CN1405554A - Far ultraviolet laser scratch measuring method and device for interface bonding strength - Google Patents
Far ultraviolet laser scratch measuring method and device for interface bonding strength Download PDFInfo
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Abstract
The invention relates to the technical field of laser detection and material performance detection, wherein a continuously loaded pulse far ultraviolet laser beam is directly loaded on the surface of a thin film of a test piece through an incident laser beam optical path system, and the material is degraded through the actions of photodissociation, photoinduced valence change, formation of lattice defects, plasma treatment and the like, and for some materials, photons can even directly break bonding bonds between molecules or crystals, so that the thin film material is peeled off. Meanwhile, the feeding system makes the test piece perform feeding movement, the laser beam forms scratches with gradually increasing depth on the surface of the film until the film-substrate interface is destroyed, and the bonding strength of the film-substrate interface is represented after the laser beam energy is processed by a certain mathematical model when the film-substrate interface is destroyed. The method is suitable for measuring the interface bonding strength of various hard tool films, decorative film systems, decorative functional films, DLC films, organic polymer materials, composite materials and other types.
Description
Affiliated technical field
The present invention relates to laser detection and material property detection technique field, refer in particular to a kind of extreme ultraviolet laser scratch measuring method and device of interface bond strength, be applicable to the mensuration of the interface bond strength of various hard tool films, decorating film system, decoration functions film, DLC film, high-molecular organic material, compound substance and other type.
Background technology
Wearing and tearing, corrosion and fatigue are topmost three kinds of forms that part or member lost efficacy in the course of the work, especially under conditions of work such as high speed, high temperature, high pressure, heavy duty, corrosive medium, often it is scrapped, finally cause equipment scrapping because of part or component surface local damage.And these failure phenomenons mostly occur in material surface, thereby take various means to improve the surface property of material, the very effective measure that increases the part safe reliability beyond doubt or increase the service life.
So-called film is the general designation of surface coating, surface coating or surface reforming layer, is divided into thick film and film.Thin film technique is one of important means of material raising surface property, properties such as part given by its material with minute quantity and component surface is wear-resisting, corrosion-resistant, heat-resisting, endurance, radiation hardness and light, heat, electricity, magnetic, play the effect that integral material was difficult to play of a large amount of costlinesses, economize on resources in a large number and the energy, can give full play to the potential of matrix material and membraneous material, reduce production costs.The surface film technology has been widely used in every field such as Aeronautics and Astronautics, machine-building, electronic technology, optical engineering and computer science.
Widespread use along with thin film technique, people are to its reliability and proposed more and more higher requirement serviceable life, and film base binding performance determined to a great extent the film reliability of applying and and serviceable life, being the pacing items of being brought into play membrane action, also is the problem of generally being concerned about in the thin film fabrication process.Film substrate bond strength is the primary index that influences the surface film quality.
Film base interfacial combined function is most important in interface science research, and direct quantitative is measured interface adhesion and remained the global problem that troubles the countries in the world scientist so far.The method of the detection film base interface binding power that has proposed at present has kind surplus the method for directly peeling off, scarification, indentation method, bending method, ballistic method, pulling method and the fracture method etc. 20.But every kind of method has its limitation Buddhist monk problem to be solved on measuring technique and Mechanics Calculation, is in particular in that the numerical value that diverse ways records differs several magnitude with a kind of method measurement data instability, even produces difference qualitatively.Its reason is that measured value is interface adhesion and film and the elasticity of matrix and the synthesis result of elastic plastic behavior, friction and relevant test parameters, and people do not understand fully the real relation of surface film rupture failure critical value and interface bond strength so far as yet.
At present, scarification and indentation method are the methods of the present characterization of membrane base interface bond strength that more generally adopts.Scarification is the present unique a kind of method that can effectively measure hard, wear-resistant film and basal body interface adhesion, and its relative indentation method is used also ripely, but has following point:
1. the factor that influences critical load Lc is a lot.Lc is not only relevant with test parameterss such as the performance of loading velocity, cut speed, membrane stress and interfacial property, testing environment and matrix, film, surfaceness, hardness, modulus, fragility, also with relating to parameters such as abrasion condition, friction force and the friction factor of pressure head point radius, pressure head, friction surface conditions.
