CN115449343A - Silicon nitride wave-absorbing material and preparation method thereof - Google Patents
Silicon nitride wave-absorbing material and preparation method thereof Download PDFInfo
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- CN115449343A CN115449343A CN202211284570.9A CN202211284570A CN115449343A CN 115449343 A CN115449343 A CN 115449343A CN 202211284570 A CN202211284570 A CN 202211284570A CN 115449343 A CN115449343 A CN 115449343A
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 47
- 239000011358 absorbing material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000011258 core-shell material Substances 0.000 claims abstract description 30
- 229910015136 FeMn Inorganic materials 0.000 claims abstract description 29
- 239000011521 glass Substances 0.000 claims abstract description 28
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 19
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 150000007524 organic acids Chemical class 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 239000012265 solid product Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000012047 saturated solution Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- JTPNRXUCIXHOKM-UHFFFAOYSA-N 1-chloronaphthalene Chemical compound C1=CC=C2C(Cl)=CC=CC2=C1 JTPNRXUCIXHOKM-UHFFFAOYSA-N 0.000 claims description 6
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 6
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 6
- 150000001732 carboxylic acid derivatives Chemical group 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- CCUWGJDGLACFQT-UHFFFAOYSA-N 2,2,3,3,4,4-hexafluoropentanedioic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(O)=O CCUWGJDGLACFQT-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- YPJUNDFVDDCYIH-UHFFFAOYSA-N perfluorobutyric acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)F YPJUNDFVDDCYIH-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- XINQFOMFQFGGCQ-UHFFFAOYSA-L (2-dodecoxy-2-oxoethyl)-[6-[(2-dodecoxy-2-oxoethyl)-dimethylazaniumyl]hexyl]-dimethylazanium;dichloride Chemical compound [Cl-].[Cl-].CCCCCCCCCCCCOC(=O)C[N+](C)(C)CCCCCC[N+](C)(C)CC(=O)OCCCCCCCCCCCC XINQFOMFQFGGCQ-UHFFFAOYSA-L 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000008422 chlorobenzenes Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 150000003613 toluenes Chemical class 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention belongs to the technical field of functional material manufacturing, and particularly relates to a silicon nitride wave-absorbing material and a preparation method thereof. A silicon nitride wave-absorbing material, which is composed of FeMn @ C 60 The core-shell structure material is compounded with silicon nitride; the FeMn @ C 60 The preparation method of the core-shell structure material comprises the following steps: step 1: metal oxide, organic acid, C 60 Filling the saturated solution into a glass tube, exhausting air in the glass tube by using nitrogen, and sealing the tube; step 2: putting the glass tube into an oven and heating; and step 3: filtering the solid product, washing for 3 times, and drying to obtain FeMn @ C 60 A core-shell structure material. FeMn @ C 60 The heterogeneous interface between the core and the shell in the core-shell structure material can also generate an interface polarization effect, so that the dielectric loss of the material is increased, the wave absorbing performance of the material is improved, the density of the material is reduced, and the dielectric loss capacity of the material is improved through multiple reflections between the core and the shell.
Description
Technical Field
The invention belongs to the technical field of functional material manufacturing, and particularly relates to a silicon nitride wave-absorbing material and a preparation method thereof.
Background
In recent years, with the widespread use of electromagnetic waves in human life, electromagnetic pollution has become an increasingly serious problem. For example, electromagnetic waves radiated by a mobile phone can affect the normal operation of a precise electronic medical instrument; electromagnetic waves can also severely interfere with communications facilities on the aircraft; electromagnetic leakage of electronic devices such as computers can cause leakage of important information; in military terms, the development of radar detection technology based on electromagnetic waves seriously threatens the viability of airplanes, tanks and ships; moreover, electromagnetic waves are also a long-term hazard to humans. Therefore, the development of the wave-absorbing material with excellent performance has important significance in both military and civil aspects.
The carbon material belongs to one of dielectric materials, has the advantages of ultralow density, high conductivity, excellent microwave absorption performance, environmental stability and the like, but the single carbon material cannot meet the requirements in the aspects of mechanical property, strength and the like. The silicon nitride has high strength, wear resistance, corrosion resistance and oxidation resistance at room temperature and high temperature, good thermal shock resistance and mechanical impact resistance, low dielectric constant and electromagnetic loss, and can mutually make up the defects of the silicon nitride and the carbon material when being used in a compounding way.
