CN1204390C - Indentor and method for producing the same - Google Patents

Indentor and method for producing the same Download PDF

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Publication number
CN1204390C
CN1204390C CN 01800695 CN01800695A CN1204390C CN 1204390 C CN1204390 C CN 1204390C CN 01800695 CN01800695 CN 01800695 CN 01800695 A CN01800695 A CN 01800695A CN 1204390 C CN1204390 C CN 1204390C
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film
diamond
penetrator
pressure head
boron
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CN 01800695
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CN1365443A (en
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姜辛
乌丁·沙麦塔特
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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
    • G01N3/40—Investigating hardness or rebound hardness
    • G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0098—Tests specified by its name, e.g. Charpy, Brinnel, Mullen
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02—Details not specific for a particular testing method
    • G01N2203/022—Environment of the test
    • G01N2203/0222—Temperature
    • G01N2203/0226—High temperature; Heating means

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a new electronic hardometer indenter which is applicable for measuring material microhardness and binding strength between a film and a base. This indenter is form by steps of vapor phase growing boron doped conductive diamond films, diamond/carbides composite films or amorphous carbon films on the diamond indenter surface. The invention innovates the traditional material hardness measuring method with advantages of easy operation, accurate measuring and possibility of on-line measuring for complex geometry workpiece.

