CN104385586A - Method for obtaining carbon black microscopic morphology enlarging entity through 3D printing - Google Patents

Method for obtaining carbon black microscopic morphology enlarging entity through 3D printing Download PDF

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Publication number
CN104385586A
CN104385586A CN201410489001.7A CN201410489001A CN104385586A CN 104385586 A CN104385586 A CN 104385586A CN 201410489001 A CN201410489001 A CN 201410489001A CN 104385586 A CN104385586 A CN 104385586A
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carbon black
microscopic appearance
printed
amplifying entity
entity
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CN201410489001.7A
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CN104385586B (en
Inventor
陈建
吴召洪
朱晓飞
罗少伶
蒋文平
朱林英
龚勇
胥会
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Sichuan University of Science and Engineering
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Sichuan University of Science and Engineering
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Abstract

The present invention discloses a method for obtaining the carbon black microscopic morphology enlarging entity through 3D printing. According to the method, based on the inorganic material microscopic carbon black primary particles or aggregates, the carbon black microscopic morphology is printed out through a 3D printer so as to establish the association between the carbon black microscopic morphology and the carbon black macroscopic morphology, ie., the macroscopy and the substantiation of the microscopy are achieved through the 3D printing technology; and the carbon black microscopic morphology picture is made out relying on the accurate data points, wherein the real data is adopted as the support, such that the obtained entity has the accurate structure. According to the present invention, the carbon black microscopic morphology is subjected to macroscopy so as to substantially promote scientific research workers to research on the carbon black structure, the particle size and the morphology, and further provide the first-hand data for the research on the carbon black aggregate reinforced rubber, and the development of the technology provides the guidance significance for the actual production.

Description

A kind of method being printed acquisition carbon black microscopic appearance amplifying entity by 3D
Technical field
The present invention relates to carbon black microscopic appearance and be converted into macroscopical entity technology, belong to research nanometer new material microscopic appearance technology.
Technical background
Carbon black microscopic appearance generally obtains with scanning probe microscopy or transmission electron microscope, a just shape appearance figure, also cannot be converted into accurate pattern entity at present, the carbon black model that market occurs only draws according to microscopic appearance figure or guess, and this can not be avoided artificial subjective factor.
At present, 3D printing technique is in the ascendant, increasingly extensive in the application of field of material preparation.The paper The 3D printing of gelatin methacrylamide cell-laden tissue-engineered constructs with high cell viability that the people such as Billiet T deliver on Biomaterials periodical take acrylamide gel as raw material, has printed mechanics of biological tissue.This structure can load cell, and this institutional framework that the survival rate 97%, 3D of its cell prints and cell have good compatibility.The paper 3D printing of cell-laden constructs for heterogeneous tissue regeneration that the people such as Pati F deliver on Manufacturing Letters periodical have employed similar method 3D and has printed regeneration isomery tissue, and the survival rate of its cell is also very high.But current this technology is all the structural objects for printing macroscopic view, and also nobody proposes the structure being printed microcosmic (nanoscale) by the method for macroscopic view, does not more use it for the report printing carbon black aggregate, primary particle.
Summary of the invention
For the problems referred to above, the invention provides a kind of method being printed acquisition carbon black microscopic appearance amplifying entity by 3D.For inorganic material microcosmic carbon black primary particle or aggregation, printed the microscopic appearance of carbon black by 3D printer, establish the contact of carbon black pattern micro-mobility protocols, namely achieved by 3D printing technique and microcosmic is carried out macroscopic view, hypostazation.
The present invention is achieved through the following technical solutions:
Printed the method obtaining carbon black microscopic appearance amplifying entity by 3D, comprise the following steps:
1) the microscopic appearance figure of carbon black is obtained;
2) described microscopic appearance figure is converted to the data file representing each point coordinate value in described microscopic appearance figure;
3) by step 2) in the data file transition of gained become the discernible form of mapping software;
4) by step 3) in the data importing mapping software of gained draw out each independently point, then hypostazation is carried out to these points, obtains the 3D solid picture amplified;
5) 3dmax software is adopted to convert the 3D solid picture of gained in step 4 to 3D printer discernible form;
6) amplifying entity that 3D printer prints performance carbon black microscopic appearance structure is opened.
This method achieves carbon black microscopic appearance amplifying entity by 3D printing technique, and rely on accurate data point to make carbon black microscopic appearance figure, have True Data as support, gained amplifying entity structure is accurate.
Alternately, in the above-mentioned methods, the microscopic appearance figure in described step 1) adopts scanning probe microscopy or transmission electron microscope to obtain.
Alternately, in the above-mentioned methods, by ultrasonic carbon black dispersion in absolute ethyl alcohol, ultrasonic 20min; Then ultrasonic good carbon black ethanol solution is dropped on clean mica sheet, dry up, mica sheet is put into scanning probe microscopy sample room, scans, obtain carbon black microscopic appearance figure.Wherein the mixing ratio of carbon black and absolute ethyl alcohol is preferably carbon black 0.1mg, absolute ethyl alcohol 200ml.
Alternately, in the above-mentioned methods, described step 2) obtain the software that carries of instrument by microscopic appearance used in step 1) and complete, such as carry software by scanning probe microscopy and be converted into Excel data, the number of data point can be chosen according to the requirement of image resolution ratio flexibly (when data provide more, image resolution ratio is higher), optional data point number comprises: 64 × 64,128 × 128,256 × 256,512 × 512,1024 × 1024 etc.Preferably 256 × 256 points.
Alternately, in the above-mentioned methods, described step 3) and 4) described in mapping software be AutoCAD.
Alternately, in the above-mentioned methods, described step 3) to be specially each coordinate value of each point between space change comma into.Concrete conversion regime can adopt MATLAB software, carries out according to following program:
clear
clc;
mm=xlsread('dat.xlsx');
mn=size(mm);
k=1;
for i=1:1:mn(1)
for j=1:1:mn(2)
xx(k,:)=[mm(1,j),mm(i,1),mm(i,j)];
k=k+1;
end
end
xlswrite('sj.xlsx',xx)
Import database, obtain x 1y 1z 1
  x 2 y 2z 2
  ……………
Coordinate group, will save File As txt form, utilize replacement function, replace " ", obtain with ", ":
x 1,y 1,z 1
x 2,y 2,z 2
……………
Coordinate system.
Alternately, in the above-mentioned methods, the hypostazation described in step 4) is specially: select the three dimensional poly-lines paint program in AutoCAD each point to be coupled together formation closed curve, and adjust multiplication factor by the distance value arranging point-to-point transmission.Because the data importing CAD of carbon black shape appearance figure is not through hypostazation, so 3D printer is None-identified, if successively by each data (256 × 256 points) hypostazation, also be unpractical, this is a difficult point, by " the three dimensional poly-lines paint program " of CAD, carbon black pattern is converted into entity.
Alternately, in the above-mentioned methods, described 3D prints and carries out at normal temperatures, and material therefor is photosensitive resin.Under adopting normal temperature, photosensitive resin prints, and energy-conservation and controllability increases, and is microcosmic carbon black macroscopic viewization also printed accurately, reflects the morphology of carbon black truly.
Alternately, in the above-mentioned methods, by ultrasonic carbon black dispersion, be the rank that carbon black pellet reaches primary particle, aggregation, adopt scanning probe microscopy to scan carbon black pattern, obtain carbon black shape appearance figure.Carry software with scan-probe AFM again shape appearance figure is derived, data are .exl form.By MATLAB software to .exl data processing, change into specific form.Then data importing CAD, drawing carbon black pattern, then be converted into entity, is the discernible .stl form of 3D printer by 3dmax data transformations.Finally, the amplifying entity of carbon black microscopic appearance is printed.
Present invention also offers a kind of macroscopical amplifying entity model of carbon black microscopic appearance, this model can adopt in said method any one obtain.
Present invention also offers a kind of application of macroscopical amplifying entity model of upper carbon black microscopic appearance, it is characterized in that, use it for teaching mode.
Present invention also offers a kind of application of macroscopical amplifying entity model of upper carbon black microscopic appearance, it is characterized in that, use it for the wind tunnel test about carbon black, explore the relation of microcosmic carbon black and macromolecular chain, simulation carbon black reinforced rubber mechanism.
All features disclosed in this description, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Beneficial effect of the present invention:
1, the present invention is directed to inorganic material microcosmic carbon black primary particle or aggregation, printed the microscopic appearance of carbon black by 3D printer, establish the contact of carbon black pattern micro-mobility protocols, namely achieved by 3D printing technique and microcosmic is carried out macroscopic view, hypostazation.And rely on accurate data point to make carbon black microscopic appearance figure, have True Data as support, gained amplifying entity structure is accurate.
2, carbon black microcosmic carry out macroscopicalization by the present invention, facilitate the research of researcher to carbon black structure, particle diameter, pattern greatly, also will provide first-hand data for research carbon black aggregate reinforced rubber, and also to actual production, there is directive significance to the exploitation of this technology.Such as can be used for doing the wind tunnel test about carbon black, explore the relation of microcosmic carbon black and macromolecular chain, simulation carbon black reinforced rubber mechanism.
Accompanying drawing explanation
Fig. 1 is the flow chart of method described in embodiment 1.
detailed description of the invention:
Detailed description of the invention is by the following examples described in further detail foregoing of the present invention again.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following example.Not departing from any amendment made within the spirit and principles in the present invention, and the equivalent replacement made according to ordinary skill knowledge and customary means or improvement, all should be included in protection scope of the present invention.
Embodiment 1:
This test first by ultrasonic carbon black dispersion, be the rank that carbon black pellet reaches primary particle, aggregation, adopt Hitachi, Ltd E-sweep scan-probe to scan carbon black pattern, obtain carbon black shape appearance figure.Carry software with scan-probe AFM again shape appearance figure is derived, data are .exl form.By MATLAB software to .exl data processing, change into specific form.Then data importing CAD, drawing carbon black pattern, then be converted into entity (.dwg file), is the discernible .stl form of 3D printer by 3dmax data transformations.Finally, the amplifying entity of carbon black microscopic appearance is printed.Idiographic flow as shown in Figure 1.
Alternately, in the above-mentioned methods, described 3D prints and carries out at normal temperatures, and material therefor is photosensitive resin.Under adopting normal temperature, photosensitive resin prints, and energy-conservation and controllability increases, and is microcosmic carbon black macroscopic viewization also printed accurately, reflects the morphology of carbon black truly.
Embodiment 2:
The microscopic appearance amplifying entity of carbon black is prepared according to following steps:
1) by ultrasonic carbon black dispersion in absolute ethyl alcohol (carbon black 0.1mg, absolute ethyl alcohol 200ml), ultrasonic 20min;
2) ultrasonic good carbon black ethanol solution is dropped on clean mica sheet, dry up.Mica sheet is put into scanning probe microscopy sample room, scans, obtain carbon black microscopic appearance figure (nanoscale);
3) carbon black microscopic appearance .xqd is converted into .xqt, then derives .exl data (256 × 256 points);
4) utilize MATLAB software, develop a program and .exl data are processed:
clear
clc;
mm=xlsread('dat.xlsx');
mn=size(mm);
k=1;
for i=1:1:mn(1)
for j=1:1:mn(2)
xx(k,:)=[mm(1,j),mm(i,1),mm(i,j)];
k=k+1;
end
end
xlswrite('sj.xlsx',xx)
Import database, obtain
x 1 y 1 z 1
 x 2 y 2 z 2
   ……………
Coordinate group, will save File As txt form, utilize replacement function, replace space, obtain with ", ":
x 1,y 1,z 1
x 2,y 2,z 2
……………
Coordinate system;
5) open AutoCAD, select three dimensional poly-lines paint program, by 3) data importing that step obtains, after AutoCAD has drawn, export " C " order, made it form closed curve, then exported " W " and order, select image to change into " block ";
6) the .dwg file that AutoCAD preserves is imported 3dmax, be converted into the discernible .stl form of 3D printer, print carbon black microscopic appearance structural solid;
7) open computer, be connected to 3D printer.Close the computer security software program such as computer fire wall and computer house keeper;
8) in the network Internet connectivity option of control panel, arrange computer static ip address: 169.254.1.3, arranging sub-mask is 255.255.0.0;
9) open 3D printer, after start, 3D printer system meeting self-inspection, opens IE8(or more version) browser, input IP address: 169.254.1.1, enters 3D printer web page control inerface;
10) click login, input account number cipher, now 3D printer can carry out preparation, (as needs more conversion materials, then need to click YES, more conversion materials) after hit OK and NO successively, webpage can show " printer is ready " printed words, now printer is ready to complete;
11) select new in print, newly-built print out task, select creat, now can eject the model cootrol window that 3D prints.Select " load CAD file ", the file of the .STL form of conversion is chosen, then select " Auto part placement " automatic centering, control Scalable by " Scale " and control direction of rotation with " Rotate ", be adjusted to required template model;
12) after moulded dimension is determined, " Generate and Preview Supports " is selected to generate and preview support, then clicking " Submit " button submits to task to arrive printing list, or from File drop-down menu, click " Submit job ", now can get back to webpage control inerface;
13) click " click here to start ", after selecting YES and NO respectively, click statr print, start print job;
14), after machine to be printed has printed, butyronitrile gloves and UV resistance special eyeglasses must be worn, then open printer, take out and print achievement, take off the model of printing with scoop and pocket knife, then put into alcohol, soak half an hour to take out, namely print carbon black appearance structure.
Alternately, in the above-mentioned methods, described 3D prints and carries out at normal temperatures, and material therefor is photosensitive resin.Under adopting normal temperature, photosensitive resin prints, and energy-conservation and controllability increases, and is microcosmic carbon black macroscopic viewization also printed accurately, reflects the morphology of carbon black truly.
Application examples
The macromodel of the carbon black appearance structure of gained in embodiment 2 is used for classroom instruction, carbon black appearance structure is understood to student there is great help.Be applied in research work and also can facilitate the research of researcher to carbon black structure, particle diameter, pattern greatly.In addition, this model is used as the wind tunnel test about carbon black, also contributes to the relation exploring microcosmic carbon black and macromolecular chain, simulation carbon black reinforced rubber mechanism.
The foregoing is only the preferred embodiments of the present invention, is only illustrative for the purpose of the present invention, and nonrestrictive; Those of ordinary skill in the art understand, and can carry out many changes in the spirit and scope that the present invention limits to it, amendment, and even equivalence is changed, but all will fall into protection scope of the present invention.
  

Claims (10)

1. printed the method obtaining carbon black microscopic appearance amplifying entity by 3D, it is characterized in that, comprise the following steps:
1) the microscopic appearance figure of carbon black is obtained;
2) described microscopic appearance figure is converted to the data file representing each point coordinate value in described microscopic appearance figure;
3) by step 2) in the data file transition of gained become the discernible form of mapping software;
4) by step 3) in the data importing mapping software of gained draw out each independently point, then hypostazation is carried out to these points, obtains the 3D solid picture amplified;
5) 3dmax software is adopted to convert the 3D solid picture of gained in step 4 to 3D printer discernible form;
6) amplifying entity that 3D printer prints performance carbon black microscopic appearance structure is opened.
2. the method being printed acquisition carbon black microscopic appearance amplifying entity by 3D according to claim 1, it is characterized in that, the microscopic appearance figure in described step 1) adopts scanning probe microscopy or transmission electron microscope to obtain.
3. the method being printed acquisition carbon black microscopic appearance amplifying entity by 3D according to claim 1, it is characterized in that, microscopic appearance figure in described step 1) adopts scanning probe microscopy to obtain, and its concrete grammar is: by ultrasonic carbon black dispersion in absolute ethyl alcohol, ultrasonic 20min; Then ultrasonic good carbon black ethanol solution is dropped on clean mica sheet, dry up, mica sheet is put into scanning probe microscopy sample room, scans, obtain carbon black microscopic appearance figure.
4. according to claim 1ly printed the method obtaining carbon black microscopic appearance amplifying entity by 3D, it is characterized in that, described step 2) obtain by microscopic appearance used in step 1) the software that instrument carries and complete.
5. according to claim 1ly printed the method obtaining carbon black microscopic appearance amplifying entity by 3D, it is characterized in that, described step 3) and 4) described in mapping software be AutoCAD.
6. according to claim 5ly printed the method obtaining carbon black microscopic appearance amplifying entity by 3D, it is characterized in that, the space between described step 3) is specially each coordinate value of each point changes comma into.
7. the method being printed acquisition carbon black microscopic appearance amplifying entity by 3D according to claim 5, it is characterized in that, hypostazation described in step 4) is specially: select the three dimensional poly-lines paint program in AutoCAD each point to be coupled together formation closed curve, and adjust multiplication factor by the distance value arranging point-to-point transmission.
8. a macroscopical amplifying entity model for carbon black microscopic appearance, is characterized in that, adopts as the method in claim 1 ~ 7 as described in any one obtains.
9. the application of macroscopical amplifying entity model of carbon black microscopic appearance according to claim 8, is characterized in that, use it for teaching mode.
10. the application of macroscopical amplifying entity model of carbon black microscopic appearance according to claim 8, is characterized in that, use it for the wind tunnel test about carbon black, explores the relation of microcosmic carbon black and macromolecular chain, simulation carbon black reinforced rubber mechanism.
CN201410489001.7A 2014-09-23 2014-09-23 A kind of method printing acquisition white carbon black microscopic appearance amplifying entity by 3D Active CN104385586B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107505480A (en) * 2017-08-16 2017-12-22 四川理工学院 A kind of method for detecting filler dispersiveness in rubber composite material
CN109087288A (en) * 2018-07-20 2018-12-25 四川理工学院 A kind of measurement method that carbon black is dispersed in rubber
CN109614695A (en) * 2018-12-10 2019-04-12 可脉检测(南京)有限公司 A kind of method and its application for analyzing fracture micromorphology by 3D printing technique
CN115142103A (en) * 2022-07-01 2022-10-04 南通大学 Micro-nano scale rapid reading and writing system and method based on glass microprobe
WO2023049395A1 (en) * 2021-09-23 2023-03-30 Birla Carbon U.S.A., Inc. Systems, devices, and methods for three-dimensional analysis of carbon black

