CN114538447B - Low-cost rapid B4C powder surface modification method for inhibiting interface brittle phase of B4C/Al composite material - Google Patents
Low-cost rapid B4C powder surface modification method for inhibiting interface brittle phase of B4C/Al composite material Download PDFInfo
- Publication number
- CN114538447B CN114538447B CN202210283319.4A CN202210283319A CN114538447B CN 114538447 B CN114538447 B CN 114538447B CN 202210283319 A CN202210283319 A CN 202210283319A CN 114538447 B CN114538447 B CN 114538447B
- Authority
- CN
- China
- Prior art keywords
- powder
- composite material
- low
- surface modification
- cost
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/991—Boron carbide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1027—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention relates to a low-cost rapid B4C powder surface modification method for inhibiting a B4C/Al composite material interfacial brittle phaseAnd a low-cost rapid B4C powder surface modification method for inhibiting the interfacial brittle phase of the B4C/Al composite material. The invention aims to solve the problems of the prior B 4 B in C reinforced Al-based composite material 4 Sharp angle of C particles, B 4 And C and the metal Al matrix, the interface combination is poor, the interface reaction is serious, brittle intermetallic compounds are generated at the interface, and the like. The method comprises the following steps: will B 4 Placing the C powder in a heating device and simultaneously charging O 2 Heating the reaction temperature from room temperature to 500-800 ℃, and preserving the heat for 5-120 min to obtain the B with the core-shell structure 4 C@B 2 O 3 And (3) particles. The invention is used for preparing the B4C/Al composite material and solves the problem of B 4 C, when used as a reinforcement in an Al-based composite material, has a problem of poor interfacial bonding with an Al matrix and of suppressing the formation of an interfacial brittle phase.
Description
Technical Field
The invention relates to a low-cost rapid B4C powder surface modification method for inhibiting a B4C/Al composite material interfacial brittle phase.
Background
In nature, B 4 The hardness of C is as high as 30GPa, which is inferior to that of diamond and cubic boron nitride, and has the advantages of high temperature resistance, low density, strong thermal neutron absorption capacity, good thermal stability and the like, and is widely applied to the fields of tank bulletproof armor, control rods of nuclear reactors, neutron shielding and the like. However, micron-sized B obtained by mechanical disruption 4 The C powder particles have obvious sharp angle characteristics and have an insoluble or severe interface with the interface between the metal Al matrixReaction, decrease B 4 And C, enhancing the mechanical property of the Al-based composite material.
The interfacial properties determine the properties of the composite material and also determine the fracture mode of the composite material. B (B) 4 When the interface bonding between C and the metal Al matrix is weak, advanced destruction of the material can be caused. When chemical bonding exists at the interface, the bonding energy can be effectively improved, but the generation of brittle intermetallic compounds is often accompanied, and the brittle intermetallic compounds become crack sources in the deformation process, so that the mechanical properties of the material are reduced. B prepared by the cast-hot extrusion method is indicated in the patent No. US5722033 (A) under the name "Fabrication methods for metal matrix composites 4 The C/Al composite material has serious interface reaction to form AlB 2 、Al 4 C 3 、Al 4 BC、AlB 24 C 4 And the second phase is equal, so that the mechanical property of the material is reduced. Furthermore, B 4 The sharp corner structure of the powder C remains in the prepared composite material, and the sharp corner is the most serious stress concentration area, so that the cracking of the material is induced.
