CN1405553A - Quasi-static laser scratch measuring method and device for interface bonding strength - Google Patents
Quasi-static 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, which utilizes a continuously loaded long pulse laser to quasi-statically load the surface of a coating or a film test piece, utilizes the thermal action of the laser to heat a thin layer (only dozens of nm thick) on the surface of the film and then heat conduction of heat to form a temperature field in the test piece, and because of the difference between the thermal expansion coefficient and the temperature of a film-base material, when the thermal stress formed in the coating reaches a certain value, the material is debonded, further material warping and peeling occur, and simultaneously, a feeding system enables the test piece to make feeding motion, thereby forming scratches on the surface of the coating. The interface bonding strength can be represented by laser energy corresponding to the peeling of the film-substrate interface, and the bonding strength of the film-substrate interface can be obtained by theoretical analysis and numerical calculation. The method is suitable for measuring the interface bonding strength of various hard tool films, decorative film systems, decorative functional films, DLC films, composite materials and other types.
Description
Technical field
The present invention relates to laser detection and material property detection technique field, refer in particular to a kind of quasistatic 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
The surface film technology is to improve the important means of material surface performance, and so-called film is the general designation of surface coating, surface coating or surface reforming layer, is divided into thick film and film.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, yet but have such undisputable fact: no matter how advanced you adopt technology, produce how excellent surface film, if it is bad with matrix bond, peel off easily, cracked or lost efficacy, its performance is good again, does not also have use value.As seen, film base binding performance determined to a great extent the film reliability of applying and and serviceable life, be the pacing items of being brought into play membrane action, also be 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, is very important in surface engineering technology and an interface science mechanical property parameter.
In practice, accurately measuring film substrate bond strength has many-sided importance: at first, it is the important indicator of various surface engineering technology product quality monitorings; Secondly it is that various technological means, technological parameter are carried out improved foundation; The 3rd, it is the basis of Surface Engineering structural design, for example, cylinder ceramic-lined, if bond strength does not reach requirement, its design obviously is irrational; The 4th, it can instruct and use the surface engineering technology product effectively and reasonably, for example corrosion-resistant and wear-resisting workplace, and its requirement to film substrate bond strength obviously is different; Or the like.
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 present invention proposes a kind of quasistatic laser scratch measuring method and device thereof that overcomes the interface bond strength of above-mentioned indentation method, laser slabbing method shortcoming.
The inventive method is characterised in that with the long pulse infrared laser beam and heats through the quasistatic of incoming laser beam light path system to the film test piece surface, film produced peel off.Simultaneously, the piece fixture system that brings into to system makes test specimen do feed motion, laser beam forms cut at film surface, and 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.The signal acquisition testing system adopts with microscope, CCD camera and detects test specimen pattern and acoustic emission detection system detection waviness of the surface combine detection.
Energy load mode of the present invention is for increasing continuously energy of lasers by laser power supply and control system and make feed system do retarded motion by feed system control, thereby increases the action time of laser at film surface.
The device of realization the inventive 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 long pulse CO
2, the YAG infrared 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.Control system is made up of controller, feed system control, laser power supply and control; Frame is used for above-mentioned each system is coupled together.Signal acquisition testing system signal acquisition testing system is made up of microscope, CCD camera, acoustic emission detection system.The signal analysis and processing system is made up of computing machine, printer and special signal process software etc.
Its course of work is:
The long pulse infrared laser beam is through the incoming 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, utilize the quasistatic heating of laser beam to film surface tens nm thickness layers, and heat heat conduction subsequently, formation temperature field in test specimen, because the difference of thin film basal body material coefficient of thermal expansion coefficient and temperature, in film, form thermal stress, when thermal stress reaches certain value, crack propagation, warpage further take place, rupture and peel off in the material production unsticking.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, thereby at film surface generation cut.Along with the increase of laser energy, peel off the position and move to matrix.Microscope, CCD camera detect the test specimen pattern, and acoustic emission detection system detects waviness of the surface, and input is formed the signal analysis and processing system by computing machine, printer and special signal process software etc., the point of judgement film base interfacial failure.Peel off pairing laser energy with the thin film basal body interface place and can characterize interfacial combined function, the laser beam energy when destroying with the film base is handled the bond strength of characterization of membrane basal body interface afterwards through the mathematical model of certain theoretical analysis and numerical evaluation.
