CN106525667B - A kind of detection method and application for managing nanoscale soot particulate matter characteristic - Google Patents
A kind of detection method and application for managing nanoscale soot particulate matter characteristic Download PDFInfo
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- 239000004071 soot Substances 0.000 title claims abstract description 172
- 238000001514 detection method Methods 0.000 title claims abstract description 20
- 239000013618 particulate matter Substances 0.000 title claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 118
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 45
- 238000001179 sorption measurement Methods 0.000 claims abstract description 20
- 238000005411 Van der Waals force Methods 0.000 claims abstract description 19
- 238000000418 atomic force spectrum Methods 0.000 claims abstract description 19
- 238000005087 graphitization Methods 0.000 claims abstract description 17
- 239000000523 sample Substances 0.000 claims description 56
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 22
- 238000009792 diffusion process Methods 0.000 claims description 18
- 239000010445 mica Substances 0.000 claims description 15
- 229910052618 mica group Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 11
- 239000000446 fuel Substances 0.000 claims description 6
- 238000005381 potential energy Methods 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001237 Raman spectrum Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000009795 derivation Methods 0.000 claims description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 3
- 239000002210 silicon-based material Substances 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 230000005622 photoelectricity Effects 0.000 claims 1
- 238000002485 combustion reaction Methods 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 230000002265 prevention Effects 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 101100042474 Homo sapiens SFTPD gene Proteins 0.000 description 2
- 230000005483 Hooke's law Effects 0.000 description 2
- 102100027845 Pulmonary surfactant-associated protein D Human genes 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 235000019504 cigarettes Nutrition 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000011217 control strategy Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N2015/0038—Investigating nanoparticles
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Abstract
The invention discloses a kind of detection methods for managing nanoscale soot particulate matter characteristic, three-dimensional appearance, mechanical characteristic and degree of graphitization at the same position of nanoscale soot particle are detected simultaneously using atomic force microscope and Raman spectrometer combined system, are included the following steps：Three-dimensional appearance, force curve and the Raman spectrogram for obtaining nanoscale soot particulate samples carry out swarming fitting to evaluate the degree of graphitization of nanoscale soot particulate samples with origin softwares to Raman spectrogram；The mechanical characteristic of all nanoscale soot particulate samples is finally obtained, the mechanical characteristic includes adsorption capacity, Van der Waals force and adhesion strength.The present invention can study the development law of the three-dimensional appearance of the soot particle generated in separate sources combustion process, mechanical characteristic and degree of graphitization, its result of study contributes to the deep generation for understanding soot particle and evolution mechanism, to provide theoretical direction to reduce the discharge of soot particle and the prevention of air environmental pollution.
Description
Technical field
The present invention relates to a kind of detection method of soot particle more particularly to it is a kind of to nanoscale soot particulate matter manage characteristic
Detection method.
Background technology
Influence of the soot particle being discharged to environment and human health of burning increasingly attracts attention, and countries in the world are to soot
Relevant policy has also all been formulated in the discharge of particle.Deeply understand soot particle generation in combustion, evolution mechanism, tool
There is very important meaning.It is low to realize to controlling the discharge of pollutant to proposing corresponding control strategy in terms of principle
Soot particle discharges.Although related research institutes in terms of soot particle formation mechenism to having done a large amount of work both at home and abroad,
And make great progress, but since soot particle forming process is extremely complex so that it generates evolution mechanism about it and arrives
It is not yet fully apparent from so far.
The combination of atomic force microscope and Raman spectrum can be used as a kind of effective method in nanoscale
Upper research soot particle three-dimensional appearance, mechanical characteristic and corresponding degree of graphitization development law in combustion, this grinds
Study carefully achievement contribute to it is deep understand that soot particle generates mechanism of Evolution, to provide theory for the discharge of reduction soot particle and refer to
It leads.
Invention content
Object of the invention it is proposed a kind of detection method for managing nanoscale soot particulate matter characteristic, atomic force microscope
Three-dimensional appearance, the mechanical characteristic at the soot particle same position to separate sources may be implemented with Raman spectrometer combined system
And degree of graphitization synchronizes the purpose of detection, while also ensuring the consistency of data.
