CN1605414A - Method for preparing vacuum hotpressing autogeny titanium-base composite material - Google Patents
Method for preparing vacuum hotpressing autogeny titanium-base composite material Download PDFInfo
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- CN1605414A CN1605414A CN 200410043964 CN200410043964A CN1605414A CN 1605414 A CN1605414 A CN 1605414A CN 200410043964 CN200410043964 CN 200410043964 CN 200410043964 A CN200410043964 A CN 200410043964A CN 1605414 A CN1605414 A CN 1605414A
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000007731 hot pressing Methods 0.000 title claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 61
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 39
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000001125 extrusion Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 10
- 239000010959 steel Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 5
- 239000010439 graphite Substances 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims abstract 3
- 239000011812 mixed powder Substances 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 20
- 238000001192 hot extrusion Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 238000007872 degassing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000002787 reinforcement Effects 0.000 abstract description 7
- 239000012467 final product Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 19
- 239000000835 fiber Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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Abstract
真空热压反应自生钛基复合材料的制备方法，它涉及一种钛基复合材料的制备方法。本发明首先将Ti粉和B4C粉按重量比配好放入罐中，在罐中再加入钢球，将罐密封后在行星式球磨机上混合均匀，将混合好的粉末装入石墨模具进行冷压，再进行真空热压烧结，将烧结后的复合材料和挤压模具分开加热，复合材料单独加热至800－1400℃，保温一小时后放入保温温度为650℃的挤压模具中进行挤压，挤压比为16∶1，挤压成形即可。本发明将纤维增强钛基复合材料的制备工艺和颗粒增强钛基复合材料的制备工艺简化为一体，具有方法简单、制作容易，制作的钛基复合材料更加致密、增强体分布均匀、质量高的优点。
The invention discloses a method for preparing a self-generated titanium-based composite material by vacuum hot-pressing reaction, which relates to a method for preparing a titanium-based composite material. In the present invention, Ti powder and B 4 C powder are prepared according to the weight ratio and put into the tank, then steel balls are added into the tank, the tank is sealed and mixed evenly on a planetary ball mill, and the mixed powder is put into a graphite mold Carry out cold pressing, and then carry out vacuum hot pressing sintering, heat the sintered composite material and the extrusion mold separately, heat the composite material separately to 800-1400°C, keep it warm for one hour, and put it into the extrusion mold with a heat preservation temperature of 650°C Carry out extrusion, extrusion ratio is 16: 1, extrusion molding gets final product. The invention simplifies the preparation process of fiber-reinforced titanium-based composite material and the preparation process of particle-reinforced titanium-based composite material, and has the advantages of simple method, easy production, denser titanium-based composite material, uniform reinforcement distribution and high quality. advantage.
Description
Technical field:
The present invention relates to a kind of preparation method of titanium matrix composite, being specifically related to a kind of is the preparation method that titanium boride whisker and titanium carbide granule strengthen titanium matrix composite by titanium and boron carbide self-formed from reaction enhancing body.
Background technology:
Metal-base composites owing to characteristic with metal, also have the combination property that height ratio is strong, height ratio is firm, heat-resisting, wear-resisting and be subjected to extensive attention.In these composites, titanium or titanium alloy has characteristics such as light specific gravity, corrosion-resistant, resistance to oxidation intensity height, is a kind of alloy that can use under 450～650 ℃ of conditions and being favored.Titanium matrix composite has better resistance to elevated temperatures than Al, Mg based composites, has caused people's attention.Titanium matrix composite (TMCs) becomes the candidate material of superelevation velocity of sound aerospace vehicle and advanced aero-engine of future generation.TMCs is broadly divided into fiber and particle strengthens two classes.Fiber reinforcement TMCs is because the manufacturing process complexity costs an arm and a leg, and development is restricted, and only is used for Ministry of Aero-Space Industry's door on a small quantity.Granule intensified titanium-base compound material is compared with the fiber reinforcement titanium matrix composite, particle wild phase cost with use is low, and the designability of performance and function is strong, manufacturing process technology relatively economical simple possible, prepared material has isotropism, can obtain advantages such as near-net-shape part.The adding of particle wild phase has improved the normal temperature of titanium alloy and high temperature effectively than elastic modelling quantity, specific strength and creep resistance.But the plasticity of this titanium alloy material, toughness descend.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of vacuum hotpressing self-formed from reaction titanium matrix composite, this method is reduced to one with the preparation technology of fiber reinforcement titanium matrix composite and the preparation technology of granule intensified titanium-base compound material, not only fiber reinforcement titanium matrix composite complicated process of preparation, expensive shortcoming have been overcome but also have solved the deficiency that granule intensified titanium-base compound material plasticity, toughness descend, have method simple, make easily, the titanium matrix composite of making is fine and close more, strengthen the characteristics that body is evenly distributed, quality is high.Method of the present invention the steps include: that (1) mix powder: at first with Ti powder and B
4The C powder prepares by weight puts into jar, adds steel ball in jar again, and jar sealing back is mixed on planetary ball mill, and incorporation time is 10-14 hour; (2) vacuum-sintering: the powder that the mixes graphite jig of packing into is colded pressing, carry out vacuum heating-press sintering again, before the sintering under 500-800 ℃ of condition degasification 0.4-1 hour, carry out sintering then, sintering temperature is 1000-1250 ℃, and sintering pressure is 15-25MPa, and sintering time is 0.4-1 hour; (3) hot extrusion: with the separately heating of the composite behind the sintering and extrusion die, composite is heated to 800-1400 ℃ separately, and being incubated and putting into holding temperature after one hour is that 650 ℃ extrusion die pushes, and extrusion ratio is 16: 1, and extrusion molding gets final product.Described Ti powder and B
4The weight ratio of C powder is 160: 1; Described Ti powder and B
4The weight ratio of C is 100: 1; Described Ti powder and B
4The weight ratio of C powder is 50: 1; The granularity of described Ti powder is 1-50 μ m; Described B
4The granularity of C powder is 1-10 μ m; The diameter of described steel ball is 5-20mm; Described steel ball and Ti powder and B
4The ratio of grinding media to material of C powder is 1: 1; The present invention is reduced to one with the preparation technology of fiber reinforcement titanium matrix composite and the preparation technology of granule intensified titanium-base compound material, not only fiber reinforcement titanium matrix composite complicated process of preparation, expensive shortcoming have been overcome but also have solved the deficiency that granule intensified titanium-base compound material plasticity, toughness descend, have method simple, make easily, the titanium matrix composite of making is fine and close more, strengthen the advantage that body is evenly distributed, quality is high.Thereby improved its serviceability as structural material.