2. cut mechanism complexity.The mechanism that scarification is surveyed adhesion is unclear fully as yet, does not set up critical load Lc and film base interface binding power accurate quantification relation at present as yet.
3. contact type measurement, the film that mechanicals efforts and friction force cause and the elastic-plastic deformation of matrix are very big to the influence of measurement result.
4. be only applicable to the measurement of ganoine thin film, can't measure flexible film; In addition, thickness being required usually should be greater than 2 μ m.
Laser technology is since coming out the sixties in 20th century, and its application spreads all over every field such as science, culture and education, medical and health, industrial or agricultural, Aero-Space and national defence.Laser Processing (cutting, welding, surface treatment, punching, laser marking) and laser measurement control technology development in recent years are rapid.External existing more jewel cut patented technology report, as Chinese patent 96199289.6, United States Patent (USP) 4392476,4467172,5410125,5149938, Jap.P. JP00-48489, JP00-77989 etc., its essence is and utilize Ultra-Violet Laser mark on jewel.China's utility model patent 90218138.6 has been reported scarification and has been measured the scratch method film adherometer.China's utility model patent 98225674.4 and Chinese invention patent 911051103.1,9113400.5,00223444.0 have been reported Ultra-Violet Laser mark (photoetching) apparatus and method, and Chinese invention patent 97109296.6 has been reported CO
2The infrared laser marking device.
The research that utilizes laser technology to measure film base interface bond strength is the hot issue of various countries scientist common concern, people such as the Gupta of Massachusetts Institute Technology take the lead in carrying out laser slabbing standard measure and measure plane film interface bond strength, and apply for a patent: System and methodfor measuring the interface tensile strength of planar interfaces (measuring method and the device of plane film interface pulling strengrth), approval number is US5438402.Its principle is to use short-pulse laser (pulsewidth is generally 2ns-8ns) impact specimen, relies on the stretching ripple and the incident compression stress wave tension when meeting at the interface that form from free-surface reflection to produce slabbing.Its shortcoming is that restricted (0.1～0.2mm), simultaneously film surface should form reflecting surface through special disposal to specimen thickness.
Summary of the invention
The objective of the invention is to propose a kind of extreme ultraviolet laser scratch measuring method and device that overcomes the interface bond strength of above-mentioned indentation method, laser slabbing method shortcoming.
Its method is characterised in that the film surface that directly loads on test specimen with continuous loading pulse extreme ultraviolet laser beam by the incoming laser beam light path system, by photodissociation, the photic processing of degrading of appraising at the current rate, form effects realizations such as lattice imperfection, plasma to material, membraneous material is produced peel off.Simultaneously, the piece fixture system that brings into to system makes test specimen do feed motion, and laser beam forms the cut that the degree of depth increases gradually at film surface, destroys until film-basal body interface; Detection signal beam path system transmissions after testing detects judgement to the signal acquisition testing system that links to each other with control system, signal analysis and processing system, simultaneously, lasing light emitter parameter acquisition system measures the collection parameters of laser beam in real time, and the laser beam energy during with film base interfacial failure is handled the bond strength of characterization of membrane basal body interface afterwards through certain mathematical model.
The signal acquisition testing system adopts with microscope, CCD camera and detects test specimen pattern, laser-ultrasound detection or laser plasma detection system detection waviness of the surface combine detection mode.
The related device of this method is made up of cut system, piece fixture system, detection system, control system and frame.