In order to solve the above-mentioned technical problem, a kind of detection side managing nanoscale soot particulate matter characteristic proposed by the present invention
Method is detected using atomic force microscope and Raman spectrometer combined system at the same position of nanoscale soot particle simultaneously
Three-dimensional appearance, mechanical characteristic and degree of graphitization, include the following steps：
Step 1: the nanoscale soot particle obtained under different operating modes is collected respectively on one group of mica sheet, by every
Mica sheet with nanoscale soot particulate samples is individually positioned in after being labeled in a culture dish, is waited to be analyzed；
Step 2: by laser, monitor, white light source, the meter of atomic force microscope and Raman spectrometer combined system
Calculation machine, display and controller power source are opened；
Step 3: the three-dimensional appearance and Raman spectrogram of nanoscale soot particulate samples are obtained, including：
The wherein a piece of mica sheet with nanoscale soot particulate samples 3-1) is fixed on atomic force microscope and Raman
On the example platform of spectrometer combined system；
The laser beam position for 3-2) adjusting atomic force microscope in atomic force microscope and Raman spectrometer combined system, makes
Vertical irradiation overarm probe front；Adjustment reflection laser is allowed to position sensing of the vertical irradiation in atomic force microscope
On the center of photodetector (position-sensitive photodetector, be abbreviated as PSPD)；Then it adjusts
Optical focus and focal length so that probe is close to clear sample；
The lasing light emitter of Raman spectrometer selects He-Ne, the laser in atomic force microscope and Raman spectrometer combined system
The launch wavelength in source is 532nm, object lens are selected as 50X, eyepiece is selected as 10X；Then the three-dimensional automatic controls of the XYZ of adjustment Raman spectrometer
Platform processed so that the image under microscope is clear, and the needle point of atomic force microscope is in the center of field range；
Set the afm scan pattern of atomic force microscope and Raman spectrometer combined system as tapping-mode,
Scanning range is X to being all 1 μm, sweep speed 1Hz with Y-direction；
Nanoscale soot particulate samples are scanned with Raman spectrometer combined system with atomic force microscope, are obtained simultaneously
Obtain three-dimensional appearance, force curve and the Raman spectrogram of the nanoscale soot particulate samples；
Step 4: the Raman spectrogram for the nanoscale soot particulate samples that step 3 obtains is divided with origin softwares
Peak is fitted, and is fitted to D1Peak, D3Peak, D4Peak and the peaks G, use D1Peak area ratio, that is, the A at peak and the peaks GD1/AGTo evaluate nanoscale soot
The degree of graphitization of particulate samples；
Step 5: obtaining the mechanical characteristic of above-mentioned nanoscale soot particulate samples, the mechanical characteristic includes adsorption capacity, model
De Huali and adhesion strength, including
5-1) seek adsorption capacity, Van der Waals force and the adhesion strength of a soot particle in nanoscale soot particulate samples：
Atomic force microscope probe is navigated to a soot particle of nanoscale soot particulate samples three-dimensional appearance, is utilized
Adsorption capacity F during Hooke's law calculating inserting needle between probe tip and the soot particleat：
Fat=kc×DJTC (1)
In formula (1), kcFor the coefficient of elasticity of atomic force microscope cantilever, DJTCIt is prominent for probe tip and the soot particle
The amount of deflection of atomic force microscope cantilever when so contacting；
Under atomic force microscope, the probe tip and the soot particle are two small balls, calculate the probe needle
Potential energy E between the sharp and described soot particle,
In formula (2), A is Hamann gram constant, R1And R2The volume of respectively probe tip radius of curvature and the soot particle is worked as
Measure radius, wherein R1For 10nm, dsFor the minimum range between probe tip and the soot particle, since soot particle is mainly
It is made of graphite flake layer, therefore, dsValue is chosen for 0.3354nm；Atomic force microscope probe needle point selects single crystal silicon material, A values
It is chosen for 2.5 × 10-19J；
To can be obtained the Van der Waals force F between probe tip and the soot particle after above-mentioned potential energy E progress derivationsvdw：
Adhesion strength F during the calculating withdraw of the needle between probe tip and the soot particlead：
Fad=kc×DJOC (4)
In formula (4), DJOCThe amount of deflection of atomic force microscope cantilever when being detached suddenly with the soot particle for probe tip；
5-2) repeat the above steps 5-1), the suction of 60~80% soot particles in nanoscale soot particulate samples is acquired respectively
Attached power, Van der Waals force and adhesion strength；
It is lifted the probe of atomic force microscope in atomic force microscope and Raman spectrometer combined system, and removes nanoscale
Soot particle sample；
Using the average value of the adsorption capacity of above-mentioned soot particle, Van der Waals force and adhesion strength as nanoscale soot particle
Adsorption capacity, Van der Waals force and the adhesion strength of sample；Another mica sheet with nanoscale soot particulate samples is fixed on original
Sub- force microscope returns to 3-2 on the example platform of Raman spectrometer combined system) sequence executes, until completing all nanometers
The detection of grade soot particle sample.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) with Flied emission transmission electron microscope and scanning electron microscope in the critical operations item such as ultravacuum and superhigh temperature
It is compared under part, the working environment of the system is relatively easy；Compared with Flied emission transmission electron microscope, it can be ensured that sample it is true
Reality, damage is small caused by sample.
