CN110256102B - Preparation method of novel TiN-based light efficient wave-absorbing material - Google Patents
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Abstract
The invention relates to the technical field of wave-absorbing material preparation, and discloses a preparation method of a novel TiN-based light high-efficiency wave-absorbing material, which comprises the following steps: carrying out primary ball milling treatment on 10-30 parts of light filler 3M hollow glass microspheres to obtain a primary ball milling product; carrying out secondary ball milling treatment on the primary ball-milled product and 40-50 parts of wave-absorbing matrix nano titanium nitride (TiN) to obtain a secondary ball-milled product; mixing the secondary ball-milling product with 10-20 parts of wave-absorbing filler nano ferroferric oxide (Fe)3O4) Carrying out three ball milling treatments to obtain three ball milling products; and pressing and molding the third ball-milled product under the pressure of 20-30 MPa to obtain a precursor, and finally performing hot-pressing sintering treatment on the precursor to prepare the novel TiN-based light high-efficiency wave-absorbing material. The invention solves the technical problems that the nano TiN particles are easy to agglomerate and the wave absorbing mechanism is single, and the required filler content is high (about 45 wt%) in order to embody enough wave absorbing performance, so that the requirements of the light high-efficiency wave absorbing material are difficult to meet.
Description
Technical Field
The invention relates to the technical field of wave-absorbing material preparation, in particular to a preparation method of a novel TiN-based light high-efficiency wave-absorbing material.
Background
In recent years, with the continuous expansion of the application field of the wave-absorbing material, researches on the improvement of the loss performance of the wave-absorbing material, the widening of the effective loss frequency band and the like are increasingly active at home and abroad, and the requirements on the wave-absorbing material are more and more strict. However, the traditional wave-absorbing materials such as ferrite, magnetic metal particles and oxides thereof have high density, large filler content and poor environmental stability, and thus the requirements of light weight and high efficiency of the wave-absorbing materials are difficult to meet. Therefore, the development of a novel efficient wave-absorbing material with thin thickness, light weight, wide frequency band and strong absorption is urgently needed.
Titanium nitride (TiN) has lower density and excellent wave-absorbing performance, and is a potential light wave-absorbing material. However, because the nano TiN particles are easy to agglomerate and the wave-absorbing mechanism is single, in order to embody sufficient wave-absorbing performance, the required filler content is high (about 45 wt%), and the requirements of the light high-efficiency wave-absorbing material are difficult to meet. Therefore, the method adopts a proper method to improve the dispersion behavior of the TiN nano particles and endows the material with more wave-absorbing mechanisms, and is a key solution for reducing the filler content and preparing the TiN-based light high-efficiency wave-absorbing material.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a novel TiN-based light high-efficiency wave-absorbing material, which solves the technical problems that the nano TiN particles are easy to agglomerate and the wave-absorbing mechanism is single, and the required filler content is high (about 45 wt%) in order to embody enough wave-absorbing performance, so that the requirements of the light high-efficiency wave-absorbing material are difficult to meet.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a novel TiN-based light high-efficiency wave-absorbing material comprises the following steps:
the method comprises the following steps: carrying out primary ball milling treatment on 10-30 parts of light filler 3M hollow glass microspheres to obtain a primary ball milling product;
step two: carrying out secondary ball milling treatment on the primary ball-milled product and 40-50 parts of wave-absorbing matrix nano titanium nitride (TiN) to obtain a secondary ball-milled product;
step three: mixing the secondary ball-milling product with 10-20 parts of wave-absorbing filler nano ferroferric oxide (Fe)3O4) Carrying out three ball milling treatments to obtain three ball milling products;
step four: and pressing and molding the third ball-milled product under the pressure of 20-30 MPa to obtain a precursor, and finally performing hot-pressing sintering treatment on the precursor at the temperature of 1300-1500 ℃ and under the pressure of 120-150 MPa to prepare the novel TiN-based light high-efficiency wave-absorbing material.
Preferably, the first step: the light filler 3M hollow glass beads are placed on a ball mill, the ball milling speed is 300r/min, the interval of each ball milling is 30min and 5min, and the ball milling time is 2 h.
Preferably, the step four: the temperature rise rate of the vacuum furnace was 10 ℃/min.