Thus, for B 4 The surface modification of the C powder is an effective solution to the key problem of its use as reinforcement in Al-based composites. In the related report, the method of coating the reinforcement or regulating the matrix composition is often used to avoid harmful interface reaction and improve wettability, but the operation process is complex and the cost is high. The patent number CN102730689a, entitled "surface treatment method of boron carbide powder" indicates that surface activation of boron carbide powder is achieved by an acid treatment process, which undoubtedly aggravates chemical reaction of boron carbide with aluminum alloy, forming brittle phase that is liable to fracture. Metal composite material of Harbin university and engineering institute realize B 4 Surface modification of C powder to form B on its surface by controlling the temp. and time of high-temp. oxidation process 2 O 3 The phase can effectively improve the mechanical property, but B is under the condition of low temperature and shorter oxidation time 4 B of powder surface 2 O 3 The phase distribution is uneven, and the high-temperature and long-time oxidation process can cause the problems of high cost and difficult opening of the mutual adhesion of the powder.
Disclosure of Invention
The invention aims to solve the problems of the prior B 4 B in C reinforced Al-based composite material 4 Sharp angle of C particles, B 4 And C and the metal Al matrix, the interface combination is poor, the interface reaction is serious, brittle intermetallic compounds are generated at the interface, and the like. And provides a low-cost rapid B4C powder surface modification method for inhibiting the interfacial brittle phase of the B4C/Al composite material.
The low-cost rapid B4C powder surface modification method for inhibiting the interfacial brittle phase of the B4C/Al composite material comprises the following steps:
will B 4 Placing the C powder in a heating device and simultaneously charging O 2 Heating the reaction temperature from room temperature to 500-800 ℃, and preserving the heat for 5-120 min at the temperature of 500-800 ℃ to obtain the B with the core-shell structure 4 C@B 2 O 3 Particles; charging O 2 The concentration of (2) is 21% -90%.
The invention has the beneficial effects that:
the invention can be applied to the B 4 The surface of the powder particles of the C form a layer of compact B which is uniformly distributed 2 O 3 A coating layer, and B 2 O 3 The thickness of the coating layer is controllable and is connected with the core B 4 C has good interfacial bonding. Modified B 4 C@B 2 O 3 The particles can be used as reinforcement in the Al-based composite material to effectively improve interface bonding and inhibit the formation of brittle intermetallic compounds between the particles and an Al matrix, and have wide application prospect. The invention has the advantages of simple equipment and operation, strong controllability, low cost, high yield and the like.
Drawings
FIG. 1 is untreated raw B 4 SEM (scanning electron microscope) photograph of the C powder;
FIG. 2 is B 4 C typical SEM (scanning electron microscope) photograph after the surface modification treatment of the powder particles;
FIG. 3 is B 4 C typical TEM (transmission electron microscope) photograph of the powder particles after surface modification treatment.
Detailed Description
The first embodiment is as follows: the low-cost rapid B4C powder surface modification method for inhibiting the interfacial brittle phase of the B4C/Al composite material in the embodiment specifically comprises the following steps:
will B 4 Placing the C powder in a heating device and simultaneously charging O 2 Heating the reaction temperature from room temperature to 500-800 ℃, and preserving the heat for 5-120 min at the temperature of 500-800 ℃ to obtain the B with the core-shell structure 4 C@B 2 O 3 Particles; charging O 2 The concentration of (2) is 21% -90%.
The present embodiment is based on chemical reaction equation B 4 C+4O 2 ＝2B 2 O 3 +CO 2 And the thermodynamics of the reaction are known, B 4 The powder particles of C can be mixed with O at a set temperature 2 The chemical reaction takes place, the invention leads O to be formed by controlling the temperature, the time and the atmosphere condition 2 The molecule can be combined with B 4 C powder particle surface B 4 The C molecules react to oxidize the C molecules layer by layer to form compact B 2 O 3 The film is obtained to obtain the core-shell structure B 4 C@B 2 O 3 And (3) particles. Thus, pair B is realized 4 And C, surface modification of the powder particles. At the same time, the shell B can be realized by controlling the reaction temperature, time and atmosphere conditions 2 O 3 And (3) controlling the layers.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the B is 4 And C, carrying out surface activation treatment on the powder: the concrete process is that B 4 Dispersing the powder C in a dilute hydrochloric acid aqueous solution for pickling, standing, washing with deionized water, performing suction filtration, and drying to obtain surface-activated B 4 C, powder; b (B) 4 The mass ratio of the powder C to the dilute hydrochloric acid aqueous solution is 1 (3-5). The other is the same as in the first embodiment.
