CN106610389B - A method of measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature - Google Patents
A method of measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature Download PDFInfo
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Abstract
The present invention is suitable for coating technology field, provides a kind of method for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature, comprising the following steps: prepares a-C:H coating sample: A sample and B sample with two kinds of various substrates；A sample and B sample are successively measured in T0、T1Under radius of curvature RA0And RB0、RA1And RB1；A sample and B sample are calculated separately in Δ T=T using Stoney formula1‑T0The stress variation Δ σ of lower sampleA1With Δ σB1, the thermalexpansioncoefficientα of a-C:H coating is obtained after deformingf1；Repeat the above steps operation, obtains T2、T3…Ti‑1、TiAt a temperature of the a-C:H coating in different temperature range Ti‑1→TiInterior average linear expansion coefficient αfi, wherein i=1,2,3 ..., obtain the linear expansion coefficient variation with temperature curve of the a-C:H coating.
Description
Technical field
The invention belongs to coating technology field more particularly to it is a kind of measure hydrogeneous diamond-like coating at low temperature heat it is swollen
The method of swollen coefficient.
Background technique
Containing hydrogen diamond (a-C:H) coating due to its under vacuum and dry environment with extremely low coefficient of friction (<
0.01), especially suitable for the solid lubrication components in spacecraft, such as airship or the separating mechanism of space station, retaining mechanism, right
Connection mechanism, the ball bearing of solar energy sailboard mechanism, oxygen regulating valve automatic control system, gyroscope and inertial control system with
And transmission mechanism of space resources drilling equipment etc. needs the space components of solid lubrication.
As the solid lubricant coating of space components, working environment and conventional ground environment difference are very big, in addition to height
Outside vacuum condition, space components still suffer from the ultra-low temperature surroundings (about -250 DEG C of minimum temperature) of space.A-C:H coating sinks
Accumulated temperature degree is generally 200-500 DEG C, much higher than its use temperature in space, since the heat of DLC coating and base material is swollen
Swollen coefficient (Coefficient of Thermal Expansion, CTE) has differences, and certainly will generate biggish heat in the coating
Stress is easy crack initiation in the coating and even results in disbonding.In order to avoid the generation of this problem, it is necessary to selection thermal expansion
Coefficient and the lesser base material of a-C:H coating difference, or selection thermal expansion coefficient is between a-C:H coating and substrate
Material is as buffer layer.But, it carries out substrate or buffer layer is preferred on condition that necessary known a-C:H coating is in ultra-low temperature surroundings
Under thermal expansion coefficient, however the research of hot expansibility of the DLC coating under ultra-low temperature surroundings is rarely reported at present.Therefore,
Hot expansibility of the a-C:H coating under ultra-low temperature surroundings is studied, there is important promotion for its application in space field
Effect.
Currently, a-C:H coating hot expansibility report is less, Champi et al. (A.Champi, R.G.Lacerda,
G.A.Viana and F.C.Marques.Journal of Non-Crystalline Solids,2004(338-340):
The thermal expansion coefficient of a-C:H 499-502) is studied using thermal induction bending method (Thermally induced bending, TIB),
So-called thermal induction bending method is thermal stress formula and Stoney formula based on coating, it may be assumed that Δ σ=Ef/(1-νf)(αs-αf)(T-
T0), σ=[Es/(1-νs)]ts2/6tf(1/R-1/R0)；In formula, E, ν, α and t are respectively Young's modulus, Poisson's ratio, line expansion
Coefficient and thickness；Subscript s and f respectively indicate substrate and coating；R0For in temperature T0When sample radius of curvature, R be in temperature T
When sample radius of curvature；Make coating sample temperature by T by heating0It is increased to T, due to coating and substrate thermal expansion coefficient
It mismatches, thermal stress can be generated in coating, and sample radius of curvature under thermal stress effect can change, then by curvature half
The knots modification of diameter substitutes into Stoney formula, and then calculates the thermal stress of coating, and thermal stress result is then substituted into thermal stress formula
The thermal expansion coefficient of coating is calculated.
