CN1261611C - Method for preparing tension specimen made from composite material of Ti alloy base enhanced by continuous SiC fibre - Google Patents
Method for preparing tension specimen made from composite material of Ti alloy base enhanced by continuous SiC fibre Download PDFInfo
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- CN1261611C CN1261611C CN 03110901 CN03110901A CN1261611C CN 1261611 C CN1261611 C CN 1261611C CN 03110901 CN03110901 CN 03110901 CN 03110901 A CN03110901 A CN 03110901A CN 1261611 C CN1261611 C CN 1261611C
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Abstract
The present invention discloses a method for preparing continuous SiC fiber reinforcement Ti alloy base composite material tensile samples. The method comprises the following operating procedures: (1) continuous SiC fiber reinforcement Ti alloy base composite material precursor wires as raw materials are wound on a circular stainless steel cylinder by a winding machine set, and the surface of the wires is coated to be flat and fixed with agglomerants so that a precast slab is manufactured; then, the precast slab is tailored for use; (2)before the precast slab is processed by hot pressing, firstly, metal plates are placed on the upper-lower sides of the stacking layer of the precast slab; the precast slab with the metal plates are put into a mold, and the mold is put into a hot pressing furnace; the agglomerants are processed by thermal decomposition and degassing at a temperature interval of 250 DEG C to 600 DEG C so that the agglomerants are cleaned; a slab sample is obtained by heating up to a hot pressing temperature and pressurizing; (3)the slab sample is treated by wire-cut; the working section metal slabs of the sample are treated, and the clamping parts are processed by protective treatment. By the method of the present invention, the property of the material is clearly and accurately characterized, and the arrangement evenness is guaranteed.
Description
Technical field
The present invention relates to the Composite Preparation technology, specifically a kind of method for preparing continuous SiC fiber reinforced Ti alloy-based composite stretching sample.
Background technology
The demand for development high-temperature material of Aeronautics and Astronautics and space technology has less dense, more high strength and elevated operating temperature more.Yet therefore conventional high-temperature materials such as titanium alloy and nickel base superalloy must develop the new type high temperature material, to satisfy the requirement that the aircraft engine working temperature improves constantly near its maximum operation (service) temperature.It is a developing direction of novel high-performance space structure material that continuous SiC fiber strengthens titanium matrix composite.The SiC fiber has high specific strength, high ratio modulus and well thermostability, feature performance benefit such as anticorrosive and wear-resisting, therefore can be used as the enhancing body of high-temperature material, to improve the use temperature and the mechanical property of material.Continuous SiC fiber strengthens titanium matrix composite can significantly improve creep resistance and rigidity, has broad application prospects.
The test of continuous SiC fiber reinforced Ti alloy-based composite performance accuracy is a raw material with the continuous SiC fiber reinforced Ti alloy-based composite precursor wire generally, adopts tubulose or tabular stretching sample.For tabular stretching sample, exist the inhomogeneity problem of arranging, adopt random alignment mostly, and the shape of stretching sample, size all there are certain influence to the accuracy of performance test.In the tensile process, retained part all can cause sample from the fracture of anchor clamps front end to the damage of sample, thereby can't reflect the actual performance of material.
Summary of the invention
In order to overcome above-mentioned deficiency, the purpose of this invention is to provide a kind of method for preparing continuous SiC fiber reinforced Ti alloy-based composite stretching sample, adopt the inventive method can know the performance of exosyndrome material exactly, guarantee to arrange homogeneity, and provide a feasible technological line for the preparation of massive material.
To achieve these goals, technical scheme of the present invention is to operate as follows:
1) with the coiling unit, be raw material with the continuous SiC fiber reinforced Ti alloy-based composite precursor wire, the mode by nearly solid matter is wound on the circular stainless steel cylinder, with binding agent the surface of silk is coated with flatly again, fixes, and makes precoated plate; According to the size of mould, the precoated plate of making is carried out cutting then, compound in order to hot pressing;
2) before hot pressing, earlier put metal sheet in the top and bottom that precoated plate stacks layer, put into mould then, the hot pressing furnace of packing into, in 250 ℃～600 ℃ intervals binding agent is carried out the thermolysis degasification, remove binding agent; After degasification finishes, be warmed up to hot pressing temperature and pressurize, tabular sample;
3) by user's desired size described tabular sample is carried out the line cutting, make desired shape, working zone to sample removes the metal sheet processing, retained part is protected processing then, guarantees that sample ruptures at working zone, so that truly reflect the performance of material;
Wherein: complete in order to make binder decomposed, described thermolysis degasification is carried out in two stages: i.e. the degassing procedure of two differing tempss, different time, and the first step: the degasification temperature is 250 ℃～420 ℃, the time is 0.5 hour～4 hours; Second step: the degasification temperature is 420 ℃～600 ℃, and the time is 0.3 hour～3 hours;
For the superplasticity that made full use of matrix flows, described intensification pressure method is: be warming up to 650 ℃～850 ℃ at 10 minutes～20 minutes with interior earlier, be incubated 10 minutes～20 minutes, be forced into 2Mpa～14Mpa, pressurize, insulation again 0.1 hour～1 hour; And then in 0.1 hour～1 hour, be warming up to 850 ℃～950 ℃, and be incubated 10 minutes～20 minutes, be pressurized between 5Mpa～100Mpa pressurize, insulation 0.5 hour～6 hours again;
Described binding agent adopts dimethylbenzene and gathers bright ethene or polymethylmethacrylate and acetone formulated; Wherein: described dimethylbenzene and poly-bright ethene preparation part by weight are 1: 1, and polymethylmethacrylate and acetone preparation part by weight are 1: 15～20; Step 2) described plate thickness is 20 μ m～500 μ m, and described metal sheet can adopt tinsel, and quantity is 1～5; The layer structure that described precursor wire is wound on the circular stainless steel cylinder can be monolayer alignment, can also arrange for multilayer.
