CN102815957A - Nonferrous metal alloy-toughened aluminum nitride ceramic-based composite material and preparation method thereof - Google Patents
Nonferrous metal alloy-toughened aluminum nitride ceramic-based composite material and preparation method thereof Download PDFInfo
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- 239000002184 metal Substances 0.000 title abstract description 17
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title abstract description 12
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 7
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Abstract
The invention discloses a nonferrous metal alloy-toughened aluminum nitride ceramic-based composite material and a preparation method thereof. An aluminum nitride blank comprises aluminum nitride, yttrium oxide, alumina and carbon black according to a weight part ratio. The preparation method comprises the following steps of heating in a nitrogen atmosphere to obtain an aluminum nitride blank having porosity less than 43%, heating a die-casting machine, heating a copper alloy until melting, pouring the melted copper alloy into a cavity for receiving the aluminum nitride blank, pressing the melted copper alloy into the aluminum nitride blank by a pressing head, cooling a casted block, and separating the casted block from a mold. The nonferrous metal alloy-toughened aluminum nitride ceramic-based composite material has the characteristics of high elasticity modulus, high strength, high hardness, excellent frictional property and low thermal expansion coefficient. Compared with the traditional aluminum nitride ceramic materials, the nonferrous metal alloy-toughened aluminum nitride ceramic-based composite material has higher fracture toughness, and can be widely used for friction and wearing structural members of electromechanical special equipment, heat-resistant corrosion-resistant structural members of pressure-bearing special equipment, aerospace structural members and automobile structural members.
Description
Technical field
The present invention relates to a kind of metal toughening ceramic based composites and preparation method, be specifically related to toughness reinforcing aluminium nitride ceramics based composites of a kind of non-ferrous metal alloy and preparation method.
Background technology
The intensity of stupalith is high, hardness is big, high temperature resistant, anti-oxidant; Resistance to wear under the high temperature, chemical resistance is good, and thermal expansivity and proportion are little; These excellent material properties are that general common metal material, macromolecular material and matrix material thereof are not available; It more and more receives people's attention. and countries in the world all bar structure pottery regard that revolution has the hi tech and new material of significant role and gives primary study and development to futurity industry as, and have carried out the extensive hot machine research project of pyroceramic such as ceramic automobile mover, oil motor and aircraft engine in succession, ceramic heat occurred. still; Because the deadly defect-fragility of stupalith itself; Do to lack enough safeties when structured material uses, thereby the fragility of improving stupalith has become one of stupalith field problem demanding prompt solution.
The toughness reinforcing continuous ceramic matric composite of metal is a kind of ceramic/metal composite materials with brand-new compound enhancing mode that occurs in recent years.In this matrix material, the matrix ceramic enhancement phase has the internal structure of three-dimensional communication, thereby plays the metal filled in the space of ceramic skeleton of toughening effect, and it spatially also is a three-dimensional communication.Realize that this composite structure need be different from traditional composite material forming and technology of preparing.This composite structure makes continuous ceramic matric composite can pottery and metal performance characteristics separately more be retained in the final matrix material; Simultaneously, also shown and the different performance of conventional composite materials (particulate reinforced composite, fibre reinforced composites etc.), be with a wide range of applications.The classical production process of ceramic matric composite mainly contains (1), slurry method of impregnation; (2), sol-gel and polymkeric substance pyrogenic silica; (3), direct melt oxidation method; (4) melt infiltration method;
(1), slurry method of impregnation
The slurry method of impregnation is used at most on manufacturing macrofiber reinforcement glass and glass-ceramic and lower melting point ceramic composite at present, and the most effective.When hot pressed sintering temperature should near or a little more than the softening temperature of glass, the generation that helps VISCOUS FLOW like this is to promote the carrying out of densification process.But this method is but very ineffective to some now used non-oxide ceramicses; Because pottery is difficult to take place VISCOUS FLOW under the high temperature, thereby can only just can make matrix fine and close through improving hot pressing temperature, but along with the rising of hot pressing temperature; Reaction aggravation between fiber and matrix; Reduce because of fiber oxidation and fiber grain growth make fibre property, simultaneously, can produce scratch and physical abuse to fiber under the infusibility hard particles pressure.In addition, this method can only be made the matrix material of one dimension or two-dimensional fiber reinforcement, adds the restriction of process aspects such as hot pressed sintering, also can only make the structural part of some simple shape.Referring to king zero woods, < < special cermacis>>, press of Zhongnan Polytechnic Univ, 1994.