Description of drawings:
Fig. 1 is test Ti-B
4The DSC curve map of C mixture.
The specific embodiment:
Present embodiment is achieved in that (1) mix powder: at first with Ti powder and B
4The C powder prepares by weight puts into jar, adds steel ball in jar again, and jar sealing back is mixed on planetary ball mill, and incorporation time is 10-14 hour; Best mixing time is 12 hours, (2) vacuum-sintering: the powder that the mixes graphite jig of packing into is colded pressing, carry out vacuum heating-press sintering again, before the sintering under 500-800 ℃ of condition degasification 0.4-1 hour, best degasification temperature was 800 ℃; Carry out sintering then, sintering temperature is 1000-1250 ℃, and optimal sintering temperature is 1200 ℃; Sintering pressure is 15-25MPa, and sintering time is 0.4-1 hour; (3) hot extrusion: with composite behind the sintering and separately heating of extrusion die, composite is heated to 800-1400 ℃ separately, and optimal heat extruding heating-up temperature is 1150 ℃; Being incubated and putting into holding temperature after one hour is that 650 ℃ extrusion die pushes, and extrusion ratio is 16: 1, and extrusion molding gets final product.Described Ti powder and B
4The weight ratio of C powder is 160: 1; Described Ti powder and B
4The weight ratio of C is 100: 1; Described Ti powder and B
4The weight ratio of C powder is 50: 1; The granularity of described Ti powder is 1-50 μ m; Described B
4The granularity of C powder is 1-10 μ m; The diameter of described steel ball is 5-20mm; Described steel ball and Ti powder and B
4The ratio of grinding media to material of C powder is 1: 1.
In order to determine B
4The reaction optimum temperature of C and Ti has been tested Ti-B
4The DSC curve (see figure 1) of C mixture.As can be seen, Ti and B
4The reaction of C heat release occurs during since 900 ℃, illustrates that metal Ti begins and B
4Chemical reaction takes place in C.Along with the rising of temperature, it is maximum that exothermic peak to 1000 ℃ reaches, and can think Ti and B this moment
4The C reaction is the most violent, to 1250 ℃ of end.In order to make Ti and B
4C powder complete reaction, sintering temperature are chosen as 1200 ℃.The TiB whisker evenly generates in the titanium matrix, and diameter of whiskers has only about 0.075～0.3 μ m, and length is approximately 0.3～30 μ m.The TiC particle also evenly generates in the titanium matrix.Graphite jig is adopted in hot pressing.The extrusion die of using during hot extrusion, recipient adopts the 3Cr2W8V material, and the GCr15 material is adopted on die, pressure head and chassis.Because plasticity is relatively poor at normal temperatures, fragility is big for titanium matrix composite, be not easy to carry out plastic working, so thermal deformation is one of main mode of texturing of discontinuous enhancing titanium matrix composite.Optimal heat extrusion process: 1150 ℃, be incubated 1 hour, extrusion ratio 16: 1.Titanium is a close-packed hexagonal structure when being lower than 882 ℃, and slip system is fewer, and deformation ratio is difficulty.When hot extrusion, material is heated to 1150 ℃, titanium is in body-centered cubic structure, and slip system is many, and the plastic deformation ratio is easier to.If but temperature is too high, crystal grain is grown up easily, therefore, adopts suitable extrusion temperature, and is most important for the material for preparing.The density of sintered state material increases and reduces along with the volume fraction that strengthens body, and this is that the interfacial area that strengthens body and matrix increases because along with the volume fraction that strengthens body increases, thereby interface contact " loose " degree is increased.After hot extrusion, the porosity of material reduces, basically near solid density.Suitable hot extrusion technique parameter can obtain more satisfactory material.By the extruding attitude is mixed reinforced composite along the direction of extrusion (vertically) with perpendicular to the direction of extrusion microscopic examination of (laterally), after high temperature crimp, the evident characteristic of its institutional framework is that whisker has produced aligning along the direction of extrusion.The composite of sintered state is behind hot extrusion deformation, and material is fine and close more, strengthens body and is evenly distributed, thereby can obtain better institutional framework, has improved its serviceability as structural material.Result of study shows, the complete and B of Ti powder
4C reaction generates TiC and TiB, and the whisker of short fiber shape is TiB, is TiC and wait the axle shape or axle shape particle such as be similar to.By extrusion die reasonable in design and suitable extrusion process, can successfully squeeze out high-quality titanium matrix composite.
