CN117385223A - Cu- (Si) with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) Preparation method of composite material - Google Patents

Cu- (Si) with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) Preparation method of composite material Download PDF

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CN117385223A
CN117385223A CN202311353839.9A CN202311353839A CN117385223A CN 117385223 A CN117385223 A CN 117385223A CN 202311353839 A CN202311353839 A CN 202311353839A CN 117385223 A CN117385223 A CN 117385223A
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ball milling
powder
temperature
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秦永强
韦国宣
吴玉程
罗来马
马冰
张一帆
王岩
崔接武
张勇
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Hefei University of Technology
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    • C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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Abstract

Cu- (Si) with excellent comprehensive performance 3 N 4 ‑Y 2 O 3 ) The preparation method of the composite material specifically comprises the following steps: solid salt crystallizationPerforming chemical treatment; (II) high-temperature nitriding and calcining; (III) alloying at atomic level; and (IV) direct current pulse hot-pressing sintering. According to the invention, uniformly dispersed composite powder is obtained by the methods of salt solidification crystallization and nitriding calcination, and the composite powder is added into a copper matrix by using an atomic level alloying method, so that the dispersion strengthening effect is achieved; traditionally added single hard phase Y 2 O 3 It has an undesirable reinforcing effect when added alone due to coarsening at high temperature. Si (Si) 3 N 4 The material has the characteristics of high hardness, high strength, wear resistance and the like, and can inhibit coarsening of yttrium oxide particles in the preparation process of the material, so that the dispersion strengthening effect is optimized, the mechanical property of the material is greatly improved, the conductivity is maintained at a higher level, and the excellent comprehensive properties of high strength and high conductivity of the copper-based material are realized.