(2), sol-gel and polymkeric substance pyrogenic silica
It is to utilize organic precursor method cracking at high temperature and be converted into the inorganic ceramic matrix.Sol-gel method is mainly used in preparation oxide ceramics based composites, and it is to be dewatered and the polymer formation gel through further hydrolysis reaction by liquid colloidal sol, and gel forms the inorganic oxide ceramic matrix through high temperature drying and cracking.The advantage that this method possesses is: its chemical ingredients is reached very evenly; Can make composition evenly, the heterogenetic ceramic matrix, to fiber preform, be easy to infiltrate, firing temperature is low, generally is no more than 1400 ℃, this is than the low several Baidu of traditional firing temperature.But the at present main problem that exists of this method is, the fine and close cycle is longer, and the goods voidage is higher, and matrix shrinking percentage in the Pintsch process process is bigger, is easy to generate crackle and pore.Referring to Wang Xingye, Su Bo. < < progress of continuous fibre ceramic composite (CFCC)>>, aircraft industry press, 1994.
(3), direct melt oxidation method
With the ceramic fiber preformed member place molten metal above, through selecting suitable metal species and composition, furnace body temperature and atmosphere; The metal that floods to the fabric and atmosphere are reacted and form ceramic matrix and be deposited on fiber surface, form the ceramic of compact matrix that contains the small portion of residual metal, its characteristics are: mold temperature is lower; The matrix material room temperature and the mechanical behavior under high temperature of preparation are better; Production efficiency is higher, and cost is lower, is a kind of ceramic matric composite preparation technology that industrial prospect is arranged; This technology is invented by the LANXDE company of the U.S. the earliest; Thereby being called the LANXIDE method again, the existing a small amount of CMC product of the said firm is sold at present, and is applied to aspect such as ground protection plate armour.Referring to Cao Yongfu, " progress of ceramic matric composite ", Kunming University of Science and Technology's journal, 1997,22:2
(4), melt infiltration method
Though this method has obtained widespread use aspect metal-base composites.And fruitful, but the work of being done in the ceramic matric composite method so far is still few, does not also obtain enough attention.The melt infiltration method is that molten metal is impregnated in the pore of built-in ceramic foam prefab; The major advantage of this method: can once form densification and flawless basically matrix; Dimensional change is minimum between preformed member and the finished product, can obtain the part of any complicated shape, and can keep the shape of fiber reinforcement and the intensity of fiber to a certain extent. referring to Cornie J A; Processing of metal and ceramic matrix composites; Am. Ceram. Soc.Bull., 1986,65 (2): 293～304.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of production technique; Preparation cost is low; Excellent product performance; Have high elastic coefficient, HS, high firmness, the tribological properties of excellence and low thermal expansivity, the toughness reinforcing aluminium nitride ceramics based composites of a kind of non-ferrous metal alloy of high fracture toughness property.
Another object of the present invention provides the preparation method of the toughness reinforcing aluminium nitride ceramics based composites of non-ferrous metal alloy.
In order to overcome the deficiency of prior art; Technical scheme of the present invention is to solve like this: the toughness reinforcing aluminium nitride ceramics based composites of a kind of non-ferrous metal alloy; Special character of the present invention is the preceding raw materials by weight portion ratio of aluminium nitride ceramics blank sintering; Form by 50 parts～95 parts aluminium nitride AlN, 5 parts of yttrium oxide, 0 part～34 parts aluminum oxide, 0 part～11 parts carbon blacks, wherein in ceramic matric composite, add 2 parts～63 parts non-ferrous metal alloys of matrix material gross weight.
Said non-ferrous metal alloy is the cast copper alloy of various models.