The present invention has following advantage:
1. guarantee to arrange homogeneity.Adopt the inventive method precursor wire to arrange and be very neatly arranged, by pyrolysis technique, used binding agent is easy to be removed, and can not pollute sample.
2. can know the performance of exosyndrome material exactly.In the hot pressing, make full use of the superplasticity flow principles of matrix, reduced hot pressing temperature, reduced pressure, thereby avoided the damage of over-drastic surface reaction and fiber, guaranteed the compactness of material simultaneously again; The present invention adds metal sheet (as tinsel) in the upper and lower surface of material, in the tensile process, has protected material, makes it not to be subjected to external damage, allows fracture appear at working zone, the performance of having shown material truly.
3. the present invention provides a feasible technological line for the preparation of massive material.
Description of drawings
Fig. 1 is the embodiment of the invention 1 stress strain curve.
Embodiment
Below in conjunction with drawings and Examples in detail the present invention is described in detail.
Embodiment 1
Present embodiment adopts J801-7A/ZF coiling unit and ZRY45B vacuum hotpressing stove, and the technological process of experiment is as follows:
1) with the coiling unit, with the continuous SiC fiber reinforced Ti alloy-based composite precursor wire is raw material, mode winding of single layer by nearly solid matter is to the stainless steel cylinder of circle, be coated with the surface of silk flat with dimethylbenzene and poly-bright ethene with the binding agent of part by weight preparation in 1: 1 again, fixing, make precoated plate; According to the size of mould the precoated plate of making is carried out cutting then, compound in order to hot pressing;
2) before hot pressing, be stacked together at precoated plate earlier, the top and bottom storing thickness that stacks layer is 5 of 40 μ m tinsels, put into mould again, the hot pressing furnace of packing into then carries out the thermolysis degasification in 250 ℃～600 ℃ intervals to binding agent, in order to make binder decomposed complete, described thermolysis degasification is carried out in two stages: i.e. the degassing procedure of two differing tempss, different time, to remove binding agent (specifically :) 350 ℃ of degasification 2 hours, 500 ℃ of degasification 1 hour; After degasification finishes, be warmed up to hot pressing temperature and pressurization (specifically: be warming up to 650 ℃ at 10 minutes with interior earlier, be incubated 10 minutes, being forced into 2Mpa, pressurize, soaking time again is 0.5 hour, be raised to 850 ℃ again in 1 hour, be incubated 20 minutes, plus-pressure is 50Mpa, pressurize, insulation 2 hours again), here make full use of the superplasticity flow principles of matrix, made tabular sample matrix material;
3) will by user's desired size (length overall 70mm, the wide 9mm of retained part, work segment length 20, wide 4mm) sample be carried out the line cutting behind the described tabular sample; make the required writing board shape of user; working zone to sample removes the tinsel processing and protects processing (that is: the tinsel on working zone two sides to be removed to retained part then; the tinsel that thickness is 100 μ m is respectively pasted on the retained part two sides), obtain the sample that stretches.
The preparation of the used continuous SiC fiber reinforced Ti alloy-based composite precursor wire of present embodiment is: be matrix with the continuous SiC fiber, be wrapped in it with the Ti alloy and be on the specimen holder of target, put into vacuum chamber that first forvacuum feeds argon gas again; Rotary substrate carries out carrying out magnetron sputtering after the preheating to matrix; Processing parameter is: forvacuum makes vacuum tightness to 3.0 * 10
-4Magnetron sputtering power 2530W; Feed argon gas, make vacuum tightness reach 0.8Pa; The matrix movement velocity is 11 rev/mins; Substrate temperature is controlled at 260 ℃; Target-cardinal distance is 40mm.
On the stretching experiment machine described stretching sample has been carried out the tensile property test, fracture occurs in working zone, has reflected the performance of material really.Adopt the performance higher (the present embodiment sample strength reaches 1611Mpa) of the inventive method gained specimen material, its stress-strain(ed) curve as shown in Figure 1.
