CN107555994B - Preparation method of high-absorptivity terahertz material - Google Patents

Preparation method of high-absorptivity terahertz material Download PDF

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CN107555994B
CN107555994B CN201710783903.5A CN201710783903A CN107555994B CN 107555994 B CN107555994 B CN 107555994B CN 201710783903 A CN201710783903 A CN 201710783903A CN 107555994 B CN107555994 B CN 107555994B
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graphene
nano tube
carbon nano
resin
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CN107555994A (en
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张鹏
韩顺利
董杰
龚侃
吕子敬
孟鑫
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CETC 41 Institute
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Abstract

The invention provides a preparation method of a high-absorptivity terahertz material, which comprises the following steps of 1: selecting graphene powder and carbon nanotube powder; step 2: mixing the carbon nano tube and the graphene according to a ratio to prepare mixed powder; and step 3: adding ultrapure water into the mixed powder to prepare a solution, and adding 2g/L of surfactant into the solution; and 4, step 4: ultrasonic oscillation is carried out for 25 to 30 minutes; and 5: carrying out centrifugal rotation to finish the preparation of the carbon nano tube and graphene slurry; step 6: adding resin into the slurry of the carbon nano tube and the graphene; and 7: rotating the slurry by using a vacuum rotating machine to uniformly disperse the resin in the slurry; and 8: coating the slurry on a substrate; and step 9: and (5) putting the mixture into a high-temperature box for sintering to finish the preparation. By adopting the scheme, the terahertz laser has high absorptivity in a wide frequency range, the manufacturing process is simple, and the heat dissipation performance is good.

Description

Preparation method of high-absorptivity terahertz material
Technical Field
The invention belongs to the technical field of preparation of terahertz materials, and particularly relates to a preparation method of a terahertz material with high absorptivity.
Background
At present, materials with high absorptivity for terahertz laser are needed to be used in the aspects of terahertz stealth materials, terahertz detector manufacturing and the like. However, the existing absorption material is generally made of a plurality of materials through a specific process, the process is complex, the terahertz laser can be absorbed only at partial frequency points, and the terahertz laser cannot be well absorbed at 0.1 THz-10 THz.
Accordingly, the prior art is deficient and needs improvement.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a high-absorptivity terahertz material aiming at the defects of the prior art.
The technical scheme of the invention is as follows:
a preparation method of a high-absorptivity terahertz material comprises the following steps:
step 1: selecting graphene powder with the purity of not less than 98% and the length of less than 10 microns, and selecting carbon nanotube powder with the purity of not less than 95% and the length of less than 20 microns;
step 2: mixing the carbon nano tube and the graphene according to the ratio of 7:1 to prepare mixed powder;
and step 3: adding ultrapure water into the mixed powder to prepare a solution with the concentration of 80-100 g/L, and adding 2g/L of surfactant into the solution;
and 4, step 4: using an ultrasonic cleaner, and carrying out ultrasonic oscillation for 25-30 minutes under the condition that the ultrasonic frequency is 30-40 kHz;
and 5: when the rotation speed is 10000rpm, a centrifugal machine is used for carrying out centrifugal rotation on the solution after ultrasonic oscillation for 2 minutes, the carbon nano tube and graphene slurry are precipitated at the lower layer of the solution, the upper layer of the solution is clear liquid, and the clear liquid at the upper layer is poured out, so that the preparation of the carbon nano tube and graphene slurry is completed;
step 6: adding resin into the slurry of the carbon nano tube and the graphene to improve the viscosity of the slurry, wherein the ratio of the slurry to the resin is 6: 1;
and 7: rotating the carbon nano tube added with the resin and the graphene slurry for 3 to 5 minutes by using a vacuum rotating machine at the rotating speed of 6000rpm to uniformly disperse the resin in the carbon nano tube and graphene slurry;
and 8: coating the carbon nano tube containing resin and graphene slurry on a substrate;
and step 9: and (4) sintering the material in a high-temperature box to finish the preparation of the terahertz material.
In the step 1, the carbon nanotube is a single-walled carbon nanotube or a multi-walled carbon nanotube.
In the step 3, the surfactant is cetyl trimethyl ammonium bromide or an emulsifier OP.
In the step 6, the resin is polydimethylsiloxane.
In the step 8, the coating method includes magnetron sputtering, spraying or screen printing.
By adopting the scheme, the thermal conductivity of the terahertz absorption material is improved, so that the terahertz laser is absorbed more uniformly by the absorption material, and heat dissipation is facilitated. In addition, through tests, the absorption rate of the terahertz material provided by the invention on terahertz laser is more than 99% between 0.1THz and 30THz, and the terahertz material has higher absorption rate.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments.
Example 1
As shown in fig. 1, in order to overcome the defects of the prior art, the present invention provides a material having a high absorption rate for terahertz laser in a wide frequency range, and the method of the present invention comprises the following steps:
step 1: selecting graphene powder with the purity of not less than 98% and the length of less than 10 microns, and selecting carbon nanotube powder with the purity of not less than 95% and the length of less than 20 microns, wherein the carbon nanotube is a single-walled carbon nanotube or a multi-walled carbon nanotube.
Step 2: mixing the carbon nano tube and the graphene according to the ratio of 7:1 to prepare mixed powder.
And step 3: adding ultrapure water into the mixed powder to prepare a solution with the concentration of 80-100 g/L, and adding 2g/L of surfactant into the solution, wherein the surfactant is cetyl trimethyl ammonium bromide or an emulsifier OP.
And 4, step 4: an ultrasonic cleaner is used, ultrasonic oscillation is carried out for 25-30 minutes under the condition that the ultrasonic frequency is 30-40 kHz, under the action of a surfactant, the carbon nano tube and the graphene are dispersed in a solution, the agglomeration phenomenon disappears, and the terahertz material can be uniformly distributed.
And 5: and when the rotating speed is 10000rpm, a centrifugal machine is used for carrying out centrifugal rotation on the solution after ultrasonic oscillation for 2 minutes, the carbon nano tube and the graphene slurry are precipitated at the lower layer of the solution, the upper layer of the solution is clear liquid, and the clear liquid at the upper layer is poured out, so that the preparation of the carbon nano tube and the graphene slurry is completed.
Step 6: adding resin into the slurry of the carbon nano tube and the graphene to improve the viscosity of the slurry, wherein the ratio of the slurry to the resin is 6:1, and the resin is polydimethylsiloxane.
And 7: and rotating the carbon nano tube added with the resin and the graphene slurry for 3 to 5 minutes by using a vacuum rotating machine at the rotating speed of 6000rpm so as to uniformly disperse the resin in the carbon nano tube and graphene slurry.
And 8: the carbon nano tube containing resin and graphene slurry are coated on a substrate by magnetron sputtering, spraying, screen printing and the like.
And step 9: and (4) sintering the material in a high-temperature box to finish the preparation of the terahertz material.
According to the invention, the graphene is added into the carbon nano tube, so that the thermal conductivity of the terahertz absorption material is improved, the terahertz laser is absorbed by the absorption material more uniformly, and the heat dissipation is facilitated. In addition, through tests, the absorption rate of the terahertz material provided by the invention on terahertz laser is more than 99% between 0.1THz and 30 THz.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.