Disclosure of Invention
The invention provides a silicon nitride wave-absorbing material and a preparation method thereof in order to overcome the problems in the prior art.
The technical scheme provided by the invention is as follows:
a silicon nitride wave-absorbing material, which consists of FeMn @ C 60 The core-shell structure material is compounded with silicon nitride;
the FeMn @ C 60 The preparation method of the core-shell structure material comprises the following steps:
step 1: 0.07mol of metal oxide, organic acid and 1L of C 60 Filling the saturated solution into a glass tube, exhausting air in the glass tube by using nitrogen, and sealing the tube, wherein the metal oxide consists of FeO and MnO;
step 2: putting the glass tube in the step 1 into an oven, heating to 160-200 ℃, keeping for 48-96h, and then cooling to room temperature at a cooling rate of 5 ℃/h;
and step 3: the solid product in the glass tube was filtered and used for preparation C 60 Washing with saturated organic solvent for 3 times, and drying to obtain FeMn @ C 60 A core-shell structure material.
Specifically, the mol ratio of FeO to MnO is 0.8-1.2:1.
specifically, the organic acid adopts any one of heptafluorobutyric acid, hexafluoroglutaric acid and glutaric acid, and the molar ratio of the carboxylic acid functional group to the metal oxide in the organic acid is 0.5-3.
Specifically, step C in the step 1 60 The organic solvent of the saturated solution is any one of chlorobenzene, toluene and 1-chloronaphthalene.
The invention also provides a preparation method of the silicon nitride wave-absorbing material, which is prepared by reacting FeMn @ C 60 The core-shell structure material and silicon nitride are ground in a ball mill for 2-3 h.
The invention provides a silicon nitride wave-absorbing material, wherein FeMn @ C 60 The heterogeneous interface between the core and the shell in the core-shell structure material can generate an interface polarization effect, so that the dielectric loss of the material is increased, the wave-absorbing performance of the material is improved, and the density of the material is reduced. Multiple reflections between the core and the shell increase the dielectric loss capability of the material. In addition, feMn @ C 60 The core-shell structure material is compounded with the porous silicon nitride to form a more complex porous material, so that the void ratio is further improved, the number of interfaces is increased, and the wave-absorbing performance of the material is improved. The complex formed by the iron and manganese metal elements has a certain magnetic consumption effect, and the wave-absorbing performance of the material can be further improved.
Drawings
FIG. 1 is a graph of the real part of the complex dielectric constant of an example 4 of a silicon nitride wave-absorbing material varying with frequency.
FIG. 2 is a graph of the change of the imaginary part of the complex dielectric constant with frequency in example 4 of a silicon nitride wave-absorbing material.
FIG. 3 is a graph of the real part of the complex permeability constant of the silicon nitride wave-absorbing material in example 4 as a function of frequency.
FIG. 4 is a graph of the change of the imaginary part of the complex permeability constant with frequency in example 4 of the silicon nitride wave-absorbing material.
FIG. 5 is a wave-absorbing property diagram of a silicon nitride wave-absorbing material in example 4 with different thicknesses of a sample and paraffin.
Detailed Description
For a further understanding of the present invention, reference will now be made to the following preferred embodiments of the invention in conjunction with the examples, but it is to be understood that the description is intended to further illustrate the features and advantages of the invention and is not intended to limit the scope of the claims which follow.
Example 1
The silicon nitride wave-absorbing material is prepared from FeMn @ C 60 A composite material formed by a core-shell structure material and silicon nitride; the preparation method comprises the following steps: handle FeMn @ C 60 The core-shell structure material and silicon nitride are ground in a ball mill for 2 hours.
The silicon nitride is a silicon nitride nanowire.