Embodiment 2
Difference from Example 1 is:
With the continuous SiC fiber reinforced Ti alloy-based composite is precursor wire, and the mode by nearly solid matter is wound on the circular stainless steel cylinder by 3 layers, and binding agent also can adopt polymethylmethacrylate and acetone formulated, and both part by weight are 1: 20;
The top and bottom storing thickness that stacks layer at precoated plate is 1 of 400 μ m tinsel; Concrete operations when binding agent is carried out the thermolysis degasification are: 250 ℃ of degasification 4 hours, again 600 ℃ of degasification 3 hours; For the superplasticity that made full use of matrix flows, after degasification finishes, be warmed up to hot pressing temperature and pressurize, be specially: earlier 20 minutes with interior 650 ℃ of the hot pressing temperatures that are warmed up to, be incubated 20 minutes, plus-pressure 14Mpa, pressurize, insulation 0.1 hour; Be warming up to 950 ℃ then in 10 minutes, be incubated 10 minutes, be pressurized to 100Mpa, pressurize, insulation 0.5 hour make tabular stretching sample composites.
Adopt the performance of the inventive method gained specimen material higher, its result is identical with embodiment 1.
Claims (4)
1. method for preparing continuous SiC fiber reinforced Ti alloy-based composite stretching sample is characterized in that and can operate as follows:
1) with the coiling unit, be raw material with the continuous SiC fiber reinforced Ti alloy-based composite precursor wire, the mode by nearly solid matter is wound on the circular stainless steel cylinder, with binding agent the surface of silk is coated with flatly again, fixes, and makes precoated plate; Cutting then, compound in order to hot pressing;
2) before hot pressing, earlier put metal sheet in the top and bottom that precoated plate stacks layer, put into mould then, the hot pressing furnace of packing into, in 250 ℃～600 ℃ intervals binding agent is carried out the thermolysis degasification, remove binding agent; After degasification finishes, be warmed up to hot pressing temperature and pressurize, tabular sample;
3) described tabular sample is carried out the line cutting, make desired shape, the working zone to sample removes the metal sheet processing, protects processing to get final product to retained part then;
Described thermolysis degasification is carried out in two stages: the first step: the degasification temperature is 250 ℃～420 ℃, and the time is 0.5 hour～4 hours; Second step: the degasification temperature is 420 ℃～600 ℃, and the time is 0.3 hour～3 hours;
Described intensification pressure method is: earlier be warming up to 650 ℃～850 ℃ at 10 minutes～20 minutes with interior, be incubated 10 minutes～20 minutes, be forced into 2Mpa～14Mpa, pressurize, insulation again 0.1 hour～1 hour; And then in 0.1 hour～1 hour, be warming up to 850 ℃～950 ℃, and be incubated 10 minutes～20 minutes, be pressurized between 5Mpa～100Mpa pressurize, insulation 0.5 hour～6 hours again.
2. according to the described method for preparing continuous SiC fiber reinforced Ti alloy-based composite stretching sample of claim 1, it is characterized in that: described binding agent employing polymethylmethacrylate and acetone are formulated; Polymethylmethacrylate and acetone preparation part by weight are 1: 15～20.
3. according to the described method for preparing continuous SiC fiber reinforced Ti alloy-based composite stretching sample of claim 1, it is characterized in that: step 2) described plate thickness is 20 μ m～500 μ m.
4. according to the described method for preparing continuous SiC fiber reinforced Ti alloy-based composite stretching sample of claim 1, it is characterized in that: the layer structure that described precursor wire is wound on the circular stainless steel cylinder can be monolayer alignment, can also arrange for multilayer.
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| CN 03110901 CN1261611C (en) | 2003-01-20 | 2003-01-20 | Method for preparing tension specimen made from composite material of Ti alloy base enhanced by continuous SiC fibre |
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| CN 03110901 CN1261611C (en) | 2003-01-20 | 2003-01-20 | Method for preparing tension specimen made from composite material of Ti alloy base enhanced by continuous SiC fibre |
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| CN1261611C true CN1261611C (en) | 2006-06-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101750239B (en) * | 2008-12-22 | 2011-12-21 | 西安飞机工业（集团）有限责任公司 | Method for processing composite material test plate |
| CN101787505B (en) * | 2010-02-12 | 2011-12-21 | 中国航空工业集团公司北京航空制造工程研究所 | Preparation method of continuous fiber reinforcing titanium matrix composite |
| CN102252896A (en) * | 2011-04-21 | 2011-11-23 | 西北工业大学 | Test sample with two straight waist-shaped side faces and for testing tension and compression property of composite material laminated thick plate |
| US9464975B2 (en) * | 2014-08-13 | 2016-10-11 | The Boeing Company | Composite test specimen |
| CN104359729A (en) * | 2014-10-29 | 2015-02-18 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for reducing notch sensitivity in mechanical property test of titanium based intermetallic compounds |
| CN105181377B (en) * | 2015-08-27 | 2018-10-09 | 西南大学 | Sampling method on 20~50 ㎜ thickness aluminum alloy hot rolling plate thickness directions |
| CN106591744B (en) * | 2015-10-15 | 2019-01-29 | 中国航空制造技术研究院 | A kind of composite material die for preparation and preparation method |
| CN114013129A (en) * | 2021-10-09 | 2022-02-08 | 中国航发北京航空材料研究院 | Preparation method of continuous SiC fiber reinforced titanium-based composite material plate |
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