Preferably, the step four: the annealing rate of the vacuum furnace was 10 ℃/min.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adopts the technical scheme that' 10-30 parts of light filler 3M hollow glass beads are subjected to one stepPerforming secondary ball milling treatment to obtain a primary ball milling product, performing secondary ball milling treatment on the primary ball milling product and 40-50 parts of wave-absorbing matrix nano titanium nitride (TiN) to obtain a secondary ball milling product, and mixing the secondary ball milling product with 10-20 parts of wave-absorbing filler nano ferroferric oxide (Fe)3O4) Carrying out three-time ball milling treatment to obtain a three-time ball milling product, carrying out compression molding on the three-time ball milling product under the pressure of 20-30 MPa to obtain a precursor, and finally carrying out hot-pressing sintering treatment on the precursor at the temperature of 1300-1500 ℃ and under the pressure of 120-150 MPa to prepare the novel TiN-based light high-efficiency wave-absorbing material, so that the technical problem that the requirements of the light high-efficiency wave-absorbing material are difficult to meet due to the fact that nano TiN particles are easy to agglomerate and the wave-absorbing mechanism is single, and the required filler content is high (about 45 wt%) in order to embody enough wave-absorbing performance is solved;
the effective absorption frequency bandwidth range of the novel TiN-based light high-efficiency wave-absorbing material prepared by the invention is 3-18 GHz, and the density of the novel TiN-based light high-efficiency wave-absorbing material is 2.84-3.21 g/cm3。
Detailed Description
The raw materials used in the examples were as follows:
nanometer titanium nitride (TiN), average particle diameter of 40nm, and purity>99.9% and tap density of 5.4g/cm3Black powder, Shanghai Xian New Material science and technology, Inc.;
nano ferroferric oxide (Fe)3O4) Average particle diameter of 10 to 20nm, purity>99.9 percent and tap density of 4.8 to 5.1g/cm3Black powder, Nanjing Hongde nanomaterial Co., Ltd;
3M hollow glass beads with an average particle size of 15-120 um, soda lime borosilicate glass with a density of 0.125-0.6 g/cm3Pure white, Shanghai Huizi Su nanometer New Material Co.
The first embodiment is as follows:
(1) weighing 10g of 3M hollow glass microspheres and 100mL of absolute ethyl alcohol, placing the mixture in a stainless steel ball milling container, placing 15 stainless steel microspheres with the diameter of 10mm in the container, placing the container on a ball milling instrument, adjusting the ball milling rotation speed to 300r/min, and performing ball milling for 30min at an interval of 5min for 2h to obtain a primary ball milling product;
(2) weighing 40g of nano titanium nitride (TiN) and the primary ball-milled product prepared in the step (1), and ball-milling for 2 hours at a speed of 400r/min to obtain a secondary ball-milled product;
(3) weighing 10g of nano ferroferric oxide (Fe)3O4) Ball-milling the mixture and the secondary ball-milling product prepared in the step (2) for 2 hours at the speed of 400r/min to obtain a tertiary ball-milling product;
(4) putting the tertiary ball-milling product in the step (3) into an isostatic pressing die, and pressing the product into a mold under the pressure of 20MPa to prepare a precursor;
(5) putting the precursor formed by pressing in the step (4) into a vacuum furnace, heating from room temperature to 1300 ℃ at the temperature rising rate of 10 ℃/min under the pressure of 120MPa, carrying out vacuum sintering for 3h at the temperature of 1300 ℃ and the pressure of 120MPa, and then cooling to room temperature at the annealing rate of 10 ℃/min, and taking out to prepare the novel TiN-based light high-efficiency wave-absorbing material;
(6) and (4) carrying out performance test on the novel TiN-based light high-efficiency wave-absorbing material prepared in the step (5), wherein the effective absorption frequency bandwidth range is 3-18 GHz, and the density is 2.98g/cm3。
Example two:
(1) weighing 30g of 3M hollow glass microspheres and 100mL of absolute ethyl alcohol, placing the mixture in a stainless steel ball milling container, placing 15 stainless steel microspheres with the diameter of 10mm in the container, placing the container on a ball milling instrument, adjusting the ball milling rotation speed to 300r/min, and performing ball milling for 30min and 5min at intervals for 2h to obtain a primary ball milling product;
(2) weighing 50g of nano titanium nitride (TiN) and the primary ball-milled product prepared in the step (1), and ball-milling for 2 hours at a speed of 400r/min to obtain a secondary ball-milled product;
(3) weighing 20g of nano ferroferric oxide (Fe)3O4) Ball-milling the mixture and the secondary ball-milling product prepared in the step (2) for 2 hours at the speed of 400r/min to obtain a tertiary ball-milling product;
(4) putting the tertiary ball-milling product in the step (3) into an isostatic pressing die, and pressing the product into a mold under the pressure of 30MPa to prepare a precursor;
(5) putting the precursor formed by pressing in the step (4) into a vacuum furnace, heating the precursor from room temperature to 1500 ℃ at the heating rate of 10 ℃/min under the pressure of 150MPa, carrying out vacuum sintering at the temperature of 1500 ℃ and the pressure of 150MPa for 3h, and then cooling to room temperature at the annealing rate of 10 ℃/min, and taking out to prepare the novel TiN-based light high-efficiency wave-absorbing material;
(6) and (4) carrying out performance test on the novel TiN-based light high-efficiency wave-absorbing material prepared in the step (5), wherein the effective absorption frequency bandwidth range is 3-18 GHz, and the density is 3.21g/cm3。
Example three:
(1) weighing 20g of 3M hollow glass microspheres and 100mL of absolute ethyl alcohol, placing the mixture in a stainless steel ball milling container, placing 15 stainless steel microspheres with the diameter of 10mm in the container, placing the container on a ball milling instrument, adjusting the ball milling rotation speed to 300r/min, and performing ball milling for 30min at an interval of 5min for 2h to obtain a primary ball milling product;
(2) weighing 45g of nano titanium nitride (TiN) and the primary ball-milled product prepared in the step (1), and ball-milling for 2 hours at a speed of 400r/min to obtain a secondary ball-milled product;
(3) weighing 15g of nano ferroferric oxide (Fe)3O4) Ball-milling the mixture and the secondary ball-milling product prepared in the step (2) for 2 hours at the speed of 400r/min to obtain a tertiary ball-milling product;
(4) putting the tertiary ball-milling product in the step (3) into an isostatic pressing die, and pressing the product into a mold under the pressure of 25MPa to prepare a precursor;
(5) putting the precursor formed by pressing in the step (4) into a vacuum furnace, heating the precursor from room temperature to 1400 ℃ at the temperature rise rate of 10 ℃/min under the pressure of 140MPa, carrying out vacuum sintering at the temperature of 1400 ℃ under the pressure of 130MPa for 3h, and then cooling the precursor to room temperature at the annealing rate of 10 ℃/min, and taking out the precursor to prepare the novel TiN-based light high-efficiency wave-absorbing material;
(6) and (4) carrying out performance test on the novel TiN-based light high-efficiency wave-absorbing material prepared in the step (5), wherein the effective absorption frequency bandwidth range is 3-18 GHz, and the density is 2.84g/cm3。
Claims (1)
1. A preparation method of a novel TiN-based light high-efficiency wave-absorbing material is characterized by comprising the following steps:
(1) weighing 20g of 3M hollow glass microspheres and 100mL of absolute ethyl alcohol, placing the mixture in a stainless steel ball milling container, placing 15 stainless steel microspheres with the diameter of 10mm in the container, placing the container on a ball milling instrument, adjusting the ball milling rotation speed to 300r/min, and performing ball milling for 30min at an interval of 5min for 2h to obtain a primary ball milling product;
(2) weighing 45g of nano titanium nitride (TiN) and the primary ball-milled product prepared in the step (1), and ball-milling for 2 hours at a speed of 400r/min to obtain a secondary ball-milled product;
(3) weighing 15g of nano ferroferric oxide (Fe)3O4) Ball-milling the mixture and the secondary ball-milling product prepared in the step (2) for 2 hours at the speed of 400r/min to obtain a tertiary ball-milling product;
(4) putting the tertiary ball-milling product in the step (3) into an isostatic pressing die, and pressing the product into a mold under the pressure of 25MPa to prepare a precursor;
(5) putting the precursor formed by pressing in the step (4) into a vacuum furnace, heating the precursor from room temperature to 1400 ℃ at the temperature rise rate of 10 ℃/min under the pressure of 140MPa, carrying out vacuum sintering at the temperature of 1400 ℃ under the pressure of 130MPa for 3h, and then cooling the precursor to room temperature at the annealing rate of 10 ℃/min, and taking out the precursor to prepare the novel TiN-based light high-efficiency wave-absorbing material;
(6) and (4) carrying out performance test on the novel TiN-based light high-efficiency wave-absorbing material prepared in the step (5), wherein the effective absorption frequency bandwidth range is 3-18 GHz, and the density is 2.84g/cm3；
Wherein the nano titanium nitride (TiN) has an average particle size of 40nm and a purity of>99.9% and tap density of 5.4g/cm3Black powder, Shanghai Xian New Material science and technology, Inc.;
wherein the nano ferroferric oxide (Fe)3O4) Average particle diameter of 10 to 20nm, purity>99.9 percent and tap density of 4.8 to 5.1g/cm3Black powder, Nanjing Hongde nanomaterial Co., Ltd;
wherein the 3M hollow glass bead has an average particle size of 15-120 um, and the soda lime borosilicate glass has a density of 0.125-0.6 g/cm3Pure white, Shanghai Huizi Su nanometer New Material Co.
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| US9674992B2 (en) * | 2014-07-07 | 2017-06-06 | Iteq Corporation | Electromagnetic interference shielding film |
| CN105273689A (en) * | 2014-07-18 | 2016-01-27 | 广东工业大学 | Novel multi-element structure composite conductive filling material |
| CN107051343A (en) * | 2016-12-06 | 2017-08-18 | 青岛大学 | The preparation method of the sour nickel@ferriferrous oxide composite materials of the carbon@cobalts of multi-layer core-shell structure |
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