(2) the accurate measurement at same time, same position to sample may be implemented in detection method, it is ensured that
The consistency of data, and the detection of soot particle grain size limit has been extended to 1nm.
(3) detection method of characteristic is managed nanoscale soot particulate matter using the present invention can obtain soot in cylinder of diesel engine
For particle there are three types of the force curve of different characteristics, it is micro- that the force curves of three kinds of different characteristics corresponds respectively to carbonization soot in cylinder of diesel engine
Unburned liquid fuel in grain, come into being in cylinder of diesel engine soot particle and cylinder of diesel engine.Similarly, carbon in Methane Diffusion Flame is also obtained
There are two types of the force curve of different characteristics, the force curves of two kinds of different characteristics to correspond to carbonized carbonaceous in Methane Diffusion Flame respectively for cigarette particle
Nascent soot particle in cigarette particle and Methane Diffusion Flame.Using obtained force curve to being generated under different working conditions
The type of soot particle is judged, obtains its development law, which contributes to the deep generation for understanding soot particle
And evolution mechanism, to provide theoretical direction to reduce the discharge of soot particle and the prevention of air environmental pollution.
Description of the drawings
Fig. 1 is the swarming fitted figure of Raman spectrum；
Fig. 2-1 to Fig. 2-5 is the three-dimensional appearance figure of the soot particle in cylinder under different crankshaft of diesel engine corners of embodiment 1；
Fig. 3 is the degree of graphitization of the soot particle in cylinder under different crankshaft of diesel engine corners of embodiment 1；
Fig. 4 is the adsorption capacity and Van der Waals force of the soot particle in cylinder under different crankshaft of diesel engine corners of embodiment 1；
Fig. 5 is the adhesion strength of the soot particle in cylinder under different crankshaft of diesel engine corners of embodiment 1；
Fig. 6-1 to Fig. 6-3 is the three typical force curves obtained in embodiment 1；
Fig. 7-1 to Fig. 7-5 is the three-dimensional appearance figure of the soot particle at different diffusion flame height of embodiment 2；
Fig. 8 is the degree of graphitization of the soot particle at different diffusion flame height of embodiment 2；
Fig. 9 is the adsorption capacity and Van der Waals force of the soot particle at different diffusion flame height of embodiment 2；
Figure 10 is the adhesion strength of the soot particle at different diffusion flame height of embodiment 2；
Figure 11-1 and Figure 11-2 is the two typical force curves obtained in embodiment 2.
Specific implementation mode
Technical solution of the present invention is described in further detail in the following with reference to the drawings and specific embodiments, it is described specific
Embodiment is only explained the present invention, is not intended to limit the invention.
Embodiment 1
A kind of detection method for managing nanoscale soot particulate matter characteristic, is joined using atomic force microscope and Raman spectrometer
Detect three-dimensional appearance, mechanical characteristic and the degree of graphitization at the same position of nanoscale soot particle simultaneously with system,
Include the following steps：
First, it is five diesel oil of state to select model 6102BZLQ, rotating speed 1000rpm, injection pressure 100MPa, fuel
Diesel engine, therewith respectively by crankshaft of diesel engine corner be -0.5 °, 2.5 °, 7 °, 18 °, 24.5 ° under the conditions of cylinder in soot it is micro-
Grain collects on mica sheet, and the mica sheet being collected is placed on after being labeled in culture dish, is waited to be analyzed；
Secondly, by the laser of atomic force microscope and Raman spectrometer combined system, monitor, white light source, calculating
Machine, display and controller power source are opened；
The three-dimensional appearance and Raman spectrogram of nanoscale soot particulate samples are obtained, including：
The mica sheet of the soot particle sample obtained in cylinder under -0.5 ° of crankshaft of diesel engine corner is fixed on atomic force to show
On the example platform of micro mirror and Raman spectrometer combined system；
The laser beam position for adjusting atomic force microscope in atomic force microscope and Raman spectrometer combined system, is allowed to vertical
The straight probe front for being radiated at overarm；Adjustment reflection laser is allowed to vertical irradiation on the center of PSPD；Then light is adjusted
Learn focus and focal length so that probe is close to clear sample；
The lasing light emitter of Raman spectrometer selects He-Ne, the laser in atomic force microscope and Raman spectrometer combined system
The launch wavelength in source is 532nm, object lens are selected as 50X, eyepiece is selected as 10X；Then the three-dimensional automatic controls of the XYZ of adjustment Raman spectrometer