Claims (1)

1. A preparation method of a high-absorptivity terahertz material is characterized by comprising the following steps:
step 1: selecting graphene powder with the purity of not less than 98% and the length of less than 10 microns, and selecting carbon nanotube powder with the purity of not less than 95% and the length of less than 20 microns;
step 2: mixing the carbon nano tube and the graphene according to the ratio of 7:1 to prepare mixed powder;
and step 3: adding ultrapure water into the mixed powder to prepare a solution with the concentration of 80-100 g/L, and adding 2g/L of surfactant into the solution;
and 4, step 4: using an ultrasonic cleaner, and carrying out ultrasonic oscillation for 25-30 minutes under the condition that the ultrasonic frequency is 30-40 kHz;
and 5: when the rotation speed is 10000rpm, a centrifugal machine is used for carrying out centrifugal rotation on the solution after ultrasonic oscillation for 2 minutes, the carbon nano tube and graphene slurry are precipitated at the lower layer of the solution, the upper layer of the solution is clear liquid, and the clear liquid at the upper layer is poured out, so that the preparation of the carbon nano tube and graphene slurry is completed;
step 6: adding resin into the slurry of the carbon nano tube and the graphene to improve the viscosity of the slurry, wherein the ratio of the slurry to the resin is 6: 1;
and 7: rotating the carbon nano tube added with the resin and the graphene slurry for 3 to 5 minutes by using a vacuum rotating machine at the rotating speed of 6000rpm to uniformly disperse the resin in the carbon nano tube and graphene slurry;
and 8: coating the carbon nano tube containing resin and graphene slurry on a substrate;
and step 9: sintering the material in a high-temperature box to complete the preparation of the terahertz material;
in the step 1, the carbon nanotube is a single-walled carbon nanotube or a multi-walled carbon nanotube; in the step 3, the surfactant is cetyl trimethyl ammonium bromide or an emulsifier OP; in the step 6, the resin is polydimethylsiloxane; in the step 8, the coating method comprises magnetron sputtering, spraying or screen printing.
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CN110128121A (en) * 2019-05-14 2019-08-16 江苏中兴国邦环保科技有限公司 A kind of preparation method of energy-saving active Terahertz composite material
CN111551516B (en) * 2020-05-14 2023-03-14 南京邮电大学 Efficient visual terahertz detector and preparation and test methods thereof
CN113451864A (en) * 2021-06-25 2021-09-28 泉州慈光科技有限公司 Terahertz emitter and manufacturing method thereof

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN102417610A (en) * 2011-07-13 2012-04-18 青岛科技大学 Graphene/carbon nanotube hybrid polymer composite material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102417610A (en) * 2011-07-13 2012-04-18 青岛科技大学 Graphene/carbon nanotube hybrid polymer composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
材料在太赫兹波段吸收性能的研究进展;韩建龙等;《兵器材料科学与工程》;20130331;第36卷(第2期);第130-133页 *

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