B of the present embodiment 4 The powder C is a commercial product, and the purpose of acid washing is to remove B 4 Impurity on the surface of the C powder.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the heating device is a sintering furnace. The other is the same as the first or second embodiment.
The specific embodiment IV is as follows: this embodiment differs from one of the first to third embodiments in that: heating the reaction temperature from room temperature to 500-650 ℃, and preserving heat for 10-60 min at the temperature of 500-650 ℃; charging O 2 The concentration of (2) is 25% -70%. The other is the same as in one of the first to third embodiments.
Fifth embodiment: this embodiment differs from one to four embodiments in that: heating the reaction temperature from room temperature to 500-650 ℃, and preserving heat for 30min at the temperature of 500-650 ℃; charging O 2 The concentration of (2) was 21%. The others are the same as in one to one fourth embodiments.
Specific embodiment six: this embodiment differs from one to four embodiments in that: heating the reaction temperature from room temperature to 600 ℃, and preserving the heat at 600 ℃ for 30min; charging O 2 The concentration of (2) is 30% -50%. The others are the same as in one to one fourth embodiments.
Seventh embodiment: this embodiment differs from one to four embodiments in that: heating the reaction temperature from room temperature to 500-650 ℃, and preserving heat for 10-60 min at the temperature of 500-650 ℃; charging O 2 The concentration of (2) is 25% -60%. The others are the same as in one to one fourth embodiments.
Eighth embodiment: this embodiment differs from one to four embodiments in that: b of the core-shell structure 4 C@B 2 O 3 The core of the particle is B 4 C. The outer shell is B 2 O 3 ，B 2 O 3 In an amorphous state; b (B) 4 C and B 2 O 3 Interface bonding of (a) is a tight bonding on atomic scale according to initial B 4 Average diameter of powder particles C, B 2 O 3 The thickness of the coating layer is controlled between 5nm and 800nm. The others are the same as in one to one fourth embodiments.
Detailed description nine: this embodiment differs from one to four embodiments in that: the B is 2 O 3 The thickness of the coating layer is 5 nm-100 nm. The others are the same as in one to one fourth embodiments.
Detailed description ten: this embodiment differs from one to four embodiments in that: the B is 2 O 3 The thickness of the coating layer is 5 nm-300 nm. The others are the same as in one to one fourth embodiments.
The effect of the invention was verified by the following tests:
embodiment one: the low-cost rapid B4C powder surface modification method for inhibiting the interfacial brittle phase of the B4C/Al composite material comprises the following steps:
will B 4 Dispersing the powder C in a dilute hydrochloric acid aqueous solution for pickling, standing, washing with deionized water, performing suction filtration, and drying to obtain surface-activated B 4 C, powder; b (B) 4 The mass ratio of the powder C to the dilute hydrochloric acid aqueous solution is 1:4;
b activating the surface 4 Placing the C powder in a heating device and simultaneously charging O 2 Heating the reaction temperature from room temperature to 500 ℃, and preserving the heat for 30min at the temperature of 500 ℃ to obtain the B with the core-shell structure 4 C@B 2 O 3 Particles; charging O 2 Is 25%; then adopting a powder metallurgy method to prepare the B with the volume fraction of 15 percent 4 C/2024Al composite.
FIG. 1 is a diagram of acid washed B 4 Powder C, as can be seen from the figure, B 4 The powder C has smooth surface and obvious sharp corners; FIG. 2 is a surface modified B 4 C powder, forming core-shell structure, inside B 4 The powder C is coated with an oxide layer, and FIG. 3 further illustrates B 4 The oxide layer "shell" on the surface of the C powder is amorphous.