The cut system connects the incoming laser beam light path system by the cut laser instrument and forms, and the cut laser instrument is a short pulse extreme ultraviolet excimer laser.The piece fixture system is by test specimen, anchor clamps and bring into to the worktable of system and form; Detection system is formed by lasing light emitter parameter acquisition system, detection beam path system, signal acquisition testing system, signal analysis and processing system in combination; The incoming laser beam light path system is made up of adjustable diaphragm, spectroscope, the light-conducting system that contains attenuator, focus lamp; Detecting the beam path system is made up of spectroscope, catoptron; The signal acquisition testing system is made up of microscope, CCD camera, detection laser, interferometer etc.
Control system is made up of controller, feed system control, laser power supply and control photodiode trigger switch etc., and photodiode trigger switch one end light path after testing links to each other with spectroscope, and the other end links to each other with dual channel oscilloscope; Frame is used for above-mentioned each system connection; The signal analysis and processing system is made up of computing machine, printer, oscillograph and special signal process software etc., and dual channel oscilloscope one end links to each other with interferometer, and the other end links to each other with computing machine.
Its course of work is:
Pulse extreme ultraviolet laser beam is through the incident pulse laser beam light path system direct radiation film sample surface of compositions such as adjustable diaphragm, spectroscope, the light-conducting system that contains attenuator, focus lamp, by laser power supply and control system laser energy is increased continuously, simultaneously feed system make worktable and on anchor clamps and test specimen do feed motion.The extreme ultraviolet laser action is in the film sample surface, by photodissociation, photicly appraise at the current rate, form effect photochemical effect such as lattice imperfection and heat effect and realize material degraded processing (melting mechanism), to some material, photon even can directly break associative key between molecule or the crystal, make film surface produce cut, until the film matrix interfacial failure.Microscope, CCD camera detect the test specimen pattern, and detection laser, interferometer are gathered the parameters such as waviness of the surface of test specimen in the cut process in real time, and simultaneously, lasing light emitter parameter acquisition system measures the collection parameters of laser beam in real time.The data input of gathering is formed the signal analysis and processing system by printer, computing machine, dual channel oscilloscope and special signal process software, judge the point of film base interfacial failure, the laser beam energy when destroying with the film base is handled the bond strength of characterization of membrane basal body interface afterwards through certain mathematical model.
The present invention and existing film bond strength detection method ratio have following advantage:
1. non-cpntact measurement, and do not have the effect of mechanical force between film test piece.Directly peeling off film bond strength detection methods such as method, scarification, indentation method, bending method, ballistic method, pulling method and fracture method all is contact type measurement, and the film that mechanicals efforts and friction force cause and the elastic-plastic deformation of matrix are very big to the influence of measurement result.
2. laser action mechanism obviously, succinctly.Adopt Ultra-Violet Laser as the cut light source, photon may directly be broken the associative key between molecule or the crystal, by photodissociation, photicly appraise at the current rate, form effect realization such as lattice imperfection material degraded processing (melting mechanism).
3. simplified the factor that influences measurement result, compare with traditional diamond penetrator scarification, critical load is only relevant with performance of laser loading velocity, cut speed, membrane stress and interfacial property, testing environment, matrix and film etc., does not have the blunt of diamond penetrator in the scarification and the influence of friction.
4. the interaction between laser and the membraneous material can accurately be controlled, and the laser energy load measurement is accurately convenient, by spectroscope, can directly measure parameters such as the power that loads laser, energy, pattern, spot diameter.
5. laser beam is easy to focus on, and can change shape, size and energy density arbitrarily according to measuring needs.
6. the guiding of laser beam and NE BY ENERGY TRANSFER are convenient and swift, are convenient to realize measuring robotization.
7. compare with the bond strength technology at existing laser measurement film matrix interface, shape, matrix thickness and the thicknesses of layers of test specimen do not had specific (special) requirements, as long as can be placed on the worktable.
8. the critical value that the result who records once makes film break away from for pulsed laser action, little with test process parameters relationships such as laser loading velocity, cut speed.The differentiation process is succinct, convenient, practical, accurate.
Description of drawings
Fig. 1 is a course of work synoptic diagram of the present invention.