Platform processed so that the image under microscope is clear, and the needle point of atomic force microscope is in the center of field range；
Set the afm scan pattern of atomic force microscope and Raman spectrometer combined system as tapping-mode,
Scanning range is X to being all 1 μm, sweep speed 1Hz with Y-direction；
Nanoscale soot particulate samples are scanned with Raman spectrometer combined system with atomic force microscope, are obtained simultaneously
Obtain three-dimensional appearance, force curve and the Raman spectrogram of the nanoscale soot particulate samples；
The Raman spectrogram of the nanoscale soot particulate samples obtained in the above method is subjected to swarming with origin softwares
Fitting, is fitted to D1Peak, D3Peak, D4Peak and the peaks G, are fitted to that the results are shown in Figure 1, use D1The peak area ratio at peak and the peaks G is
AD1/AGTo evaluate the degree of graphitization of nanoscale soot particulate samples；
Finally, the mechanical characteristic of above-mentioned nanoscale soot particulate samples is obtained, the mechanical characteristic includes adsorption capacity, Fan De
Hua Li and adhesion strength：
Seek adsorption capacity, Van der Waals force and the adhesion strength of a soot particle in nanoscale soot particulate samples：
The soot particle that atomic force microscope probe is navigated to nanoscale soot particulate samples three-dimensional appearance, when right
During this soot particle inserting needle, there is a discontinuous jump, in unexpected contact process, probe tip and sample in needle point
Active force between product is known as adsorption capacity Fat, which is calculated by Hooke's law：
Fat=kc×DJTC(1)
In formula (1), kcFor the coefficient of elasticity of atomic force microscope cantilever, DJTCIt is prominent for probe tip and the soot particle
The amount of deflection of atomic force microscope cantilever when so contacting；
Under atomic force microscope, the probe tip and the soot particle are two small balls, calculate the probe needle
Potential energy E between the sharp and described soot particle,
In formula (2), A is Hamann gram constant, R1And R2The volume of respectively probe tip radius of curvature and the soot particle is worked as
Measure radius, wherein R1For 10nm, dsFor the minimum range between probe tip and the soot particle, since soot particle is mainly
It is made of graphite flake layer, therefore, dsValue is chosen for 0.3354nm；Atomic force microscope probe needle point selects single crystal silicon material, A values
It is chosen for 2.5 × 10-19J；
To can be obtained the Van der Waals force F between probe tip and the soot particle after above-mentioned potential energy E progress derivationsvdw：
During the soot particle withdraw of the needle, after the attraction between needle point and particle reaches maximum value, if continuing the withdraw of the needle,
Needle point will occur to detach suddenly with soot particle.Maximum force between needle point and soot particle is adhesion strength Fad, should
Power is acquired by following formula：
Fad=kc×DJOC (4)
In formula (4), DJOCThe amount of deflection of atomic force microscope cantilever when being detached suddenly with the soot particle for probe tip；
The above method is repeated, acquires adsorption capacity, the model of 60~80% soot particles in nanoscale soot particulate samples respectively
De Huali and adhesion strength；
It is lifted the probe of atomic force microscope in atomic force microscope and Raman spectrometer combined system, and removes nanoscale
Soot particle sample；
Using the average value of the adsorption capacity of above-mentioned soot particle, Van der Waals force and adhesion strength as nanoscale soot particle
Adsorption capacity, Van der Waals force and the adhesion strength of sample；
Then crankshaft of diesel engine corner is obtained respectively under the conditions of 2.5 °, 7 °, 18 ° and 24.5 ° and carries soot particle
Mica sheet be fixed on the example platform of atomic force microscope and Raman spectrometer combined system, execute according to the method described above,
Until completing the detection of all nanoscale soot particulate samples.Obtain under diesel engine difference crank angle three of soot particle in cylinder
Tie up pattern, degree of graphitization and mechanical characteristic.Three-dimensional appearance, degree of graphitization and the mechanical characteristic of the soot particle adsorb
Power, Van der Waals force and adhesion strength are respectively as shown in Fig. 2-1 to Fig. 2-5, Fig. 3, Fig. 4 and Fig. 5.Soot in cylinder of diesel engine simultaneously
Carbonization soot particle in the force curve i.e. cylinder of diesel engine of three strips is obtained in the experiment of particle, soot of coming into being in cylinder of diesel engine
Unburned liquid fuel is respectively as shown in Fig. 6-1,6-2 and 6-3 in particle and cylinder of diesel engine.