Embodiment two:
placing the powder into an O-charge 2 Heating in a heating furnace with the concentration of 60 percent at 500 ℃ for 30 minutes, and then preparing B with the volume fraction of 15 percent by adopting a powder metallurgy method 4 C/2024Al composite.
Embodiment III:
placing the powder into an O-charge 2 Heating in a heating furnace with a concentration of 25%, heating at 600deg.C for 30min, and powder metallurgyPreparation of B with 15% volume fraction 4 C/2024Al composite.
Embodiment four:
placing the powder into an O-charge 2 Heating in a heating furnace with the concentration of 25 percent at 600 ℃ for 5 minutes, and then preparing B with the volume fraction of 15 percent by adopting a powder metallurgy method 4 C/2024Al composite.
The composite material prepared by the embodiment is subjected to elastic modulus and mechanical property test, and the following table shows the test data of the composite material in two embodiment:
Claims (5)
1. the low-cost rapid B4C powder surface modification method for inhibiting the B4C/Al composite material interfacial brittleness phase is characterized by comprising the following steps of:
will B 4 Placing the C powder in a heating device and simultaneously charging O 2 Heating the reaction temperature from room temperature to 600 ℃, and preserving the heat for 30min at the temperature of 600 ℃ to obtain the B with the core-shell structure 4 C@B 2 O 3 Particles; charging O 2 The concentration of (2) is 30% -50%; the B is 4 And C, carrying out surface activation treatment on the powder: the concrete process is that B 4 Dispersing the powder C in a dilute hydrochloric acid aqueous solution for pickling, standing, washing with deionized water, performing suction filtration, and drying to obtain surface-activated B 4 C, powder; b (B) 4 The mass ratio of the powder C to the dilute hydrochloric acid aqueous solution is 1 (3-5).
2. The method for low-cost and rapid modification of B4C powder surface to suppress interfacial brittle phases of B4C/Al composites according to claim 1, wherein the heating device is a sintering furnace.
3. A suppression B4C/Al according to claim 1A low-cost rapid B4C powder surface modification method for a composite material interfacial brittle phase is characterized by comprising the following steps of 4 C@B 2 O 3 The core of the particle is B 4 C. The outer shell is B 2 O 3 ，B 2 O 3 In an amorphous state; b (B) 4 C and B 2 O 3 Interface bonding of (a) is a tight bonding on atomic scale according to initial B 4 Average diameter of powder particles C, B 2 O 3 The thickness of the coating layer is controlled to be 5-800 nm.
4. The method for low-cost rapid modification of B4C powder to suppress interfacial brittle phases of B4C/Al composites according to claim 3, wherein the B 2 O 3 The thickness of the coating layer is 5 nm-100 nm.
5. The method for low-cost rapid modification of B4C powder to suppress interfacial brittle phases of B4C/Al composites according to claim 3, wherein the B 2 O 3 The thickness of the coating layer is 5 nm-300 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210283319.4A CN114538447B (en) | 2022-03-22 | 2022-03-22 | Low-cost rapid B4C powder surface modification method for inhibiting interface brittle phase of B4C/Al composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210283319.4A CN114538447B (en) | 2022-03-22 | 2022-03-22 | Low-cost rapid B4C powder surface modification method for inhibiting interface brittle phase of B4C/Al composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114538447A CN114538447A (en) | 2022-05-27 |
| CN114538447B true CN114538447B (en) | 2023-05-23 |
Family
ID=81665805
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210283319.4A Active CN114538447B (en) | 2022-03-22 | 2022-03-22 | Low-cost rapid B4C powder surface modification method for inhibiting interface brittle phase of B4C/Al composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114538447B (en) |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4718941A (en) * | 1986-06-17 | 1988-01-12 | The Regents Of The University Of California | Infiltration processing of boron carbide-, boron-, and boride-reactive metal cermets |