Fig. 2 peels off the energy stage synoptic diagram of threshold value for film absorption surpasses it.
After Fig. 3 is the film absorption laser energy, carries out photochemistry and decompose and thermal decomposition stage synoptic diagram.
Fig. 4 goes out surface stage synoptic diagram for the gaseous state powderject of high temperature.
Fig. 5 is the microstructure SEM photo with the quasi-molecule laser etching fabrication techniques.
Fig. 6 is the device synoptic diagram of cut system.
(1) cut laser instrument (2) laser power supply and control (3) printer (4) computing machine (5) controller
(6) feed system control (7) CCD camera (8) microscope (9) photodiode trigger switch (10) bilateral
Road oscillograph (11) is brought worktable (12) anchor clamps (13) test specimens (14) interferometers (15) catoptron to system into
(16) focus lamp (17) detection laser (18) contains light-conducting system (19) the lasing light emitter parameter acquisition system of attenuator
(20) spectroscope (21) spectroscope (22) adjustable diaphragm (23) resonator cavity (24) extreme ultraviolet laser (25) swashs
Light beam (26) film (27) matrix
Embodiment
As shown in Figure 1, the related system of this method is made up of cut system, piece fixture system, detection system, control system and frame.
Its method is: the incoming laser beam light path system that the extreme ultraviolet laser 24 in the resonator cavity 23 of cut laser instrument 1 is formed via adjustable diaphragm 22, spectroscope 21,20, the light-conducting system 18 that contains attenuator, focus lamp 16 directly loads on the film surface of the sample 13 that is installed on the anchor clamps 12, test specimen 13 by matrix 27 and on film 26 form, by laser power supply and control system 2 laser energy is increased continuously, bring into simultaneously to the worktable 11 drive anchor clamps 12 of system and do feed motion with test specimen 13.The extreme ultraviolet laser action is in the film sample surface, by photodissociation, photicly appraise at the current rate, form effect photochemical effect such as lattice imperfection and heat effect and realize material degraded processing (melting mechanism), to some material, photon even can directly break associative key between molecule or the crystal, form the cut that the degree of depth increases gradually at film surface, destroy until film-basal body interface.Form the signal acquisition testing system by microscope 8, CCD camera 7, detection laser 17, interferometer 14 and gather parameters such as the pattern of test specimen in the cut process, waviness of the surface in real time, simultaneously, parameters of laser beam is gathered in the real-time measurement of lasing light emitter parameter acquisition system 19.The data of gathering are imported into by printer 3, computing machine 4, dual channel oscilloscope 10 etc. and are formed the signal analysis and processing system, judge the point of film base interfacial failure, the laser beam energy when destroying with the film base is handled the bond strength of characterization of membrane basal body interface afterwards through certain mathematical model.As shown in Figure 6, the cut system is formed by cut laser instrument 1 connection incoming laser beam light path system.The cut laser instrument is extreme ultraviolet lasing light emitters such as quasi-molecule, and the incoming laser beam light path system is made up of adjustable diaphragm 22, spectroscope 16, the light-conducting system 15 that contains attenuator, focus lamp 14.Long pulse infrared laser 20 in the resonator cavity 19 arrives spectroscope 20 via adjustable diaphragm 18, spectroscope 20 is divided into two-beam with laser beam, the film surface of a branch of light-conducting system 18, focus lamp 16 direct radiation samples 13 through containing attenuator also focuses on, and forms the cut that the degree of depth increases gradually at film surface.Another bundle enters lasing light emitter parameter acquisition system 19, and the lasing light emitter parameter of collection is through importing the computing machine 4 that links to each other with printer 3 into controller 5, so that realize real-time detection and control to the lasing light emitter parameter.Spectroscope 21 is told a branch of light to the photodiode trigger switch 9 that links to each other with oscillograph 10.22 pairs of laser beam reshapings of adjustable diaphragm are adjusted spot size and shape thereof.Laser power supply and control 2 and can realize that the real-time continuous of laser energy increases or reduces.