The preparation method of the toughness reinforcing aluminium nitride ceramics based composites of a kind of non-ferrous metal alloy, undertaken by following step:
(1), by ratio of weight and the number of copies, take by weighing aluminium nitride AlN, yttrium oxide, aluminum oxide, carbon black;
(2), with above-mentioned each material mixing that takes by weighing, be prepared into mixed powder with wet ball grinding, mixed powder is sieved processes the granulation material, in the mold cavity of packing into, die forming is the blank of different components;
(3), with the blank of different components respectively greater than the flow of 2 normal atmosphere nitrogen atmospheres, flowing nitrogen greater than 2L/min, be warmed up to 1600 ℃ of insulations 2 hours down gradually with the heat-up rate of 10 ℃/min, obtain void content less than 43% aluminium nitride AlN blank;
(4), the aluminium nitride AlN blank of each component is put into pressure die-casting machine die cavity internal heating die cavity to 700 ℃～900 ℃ respectively after the pressure die-casting machine each several part assembling, perhaps put into the pressure die-casting machine die cavity again behind the preheating aluminium nitride AlN blank to 700 ℃～900 ℃ separately earlier; Simultaneously, copper alloy is heated to 1000 ℃～1200 ℃ and reaches molten state;
(5), coat releasing agent with the part that liquid metal directly contacts in the pressure die-casting machine die cavity, with conveniently stripped;
(6), the fusion copper alloy liquid is poured in the pressure die-casting machine die cavity of placing the aluminium nitride AlN blank, the amount of being pressed into of fusion copper alloy liquid is 2%～63% of a matrix material gross weight;
(7), rely on the pressure die-casting machine seaming chuck that molten copper alloy hydraulic pressure is gone in the aluminium nitride AlN blank, form ingot bar, when pressure reaches 40～60MPa, stop pressurization, and keep-uped pressure 10 minutes, treat to take out ingot bar from die cavity after ingot bar is cooled to room temperature;
(8), ingot bar is reheated the unnecessary copper alloy in removal ingot bar outside;
(9), the ingot bar of removing unnecessary copper alloy is carried out obtaining matrix material after the T6 thermal treatment process; Said T6 thermal treatment process: ingot bar is put into retort furnace; In half a hour, furnace temperature is risen to 600 ℃ from room temperature; And be incubated 5 hours, and then ingot bar is taken out shrend, eliminated internal stress in 5 hours 150 ℃ of insulations again.
The present invention compared with prior art uses the prefab of the aluminium nitride AlN blank of carbothermic method preparation as ceramic matrix, has prepared the excellent toughness reinforcing aluminium nitride ceramics based composites of copper alloy of mechanical property in conjunction with melt infiltration method and pressure casting method.Its advantage is:
(1) the aluminium nitride AlN blank void content of carbothermic method preparation is less than 40%, and ceramic matrix phase content higher (greater than 60%) approaches the ceramic matrix content (about 70%) of traditional ceramics based composites.And can regulate aluminium nitride AlN blank void content, and then realize the target of control aluminium nitride AlN matrix volume content through the content of adjustment raw material.
(2) the aluminium nitride AlN matrix of the toughness reinforcing aluminium nitride ceramics based composites of copper alloy of this kind method preparation and the toughness reinforcing body of copper alloy have determined this performance of composites to have significant advantage at the topological framework that three-dimensional space intersection IPN distributes: because ceramic matrix is continuous at three-dimensional space, make this matrix material can hold the more ceramic phase of high-volume fractional; When stressed, help concentrating on a little or stress on the face disperses in the space body scope rapidly and transmits, thereby can improve the supporting capacity or the impact resistance of matrix material significantly; Because toughness reinforcing phase (metal) is continuous at three-dimensional space, feasible whole toughening effect to matrix material significantly strengthens; The flexible metallographic phase has higher inefficacy strain; Thereby can, crackle play the effect of crackle bridge joint after producing; The structure of this three-dimensional co-continuous also possibly cause the effect of structural interlock simultaneously, makes material have higher damage tolerance, and the danger of material failure reduces greatly.Because matrix (pottery) and toughness reinforcing (metal) mutually are the topology network architecture of interlacing three-dimensional co-continuous in the space, make toughness reinforcing phase (metal) and matrix (pottery) combine significantly improved.