The FeMn @ C 60 The preparation method of the core-shell structure material comprises the following steps:
step 1: 0.07mol of metal oxide, heptafluorobutyric acid and 1L of C 60 Filling a saturated chlorobenzene solution into a high-temperature-resistant glass tube, exhausting air in the glass tube by using nitrogen, and sealing the glass tube, wherein the metal oxide consists of FeO and MnO;
and 2, step: putting the glass tube obtained in the step 1 into a baking oven capable of heating and cooling according to a program, heating to 160 ℃, keeping for 96 hours, and then cooling to room temperature at a cooling rate of 5 ℃/h;
and step 3: filtering the solid product in the glass tube, washing with chlorobenzene for 3 times, and drying to obtain FeMn @ C 60 A core-shell structure material.
The mol ratio of FeO to MnO in step 1 is 0.8:1.
the molar ratio of the carboxylic acid functional group to the metal oxide in the heptafluorobutyric acid in the step 1 is 0.5.
Example 2
The silicon nitride wave-absorbing material is prepared from FeMn @ C 60 A composite material formed by the core-shell structure material and silicon nitride; it is composed ofThe preparation method comprises the following steps: handle FeMn @ C 60 The core-shell structure material and silicon nitride are ground in a ball mill for 2.5 hours.
The silicon nitride is a silicon nitride nanowire.
The FeMn @ C 60 The preparation method of the core-shell structure material comprises the following steps:
step 1: 0.07mol of metal oxide, hexafluoroglutaric acid, 1L of C 60 Filling the saturated toluene solution into a high-temperature-resistant glass tube, exhausting air in the glass tube by using nitrogen, and sealing the tube, wherein the metal oxide consists of FeO and MnO;
step 2: putting the glass tube obtained in the step 1 into an oven capable of heating and cooling according to a program, heating to 180 ℃, keeping the temperature for 80 hours, and then cooling to room temperature at a cooling rate of 5 ℃/h;
and step 3: filtering the solid product in the glass tube, washing with toluene for 3 times, and drying to obtain FeMn @ C 60 A core-shell structure material.
In the step 1, the mol ratio of FeO to MnO is 1:1.
the molar ratio of the carboxylic acid functional group to the metal oxide in the hexafluoroglutaric acid in step 1 was 1.
Example 3
The silicon nitride wave-absorbing material is prepared from FeMn @ C 60 A composite material formed by the core-shell structure material and silicon nitride; the preparation method comprises the following steps: handle FeMn @ C 60 The core-shell structure material and silicon nitride are ground in a ball mill for 2.5 hours.
The silicon nitride is a silicon nitride nanowire.
The FeMn @ C 60 The preparation method of the core-shell structure material comprises the following steps:
step 1: 0.07mol of metal oxide, glutaric acid and 1L of C 60 Filling a saturated 1-chloronaphthalene solution into a high-temperature resistant glass tube, exhausting air in the glass tube by using nitrogen, and sealing the tube, wherein the metal oxide consists of FeO and MnO;
step 2: putting the glass tube obtained in the step 1 into an oven capable of heating and cooling according to a program, heating to 200 ℃, keeping for 72 hours, and then cooling to room temperature at a cooling rate of 5 ℃/h;
and step 3: filtering the solid product in the glass tube, washing with 1-chloronaphthalene for 3 times, and drying to obtain FeMn @ C 60 A core-shell structure material.
In the step 1, the mol ratio of FeO to MnO is 1.1:1.
the mole ratio of carboxylic acid functional group to metal oxide in glutaric acid in step 1 was 2.
Example 4
The silicon nitride wave-absorbing material is prepared from FeMn @ C 60 A composite material formed by the core-shell structure material and silicon nitride; the preparation method comprises the following steps: handle FeMn @ C 60 The core-shell structure material and silicon nitride are ground in a ball mill for 3 hours.
The silicon nitride is a silicon nitride nanowire.
The FeMn @ C 60 The preparation method of the core-shell structure material comprises the following steps:
step 1: 0.07mol of metal oxide, glutaric acid and 1L of C 60 Filling a saturated 1-chloronaphthalene solution into a high-temperature resistant glass tube, exhausting air in the glass tube by using nitrogen, and sealing the tube, wherein the metal oxide consists of FeO and MnO;
step 2: putting the glass tube obtained in the step 1 into a drying oven capable of heating and cooling according to a program, heating to 200 ℃, keeping for 48 hours, and then cooling to room temperature at a cooling rate of 5 ℃/h;
and step 3: filtering the solid product in the glass tube, washing with 1-chloronaphthalene for 3 times, and drying to obtain FeMn @ C 60 A core-shell structure material.