However, existing test method can only provide the thermal expansion coefficient of a-C:H coating at room temperature, and can not obtain
Thermal expansion coefficient under low temperature, thus can not use to a-C:H coating as space solid lubricant coating at low ambient temperatures
Provide directive function.
Summary of the invention
The purpose of the present invention is to provide a kind of sides for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature
Method, it is intended to solve the problems, such as that the prior art can not obtain the thermal expansion coefficient containing hydrogen diamond (a-C:H) coating at low temperature.
The invention is realized in this way a kind of side for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature
Method, comprising the following steps:
(1) a-C:H coating sample is prepared using two kinds of different materials as substrate, respectively obtains A sample and B sample；
(2) in temperature T0Under, measure the radius of curvature R of the A sample and the B sample respectively using stress gaugeA0And RB0；
(3) sample temperature is increased to by T by temperature control system1, then isothermal holding measures the A sample and institute respectively
State the radius of curvature R of B sampleA1And RB1；
(4) the A sample and the B sample are calculated separately in Δ T=T using Stoney formula1-T0The stress of lower sample
Changes delta σA1With Δ σB1, expression formula is distinguished as follows:
ΔσA1=Ef/(1-νf)(αsA1-αf)(T-T0) (formula 1),
ΔσB1=Ef/(1-νf)(αsB1-αf)(T-T0) (formula 2),
(5) by the Δ σA1With the Δ σB1Expression formula be divided by, eliminate common phase Ef/(1-νf)(T-T0), through deforming
The thermalexpansioncoefficientα of available a-C:H coating afterwardsf1, expression formula is as follows:
αf1=(Δ σB1αsA1-ΔσA1αsB1)/(ΔσB1-ΔσA1) (formula 3),
In formula, αf1It is T0→T1Average linear expansion coefficient in temperature range；
(6) repeat the above steps the operations of (3)-(5), by successively measuring T2、T3…Ti-1、TiAt a temperature of the A sample
With the radius of curvature R of the B sampleA2、RA3…RAi-1、RAiAnd RB2、RB3…RBi-1、RBi, calculate separately the A sample and the B
Sample is in Δ T=Ti-Ti-1The stress variation Δ σ of lower sampleAiWith Δ σBi, the a-C:H coating is successively obtained in different temperature
Section Ti-1→TiInterior average linear expansion coefficient αfi, wherein i=1,2,3 ..., obtain
αfi(Ti-1→Ti)≈αfi[(Ti-1+Ti)/2] (formula 4),
Obtain the linear expansion coefficient variation with temperature curve of the a-C:H coating.
The method of measurement thermal expansion coefficient at low temperature Han hydrogen diamond (a-C:H) coating provided by the invention, benefit
The thermal expansion coefficient in a-C:H coating low temperature range is measured with thermal induction bending method, and obtains thermal expansion coefficient and varies with temperature
Relation curve, the relation curve that (100-300K) thermal expansion coefficient varies with temperature especially at low temperature.To be a-C:H
The use of coating at low temperature provides design parameter, and then a-C:H coating and the mismatch production of substrate thermal expansion coefficient is effectively reduced
Influence of the raw thermal stress to coating service performance.
Detailed description of the invention
Fig. 1 is the structural representation provided in an embodiment of the present invention in (100) monocrystalline substrate after deposition a-C:H coating
Figure；
Fig. 2 is the structural schematic diagram provided in an embodiment of the present invention in copper substrate after deposition a-C:H coating；
Fig. 3 is linear expansion coefficient of (100) monocrystalline silicon provided in an embodiment of the present invention within the scope of 100-300K with temperature
Variation relation curve graph；
Fig. 4 is that linear expansion coefficient of the copper provided in an embodiment of the present invention within the scope of 100-300K varies with temperature relationship song
Line chart；
Fig. 5 be (100) monocrystalline silicon provided in an embodiment of the present invention within the scope of 100-300K Young's modulus and Poisson's ratio with
Temperature change relation curve；
Fig. 6 is that copper provided in an embodiment of the present invention Young's modulus and Poisson's ratio within the scope of 100-300K vary with temperature pass
It is curve.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Accompanying drawings and embodiments, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used
To explain the present invention, it is not intended to limit the present invention.
The embodiment of the invention provides a kind of method for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature,
The following steps are included:
(1) a-C:H coating sample is prepared using two kinds of different materials as substrate, respectively obtains A sample and B sample；
(2) in temperature T0Under, measure the radius of curvature R of the A sample and the B sample respectively using stress gaugeA0And RB0；
(3) sample temperature is increased to by T by temperature control system1, then isothermal holding measures the A sample and institute respectively
State the radius of curvature R of B sampleA1And RB1；
(4) the A sample and the B sample are calculated separately in Δ T=T using Stoney formula1-T0The stress of lower sample
Changes delta σA1With Δ σB1, expression formula is distinguished as follows:
ΔσA1=Ef/(1-νf)(αsA1-αf)(T-T0) (formula 1),
ΔσB1=Ef/(1-νf)(αsB1-αf)(T-T0) (formula 2),
(5) by the Δ σA1With the Δ σB1Expression formula be divided by, eliminate common phase Ef/(1-νf)(T-T0), through deforming
The thermalexpansioncoefficientα of available a-C:H coating afterwardsf1, expression formula is as follows:
αf1=(Δ σB1αsA1-ΔσA1αsB1)/(ΔσB1-ΔσA1) (formula 3),
In formula, αf1It is T0→T1Average linear expansion coefficient in temperature range；
(6) repeat the above steps the operations of (3)-(5), by successively measuring T2、T3…Ti-1、TiAt a temperature of the A sample
With the radius of curvature R of the B sampleA2、RA3…RAi-1、RAiAnd RB2、RB3…RBi-1、RBi, calculate separately the A sample and the B
Sample is in Δ T=Ti-Ti-1The stress variation Δ σ of lower sampleAiWith Δ σBi, the a-C:H coating is successively obtained in different temperature
Section Ti-1→TiInterior average linear expansion coefficient αfi, wherein i=1,2,3 ..., obtain
αfi(Ti-1→Ti)≈αfi[(Ti-1+Ti)/2] (formula 4),
Obtain the linear expansion coefficient variation with temperature curve of the a-C:H coating.
Specifically, two kinds of different materials as substrate need to meet as the normal of substrate material in above-mentioned steps (1)
Rule require, and as having the substrate material of reflection function after polishing treatment, and also need the rigidity for having certain, prevent in use process
There is irregular or non-uniform bending deformation phenomenon.In the embodiment of the present invention, two kinds of different materials as substrate are
In T0→TiIn range, two kinds of different materials, thus can be used as under calculating known to thermal expansion coefficient, Young's modulus and Poisson's ratio
State the stress variation Δ σ of A sample described in step and the B sampleA1With Δ σB1.As substrate described in the embodiment of the present invention
The acquisition of the thermal expansion coefficient, Young's modulus and Poisson's ratio of two kinds of different materials, directly can report data by consulting literatures
It obtains, can also report data by Arranging Literatures, fit data and curves acquisition.
As a specific embodiment, the substrate of described two different materials can be respectively (100) monocrystalline substrate and
Copper substrate, the structure difference after a-C:H coating is deposited on (100) monocrystalline silicon and the copper substrate is as shown in Figure 1 and Figure 2,
Wherein 10 indicate a-C:H coating, 20,30 respectively indicate (100) monocrystalline substrate and copper substrate.It is (100) monocrystalline silicon, described
It is as shown in Figure 3, Figure 4 that linear expansion coefficient of the copper within the scope of 100-300K varies with temperature relation curve difference；Described (100) are single
Crystal silicon, the copper Young's modulus and Poisson's ratio within the scope of 100-300K vary with temperature relation curve respectively such as Fig. 5, Fig. 6 institute
Show.
In the embodiment of the present invention, used thermal expansion coefficient formula (see formula 1 and formula 2) contains there are two known variables, point
Not Wei coating twin shaft elastic modulus Ef/(1-νf) and coating thermalexpansioncoefficientαf, therefore can not be asked by an independent equation
Solution, but need to obtain two independent equations as substrate using two kinds of materials with different heat expansion coefficient, pass through simultaneous
Solve system of equation can be solved.Preferred embodiment, the thermal expansion coefficient of two kinds of different materials as substrate
Relative deviation is greater than 10%, and relative deviation is bigger, and it is smaller to calculate error.
The method that the embodiment of the present invention prepares a-C:H coating sample on substrate is unrestricted, can be normal using this field
Rule method is realized, is specifically including but not limited to using plasma enhancing chemical vapour deposition technique or ion beam deposition is realized.
In above-mentioned steps (2), the A sample and the B sample are measured respectively using stress gauge in temperature T0Under curvature
Radius RA0And RB0, the stress gauge is the stress gauge with low temperature platform, and the low temperature range includes 100-300K, i.e. temperature can
With from 100-300K linear regulation.
In above-mentioned steps (3), the radius of curvature R of the A sample and the B sample is measuredA1And RB1Before need at heat preservation
Reason, to guarantee the temperature uniformity of A sample and B sample, to obtain reliable and stable radius of curvature data.As preferred implementation
Example, time >=2min of the isothermal holding.
In the embodiment of the present invention, the T1And subsequent T2、T3…Ti-1、TiSelection, without specific actual temp point
Value requires, of course it is to be understood that Δ T, that is, Ti-Ti-1α that is smaller, then obtainingfiData it is more, thus obtain the a-C:H
The linear expansion coefficient variation with temperature curve of coating is more accurate reliable.But when the Δ T is too small, since temperature itself can
Energy bring error is amplified, and is unfavorable for obtaining the linear expansion coefficient of the accurately a-C:H coating instead.As preferred implementation
Example, the Δ T meet: 5K≤Δ T≤50K.Further, the Δ T is preferably satisfied: 10K≤Δ T≤50K.
In above-mentioned steps (4), the Stoney formula is specially
σ=[Es/(1-νs)]ts 2/6tf(1/R-1/R0) (formula 5).
By the formula 5, it can calculate and obtain the A sample and the B sample in Δ T=T1-T0The stress of lower sample becomes
Change Δ σA1With Δ σB1, specifically as shown in formula 1, formula 2.
In above-mentioned steps (5), above-mentioned formula 1, formula 2 are divided by, after eliminating common factor formula and deformation, a-C:H can be obtained
The thermalexpansioncoefficientα of coatingf1, expression formula is as shown in Equation 3, thus to obtain T0→T1Average linear expansion coefficient in temperature range
αf1。
In above-mentioned steps (6), the operation for (3)-(5) that repeat the above steps can successively obtain T2、T3…Ti-1、TiTemperature
Lower average linear expansion coefficient αfi, wherein i=1,2,3 ....
Specifically, having measured the A sample and the B sample in temperature T1Under radius of curvature RA1And RB1The case where
Under, it repeats step (3), sample temperature is continued to rise into T3, keep the temperature and measure the curvature half of the A sample and the B sample
Diameter RA2And RB2, then repeatedly step (4), (5) obtain a-C:H coating in T2→T3Average linear expansion coefficient in temperature range
αf2；After the same method, a-C:H coating is gradually measured in different temperature range Ti-1→TiInterior average line expands system
Number αfi, wherein i=1,2,3 ...；Since the linear expansion coefficient of material is usually dull linear change in 100-300K temperature range
Change, in Δ T=Ti-Ti-1In the case where sufficiently small,
It is considered that the linear expansion coefficient of a-C:H coating is approximately constant in Δ T temperature range, then have following relationship at
It is vertical:
αfi(Ti-1→Ti)≈αfi[(Ti-1+Ti)/2] (formula 4)
Thus to obtain the linear expansion coefficient variation with temperature curve of the a-C:H coating, wherein the αfiRefer to
Ti-1→TiAverage linear expansion coefficient in temperature range, and it is approximately equal to T=(Ti-1+TiLinear expansion coefficient when)/2 temperature.
In the embodiment of the present invention, the T0→TiTemperature range measurement temperature range range be 0-1000K.Herein, it answers
It is interpreted as, the T0It is minimum can be to 0K, the TiHighest can be to 1000K, i.e., the described T0≥0K；The Ti≤1000K.Further
, preferably T0=100K, Ti=300K.
As a preferred embodiment, the Δ T meets: 5K≤Δ T≤20K；Further preferably, the Δ T meets: 10K
≤ΔT≤20K.Herein, due to Δ T=Ti-Ti-1It is sufficiently small, it is believed that the linear expansion coefficient of a-C:H coating is in Δ T temperature
It is approximately a constant in range.
In the embodiment of the present invention, the TiSetting need to meet the A sample and the B sample does not occur at such a temperature
Deformation, oxidation.Therefore, the method for the embodiment of the present invention can be used for the line expansion of the a-C:H coating under room temperature, high temperature
The measurement of coefficient.As a preferred embodiment, the highest test temperature is not less than 300K.I.e. the embodiment of the present invention is used in particular for low
The measurement of the linear expansion coefficient of the a-C:H coating under warm environment.
Measurement method described in the embodiment of the present invention is based on thermal stress formula and Stoney formula, and selection has in low temperature range
There are two different materials of known thermal expansion coefficient and Young's modulus and Poisson's ratio as substrate, in two different substrates
Upper deposition a-C:H coating；Then, changed by measuring the radius of curvature of two kinds of coating samples in temperature-rise period, utilized
Stoney formula and thermal stress formula calculate the thermal expansion coefficient of a-C:H coating at different temperatures, and obtain a-C:H coating and exist
Thermal expansion coefficient variation with temperature relation curve in low temperature range.
The side of measurement thermal expansion coefficient at low temperature Han hydrogen diamond (a-C:H) coating provided in an embodiment of the present invention
Method using the thermal expansion coefficient in thermal induction bending method measurement a-C:H coating low temperature range, and obtains thermal expansion coefficient with temperature
The relation curve of variation, the relation curve that (100-300K) thermal expansion coefficient varies with temperature especially at low temperature.To be
The use at low temperature of a-C:H coating provides design parameter, and then a-C:H coating and substrate thermal expansion coefficient is not effectively reduced not
Influence of the thermal stress with generation to coating service performance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. a kind of method for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature, comprising the following steps:
(1) a-C:H coating sample is prepared using two kinds of different materials as substrate, respectively obtains A sample and B sample；
(2) in temperature T0Under, measure the radius of curvature R of the A sample and the B sample respectively using stress gaugeA0And RB0；
(3) sample temperature is increased to by T by temperature control system1, then isothermal holding measures the A sample and the B sample respectively
The radius of curvature R of productA1And RB1；
(4) the A sample and the B sample are calculated separately in Δ T=T using Stoney formula1-T0The stress variation of lower sample
ΔσA1With Δ σB1, expression formula is distinguished as follows, wherein EfFor Young's modulus, νfFor the Poisson's ratio of coating, αsA1For sample A substrate
Thermal expansion coefficient, αfFor the thermal expansion coefficient of coating, αsB1For the thermal expansion coefficient of sample B substrate,
ΔσA1=Ef/(1-νf)(αsA1-αf)(T-T0) (formula 1),
ΔσB1=Ef/(1-νf)(αsB1-αf)(T-T0) (formula 2),
(5) by the Δ σA1With the Δ σB1Expression formula be divided by, eliminate common phase Ef/(1-νf)(T-T0), it can be with after deforming
Obtain the thermalexpansioncoefficientα of a-C:H coatingf1, expression formula is as follows:
αf1=(Δ σB1αsA1-ΔσA1αsB1)/(ΔσB1-ΔσA1) (formula 3),
In formula, αf1It is T0→T1Average linear expansion coefficient in temperature range；
(6) repeat the above steps the operations of (3)-(5), by successively measuring T2、T3…Ti-1、TiAt a temperature of the A sample and institute
State the radius of curvature R of B sampleA2、RA3…RAi-1、RAiAnd RB2、RB3…RBi-1、RBi, calculate separately the A sample and the B sample
In Δ T=Ti-Ti-1The stress variation Δ σ of lower sampleAiWith Δ σBi, the a-C:H coating is successively obtained in different temperature ranges
Ti-1→TiInterior average linear expansion coefficient αfi(Ti-1→Ti), wherein i=1,2,3 ..., obtain
αfi(Ti-1→Ti)≈αfi[(Ti-1+Ti)/2](formula 4),
Obtain the linear expansion coefficient variation with temperature curve of the a-C:H coating；
In formula 4, αfi[(Ti-1+Ti)/2]It in temperature is [(T for coatingi-1+Ti)/2] thermal expansion coefficient；
The T0→TiTemperature range range be 100-300K.
2. the method for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature as described in claim 1, feature
It is, the Δ T meets: 5K≤Δ T≤50K.
3. the method for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature as claimed in claim 2, feature
It is, the Δ T meets: 10K≤Δ T≤50K.
4. the method for the thermal expansion coefficient of the hydrogeneous diamond-like coating of measurement a method according to any one of claims 1-3 at low temperature,
It is characterized in that, two kinds of different materials as substrate are in T0→TiIn range, thermal expansion coefficient, Young's modulus and pool
Pine is than known two kinds of different materials.
5. the method for measuring the thermal expansion coefficient of hydrogeneous diamond-like coating at low temperature as claimed in claim 4, feature
It is, the relative deviation of the thermal expansion coefficient of two kinds of different materials as substrate is greater than 10%.
6. the method for the thermal expansion coefficient of the hydrogeneous diamond-like coating of measurement a method according to any one of claims 1-3 at low temperature,
It is characterized in that, the time of the isothermal holding >=2min.
7. the method for the thermal expansion coefficient of the hydrogeneous diamond-like coating of measurement a method according to any one of claims 1-3 at low temperature,
It is characterized in that, the Stoney formula is
σ=[Es/(1-νs)]ts 2/6tf(1/R-1/R0) (formula 5)
In formula 5, σ is stress, EsFor Young's modulus, νsFor the Poisson's ratio of substrate, tsFor the thickness of substrate, tfFor the thickness of coating, R
For the radius of curvature of sample after heating, R0For the radius of curvature for the preceding sample that heats up.
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|---|---|---|---|---|
| SU502301A1 (en) * | 1974-04-22 | 1976-02-05 | Ордена Трудового Красного Знамени Институт Физики Ан Литовской Сср | Method for determining hermetic linear expansion coefficient |
| SU693191A1 (en) * | 1977-08-23 | 1979-10-25 | Предприятие П/Я А-1857 | Method of determining linear expansion thermal coefficient |
| JPH11281599A (en) * | 1998-03-26 | 1999-10-15 | Kyocera Corp | Method for measuring linear expansion coefficient |
| JP2012026900A (en) * | 2010-07-26 | 2012-02-09 | Japan Polypropylene Corp | Thermal expansion measuring apparatus |
| CN203688116U (en) * | 2013-12-18 | 2014-07-02 | 深圳职业技术学院 | Thin film stress tester |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU502301A1 (en) * | 1974-04-22 | 1976-02-05 | Ордена Трудового Красного Знамени Институт Физики Ан Литовской Сср | Method for determining hermetic linear expansion coefficient |
| SU693191A1 (en) * | 1977-08-23 | 1979-10-25 | Предприятие П/Я А-1857 | Method of determining linear expansion thermal coefficient |
| JPH11281599A (en) * | 1998-03-26 | 1999-10-15 | Kyocera Corp | Method for measuring linear expansion coefficient |
| JP2012026900A (en) * | 2010-07-26 | 2012-02-09 | Japan Polypropylene Corp | Thermal expansion measuring apparatus |
| CN203688116U (en) * | 2013-12-18 | 2014-07-02 | 深圳职业技术学院 | Thin film stress tester |
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