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| CN 200410043964 CN1605414A (en) | 2004-10-22 | 2004-10-22 | Method for preparing vacuum hotpressing autogeny titanium-base composite material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103443311A (en) * | 2011-03-22 | 2013-12-11 | 挪威钛组件公司 | Method for production of alloyed titanium welding wire |
| CN107130138A (en) * | 2017-05-19 | 2017-09-05 | 淮阴工学院 | The method of medical high abrasion titanium alloy composite material and 3D printing gradient in-situ nano complex phase anti-attrition medical titanium alloy |
| CN109317678A (en) * | 2018-11-20 | 2019-02-12 | 贵州大学 | A kind of synthetic method of ultra-vacuum in-situ hot-pressing sintering graphene-reinforced stone-titanium-based composite material |
| CN110592426A (en) * | 2019-08-27 | 2019-12-20 | 江苏大学 | Solid phase in situ reaction to generate high hardness and high temperature resistant TiC+TiB reinforced titanium matrix composite material and its preparation method |
| CN111822711A (en) * | 2020-07-16 | 2020-10-27 | 东北大学 | High-density titanium or titanium alloy parts and powder metallurgy filling method |
| CN113996797A (en) * | 2021-10-15 | 2022-02-01 | 中国兵器科学研究院宁波分院 | Low-cost recovery and powder preparation process for titanium alloy spherical coarse powder |
| CN115070038A (en) * | 2022-07-21 | 2022-09-20 | 西安稀有金属材料研究院有限公司 | In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof |
| CN117966052A (en) * | 2024-02-26 | 2024-05-03 | 哈尔滨工业大学 | Preparation method of titanium-based composite material with high strength and toughness and service performance at 700 DEG C |
-
2004
- 2004-10-22 CN CN 200410043964 patent/CN1605414A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103443311B (en) * | 2011-03-22 | 2016-03-09 | 挪威钛组件公司 | For the production of the method for titanium alloy welding wire |
| CN103443311A (en) * | 2011-03-22 | 2013-12-11 | 挪威钛组件公司 | Method for production of alloyed titanium welding wire |
| CN107130138A (en) * | 2017-05-19 | 2017-09-05 | 淮阴工学院 | The method of medical high abrasion titanium alloy composite material and 3D printing gradient in-situ nano complex phase anti-attrition medical titanium alloy |
| CN107130138B (en) * | 2017-05-19 | 2018-09-04 | 淮阴工学院 | The method of medical high abrasion titanium alloy composite material and 3D printing gradient in-situ nano complex phase anti-attrition medical titanium alloy |
| CN109317678A (en) * | 2018-11-20 | 2019-02-12 | 贵州大学 | A kind of synthetic method of ultra-vacuum in-situ hot-pressing sintering graphene-reinforced stone-titanium-based composite material |
| CN110592426B (en) * | 2019-08-27 | 2021-11-23 | 江苏大学 | High-hardness high-temperature-resistant TiC + TiB reinforced titanium-based composite material generated by solid-phase in-situ reaction and preparation method thereof |
| CN110592426A (en) * | 2019-08-27 | 2019-12-20 | 江苏大学 | Solid phase in situ reaction to generate high hardness and high temperature resistant TiC+TiB reinforced titanium matrix composite material and its preparation method |
| CN111822711A (en) * | 2020-07-16 | 2020-10-27 | 东北大学 | High-density titanium or titanium alloy parts and powder metallurgy filling method |
| CN113996797A (en) * | 2021-10-15 | 2022-02-01 | 中国兵器科学研究院宁波分院 | Low-cost recovery and powder preparation process for titanium alloy spherical coarse powder |
| CN113996797B (en) * | 2021-10-15 | 2023-09-15 | 中国兵器科学研究院宁波分院 | Low-cost recovery and re-pulverizing process for titanium alloy spherical coarse powder |
| CN115070038A (en) * | 2022-07-21 | 2022-09-20 | 西安稀有金属材料研究院有限公司 | In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof |
| CN115070038B (en) * | 2022-07-21 | 2022-11-04 | 西安稀有金属材料研究院有限公司 | In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof |
| CN117966052A (en) * | 2024-02-26 | 2024-05-03 | 哈尔滨工业大学 | Preparation method of titanium-based composite material with high strength and toughness and service performance at 700 DEG C |
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