Embodiment 2
Almost the same with the process of embodiment 1, difference, which is only the acquisition of soot particle sample, is：Laboratory diffusion flame combustion
Fuel is selected as methane in burner, is respectively 30mm, 34mm, 38mm by flame height, the soot particle at 50mm, 60mm collects
On mica sheet, the mica sheet that is collected is placed on after being labeled in culture dish；It is respectively 30mm by diffusion flame height,
The mica sheet with soot particle is obtained at 34mm, 38mm, 50mm, 60mm is fixed on atomic force microscope and Raman spectrometer connection
It on the example platform of system, is subsequently operated according to the method for embodiment 1, until completing all nanoscale soot particulate samples
Detection.It is special to obtain the three-dimensional appearance of soot particle, degree of graphitization and mechanics at the diffusion flame difference flame height of laboratory
Property.The three-dimensional appearance of the soot particle, degree of graphitization and mechanical characteristic, that is, adsorption capacity, Van der Waals force and adhesion strength are respectively as schemed
Shown in 7-1 to Fig. 7-5, Fig. 8, Fig. 9 and Figure 10.It is obtained in the soot particle experiment that laboratory diffusion flame is obtained simultaneously
Two typical force curves correspond respectively to the soot of coming into being that is carbonized in soot particle and Methane Diffusion Flame in Methane Diffusion Flame
Particle, as shown in Figure 11-1 and 11-2.
Be carbonized soot particle, come into being in cylinder of diesel engine soot particle and bavin in the cylinder of diesel engine as shown in Fig. 6-1,6-2 and 6-3
In oil machine cylinder in Methane Diffusion Flame shown in the force curve of unburned liquid fuel and Figure 11-1 and Figure 11-2 carbonization soot particle and
It comes into being in Methane Diffusion Flame the force curve of soot particle, using obtained force curve to being generated under different working conditions
The type of soot particle is judged, it can be deduced that its development law, the result of study help deep to understand soot particle
Generation and evolution mechanism, to provide theoretical direction to reduce the discharge of soot particle and the prevention of air environmental pollution.
To sum up, the present invention proposes a kind of detection method for managing nanoscale soot particulate matter characteristic, to separate sources
The development law of the three-dimensional appearance of the soot particle generated in combustion process, mechanical characteristic and degree of graphitization is ground
Study carefully, which contributes to the deep generation for understanding soot particle and evolution mechanism, to the discharge for reduction soot particle
And the prevention of air environmental pollution provides theoretical direction.
Claims (3)
1. a kind of detection method for managing nanoscale soot particulate matter characteristic, which is characterized in that utilize atomic force microscope and drawing
Graceful spectrometer combined system detects three-dimensional appearance, mechanical characteristic and the stone at the same position of nanoscale soot particle simultaneously
Blackization degree, includes the following steps：
Step 1: the nanoscale soot particle obtained under different operating modes is collected respectively on one group of mica sheet, every is carried
The mica sheet of nanoscale soot particulate samples is individually positioned in after being labeled in a culture dish, is waited to be analyzed；
Step 2: by the laser of atomic force microscope and Raman spectrometer combined system, monitor, white light source, computer,
Display and controller power source are opened；
Step 3: the three-dimensional appearance and Raman spectrogram of nanoscale soot particulate samples are obtained, including：
The wherein a piece of mica sheet with nanoscale soot particulate samples 3-1) is fixed on atomic force microscope and Raman spectrum
On the example platform of instrument combined system；
The laser beam position for 3-2) adjusting atomic force microscope in atomic force microscope and Raman spectrometer combined system, is allowed to vertical
The straight probe front for being radiated at overarm；Adjustment reflection laser is allowed to position sensing photoelectricity of the vertical irradiation in atomic force microscope
On the center of detector；Then optical focus and focal length are adjusted so that probe is close to clear sample；
The lasing light emitter of Raman spectrometer selects He-Ne in atomic force microscope and Raman spectrometer combined system, the lasing light emitter
Launch wavelength is 532nm, object lens are selected as 50X, eyepiece is selected as 10X；Then the XYZ three-dimensionals of adjustment Raman spectrometer automatically control flat
Platform so that the image under microscope is clear, and the needle point of atomic force microscope is in the center of field range；