Description

Penetrator
Technical field
The present invention relates to be applied to measure material microhardness and the employed penetrator of film bond strength.The Vickers or the Knoop hardness tester pressure head that for example are used for the material micro-hardness measurement.
Background technology
The measuring method of material microhardness adopts Vickers method (ISO-Norm6507) or Nu Shi method (ISO-Norm4545) usually.In these two kinds of measuring methods, all must use the pressure head of a hard, pressure head is pushed down into sample surfaces in given load, by the width of experimenter at microscopically measurement impression, calculates hardness number more then.The prerequisite that obtains accurate hardness number in this way is to use the pressure head of high rigidity.If the not sufficiently high words of the hardness of pressure head material, its elasticity will cause system errors for measurement.Therefore, the pressure head great majority adopt adamas to make.And these adamass mainly are from natural diamond or by the synthetic adamas of high temperature and high pressure method.The shortcoming of said method is the recovery of elasticity of tested sample impression.Under these circumstances, different when the degree of depth of impression or width are pressed into the back with pressure head, produce measuring error.
For avoiding this systematic error, another kind of method is when pressure head is pressed into, the degree of depth of synchro measure impression.In other words, it is not to produce the back at impression to go to measure its degree of depth with method of optics, but removes to measure the resistance between pressure head and tested sample when impression produces.The most important condition that realizes this measurement is: pressure head must conduct electricity, and tested sample is semiconductor at least.Because resistance is directly proportional with the length of object, so the resistance value of measurement reduces with the increase of pressure head compression distance.This method can be avoided the above-mentioned systematic error that is caused by the elastic properties of materials recovery, and can realize the robotization of hardness measurement.This also makes the hardness measurement of the higher object of difficulty of test become simply, and can realize in-site measurement.That is to say that even if tested object has the complex surfaces shape, the also available the method for its hardness is measured, this is its another advantage.
People's such as Enomoto United States Patent (USP) (US 4,984,453) has provided a kind of sclerometer of being made as the pressure head of pedestal and conduction by insulator.Its pressure head can be by the material such as the boron carbide (B of monolithic conductive 4C) or II type adamas constitute.According to US4,984,453 patents, this II type adamas should be boron doped P-type semiconductor adamas.Another kind method is that the surface of diamond penetrator is carried out the ion injection and made it conduction.
US4, the diamond by boron doping preparation of 984,453 suggestions are to have only very small amount of boron to be impregnated in the adamantine process of preparation in the process of mixing as the problem that pressure head brings.The typical dopant amount is in the ppm scope.Owing to technical reason, high dopant dose can not realize that it is very low that this makes its electricity lead.If adopt the ion injection method of people's suggestion such as Enomoto, conduction is realized on surface that then can diamond penetrator.But the shortcoming that ion injects is that the physical strength on surface is descended, and causes the life-span of pressure head to be reduced.This is to cause the graphitization on diamond penetrator surface because ion injects.The variation of this lattice structure can not reverse with the way of additive method such as thermal treatment or heating.Because this variation is irreversible.Because the generation of surperficial soft rock China ink phase makes the hardness of pressure head reduce on the one hand, can make the surface undesirable lubricated phenomenon occur on the other hand, because graphite is good kollag mutually.The not anti-zoned property of this soft rock China ink phase makes the life-span of pressure head reduce in addition.This is distinct issues to hardness test, because hardness measurement is very high to the machine requirement of strength of pressure head, therefore, and US4, the range of application of 984,453 pressure heads of being advised is very limited.
The Another Application of pressure head is MEASUREMENTS OF THIN and high base strength.The measuring method of film and high base strength has a lot, and a kind of method is the surface of delineating the transverse movement sample with the tip of diamond penetrator with the load that increases gradually.Acoustical signal that the inefficacy of film and substrate combinating strength is discharged by detection system or the optics behind the cut and chemical analysis are determined.The method of back is very complicated, and the Acoustic detection method is the non-direct method of a kind of suitable hard brittle material.Owing to these reasons, the known method with diamond penetrator measurement bond strength has significant limitation.
Summary of the invention
The present invention comes from and solves shortcoming and the problem that exists on the prior art, and prepare a kind of on electricity the diamond penetrator for the hard wear resistant of conductor or semiconductor conduction.
According to invention, this technical matters can be solved by the chemical vapour deposition film pressure head by a kind of.This diamond thin by the chemical vapor deposition preparation has existed for many years and has been proved to be to have with the identical hardness of rusty gold hard rock.Because such diamond thin has the crystal structure identical with natural diamond.Such chemical vapor deposition processes permission realizes the chemical doping on the throne of film in simple mode and can modulate and select the conductivity of film.Its conductivity is generally at 0.1-100 Ω -1Cm -1Between, diamond penetrator is done as a whole, and its resistance will be 100 to 1500 ohm.
In chemical vapor deposition processes, reacting gas is by warm or plasma-activated, and this makes it originally is that the graphite that metastable adamas replaces the thermodynamics stable state mutually deposits.Macroscopical physics of these films and chemical characteristic and natural diamond crystal are roughly the same.By chemical vapor deposition, diamond thin can be deposited on the matrix of complex geometry, makes to widely apply to be achieved.This chemical vapor deposition processes also can as matrix is applied bias voltage, obtain different membrane structures and pattern by different control.