| JP4969372B2 (en) * | 2007-02-27 | 2012-07-04 | 京セラ株式会社 | Boron carbide powder, method for producing the same, boron carbide molded body and boron carbide sintered body using the same |
| CN104164601B (en) * | 2014-08-13 | 2016-02-24 | 扬州峰明金属制品有限公司 | A kind of heat resistance magnesium alloy of polynary enhancing and manufacture method thereof |
| CN108018451A (en) * | 2016-11-04 | 2018-05-11 | 中国科学院金属研究所 | Al bases B is quickly prepared under a kind of low temperature4The method of C composite |
| CN111349805B (en) * | 2020-03-23 | 2021-11-09 | 中国科学院金属研究所 | High-temperature structure function integrated Mg (Al) B2And B4C-co-enhanced aluminum-based neutron absorption material and preparation method thereof |
| CN112341201A (en) * | 2020-11-10 | 2021-02-09 | 宜兴市丁山耐火器材有限公司 | Self-bonding silicon carbide refractory material and preparation method thereof |
-
2022
- 2022-03-22 CN CN202210283319.4A patent/CN114538447B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN114538447A (en) | 2022-05-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106435323B (en) | A kind of oxide dispersion intensifying ODS high-entropy alloys and preparation method thereof | |
| JP2022517021A (en) | Method of preparing metal material or metal composite material | |
| CN108585897B (en) | Refractory metal high-temperature oxidation-resistant Si-Mo-YSZ coating and preparation method thereof | |
| CN107142398B (en) | A kind of Al4C3Modification on Al based composites and preparation method thereof | |
| CN107034386B (en) | A kind of anti-fused salt corrosion high-temperature composite material and molten salt reactor core structure part | |
| CN108913928A (en) | A method of preparing oxide dispersion intensifying carbon/carbon-copper composite material | |
| CN112226662B (en) | Double-nanostructure tungsten alloy with good high-temperature stability and preparation method and application thereof | |
| CN109797309A (en) | A kind of structure-function integration neutron absorber material High-Temperature Strengthening method | |
| CN108570572A (en) | A kind of nano oxide dispersion strengthens Cu-Ti alloys and preparation method thereof | |
| CN107164661A (en) | A kind of high corrosion resistance aluminum alloy composite and preparation method thereof | |
| CN110306074B (en) | Discharge plasma sintering preparation method of CERMET fuel pellet | |
| CN114574789B (en) | Silicon carbide fiber, medium-high entropy ceramic reinforced metal matrix composite material and preparation method | |
| CN106282633A (en) | The preparation method of one kind garnet structure enhanced ceramic aluminum/cuprio high damping composite material | |
| CN114538447B (en) | Low-cost rapid B4C powder surface modification method for inhibiting interface brittle phase of B4C/Al composite material | |
| CN107299269B (en) | A kind of W-Cr-Al composite material and preparation method of resistance to high temperature oxidation | |
| CN114591084B (en) | Method for rapidly preparing compact TiC ceramic at low temperature | |
| CN108754350A (en) | A kind of oxide dispersion intensifying steel and preparation method thereof | |
| CN106876042A (en) | A kind of method that high-temperature sintering process prepares niobium aluminium superconductor | |
| Liu et al. | Effect of Al2O3np on the Properties and Microstructure of B4Cp/Al Composites | |
| CN108447576B (en) | Preparation method of MAX phase improved uranium dioxide pellet | |
| CN115652161B (en) | Preparation method of polymer carbonized porous coated nano carbide strengthening and toughening molybdenum alloy | |
| CN105970608B (en) | A method of titanium carbide is prepared based on slurry cladding process and coats carbon fiber | |
| Qian et al. | Improving the Cyclic‐Oxidation Resistance of Ti3AlC2 at 550° C and 650° C by Preoxidation at 1100° C | |
| JP3882114B2 (en) | Neutron multiplier for fusion reactor | |
| CN111809098B (en) | Composite material for spent fuel storage and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |