CN104385586A - A method for obtaining carbon black microscopic morphology enlarged entity by 3D printing - Google Patents

Abstract

The invention discloses a method for obtaining the enlarged entity of carbon black microscopic appearance through 3D printing. The method aims at the microscopic carbon black primary particles or aggregates of inorganic materials, and prints the microscopic appearance of carbon black through a 3D printer, and establishes a carbon black The connection between the microcosm and the macrocosm of the morphology means that the microcosm is macroscopically realized and materialized through 3D printing technology. And rely on accurate data points to make carbon black microscopic topography map, with real data as support, the obtained enlarged entity structure is accurate. In the present invention, carbon black is microscopically macroscopic, which greatly promotes research workers' research on carbon black structure, particle size, and morphology, and will also provide first-hand information for the study of carbon black aggregates to reinforce rubber. The development of this technology also has guiding significance for actual production.

Description

A method for obtaining carbon black microscopic morphology enlarged entity by 3D printing

technical field

The invention relates to the technology of transforming the microscopic appearance of carbon black into a macroscopic entity, and belongs to the technology of studying the microscopic appearance of nano new materials. the

technical background

The microscopic morphology of carbon black is generally obtained by scanning probe microscope or transmission electron microscope, which is just a topographical map, which cannot be converted into an accurate physical appearance at present. The carbon black models that appear on the market are only based on microscopic topographical maps or conjectures. Drawn, which cannot avoid human subjective factors. the

At present, 3D printing technology is in the ascendant, and its application in the field of material preparation is becoming more and more extensive. The paper The 3D printing of gelatin methacrylamide cell-laden tissue-engineered constructs with high cell viability published in the Biomaterials journal by Billiet T et al. uses acrylamide gel as a raw material to print out biological tissue structures. This structure can be loaded with cells, and its cell survival rate is as high as 97%. The 3D printed tissue structure has good compatibility with cells. In the paper 3D printing of cell-laden constructs for heterogeneous tissue regeneration published in the journal Manufacturing Letters, Pati F et al. used a similar method to 3D print regenerated heterogeneous tissues, and the survival rate of the cells was also high. But at present, this technology is only used to print macroscopic structural objects. No one has proposed to print microscopic (nanoscale) structures through macroscopic methods, and there is no report of using it to print carbon black aggregates and primary particles. . the

Contents of the invention

In view of the above problems, the present invention provides a method for obtaining carbon black microscopic morphology enlarged entity by 3D printing. For the primary particles or aggregates of microscopic carbon black of inorganic materials, the microscopic morphology of carbon black is printed by 3D printers, and the connection between the microscopic and macroscopic of carbon black morphology is established, that is, the microscopic is macroscopically realized through 3D printing technology. change. the

The present invention is realized through the following technical solutions:

A kind of method that obtains carbon black microscopic appearance and enlarged entity by 3D printing, comprises the following steps:

1) Obtain the microscopic topography of carbon black;

2) converting the microscopic topography diagram into a data file representing the coordinate values of each point in the microscopic topography diagram;

3) Convert the data file obtained in step 2) into a form recognizable by the drawing software;

4) Import the data obtained in step 3) into the drawing software to draw each independent point, and then materialize these points to obtain an enlarged three-dimensional solid picture;

5) Use 3dmax software to convert the 3D solid image obtained in step 4 into a format recognizable by the 3D printer;

6) Turn on the 3D printer to print an enlarged entity showing the microscopic structure of carbon black.

This method realizes the magnification and materialization of the microscopic morphology of carbon black through 3D printing technology, and relies on accurate data points to make a microscopic morphology map of carbon black, supported by real data, and the obtained enlarged entity structure is accurate. the

As an option, in the above method, the microscopic topography in step 1) is obtained by scanning probe microscope or transmission electron microscope. the

As an alternative, in the above method, disperse the carbon black in absolute ethanol by ultrasound, ultrasonic 20min; Enter the scanning probe microscope sample chamber, scan, and obtain the microscopic topography of carbon black. Wherein the blending ratio of carbon black and dehydrated alcohol is preferably 0.1 mg of carbon black and 200 ml of dehydrated ethanol. the

As an optional way, in the above method, the step 2) is completed by the software that comes with the microscopic morphology acquisition tool used in step 1), for example, it is converted into Excel data by the software that comes with the scanning probe microscope, and the number of data points The number can be flexibly selected according to the requirements of image resolution (the more data provided, the higher the image resolution), the optional number of data points includes: 64×64, 128×128, 256×256, 512×512 , 1024×1024, etc. Preferably 256x256 points. the

As an optional mode, in the above method, the drawing software described in steps 3) and 4) is AutoCAD. the

As an optional manner, in the above method, the step 3) specifically replaces spaces between coordinate values of each point with commas. The specific conversion method can be carried out by using MATLAB software according to the following procedure:

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 the database and get x ₁ y ₁ z ₁

x ₂ y ₂ z ₂

                              ...

Coordinate group, save the file as txt format, use the replacement function, replace " " with "," to get:

x ₁ , y ₁ , z ₁

x ₂ , y ₂ , z ₂

                                     ...

Coordinate System.

As an optional way, in the above method, the solidification described in step 4) is specifically: select the 3D polyline drawing program in AutoCAD to connect the points to form a closed curve, and set the distance value between the two points to Adjust the magnification. Because the data of the carbon black topography map has not been materialized into CAD, the 3D printer cannot recognize it. It is also unrealistic to materialize each data (256×256 points) in turn. This is a difficulty. Through CAD's "3D polyline drawing program" converts the carbon black shape into a solid. the

As an optional way, in the above method, the 3D printing is carried out at room temperature, and the material used is photosensitive resin. It uses photosensitive resin printing at room temperature, which saves energy and increases controllability. It is to macroscopically and accurately print out microscopic carbon black, which truly reflects the morphology and structure of carbon black. the

As an optional way, in the above method, the carbon black is dispersed by ultrasound, so that the carbon black particles reach the level of primary particles and aggregates, and the morphology of the carbon black is scanned by a scanning probe microscope to obtain a carbon black morphology map. Then use the software that comes with the scanning probe atomic force microscope to export the topography map, and the data is in .exl format. The .exl data is processed by MATLAB software and converted into a specific format. Then import the data into CAD, draw the shape of carbon black, and then convert it into a solid, and convert the data into .stl format that can be recognized by 3D printers through 3dmax. Finally, a magnified entity of the carbon black's microscopic topography is printed. the

The present invention also provides a macroscopic enlarged solid model of the microscopic appearance of carbon black, which can be obtained by any one of the above-mentioned methods. the

The present invention also provides the application of a macroscopic enlarged solid model of the microscopic appearance of carbon black, which is characterized in that it is used as a teaching model. the

The present invention also provides an application of a macro-enlarged solid model of the microscopic morphology of carbon black, which is characterized in that it is used in wind tunnel tests related to carbon black to explore the relationship between microscopic carbon black and polymer chains, and to simulate carbon black. Mechanism of black reinforced rubber. the

All features disclosed in this specification, or steps in all methods or processes disclosed, may be combined in any manner, except for mutually exclusive features and/or steps. the

Beneficial effects of the present invention:

1. The present invention aims at the microcosmic carbon black primary particles or aggregates of inorganic materials, prints out the microcosmic morphology of carbon black through a 3D printer, and establishes the connection between the microcosmic and macrocosmic aspects of carbon black, that is, realizes the microcosmic process through 3D printing technology. Macroscopicalization and materialization. And rely on accurate data points to make carbon black microscopic topography map, with real data as support, the obtained enlarged entity structure is accurate.

2. The present invention has carried out the microcosmization of carbon black, which has greatly promoted the research of carbon black structure, particle size and morphology by scientific researchers, and will also provide first-hand information for the study of carbon black aggregates to reinforce rubber, and The development of this technology is also instructive for actual production. For example, it can be used to conduct wind tunnel tests on carbon black, explore the relationship between microscopic carbon black and polymer chains, and simulate the mechanism of carbon black reinforcing rubber. the

Description of drawings

FIG. 1 is a flowchart of the method described in Example 1. the

Detailed ways:

The above-mentioned content of the present invention will be further described in detail through the specific implementation of the examples below. However, this should not be construed as limiting the scope of the above-mentioned subject matter of the present invention to the following examples. Any modification made without departing from the spirit and principles of the present invention, as well as equivalent replacements or improvements made according to ordinary technical knowledge and conventional means in the field shall be included in the protection scope of the present invention.

Example 1:

In this experiment, the carbon black was first dispersed by ultrasound, so that the carbon black particles reached the level of primary particles and aggregates, and the carbon black morphology was scanned with Hitachi E-sweep scanning probe to obtain the carbon black morphology map. Then use the software that comes with the scanning probe atomic force microscope to export the topography map, and the data is in .exl format. The .exl data is processed by MATLAB software and converted into a specific format. Then import the data into CAD, draw the shape of carbon black, and then convert it into a solid (.dwg file), and convert the data into a .stl format that can be recognized by the 3D printer through 3dmax. Finally, a magnified entity of the carbon black's microscopic topography is printed. The specific process is shown in Figure 1.

As an optional way, in the above method, the 3D printing is carried out at room temperature, and the material used is photosensitive resin. It uses photosensitive resin printing at room temperature, which saves energy and increases controllability. It is to macroscopically and accurately print out microscopic carbon black, which truly reflects the morphology and structure of carbon black. the

Example 2:

The microscopic morphology enlarged entities of carbon black were prepared according to the following steps:

1) Disperse carbon black in absolute ethanol by ultrasonic (0.1mg carbon black, 200ml absolute ethanol), ultrasonic 20min;

2) Drop the sonicated carbon black anhydrous ethanol solution on the clean mica sheet and dry it. Put the mica sheet into the sample chamber of the scanning probe microscope and scan it to obtain the microscopic topography of carbon black (nanoscale);

3) Convert the microscopic morphology of carbon black from .xqd to .xqt, and then export the .exl data (256×256 points);

4) Use MATLAB software to develop a program to process the .exl data:

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 the database and get

x ₁ y ₁ z ₁

x ₂ y ₂ z ₂

……………

Coordinate group, save the file as txt format, use the replacement function, replace the space with "," to get:

x ₁ , y ₁ , z ₁

x ₂ , y ₂ , z ₂

                                   ...

Coordinate System;

5) Open AutoCAD, select the 3D polyline drawing program, and import the data obtained in step 3). After the AutoCAD drawing is completed, output the "C" command to make it form a closed curve, and then output the "W" command to convert the image into "blocks";

6) Import the .dwg file saved by AutoCAD into 3dmax, convert it into a .stl format recognizable by the 3D printer, and print out the carbon black microscopic structure entity;

7) Turn on the computer and connect to the 3D printer. Turn off computer security software programs such as computer firewall and computer housekeeper;

8) In the Internet connection option of the control panel, set the static IP address of the computer: 169.254.1.3, and set the submask to 255.255.0.0;

9) Turn on the 3D printer, the 3D printer system will perform a self-test after starting up, open the IE8 (or above version) browser, enter the IP address: 169.254.1.1, and enter the 3D printer web page control interface;

10) Click login and enter the account password. At this time, the 3D printer will be ready for work. After clicking OK and NO in turn (if you need to change the material, you need to click YES to change the material), the web page will display the words "printer is ready". When the printer is ready;

11) Select new in print, create a new print task, select creat, and the 3D printing model control window will pop up. Select "load CAD file", select the converted .STL format file, and then select "Auto part placement" to automatically center, and use "Scale" to control the zoom in and out and "Rotate" to control the rotation direction to adjust to the required template model;

12) After the model size is determined, select "Generate and Preview Supports" to generate and preview supports, and then click the "Submit" button to submit the job to the print list, or click "Submit job" from the File drop-down menu, and you will return to the web page control interface;

13) Click "click here to start", select YES and NO respectively, and click statr print to start printing;

14) After the printer is finished printing, you must wear nitrile gloves and special UV-proof glasses, then turn on the printer, take out the printed results, take off the printed model with a shovel and a knife, then put it in alcohol, soak it for half an hour, take it out, and then print Morphological structure of carbon black.

As an optional way, in the above method, the 3D printing is carried out at room temperature, and the material used is photosensitive resin. It uses photosensitive resin printing at room temperature, which saves energy and increases controllability. It is to macroscopically and accurately print out microscopic carbon black, which truly reflects the morphology and structure of carbon black. the

Application example

Using the macroscopic model of the carbon black morphology and structure obtained in Example 2 for classroom teaching is of great help to students in understanding the carbon black morphology and structure. The application in scientific research can also greatly promote the research of carbon black structure, particle size and morphology. In addition, using this model as a wind tunnel test related to carbon black is also helpful to explore the relationship between microscopic carbon black and polymer chains, and to simulate the mechanism of carbon black reinforcing rubber.

The above description is only a preferred embodiment of the present invention, and it is only illustrative and non-restrictive for the present invention; those of ordinary skill in the art understand that many modifications can be made to it within the spirit and scope of the present invention. Changes, modifications, and even equivalent changes all fall within the protection scope of the present invention. the

the

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.