The piece fixture system is by test specimen 13, anchor clamps 12 and bring into to the worktable 11 of system and form.Test specimen 13 is installed in the anchor clamps 12, and anchor clamps 12 are fixed on the worktable of bringing into to system 11.Worktable 11 is used for supporting and the clamping test pieces anchor clamps, and when feed system was used to realize that laser loads continuously, test specimen moved with respect to laser beam, forms cut to be implemented in film surface.
Detection system is formed by lasing light emitter parameter acquisition system 19, detection beam path system, signal acquisition testing system, signal analysis and processing system in combination.Parameters of laser beam is gathered in the real-time measurement of lasing light emitter parameter acquisition system 19; Detect the beam path system and form, make film surface accept the detection resources signal and detection signal conducted signal acquisition testing system and signal analysis and processing system by spectroscope 20,21, catoptron 15; The signal acquisition testing system is by microscope 8, CCD camera 7, detection laser 17, interferometer 14 is formed, gather the pattern of test specimen in the cut process in real time, parameters such as waviness of the surface, interferometer 14 is connected with test specimen 13, be used to gather the waveform signal on test specimen surface: the signal analysis and processing system is by computing machine 4, printer 3, compositions such as oscillograph 10 and special signal process software, be used for the analyzing and processing detection signal, output and printing testing result, dual channel oscilloscope 10 1 ends link to each other with interferometer 14, receive waveform signal, its other end links to each other with computing machine 4, and waveform signal is transferred out.
Control system is made up of controller, feed system control, laser power supply and control photodiode trigger switch etc., is used for the speed of feed and the laser power of real-time Control work platform.Photodiode trigger switch 9 one ends light path after testing link to each other with spectroscope 21, and the other end links to each other with dual channel oscilloscope 10, real-time or its unlatching of time-delay control.
Frame is used for above-mentioned each system connection, simultaneously the distance on scalable focal beam spot and test specimen surface.
Fig. 2～Fig. 4 is etching process (the melt mechanism) synoptic diagram of Ultra-Violet Laser to film.Whole process is to finish in moment, and pulse width general and laser is close, and is little to the heat affecting of neighboring area.Fig. 2 film absorption surpasses it and peels off the energy stage of threshold value.Behind Fig. 3 film absorption laser energy, carry out that photochemistry is decomposed and thermal decomposition, chemical bond rupture, resolve into " powder " process synoptic diagram of " gaseous state ", at this moment, small local specific volume sharply increases.The gaseous state powder of Fig. 4 high temperature sharply expands, explodes, and ejects the surface process synoptic diagram.
Fig. 5 is the microstructure SEM pattern with the quasi-molecule laser etching fabrication techniques, the dark 50 μ m of indentation, and indentation wall portion is steep, and the bottom is smooth.
Film destruction criterion of the present invention is:
1. surface topography is differentiated.Through catoptron 15 usefulness microscopes 8 viewing film surface topographies, whether warpage, crackle take place, the destruction defective such as peel off for turning traitor criterion with film surface.
2.CCD surface topography is differentiated.Detect coating (or film) surface topography in real time and import computing machine 4 with CCD camera 7.
3. other differentiations such as laser-ultrasound or microwave, plasma signal, when laser instrument 1 sends the ultraviolet pulse laser bundle, 9 whiles of photodiode trigger switch or quantitative delayed start-up dual channel oscilloscope 10, interferometer 14 is gathered laser-ultrasound or the waveform signals such as microwave, plasma signal through specimen surface in real time, and input dual channel oscilloscope 10 and computing machine 4, according to the film surface cut process of record and signal and the variation thereof before and after the cut breakage, differentiate film and whether destroy.
Calculate the interface with the stress history that laser loads through the dedicated computing software processes, get critical interface peel value, be interface tension strength.Test files such as test report and surface topography, signal waveform curve are exported by printer 3 output devices such as grade at last.
