CN1540309A - Measuing and testing techniques for detecting adhesive strength of diamond coat by method of innor expand and bubbling - Google Patents
Measuing and testing techniques for detecting adhesive strength of diamond coat by method of innor expand and bubbling Download PDFInfo
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- CN1540309A CN1540309A CNA2003101083075A CN200310108307A CN1540309A CN 1540309 A CN1540309 A CN 1540309A CN A2003101083075 A CNA2003101083075 A CN A2003101083075A CN 200310108307 A CN200310108307 A CN 200310108307A CN 1540309 A CN1540309 A CN 1540309A
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Abstract
A window cavity is made on back face of basal body of diamond coat through chemical corrosion, microprocessing or other method in order to expose inner surface, which is contacted to basal body before window cavity is made. Pressure is applied to the coat by using pressure oil through window cavity. The coat is deformed under action of even load. Based on Pascal law and theory of plate and shell, theoretical model of inner expand and bubbling method for detecting adhesive strength of coat is deduced, and calculating program is converted from the said model. Thus, testing the deformation of diamond coat and relevant pressure can calculate out adhesive strength of diamond coat. The method calculates strength with accuracy without limit of shape of basal body and magnitude of intensity.
Description
Technical field
The present invention relates to the measuring technology of diamond coatings adhesive strength on a kind of detection by quantitative different shape carbide-tipped tool matrix, particularly a kind of measuring technology that adopts internal expanding Bubbling method accurate quantification to detect the diamond coatings adhesive strength belongs to machine cut coated cutting tool coating performance detection technique field.
Background technology
Adamas becomes desirable tool materials because of having excellent properties such as high rigidity, high thermal conductivity coefficient, low-friction coefficient, low thermal coefficient of expansion and chemical stability be good; obtained using widely in diamond coatings cutting tool field, but do not accomplished scale production yet at present.Its one of the main reasons is: lack unified standard about diamond coatings inherent quality (mainly being mechanical property) evaluation.In the prior art, comprise indentation test, stretched vertically method and scrape stripping formula mensuration etc.Wherein indentation test is a kind of most widely used, simple to operate, result's observational measurement method comparatively intuitively, it is pressed into a hard pressure head (being generally natural diamond monocrystalline pressure head) in the material with a known load, and then measure thus the area of indentation or the degree of depth residual in material, being pressed into of pressure head can produce a hemispherical plastic zone, material is outwards extruded and around coating, is produced compressive stress, if coating will be bubbled, peel off and from phenomenons such as matrix are bent upwards, then these compressive stress can access release, and this method is the size of comparative coatings adhesion qualitatively.And the stretched vertically rule can provide the adhesion of chemical vapor deposition (CVD) diamond coatings more intuitively, it adopts a pair of stretching bar firm with epoxy bond with the diamond coatings surface and the matrix back side with one heart respectively, measurement is used for being pulled away from and sticks on the required stress of coating on the matrix to determine a kind of method of diamond coatings adhesion, the result of test is subjected to thickness effect that institute adds the angle variation of stress and adhesive glue greatly, and the scope of test is limited by the cohesive strength of adhesive glue also.Scraping the stripping formula measures rule and is to use the special broach tool of scraping, coating being stripped down from matrix along coating/basal body interface with the similar load mode of scraping, and the measuring method of measuring as adhesive strength between coating/matrix with the energy that is consumed in the release coating process.This shows, said method all be qualitative, indirectly adhesive force of coatings is described, test specification is subjected to effects limit such as adhesive strength size, base shape, lacks comparability each other.Therefore, make the diamond coatings material really be applied to the cutter field and realize industrialization production, must have and perfect the diamond coatings adhesive strength is carried out the technology that direct quantitative detects guarantee.
Summary of the invention
Can not carry out accurate quantification and detect and be subjected to many deficiencies such as base shape restriction in order to overcome existing diamond coatings adhesive strength detection method, the invention provides a kind of internal expanding bubbling measuring method, this measuring method can not only accurate quantification be measured the adhesive strength of diamond coatings, and not being subjected to the restriction of base shape, the adhesive strength that can be advantageously used in complicated shape matrix diamond coatings is measured.
The technical solution adopted for the present invention to solve the technical problems is: chemical corrosion is adopted at the back side at the diamond coatings matrix, micro-manufactured or other method process outside a window cavity volume makes that the coating inner surface that originally contacts with matrix is exposed to, be not damaged to simultaneously diamond coatings, originally with on the coating inner surface that matrix contacts applying hydraulic pressure or air pressure then, make diamond coatings be subjected to the effect of uniformly distributed load and produce distortion, derive the theoretical model that the internal expanding Bubbling method is measured coating adhesive strength according to Pascal law and Plate Theory, see shown in formula (1) and the formula (2) that wherein h is the perpendicular displacement (height of bubble) in window central authorities; A is a windows radius; P is a pressure; k
1, k
2Be design factor; k
vIt is volumetric coefficient; G
cIt is the critical crack expansion stresses of quantitative description diamond coatings adhesive strength; V is a cavity volume internal pressure oil volume.This computation model can be changed into calculation procedure by application software such as Matlab.By computer programming, establishment internal expanding bubbling metering computer control system software, and it is installed in the computing machine so that in experimentation, finish control and collection of experiment data, storage and analysis to whole measurement links.Can know that from formula (1) product ph is only about (h/a)
2Function.Therefore, energy release rate G
cBe one about (h/a)
2Function.Remain unchanged if this means the critical crack extension stress Gc that runs in experiment, then h/a is also constant, and the section of bubble still keeps self similarity when it increases.Thereby (h/a) change instantaneous, coating will be peeled off, at this moment measure corresponding pressure p by the perpendicular displacement h and the pressure-measuring system of the accurate measurement window of He-Ne laser interferometry system central authorities, just can obtain the relation between the suffered load of diamond coatings and its distortion, calculate windows radius a by volume equation (3) again, and then just can calculate the adhesive strength of diamond coatings according to equation (2) accurate quantification.
V＝k
va
2h (3)
The invention has the beneficial effects as follows, can detect the adhesive strength of diamond coatings accurate quantification, and measurement range is not subjected to the restriction of base shape and adhesive strength size, have remarkable economic efficiency.
Description of drawings
Fig. 1 is that sample window produces the elastic-plastic deformation synoptic diagram in internal expanding bubbling measuring process.
Fig. 2 is an internal expanding bubbling measuring system synoptic diagram of the present invention.
1 is diamond coatings among the figure, the 2nd, coated substrate, the 3rd, the window cavity volume that processes, the 4th, He-Ne laser interferometry system, the 5th, the diamond coatings sample window, the 6th, sample holder, the 7th, pressure-measuring system, the 8th, pressure feeding system, the 9th, measure pedestal, the 10th, unloader, the 11st, signal amplifier, the 12nd, computer control system.
Embodiment
Below in conjunction with accompanying drawing concrete enforcement of the present invention is further described.As shown in Figure 1 and Figure 2, concrete enforcement of the present invention can be carried out according to the following steps:
The first step: according to the know-why of this invention, developed a whole set of internal expanding bubbling measuring system, it mainly comprises measures pedestal 9, He-Ne laser interferometry system 4, pressure-measuring system 7 and pressure feeding system 8, wherein He-Ne laser interferometry system 4, pressure-measuring system 7 and pressure feeding system 8 can adopt the product of existing sale on the market to reduce the cost of total system, the shortening product development cycle.Measuring pedestal 9 is that the length of side of making of plexiglass block is the cube platform of 7cm, have four holes at the center of four faces of cube, the bottom in four holes interconnects, wherein end face hole and sample holder 6 be by being threaded, and sample holder 6 is to adopt the non-shrinkage steel bolt of opening the hole along central axis to process.The bottom hole corresponding with the end face hole then is connected with unloader 10, and unloader 10 directly is screwed into by being threaded to be measured in the pedestal 9, and the bolt end that is screwed in the plexiglass block seals with the O RunddichtringO.Measuring pedestal 9 left side hole exits links to each other with pressure-measuring system 7, pressure-measuring system 7 mainly is made up of pressure transducer and data acquisition and transfer member, wherein pressure transducer directly is screwed into by being threaded and measures in the pedestal 9, connect screw thread and adopt polytetrafluoroethylraw raw material band to seal, the measuring-signal of being gathered is sent in the computer control system 12 by the data line connection.Measure pedestal 9 right side hole exits and 8 connections mutually of pressure feeding system, pressure feeding system 8 is made up of syringe pump and step motor, the drive signal line of step motor is connected with computer control system 12, can come the rotation of control step motor thus by computing machine, thereby promote syringe pump injection pressure oil control in measuring pedestal 9 endoporus to realize system is pressurizeed.
Second step: preparation diamond coatings sample window 5, adopt chemical corrosion, micro-manufactured or other method to process outside a window cavity volume 3 makes that the coating inner surfaces that originally contact with matrix are exposed at the back side of diamond coatings matrix 2, the while is not damaged to diamond coatings 1.
The 3rd step: adopt diglycidyl ethers propane type epoxy resin of di phenolic group cementing agent diamond coatings sample window 5 epoxidations that prepare to be fixed on the top of sample holder 6, coated substrate 2 will be sticked on the top of sample holder 6 firmly like this, and the center of sample holder 6 top through holes is then aimed at the center of diamond coatings sample window 5.
The 4th step: 8 pairs of systems pressurize by computer control system 12 controlled pressure feeding systems, step motor is promoting syringe pump injection pressure oil in measuring pedestal 9 endoporus under the driving of computer control system 12, write down the variation of the volume of the pressure oil that per step of step motor exported with working sample window 5 radius a simultaneously.At this moment elastic-plastic deformation takes place in diamond coatings 1 under the effect of pressure oil internal pressure, and the fractional increments of da can effectively improve the radius dh of window.The increase of radius has caused the increase of the total area of coating internal stress and distortion coating, so the deformation energy of coating also increases.The merit of being done by the pressure fluid extrusion coating is bigger compared with the increase of coating internal strain energy.These two measure poor, can be expressed as: energy release rate G, it can represent release coating energy needed effectively.Only when G was equal to or greater than the energy that coating is consumed on the per unit area when matrix is peeled off, coating just can be peeled off, and the energy that is consumed on this per unit area can be remembered as critical crack expansion stresses (G
c), it comprises the chemical bond energy at interface and the additional energy that elastic-plastic deformation consumed takes place near the Interface Crack tip.Get final product the adhesive strength that diamond coatings is described on accurate quantification ground with it.
The 5th step: when 8 pairs of systems of computer control system 12 controlled pressure feeding systems pressurize, by the variation of pressure p in the pressure-measuring system 7 The real time measure systems, and the measuring-signal that collected is transmitted, is stored in the computing machine to make things convenient for subsequent treatment by data line by computer control system 12.
The 6th step: when 8 pairs of systems of computer control system 12 controlled pressure feeding systems pressurize, by the variation of the He-Ne laser interferometry system 4 The real time measure diamond coatings sample windows 5 height h of central authorities.By adjusting support, perpendicular displacement when the Laser Measuring measuring device of He-Ne laser interferometry system 4 is directly aimed at sample window 5 central authorities with the distortion of measurement coating, the measuring-signal that is obtained is imported in the signal amplifier 11 by the data line connection, by computer control system 12 measuring-signal that is collected is stored in the computing machine to make things convenient for subsequent treatment after amplifying.
The 7th step: the adhesive strength that calculates coating 1 by calculation procedure.Learn according to theoretical model analysis, when the ratio of the variation of the sample window the measured 5 height h of central authorities and the variation of windows radius a changes, coating 1 will be peeled off, at this moment pass through the variation of the diamond coatings sample window measured 5 height h and corresponding pressure p just can by the calculation procedure accurate quantification in the computing machine calculate the adhesive strength of diamond coatings 1.
Claims (1)
1. an internal expanding Bubbling method detects the measuring technology of diamond coatings adhesive strength, it is characterized in that this measuring technology comprises following testing procedure:
[1] preparation diamond coatings sample window (5): adopt chemical corrosion, micro-manufactured or other method to process outside a window cavity volume (3) makes that the coating inner surface that originally contacts with matrix is exposed at the back side of diamond coatings matrix (2), the while is not damaged to diamond coatings (1);
[2] adopt diglycidyl ethers propane type epoxy resin of di phenolic group cementing agent that diamond coatings sample window (5) the substrate ring oxidation for preparing is fixed on the top of sample holder (6), the center of sample holder (6) top through hole is then aimed at the center of diamond coatings sample window (5);
[3] by computer control system (12) controlled pressure feeding system (8) system is pressurizeed, step motor writes down the volume of injection pressure oil in measuring pedestal (9) endoporus of per step of step motor simultaneously at the injection pressure oil in measuring pedestal (9) endoporus of promotion syringe pump under the driving of computer control system (12);
[4] when computer control system (12) controlled pressure feeding system (8) pressurizes to system, by the variation of pressure in pressure-measuring system (7) the The real time measure system, and the measuring-signal that collected is transmitted, is stored in the computing machine to make things convenient for subsequent treatment by data line by computer control system (12).