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 the long pulse infrared laser as the cut light source, utilize of the quasistatic loading of the long pulse infrared laser of loading continuously to the test specimen surface, utilize the heating of the heat effect of laser to film surface thin layer (tens nm are thick), and heat heat conduction subsequently, formation temperature field in test specimen is because the difference of thin film basal body material coefficient of thermal expansion coefficient and temperature, in film, form thermal stress, when thermal stress reaches certain value, material production unsticking, further generating material warpage and peeling off.Along with the increase of laser energy, peel off the position and move to matrix, peel off pairing laser energy with the thin film basal body interface place and can characterize interfacial combined function.
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 result who records loads for the Long Pulse LASER quasistatic, and the critical value that film is peeled off is little than the kinetic measurement value, more approaching actual interface bond strength.
Description of drawings
The structured flowchart and the description of drawings of specific embodiments of the invention are as follows:
Fig. 1 is a course of work synoptic diagram of the present invention.
Fig. 2 begins to act on the pellicular stage synoptic diagram for laser.
Fig. 3 is that film base interface produces unsticking stage synoptic diagram.
Fig. 4 is unsticking district, a film base interface extension phase synoptic diagram.
Fig. 5 is unsticking district, a film base interface warpage stage synoptic diagram.
Fig. 6 is through-wall crack germinating of unsticking district and extension phase synoptic diagram.
Fig. 7 is a film separation stage synoptic diagram.
Fig. 8 is the device sketch 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) bring worktable into to system, (10) anchor clamps, (11) test specimen, (12) acoustic emission detection system, (13) catoptron, (14) focus lamp, (15) contain the light-conducting system of attenuator, (16) spectroscope, (17) lasing light emitter parameter acquisition system, (18) adjustable diaphragm, (19) resonator cavity, (20) infrared laser, (21) laser beam, (22) film, (23) matrix
Embodiment
The present invention proposes a kind of method of measuring film base interface bond strength.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 etc.
Long pulse infrared laser 20 in the resonator cavity 19 of cut laser instrument 1 is via adjustable diaphragm 18, spectroscope 16, the light-conducting system 15 that contains attenuator, the incoming laser beam light path system direct radiation of compositions such as focus lamp 14 is installed in the surface of the film sample 11 on the anchor clamps 10, test specimen 11 by matrix 23 and on film 22 form, utilize the quasistatic heating of 21 pairs of films of laser beam, 22 surperficial tens nm thickness layers, and heat heat conduction subsequently, formation temperature field in test specimen, because film 22, the material thermal expansion coefficient of matrix 23 and the difference of temperature, in film, form thermal stress, when thermal stress reaches certain value, crack propagation further takes place in the material production unsticking, warpage, the fracture and peel off.By laser power supply and control system 2 laser energy is increased continuously, bring into simultaneously to the worktable 9 drive anchor clamps and the test specimen of system and do feed motion.Thereby produce cut at film surface.Along with the increase of laser energy, peel off the position and move (if thermal stress is peeled off threshold value less than membraneous material, but greater than interface bond strength, then film inside does not produce and peels off, and is producing unsticking, crack propagation, warpage at the interface, ruptures and is peeling off) to matrix 23.The signal acquisition testing system that is made up of microscope 8, CCD camera 7, acoustic emission detection system 12 etc. gathers parameters such as the pattern, waviness of the surface of parameters of laser beam in the cut process and test specimen in real time, simultaneously, lasing light emitter parameter acquisition system 17 gathers parameters of laser beam in real time, input is formed the signal analysis and processing system by computing machine 4, printer 3 and special signal process software etc., judges the point of film base interfacial failure.Peel off pairing laser energy at the interface with the film base and can characterize interfacial combined function, the laser beam energy when destroying with the film base is handled the bond strength of characterization of membrane basal body interface afterwards through the mathematical model of certain theoretical analysis and numerical evaluation.
As shown in Figure 8, the cut system is formed by cut laser instrument 1 connection incoming laser beam light path system.The cut laser instrument is long pulse CO
2, the YAG infrared laser source, the incoming laser beam light path system is made up of adjustable diaphragm 18, 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 16 via adjustable diaphragm 18, spectroscope 17 is divided into two-beam with laser beam, a branch of light-conducting system 15 through containing attenuator, the film surface of focus lamp 14 direct radiation samples 11 also focuses on, utilize the quasistatic heating of 21 pairs of films of laser beam, 22 surperficial tens nm thickness layers, and heat heat conduction subsequently, formation temperature field in test specimen, because film 22, the difference of matrix 23 material coefficient of thermal expansion coefficients and temperature, in film, form thermal stress, when thermal stress reaches certain value, crack propagation further takes place in the material production unsticking, warpage, the fracture and peel off.Another bundle enters lasing light emitter parameter acquisition system 17, 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.18 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 11, anchor clamps 10 and bring into to the worktable 9 of system and form.Test specimen 11 is installed in the anchor clamps 10, and anchor clamps 10 are fixed on the worktable of bringing into to system 9.Worktable 9 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.Frame is used for above-mentioned each system connection, simultaneously the distance on scalable focal beam spot and test specimen surface.