(3) make the fusion copper alloy liquid make a forcible entry into aluminium nitride AlN blank inner air vent through mechanical pressure; Pressure remains to always and solidifies end; The mechanical pressure that applies not only can overcome prefabricated intravital various resistances; And the hot gas flow that can also make fusion copper alloy liquid forward position discharges die cavity, improved the filling capacity of fusion copper alloy liquid to the small pore of aluminium nitride AlN blank, and the matrix material density after the die casting is raise significantly.So through combining the advantage of melt infiltration method and pressure die casting technology, the toughness reinforcing aluminum-nitride-based composite material of the copper alloy of preparation has the density height, the mechanical property excellent characteristics.Be widely used in aspects such as electrical category special equipment frictional wear structural part, pressure-bearing class special equipment corrosion-and high-temp-resistant structural part, aerospace structure spare, automobile structure.
Description of drawings
Fig. 1 is the aluminium nitride AlN blank microstructure photo before embodiment 6 die casting.
Fig. 2 is the toughness reinforcing aluminium nitride ceramics based composites of the copper alloy microstructure photo after embodiment 6 die casting.
Embodiment
Below in conjunction with specific embodiment summary of the invention is done further to specify:
Embodiment 1
The toughness reinforcing aluminium nitride ceramics based composites of a kind of non-ferrous metal alloy; Raw materials by weight portion ratio before the aluminium nitride ceramics blank sintering; Form by 50 parts～95 parts aluminium nitride AlN, 5 parts of yttrium oxide, 0 part～34 parts aluminum oxide, 0 part～11 parts carbon blacks, wherein in ceramic matric composite, add 2 parts～63 parts non-ferrous metal alloys of matrix material gross weight.
Said non-ferrous metal alloy is the cast copper alloy of various models.
The preparation method of the toughness reinforcing aluminium nitride ceramics based composites of a kind of non-ferrous metal alloy, undertaken by following step:
(1), by ratio of weight and the number of copies, take by weighing aluminium nitride AlN, yttrium oxide, aluminum oxide, carbon black;
(2), with above-mentioned each material mixing that takes by weighing, be prepared into mixed powder with wet ball grinding, mixed powder is sieved processes the granulation material, in the mold cavity of packing into, die forming is the aluminium nitride AlN blank of different components;
(3), with the blank of different components respectively greater than the flow of 2 normal atmosphere nitrogen atmospheres, flowing nitrogen greater than 2L/min, be warmed up to 1600 ℃ of insulations 2 hours down gradually with the heat-up rate of 10 ℃/min, obtain void content less than 43% aluminium nitride AlN blank;
(4), the aluminium nitride AlN blank of each component is put into pressure die-casting machine die cavity internal heating die cavity to 700 ℃～900 ℃ respectively after the pressure die-casting machine each several part assembling, perhaps put into the pressure die-casting machine die cavity again behind the preheating aluminium nitride AlN blank to 700 ℃～900 ℃ separately earlier; Simultaneously, copper alloy is heated to 1000 ℃～1200 ℃ and reaches molten state;
(5), coat releasing agent with the part that liquid metal directly contacts in the pressure die-casting machine die cavity, with conveniently stripped;
(6), the fusion copper alloy liquid is poured in the pressure die-casting machine die cavity of placing the aluminium nitride AlN blank, the amount of being pressed into of fusion copper alloy liquid is 2%～63% of a matrix material gross weight;
(7), rely on the pressure die-casting machine seaming chuck that molten copper alloy hydraulic pressure is gone in the aluminium nitride AlN blank, form ingot bar, when pressure reaches 40～60MPa, stop pressurization, and keep-uped pressure 10 minutes, treat to take out ingot bar from die cavity after ingot bar is cooled to room temperature;
(8), ingot bar is reheated the unnecessary copper alloy in removal ingot bar outside;
(9), the ingot bar of removing unnecessary copper alloy is carried out obtaining matrix material after the T6 thermal treatment process; Said T6 thermal treatment process: ingot bar is put into retort furnace; In half a hour, furnace temperature is risen to 600 ℃ from room temperature; And be incubated 5 hours, and then ingot bar is taken out shrend, eliminated internal stress in 5 hours 150 ℃ of insulations again.