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CN102426711A (en) * 2011-09-08 2012-04-25 上海大学 Three-dimensional porous bone scaffold discrete model construction method capable of controlling discrete interval
CN103284815A (en) * 2013-05-17 2013-09-11 中山大学 3D-printing fast forming method of nano composite degradable bone repair material

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WO2003016030A1 (en) * 2001-05-24 2003-02-27 Vantico Gmbh Three-dimensional structured printing
CN101301107A (en) * 2007-05-10 2008-11-12 赖维祥 Method for producing three-dimensional contouring food product with rapid prototyping technology
CN102254354A (en) * 2011-06-27 2011-11-23 中国科学院武汉岩土力学研究所 Method for implementing microstructure surface morphology three-dimensional visualization of soil
CN102426711A (en) * 2011-09-08 2012-04-25 上海大学 Three-dimensional porous bone scaffold discrete model construction method capable of controlling discrete interval
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107505480A (en) * 2017-08-16 2017-12-22 四川理工学院 A kind of method for detecting filler dispersiveness in rubber composite material
CN107505480B (en) * 2017-08-16 2020-05-08 四川理工学院 Method for detecting filler dispersibility in rubber composite material
CN109087288A (en) * 2018-07-20 2018-12-25 四川理工学院 A kind of measurement method that carbon black is dispersed in rubber
CN109087288B (en) * 2018-07-20 2021-11-23 四川理工学院 Method for measuring dispersibility of carbon black in rubber
CN109614695A (en) * 2018-12-10 2019-04-12 可脉检测(南京)有限公司 A kind of method and its application for analyzing fracture micromorphology by 3D printing technique
WO2023049395A1 (en) * 2021-09-23 2023-03-30 Birla Carbon U.S.A., Inc. Systems, devices, and methods for three-dimensional analysis of carbon black
CN115142103A (en) * 2022-07-01 2022-10-04 南通大学 Micro-nano scale rapid reading and writing system and method based on glass microprobe

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