Detection system is formed by lasing light emitter parameter acquisition system 17, detection beam path system, signal acquisition testing system, signal analysis and processing system in combination.Lasing light emitter parameter acquisition system 17 gathers the lasing light emitter parameter in real time; Detect the beam path system and form, make the detection signal of film surface pass to signal acquisition testing system and signal analysis and processing system by spectroscope 16, catoptron 13; The signal acquisition testing system adopts with microscope 8, CCD camera 7 and detects test specimen pattern and acoustic emission detection system 12 detection waviness of the surface combine detection, acoustic emission detection system 12 is connected with test specimen 11, is used for gathering in real time the acoustic signals of cut process neutralized film breakage front and back; The signal analysis and processing system is made up of computing machine 4, printer 3 and special signal process software etc., is used for analyzing and processing detection signal, output and printing testing result.
Control system is by controller 5, feed system control 6, laser power supply and control 2 etc. and form, and is used for the speed of feed and the laser power of real-time Control work platform.
Fig. 2～Fig. 7 be laser action in film, the process synoptic diagram that makes its interface produce unsticking, expansion, warpage, crack initiation and extension phase, peel off.
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 film surface appearance in real time and import computing machine 4 with CCD camera 7.
3. acoustic emission detection.With acoustic emission detection system 12 real-time acoustical signal and the variations thereof that detect cut process and cut breakage front and back film surface, differentiate film and whether unsticking, warpage take place, rupture, peel off.
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 quasistatic laser scratch measuring method of interface bond strength is characterized in that heating through the quasistatic of incoming laser beam light path system to the film test piece surface with the long pulse infrared laser beam of continuous loading, film is produced peel off.Simultaneously, feed system makes test specimen do feed motion, and laser beam forms cut at film surface, and 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.
2. the quasistatic 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 acoustic emission detection system (12) detection waviness of the surface combine detection.
3. the quasistatic 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 the incoming laser beam light path system by cut laser instrument 1 and forms.
4. the quasistatic laser scratch measurement mechanism of interface bond strength according to claim 3 is characterized in that the cut laser instrument is long pulse CO
2, the YAG infrared laser.
5. the quasistatic laser scratch measurement mechanism of interface bond strength according to claim 4 is characterized in that detection system is formed by lasing light emitter parameter acquisition system (17), detection beam path system, signal acquisition testing system, signal analysis and processing system in combination.
6. the quasistatic laser scratch measurement mechanism of interface bond strength according to claim 4 is characterized in that the incoming laser beam light path system is made up of adjustable diaphragm (18), spectroscope (16), the light-conducting system (15) that contains attenuator, focus lamp (14).
7. the quasistatic laser scratch measurement mechanism of interface bond strength according to claim 4 is characterized in that detecting the beam path system and is made up of spectroscope (16), catoptron (13).
8. the quasistatic laser scratch measurement mechanism of interface bond strength according to claim 4 is characterized in that the piece fixture system is made up of test specimen (11), anchor clamps (10) and the worktable (9) brought into to system.
9. the quasistatic laser scratch measurement mechanism of interface bond strength according to claim 4 is characterized in that the signal acquisition testing system is made up of microscope (8), CCD camera (7), acoustic emission detection system (12).
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| SU1280498A1 (en) * | 1985-05-22 | 1986-12-30 | Ленинградский технологический институт целлюлозно-бумажной промышленности | Method of determining strength of coating-base adhesion |
| SU1716394A2 (en) * | 1989-05-11 | 1992-02-28 | Ленинградский технологический институт целлюлозно-бумажной промышленности | Method of determining adhesion force between coating and substrate |
| CN1037372C (en) * | 1991-07-01 | 1998-02-11 | 中国科学院金属研究所 | Method and device for detecting membrane/base bonding strength |
| CN1215320C (en) * | 2001-11-30 | 2005-08-17 | 江苏大学 | Interface bonding strength laser impact quantitative determination method and device |
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