By mix the boracic gaseous reactant in reacting gas, as the tetramethyl borine, the present invention can be on the general chemistry vapor deposition apparatus, the preparation diamond penetrator.It is controlled that the content that mixes the boron in the diamond film can mix the flow of gaseous state boracic reactant by modulation.This process not only can prepare weak boron doped effect of semiconducting diamond films, also make heavy boron doped almost be that the preparation of the diamond film of conductor becomes a reality.The conductivity of diamond film roughly is positioned at 0.1-100 Ω -1Cm -1Between.The content of corresponding boron is 10 19Cm -3To 10 23Cm -3Between.Diamond penetrator by this invention preparation can make the hardness measurement of material have extraordinary S-N ratio, therefore, and measurement result degree of accuracy height.Use unadulterated adamas can only provide signal by playing intrinsic conductivity as pressure head material the method.
Can realize another kind of electrically conducting manner as in diamond, mixing boron.With US4, the doping method in material bodies of 984,453 suggestions is compared, and can mix obviously a large amount of boron with chemical vapor deposition in diamond film.US4, the doping content that the doping method in material bodies of 984,453 patents suggestions can realize be in the ppm scope, and the content that mixes boron in the chemistry for gas phase depositing diamond film can reach 10000ppm.Therefore, the conductivity of mixing the boron diamond penetrator of this patent invention is much larger than the prepared pressure head of prior art.Reach technical desirable signal to noise ratio (S/N ratio) therefrom.
Another technology contents of the present invention is, the another kind of film of growth on diamond penetrator, and carbonide/diamond compound film for example, it compoundly is made of with adamantine mutually carbonide.For realizing this compound phase growth for Thin Film, must be in thin film growth process, in vapour phase, mix and can be carbonized and form metal and other materials of carbonide, such as elements such as silicon, tungsten, titaniums.This compound phase mechanical properties in films is determined by the mean value of two-phase performance, and can be obtained modulation by the ratio of two-phase.The carbonide that in most of the cases contains 1%-10% just can meet the demands.The resistivity of pressure head can be regulated by the content of carbonide phase, promptly from 1 Ω cm to 10 8Ω cm, adjusted in a plurality of order of magnitude scopes.This will be different from that boron mixes and the situation that obtains semiconductive thin film, but directly obtain the conductor thin film that conducts electricity, i.e. ohm conducting film.
The optimum film thickness that is deposited is generally between 1 nanometer to 20 micron.
Because extremely thin thin film deposition is repeated wayward, film thickness preferably is controlled between 0.5 micron to 10 microns.The resistivity of using desired pressure head is finally depended in the selection of film thickness.The conductivity of desired pressure head is high more, and film thickness should be thick more.Therefore thickness also may be applied greater than 20 microns film under special circumstances.Conductivity is regulated continuously.The resistance of pressure head self is between 100 Ω and 1500 Ω.
The method of this deposit film has tangible advantage, and pressure head is made of the diamond body of insulation and the diamond thin of conduction, and film and matrix have extraordinary bond strength, and the life-span of pressure head improves greatly.
The Another Application field of the pressure head that the present invention makes is MEASUREMENTS OF THIN and high base strength.If a kind of film growth of insulation is on a kind of matrix of conduction, we can obtain measuring to the inefficacy of this film rapid whereabouts by the resistance between pressure head and matrix with the diamond penetrator of a conduction.
The deposition process of diamond thin has conventional plasma enhanced chemical vapor deposition and hot-wire chemical gas-phase deposition.By contrast, microwave plasma strengthens chemical gaseous phase depositing process (MWCVD) and has tangible advantage, it under given conditions, can be on (001) Si matrix surface the epitaxial growth diamond thin.
Description of drawings
Fig. 1 has provided the reaction unit of plasma enhanced chemical vapor deposition.
Fig. 2 has provided the scanning electron microscope microphoto of a diamond penetrator.
Fig. 3 has provided the resistance and the relation curve that is pressed into F that high speed steel substrate is exerted pressure (N) of a diamond penetrator.
Embodiment
Fig. 1 has provided the reaction unit 1 of plasma enhanced chemical vapor deposition.This reactor is made up of stainless steel reaction chamber 2 and microwave generator 3.Microwave power can transfer to 1.5 kilowatts.High-frequency induction heating system 4 is used for heating the diamond penetrator that directly is placed on the molybdenum plate sample stage.Diamond penetrator can be bought on market.
Above-mentioned molybdenum plate 5 is directly lain on the graphite heating platform 6.This warm table is existing the description in German patent DE 19905980A1.By regulating the temperature of graphite heating platform, the basic temperature of sample can be controlled continuously in the 200K-1100K scope.The surface temperature of sample matrices can directly be measured by a thermo detector 7.
Matrix is put into after the reaction chamber, reaction chamber is evacuated to 10Pa to 30Pa.Matrix 1 is heated to 600 to 800 ℃ then.Then reacting gas hydrogen, methane and tetramethyl borine are fed in the reaction chamber by air hole 9.The flow of gas is respectively hydrogen 300 to 1150sccm, between methane 1 to 10sccm and the tetramethyl borine 0.001 to 0.1sccm.Sample matrices can add a bias voltage by 150V to 150V.After starting generation microwave plasma 8, produce the gaseous reactant of growing diamond in gas phase.By regulating the pattern and the purity of technological parameter may command diamond film.The resistance of film can pass through substrate bias, the boron impurity content decision of film thickness and film.The bias voltage of matrix can influence the surface topography of film, and the purity of phase also directly influences the resistance of film.
We have carried out a large amount of film growth experiments, and resulting film thickness is between 0.01 and 20 micron, but result of use the best of the film of 0.5 to 10 micron thickness.Boron impurity content should be between 0.01% to 0.6%.The resistance of film can be positioned at 1 ohm to 10 8Ohm.
Fig. 2 has provided the scanning electron microscope microphoto of a diamond penetrator.In the superficial growth of this pressure head the diamond thin of one deck boron-doping.Can know the surface topography of seeing diamond film among the figure.
Fig. 3 has provided the resistance and the relation curve that is pressed into F that high speed steel substrate is exerted pressure (N) of a diamond penetrator.From the resistance that records, can calculate the vertical contact area of pressure head, and the relation of contact area and pressure at right angle draws the hardness number of high speed steel substrate thus with matrix.