[5] when computer control system (12) controlled pressure feeding system (8) pressurizes to system, by the variation of He-Ne laser interferometry system (4) The real time measure diamond coatings sample window (5) central authorities height.By adjusting support, perpendicular displacement when the Laser Measuring measuring device of He-Ne laser interferometry system (4) is directly aimed at sample window (5) central authorities with the distortion of measurement coating, the measuring-signal that is obtained is imported in the signal amplifier (11) by the data line connection, by computer control system (12) measuring-signal that is collected is stored in the computing machine to make things convenient for subsequent treatment after amplifying.
[6] calculate the adhesive strength of coating by calculation procedure, learn according to theoretical model analysis, when the ratio of the variation of the height h of the sample window measured central authorities and the variation of windows radius a changes, coating will be peeled off, at this moment pass through the variation h of the diamond coatings sample window height measured and corresponding pressure p just can by the calculation procedure accurate quantification in the computing machine calculate the adhesive strength of diamond coatings.
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|---|---|---|---|
| CNA2003101083075A CN1540309A (en) | 2003-10-30 | 2003-10-30 | Measuing and testing techniques for detecting adhesive strength of diamond coat by method of innor expand and bubbling |
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|---|---|---|---|
| CNA2003101083075A CN1540309A (en) | 2003-10-30 | 2003-10-30 | Measuing and testing techniques for detecting adhesive strength of diamond coat by method of innor expand and bubbling |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101122561B (en) * | 2007-08-02 | 2010-06-30 | 上海交通大学 | Back penetration measuring method for film base binding performance |
| CN104359835A (en) * | 2014-11-24 | 2015-02-18 | 湘潭大学 | Method for measuring interfacial bonding strength of flexible thin film |
| CN106323871A (en) * | 2016-08-18 | 2017-01-11 | 温州市大荣纺织仪器有限公司 | Fabric film covering fastness testing method |
| CN107389459A (en) * | 2017-07-12 | 2017-11-24 | 东北大学 | A kind of thin film mechanical performance real-time test device |
| CN108931429A (en) * | 2018-07-13 | 2018-12-04 | 中国科学院半导体研究所 | A kind of test method of laser cladding layer and substrate combinating strength |
| CN113484155A (en) * | 2021-07-06 | 2021-10-08 | 中国工程物理研究院激光聚变研究中心 | Ultrathin film mechanical property measuring device and method |
-
2003
- 2003-10-30 CN CNA2003101083075A patent/CN1540309A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101122561B (en) * | 2007-08-02 | 2010-06-30 | 上海交通大学 | Back penetration measuring method for film base binding performance |
| CN104359835A (en) * | 2014-11-24 | 2015-02-18 | 湘潭大学 | Method for measuring interfacial bonding strength of flexible thin film |
| CN106323871A (en) * | 2016-08-18 | 2017-01-11 | 温州市大荣纺织仪器有限公司 | Fabric film covering fastness testing method |
| CN107389459A (en) * | 2017-07-12 | 2017-11-24 | 东北大学 | A kind of thin film mechanical performance real-time test device |
| CN108931429A (en) * | 2018-07-13 | 2018-12-04 | 中国科学院半导体研究所 | A kind of test method of laser cladding layer and substrate combinating strength |
| CN108931429B (en) * | 2018-07-13 | 2020-02-21 | 中国科学院半导体研究所 | Method for testing bonding strength of laser cladding layer and substrate |
| CN113484155A (en) * | 2021-07-06 | 2021-10-08 | 中国工程物理研究院激光聚变研究中心 | Ultrathin film mechanical property measuring device and method |
| CN113484155B (en) * | 2021-07-06 | 2024-05-24 | 中国工程物理研究院激光聚变研究中心 | Ultrathin film mechanical property measuring device and mechanical property measuring method |
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