, and resistance wire is uniformly arranged along the inwall of heating furnace body, and the top of heating furnace body is provided with an observation window.
Thin film high temperature mechanical property measuring device the most according to claim 2, it is characterised in that: optical measurement components passes through
The observation window at heating furnace top is observed.
Thin film high temperature mechanical property measuring device the most according to claim 1, it is characterised in that: optical measurement components includes
Light source, speckle parts processed, lens assembly and photographic head parts, light source, speckle parts processed, telecentric lens are sequentially connected to send light path
In, photographic head parts are connected in receiving light path.
Thin film high temperature mechanical property measuring device the most according to claim 4, it is characterised in that: lens assembly includes telecentricity
Camera lens, is used for dot projection to film sample surface to be measured.
Thin film high temperature mechanical property measuring device the most according to claim 1, it is characterised in that: power charging assembly includes
Motor, piston, oil pocket and pressure transducer.
Thin film high temperature mechanical property measuring device the most according to claim 6, it is characterised in that: oil pocket is built with high temperature resistant
Silicone oil, oil pocket side is connected with piston, and opposite side is connected with film sample to be measured.
Thin film high temperature mechanical property measuring device the most according to claim 1, it is characterised in that: measurement apparatus also includes one
Base, base is placed in bottom power charging assembly.
Thin film high temperature mechanical property measuring device the most according to claim 1, it is characterised in that: sample stage is lifting knot
Structure, needs to carry out lift adjustment according to the focusing of photographic head parts.
10. using a measuring method for thin film high temperature mechanical property measuring device according to claim 1, its feature exists
In, measuring method comprises the steps:
A. thin film is fixed in sample stage, unlatching light source and data handling component；
B. being enclosed within sample stage by heating furnace, regulate film sample to be measured and be positioned at the center of optical lens visual field, speckle imaging is clear
Clear；
C. start controller, film sample to be measured is heated；
D. power charging assembly applies uniform pressure to film sample to be measured, and data process and display module is for controlled loading
Speed；
E. pressure transducer Real-time Collection pressure data, corresponding deformation of thin membrane amount of deflection is recorded by Digital Speckle Correlation Method, from
And obtain pressure (p)-central point amount of deflection (w) curve；
F. processed by data and image and data are analyzed by display module, obtain the mechanical property ginseng of film sample to be measured
Number；
G. change heating-up temperature, repeat step a～f, obtain the mechanical property of film sample to be measured under different temperatures.
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