Claims (9)
1. the extreme ultraviolet laser scratch measuring method of interface bond strength, it is characterized in that loading on by outside optical system the film surface of test specimen with continuous loading pulse extreme ultraviolet laser beam, by photodissociation, the photic processing of degrading of appraising at the current rate, form effects realizations such as lattice imperfection, plasma to material, membraneous material is produced peel off.Simultaneously, feed system makes test specimen do feed motion, and laser beam forms the cut that the degree of depth increases gradually at film surface, destroys until film-basal body interface.Detection signal beam path system transmissions after testing detects judgement to the signal acquisition testing system that links to each other with control system, signal analysis and processing system, simultaneously, lasing light emitter parameter acquisition system measures the collection parameters of laser beam in real time, and the laser beam energy during with film base interfacial failure is handled the bond strength of characterization of membrane basal body interface afterwards through certain mathematical model.
2. the extreme ultraviolet laser scratch measuring method of interface bond strength according to claim 1 is characterized in that the signal acquisition testing system adopts with microscope (8), CCD camera (7) detection test specimen pattern and laser-ultrasound detects or the laser plasma detection system detects the waviness of the surface combine detection.
3. the extreme ultraviolet laser scratch measurement mechanism of interface bond strength, it comprises cut system, piece fixture system, control system, detection system, it is characterized in that the cut system connects incident laser light pulse beam road system by cut laser instrument (1) and forms.
4. the extreme ultraviolet laser scratch measurement mechanism of interface bond strength according to claim 3 is characterized in that the cut laser instrument is a short pulse extreme ultraviolet excimer laser.
5. the extreme ultraviolet laser scratch measurement mechanism of interface bond strength according to claim 3 is characterized in that detection system is formed by lasing light emitter parameter acquisition system 19, detection beam path system, signal acquisition testing system, signal analysis and processing system in combination.
6. the extreme ultraviolet laser scratch measurement mechanism of interface bond strength according to claim 3 is characterized in that incident pulse laser beam light path system is made up of adjustable diaphragm (22), spectroscope (21), (20), the light-conducting system (18) that contains attenuator, focus lamp (14).
7. the extreme ultraviolet laser scratch measurement mechanism of interface bond strength according to claim 3 is characterized in that detecting the beam path system and is made up of spectroscope (20), (21), catoptron (15).
8. the extreme ultraviolet laser scratch measurement mechanism of interface bond strength according to claim 3 is characterized in that the piece fixture system is made up of test specimen (13), anchor clamps (12) and the worktable (11) brought into to system.
9. the extreme ultraviolet laser scratch measurement mechanism of interface bond strength according to claim 3 is characterized in that the signal acquisition testing system is made up of microscope (8), CCD camera (7), detection laser (17), interferometer (14).
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2008009165A1 (en) * | 2006-07-03 | 2008-01-24 | He Jian Technology(Suzhou)Co.Ltd. | AN OPTICAL INSPECTING METHOD OF A PLASMA PROCESSING DEGREE OF A SiON FILM |
| CN101876627A (en) * | 2010-03-16 | 2010-11-03 | 江苏大学 | Optical power meter technology-based method for detecting interface bonding state of laser scratch |
| CN101936876A (en) * | 2010-07-28 | 2011-01-05 | 泰州市天创仪器有限公司 | Infrared laser grinding crack detecting device |
| CN102012552A (en) * | 2010-09-27 | 2011-04-13 | 江苏大学 | Light path automatic adjusting system for multi-window multi-wavelength laser |
| CN102294543A (en) * | 2011-06-22 | 2011-12-28 | 北京工业大学 | Method for observing transparent melt layer in material laser-cutting process |
| CN105737773A (en) * | 2010-11-12 | 2016-07-06 | Ev 集团 E·索尔纳有限责任公司 | Measurement device and method used for measuring layer thickness of stacked wafers and lattice imperfection |
| WO2017148208A1 (en) * | 2016-03-03 | 2017-09-08 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Surface wave plasmon apparatus |
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