In the step 1, the mol ratio of FeO to MnO is 1.2:1.
the molar ratio of carboxylic acid functional groups to metal oxide in glutaric acid in step 1 was 3.
Claims (5)
1. A silicon nitride wave-absorbing material is characterized by consisting of FeMn @ C 60 The core-shell structure material is compounded with silicon nitride;
the FeMn @ C 60 The preparation method of the core-shell structure material comprises the following steps:
step 1: 0.07mol of metal oxide, organic acid and 1L of C 60 Filling the saturated solution into a glass tube, exhausting air in the glass tube by using nitrogen, and sealing the tube, wherein the metal oxide consists of FeO and MnO;
step 2: putting the glass tube in the step 1 into an oven, heating to 160-200 ℃, keeping for 48-96h, and then cooling to room temperature at a cooling rate of 5 ℃/h;
and step 3: the solid product in the glass tube was filtered and used to prepare C 60 Washing with organic solvent of saturated solution for 3 times, and drying to obtain FeMn @ C 60 A core-shell structure material.
2. The silicon nitride wave-absorbing material of claim 1, wherein the molar ratio of FeO to MnO is 0.8-1.2:1.
3. the silicon nitride wave-absorbing material according to claim 1, wherein any one of heptafluorobutyric acid, hexafluoroglutaric acid and glutaric acid is used as the organic acid, and the molar ratio of carboxylic acid functional group to metal oxide in the organic acid is 0.5-3.
4. The silicon nitride wave-absorbing material of claim 1, wherein C in step 1 60 The organic solvent of the saturated solution is any one of chlorobenzene, toluene and 1-chloronaphthalene.
5. A preparation method of a silicon nitride wave-absorbing material adopts the silicon nitride wave-absorbing material of claims 1-4, and is characterized in that FeMn @ C is adopted 60 The core-shell structure material and silicon nitride are ground in a ball mill for 2-3 h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105032355A (en) * | 2015-08-24 | 2015-11-11 | 东华大学 | Preparation method for core-shell structure type carbon-coated magnetic nano particles |
| CN111320165A (en) * | 2018-12-13 | 2020-06-23 | 山东欧铂新材料有限公司 | Graphene oxide/carbonyl iron composite material, preparation method thereof and graphene-based wave-absorbing material |
| CN111517372A (en) * | 2020-05-11 | 2020-08-11 | 山西医科大学 | Fullerene coated Fe3O4Composite nano material and preparation method thereof |
| CN111970778A (en) * | 2020-08-25 | 2020-11-20 | 昆明理工大学 | Method and device for microwave high-flux sintering of powder block |
| CN115003142A (en) * | 2022-04-13 | 2022-09-02 | 哈尔滨工业大学（威海） | Preparation method of carbon-based/metal simple substance/boron nitride core-shell structure microwave absorbing material |
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- 2022-10-17 CN CN202211284570.9A patent/CN115449343B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105032355A (en) * | 2015-08-24 | 2015-11-11 | 东华大学 | Preparation method for core-shell structure type carbon-coated magnetic nano particles |
| CN111320165A (en) * | 2018-12-13 | 2020-06-23 | 山东欧铂新材料有限公司 | Graphene oxide/carbonyl iron composite material, preparation method thereof and graphene-based wave-absorbing material |
| CN111517372A (en) * | 2020-05-11 | 2020-08-11 | 山西医科大学 | Fullerene coated Fe3O4Composite nano material and preparation method thereof |
| CN111970778A (en) * | 2020-08-25 | 2020-11-20 | 昆明理工大学 | Method and device for microwave high-flux sintering of powder block |
| CN115003142A (en) * | 2022-04-13 | 2022-09-02 | 哈尔滨工业大学（威海） | Preparation method of carbon-based/metal simple substance/boron nitride core-shell structure microwave absorbing material |
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