The embodiment that table 1 is formed for the raw material of aluminium nitride AlN blank of the present invention
The preparation method of embodiment 2～embodiment 17 is with embodiment 1.
Table 2 is copper alloy of the present invention toughness reinforcing aluminum-nitride-based composite material die casting condition and performance
Can find out that from table 2 temperature at pressure die-casting machine is 700～900 ℃, the copper alloy Heating temperature is 1000～1200 ℃, and die casting pressure is the interior die casting of the scope of 40～60MPa, and matrix material has shown very high flexural strength, fracture toughness property and microhardness.Reach as high as 565.9MPa respectively;
, 1345.3 HV.
Mercury penetration method is measured the ventilate rate of aluminium nitride AlN blank and matrix material.Sem is observed microstructure on sample section.The toughness reinforcing aluminium nitride ceramics matrix material of embodiment 2-17 metal by aforesaid method obtains is measured three-point bending strength and fracture toughness property under the room temperature, carries out microhardness testing with the Vickers' hardness appearance.The results of property of these void content and mechanical property is as shown in table 2.
Shown in Figure 1 is the preceding aluminium nitride AlN blank microstructure photos of embodiment 6 die casting.Can know that from Photomicrograph the space of aluminium nitride AlN blank is flourishing, crystal arrangement is disperseed, less dense.
Shown in Figure 2 is the toughness reinforcing aluminium nitride ceramics based composites of copper alloy Photomicrograph after embodiment 6 die casting.Can know from Photomicrograph, the toughness reinforcing aluminium nitride ceramics base of the copper alloy after the die casting, crystal arrangement is more neat, and there is tabular crystal the centre, and fracture is more closely knit.
Claims (3)
1. toughness reinforcing aluminium nitride ceramics based composites of non-ferrous metal alloy; It is characterized in that the preceding raw materials by weight portion ratio of aluminium nitride ceramics blank sintering; Form by 50 parts～95 parts aluminium nitride AlN, 5 parts of yttrium oxide, 0 part～34 parts aluminum oxide, 0 part～11 parts carbon blacks, wherein in ceramic matric composite, add 2 parts～63 parts non-ferrous metal alloys of matrix material gross weight.
2. the toughness reinforcing aluminium nitride ceramics based composites of copper alloy according to claim 1 is characterized in that said non-ferrous metal alloy is the cast copper alloy of various models.
3. the preparation method of the toughness reinforcing aluminium nitride ceramics based composites of a kind of non-ferrous metal alloy as claimed in claim 1, undertaken by following step:
(1), by ratio of weight and the number of copies, take by weighing aluminium nitride AlN, yttrium oxide, aluminum oxide, carbon black;
(2), with above-mentioned each material mixing that takes by weighing, be prepared into mixed powder with wet ball grinding, mixed powder is sieved processes the granulation material, in the mold cavity of packing into, die forming is the blank of different components;
(3), with the blank of different components respectively greater than the flow of 2 normal atmosphere nitrogen atmospheres, flowing nitrogen greater than 2L/min, be warmed up to 1600 ℃ of insulations 2 hours down gradually with the heat-up rate of 10 ℃/min, obtain void content less than 43% aluminium nitride AlN blank;
(4), the aluminium nitride AlN blank of each component is put into pressure die-casting machine die cavity internal heating die cavity to 700 ℃～900 ℃ respectively after the pressure die-casting machine each several part assembling, perhaps put into the pressure die-casting machine die cavity again behind the preheating aluminium nitride AlN blank to 700 ℃～900 ℃ separately earlier; Simultaneously, copper alloy is heated to 1000 ℃～1200 ℃ and reaches molten state;
(5), coat releasing agent with the part that liquid metal directly contacts in the pressure die-casting machine die cavity, with conveniently stripped;
(6), the fusion copper alloy liquid is poured in the pressure die-casting machine die cavity of placing the aluminium nitride AlN blank, the amount of being pressed into of fusion copper alloy liquid is according to the void content decision of aluminium nitride AlN blank, and the amount of being pressed into of fusion copper alloy liquid is 2%～63% of a matrix material gross weight;
(7), rely on the pressure die-casting machine seaming chuck that molten copper alloy hydraulic pressure is gone in the aluminium nitride AlN blank, form ingot bar, when pressure reaches 40～60MPa, stop pressurization, and keep-uped pressure 10 minutes, treat to take out ingot bar from die cavity after ingot bar is cooled to room temperature;
(8), ingot bar is reheated the unnecessary copper alloy in removal ingot bar outside;
(9), the ingot bar of removing unnecessary copper alloy is carried out obtaining matrix material after the T6 thermal treatment process; Said T6 thermal treatment process: ingot bar is put into retort furnace; In half a hour, furnace temperature is risen to 600 ℃ from room temperature; And be incubated 5 hours, and then ingot bar is taken out shrend, eliminated internal stress in 5 hours 150 ℃ of insulations again.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105886873A (en) * | 2016-06-22 | 2016-08-24 | 陈林美 | Wear-resistant nitride-based metal ceramic knife and manufacturing method thereof |
| CN113773053A (en) * | 2021-09-14 | 2021-12-10 | 西安特种设备检验检测院 | Gradient porous ceramic preform, aluminum alloy toughened ceramic composite material and preparation |
| CN116573947A (en) * | 2023-04-27 | 2023-08-11 | 郑州航空工业管理学院 | A kind of three-dimensional toughened ceramic tool material and its preparation method |
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| CN1422827A (en) * | 2002-12-24 | 2003-06-11 | 山东大学 | Nitride/alumina based composite ceramic material and process of preparing the same |
| CN101058506A (en) * | 2007-02-12 | 2007-10-24 | 河北理工大学 | Al-AlN-ZrO2 thermal shock resistant ceramic material |
| CN101531521A (en) * | 2008-12-29 | 2009-09-16 | 中国地质大学（北京） | Fe/Mo-Sialon-based ceramic composite material with resistance to high temperature, erosion and wear and preparation method thereof |
| CN102249690A (en) * | 2011-04-26 | 2011-11-23 | 燕山大学 | Aluminum nitride ceramic material molten rapidly at low temperature and molding method thereof |
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| CN1422827A (en) * | 2002-12-24 | 2003-06-11 | 山东大学 | Nitride/alumina based composite ceramic material and process of preparing the same |
| CN101058506A (en) * | 2007-02-12 | 2007-10-24 | 河北理工大学 | Al-AlN-ZrO2 thermal shock resistant ceramic material |
| CN101531521A (en) * | 2008-12-29 | 2009-09-16 | 中国地质大学（北京） | Fe/Mo-Sialon-based ceramic composite material with resistance to high temperature, erosion and wear and preparation method thereof |
| CN102249690A (en) * | 2011-04-26 | 2011-11-23 | 燕山大学 | Aluminum nitride ceramic material molten rapidly at low temperature and molding method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105886873A (en) * | 2016-06-22 | 2016-08-24 | 陈林美 | Wear-resistant nitride-based metal ceramic knife and manufacturing method thereof |
| CN113773053A (en) * | 2021-09-14 | 2021-12-10 | 西安特种设备检验检测院 | Gradient porous ceramic preform, aluminum alloy toughened ceramic composite material and preparation |
| CN113773053B (en) * | 2021-09-14 | 2023-02-17 | 西安特种设备检验检测院 | Gradient porous ceramic preform, aluminum alloy toughened ceramic composite material and preparation |
| CN116573947A (en) * | 2023-04-27 | 2023-08-11 | 郑州航空工业管理学院 | A kind of three-dimensional toughened ceramic tool material and its preparation method |
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| CN102815957B (en) | 2014-05-07 |
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