The afm scan pattern of atomic force microscope and Raman spectrometer combined system is set as tapping-mode, scanning
Ranging from X is to being all 1 μm, sweep speed 1Hz with Y-direction；
Nanoscale soot particulate samples are scanned with Raman spectrometer combined system with atomic force microscope, while being somebody's turn to do
Three-dimensional appearance, force curve and the Raman spectrogram of nanoscale soot particulate samples；
Intend Step 4: the Raman spectrogram for the nanoscale soot particulate samples that step 3 obtains is carried out swarming with origin softwares
It closes, is fitted to D1Peak, D3Peak, D4Peak and the peaks G, use D1Peak area ratio, that is, the A at peak and the peaks GD1/AGTo evaluate nanoscale soot particle
The degree of graphitization of sample；
Step 5: obtaining the mechanical characteristic of above-mentioned nanoscale soot particulate samples, the mechanical characteristic includes adsorption capacity, Van der Waals
Power and adhesion strength, including
5-1) seek adsorption capacity, Van der Waals force and the adhesion strength of a soot particle in nanoscale soot particulate samples：
The soot particle that atomic force microscope probe is navigated to nanoscale soot particulate samples three-dimensional appearance, utilizes Hooke
Adsorption capacity F during law calculating inserting needle between probe tip and the soot particleat：
Fat=kc×DJTC (1)
In formula (1), kcFor the coefficient of elasticity of atomic force microscope cantilever, DJTCIt is contacted suddenly with the soot particle for probe tip
When atomic force microscope cantilever amount of deflection；
Under atomic force microscope, the probe tip and the soot particle are two small balls, calculate the probe tip and
Potential energy E between the soot particle,
In formula (2), A is Hamann gram constant, R1And R2The respectively volume of probe tip radius of curvature and the soot particle half
Diameter, wherein R1For 10nm, dsFor the minimum range between probe tip and the soot particle, since soot particle is mainly by stone
Ink sheet layer forms, therefore, dsValue is chosen for 0.3354nm；Atomic force microscope probe needle point selects single crystal silicon material, A values to choose
It is 2.5 × 10-19J；
To can be obtained the Van der Waals force F between probe tip and the soot particle after above-mentioned potential energy E progress derivationsvdw：
Adhesion strength F during the calculating withdraw of the needle between probe tip and the soot particlead：
Fad=kc×DJOC (4)
In formula (4), DJOCThe amount of deflection of atomic force microscope cantilever when being detached suddenly with the soot particle for probe tip；
5-2) repeat the above steps 5-1), the absorption of 60~80% soot particles in nanoscale soot particulate samples is acquired respectively
Power, Van der Waals force and adhesion strength；
It is lifted the probe of atomic force microscope in atomic force microscope and Raman spectrometer combined system, and removes nanoscale soot
Particulate samples；
Using the average value of the adsorption capacity of above-mentioned soot particle, Van der Waals force and adhesion strength as nanoscale soot particulate samples
Adsorption capacity, Van der Waals force and adhesion strength；
Another mica sheet with nanoscale soot particulate samples is fixed on atomic force microscope to be combined with Raman spectrometer
On the example platform of system, 3-2 is returned) sequence executes, until completing the detection of all nanoscale soot particulate samples.
2. a kind of application of nanoscale soot particulate matter reason characteristic detecting method, which is characterized in that using as described in claim 1
The detection method for managing nanoscale soot particulate matter characteristic obtains the power song of different characteristics there are three types of soot particles in cylinder of diesel engine
Line, it is micro- that the force curves of three kinds of different characteristics corresponds respectively to carbonization soot particle in cylinder of diesel engine, soot of coming into being in cylinder of diesel engine
Unburned liquid fuel in grain and cylinder of diesel engine.
3. a kind of application of nanoscale soot particulate matter reason characteristic detecting method, which is characterized in that using as described in claim 1
Obtaining soot particle in Methane Diffusion Flame to the detection method of nanoscale soot particulate matter reason characteristic, there are two types of different characteristics
Force curve, the force curve of two kinds of different characteristics, which is corresponded to respectively in Methane Diffusion Flame, to be carbonized in soot particle and Methane Diffusion Flame
Nascent soot particle.
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| CN103743620A (en) * | 2013-12-27 | 2014-04-23 | 天津大学 | Method for carrying out non-contact measurement on plane transformation by using low-dimensional nano material |
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