Claims (10)

1. a penetrator is characterized in that, pressure head itself is made by adamas as the matrix of deposit film, has the semiconductor conductive film at least on the pressure head surface, and this film is the diamond thin that boron mixes and makes.
2. penetrator according to claim 1 is characterized in that, described film is the diamond thin by the chemical gaseous phase depositing process preparation.
3. penetrator according to claim 1 is characterized in that, the boron content of boron-doping film is between 0.01% and 0.6%.
4. penetrator according to claim 1 is characterized in that described film thickness is between 0.01 micron to 20 microns.
5. penetrator according to claim 4 is characterized in that, the thickness range of film is between 0.5 micron to 10 microns.
6. penetrator according to claim 1, the resistance range that it is characterized in that described film are 1 ohm to 108 ohm.
7. according to the described penetrator of one of claim 1 to 6, it is characterized in that the film on the pressure head is carbonide/diamond compound film.
8. the application of the described penetrator of one of claim 1 to 7 is characterized in that, is applied to measure microhardness.
9. application according to claim 8 is characterized in that, described microhardness is Vickers or Knoop hardness.
10. the application of the described penetrator of one of claim 1 to 7 is characterized in that, is applied to MEASUREMENTS OF THIN and high base strength.
CN 01800695 2000-01-28 2001-01-25 Indentor and method for producing the same Expired - Fee Related CN1204390C (en)

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DE2000103836 DE10003836C2 (en) 2000-01-28 2000-01-28 Indentor and use of the same
DE10003836.0 2000-01-28

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CN1204390C true CN1204390C (en) 2005-06-01

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1782039B1 (en) * 2004-07-02 2008-09-10 Ernst, Erik Hardness tester with indenter of hard metal or compound and oscillating crown for testing at high load and method of comparative assessment of the hardness/depth profile
CN103695863B (en) * 2013-12-09 2016-04-13 四川大学 The preparation method of a kind of boron-doped diamond film/carbon film combination electrode material
CN105158097B (en) * 2015-08-18 2018-06-12 哈尔滨工业大学 A kind of diamond Bo Shi pressure head design methods based on intensity factor
JP2024512203A (en) * 2021-03-25 2024-03-19 華僑大学 Method for detecting tribochemical reaction between abrasive grains and diamond wafer substrate interface

Family Cites Families (11)

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Publication number Priority date Publication date Assignee Title
JPS62503052A (en) * 1985-05-03 1987-12-03 ユニサ−チ・リミテッド hardness measurement
WO1988003644A1 (en) * 1986-11-12 1988-05-19 Unisearch Limited Hardness measuring with a diamond indenter having surface treatment or coating
GB8818445D0 (en) * 1988-08-03 1988-09-07 Jones B L Stm probe
JPH0621849B2 (en) * 1989-02-13 1994-03-23 工業技術院長 Conductive indenter for material testing machine
IT1247645B (en) * 1990-10-24 1994-12-28 Alfred Ernst DUROMETER AND METHOD OF MEASUREMENT OF THE HARDNESS OF METAL MATERIALS
NL9101169A (en) * 1991-07-05 1993-02-01 Drukker Int Bv ELECTRONIC PROBE NEEDLE AND METHOD FOR MANUFACTURING IT.
JPH0617252A (en) * 1992-05-01 1994-01-25 Idemitsu Petrochem Co Ltd Member coated with diamonds and its production
IT1265986B1 (en) * 1993-09-10 1996-12-16 Alfred Ernst ELECTRIC RESISTANCE HARD GAUGE FOR DETERMINING THE HARDNESS OF METALLIC MATERIALS
US5618619A (en) * 1994-03-03 1997-04-08 Monsanto Company Highly abrasion-resistant, flexible coatings for soft substrates
FR2739494B1 (en) * 1995-09-29 1997-11-14 Suisse Electronique Microtech PROCESS FOR MANUFACTURING MICROMECHANICS PARTS WITH A DIAMOND PART CONSISTING OF AT LEAST ONE TIP, AND MICROMECHANICAL PARTS WITH AT LEAST ONE DIAMOND TIP
DE19622701A1 (en) * 1996-06-05 1997-12-18 Fraunhofer Ges Forschung Cantilever chip for atomic force microscopy

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WO2001055695A1 (en) 2001-08-02
DE10003836A1 (en) 2001-08-16
CN1365443A (en) 2002-08-21
DE10003836C2 (en) 2002-04-25

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