Description

Cu- (Si) with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) Preparation method of composite material
Technical Field
The invention belongs to the technical field of preparation of copper-based composite materials for high strength and high conductivity, and in particular relates to a Cu- (Si) composite material with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is a preparation method of a high-strength high-conductivity copper-based composite material for communication cables.
Background
Copper and its alloy are widely used in communication cable, resistance welding electrode and electrical contact material due to the characteristics of high conductivity and high strength, however, along with the development of technology, various materials, especially the field of communication cable, put higher demands on the strength of copper and its alloy. Dispersion strengthened copper (DS-Cu) is a metallic material strengthened by adding second phase ceramic particles insoluble in the base metal to the copper matrix. It is usually generalThrough powder metallurgy preparation, the second phase is uniformly distributed in the base metal, and the DS-Cu can keep high-level conductivity and dispersion strengthening effect at high temperature, so that the DS-Cu becomes one of main stream copper alloys widely applied to various industries. Conventionally added hard phase Y 2 O 3 Since it has an undesirable reinforcing effect when added alone due to coarsening at high temperature, it is considered to add another nonmetallic ceramic phase to be combined therewith, further improving the dispersion strengthening effect. Si (Si) 3 N 4 The material has the characteristics of high hardness, high strength, wear resistance and the like, and can inhibit coarsening of yttrium oxide particles in the preparation process of the material, so that the dispersion strengthening effect is optimized.
Disclosure of Invention
The invention aims to provide Cu- (Si) with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) Preparation method of composite material, cu- (Si) prepared by the method 3 N 4 -Y 2 O 3 ) The copper-based composite material not only can improve the mechanical property of the material, but also can improve the conductivity of the material, thereby meeting the use requirement.
In order to achieve the above object, the present invention adopts the following technical solutions:
cu- (Si) with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) The preparation method of the composite material specifically comprises the following steps:
(one) solid salt crystallization
(1) Yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 O) dissolving the powder in deionized water, fully stirring, and adding pure Si powder into the solution;
(2) Heating and stirring the mixture in a magnetic stirrer until the solution is evaporated, and completely precipitating yttrium salt for crystallization to obtain a precursor;
(3) Fully grinding the precursor obtained in the step (2) in a mortar to finally obtain the Si-Y (NO) with uniform dispersion 3 ) 3 Precursor powder;
(II) high temperature nitriding calcination
Step 1The prepared precursor powder is put into a high-temperature tube furnace and is nitrided and calcined in nitrogen atmosphere to obtain Si 3 N 4 -Y 2 O 3 The composite powder is prepared by heating from room temperature to 300 ℃ at a rate of 10 ℃ per minute and then preserving the temperature for 1 hour to ensure complete decomposition of yttrium nitrate, heating to 1000 ℃ at a rate of 10 ℃ per minute, heating to 1300 ℃ to 1400 ℃ at a rate of 5 ℃ per minute and preserving the temperature for 2 to 3 hours, heating to 1000 ℃ at a rate of 5 ℃ per minute, heating to 500 ℃ at a rate of 10 ℃ per minute and then cooling with a furnace to obtain Si 3 N 4 -Y 2 O 3 A powder;
(III) atomic level alloying
Si obtained in the step (II) 3 N 4 -Y 2 O 3 Placing the powder and copper powder in a ball milling tank, si 3 N 4 -Y 2 O 3 The powder accounts for 2% -6% of the mass ratio, the ball milling rotating speed (autorotation speed) is 200-300 rpm, the ball milling time is 12-18 hours, the assembly of a ball milling tank is completed under the argon atmosphere in a vacuum glove box, the ball milling process is ensured to be carried out under the protection of the argon atmosphere so as to reduce the influence of oxygen oxidation powder in air in the atomic level alloying process, the ball milling tank and the ball milling medium are made of hard alloy, after the assembly is completed, the ball milling tank is placed in a planetary ball mill for ball milling, and after the ball milling tank is taken out for grinding, the dispersed Cu- (Si) is finally obtained 3 N 4 -Y 2 O 3 ) A composite powder;
(IV) direct-current pulse hot-pressing sintering
(1) Cu- (Si) obtained in the step (III) 3 N 4 -Y 2 O 3 ) Loading the composite powder into a graphite mold, prepressing, then placing the mold into a direct current pulse hot-pressing sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ and preserving heat for 5 min;
(2) Heating to 750-850 deg.C, maintaining for 5min, and cooling to room temperature to obtain Cu- (Si) 3 N 4 -Y 2 O 3 ) A composite material.
In the step (one), yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 The purity of O) and silicon powder is 99 percent.
And (3) in the step (II), the model GSL-1200X of the tube furnace has the temperature rising rate of 5-10 ℃ per minute and the temperature reducing rate of 5-10 ℃ per minute.
Si in the step (II) 3 N 4 And Y 2 O 3 The mass ratio of (2) is 1:1.
The copper powder in step (three) had a purity of 99.5% and a particle size of 25 μm and was purchased from Chengdu Kogyo Co.
In the step (III), the model of a vacuum glove box is ZKX, the planetary ball mill is a QM-QX4 omnibearing planetary ball mill, the ball-material ratio is 7:1, the ball milling rotating speed (autorotation speed) is 200-300 rpm, the ball milling time is 12-18 hours, the assembly of a ball milling tank is completed in the vacuum glove box, the pure ball milling environment is ensured, the ball milling medium and the pellets are all hard alloy, and the hard alloy component is WC-Co.
The graphite mold diameter in the step (four) is 20 mm.
In the step (IV), the temperature rising rate is 100 ℃ per minute, and the temperature reducing rate is 100 ℃ per minute.
The type of the sintering furnace for direct current pulse hot-pressing sintering in the step (IV) is Labox (TM) -300, the pre-pressing pressure is 10 MPa, the sintering temperature is 750-850 ℃, the heat preservation time is 5min, and the final pressure is 50 MPa.
And (3) in the step (IV), the heating rate of the direct current pulse hot-pressing sintering is 100 ℃/min, the temperature is kept at 600 ℃ for 5min in the heating process, and the process from pre-pressing to final pressing is completed in the heating process from 600 ℃ to the sintering temperature.
The invention has the beneficial effects that: different from the contradiction between the mechanical property and the conductivity of the traditional copper alloy, the invention obtains uniformly dispersed composite powder by the methods of salt fixation crystallization and nitriding calcination, and adds the composite powder into a copper matrix by using an atomic level alloying method, thereby achieving the effect of dispersion strengthening; traditionally added single hard phase Y 2 O 3 Because of its coarsening at high temperature, it has undesirable strengthening effect when added alone, and another nonmetallic ceramic phase is added to be matched with itThe dispersion strengthening effect can be further improved. Si (Si) 3 N 4 The material has the characteristics of high hardness, high strength, wear resistance and the like, and can inhibit coarsening of yttrium oxide particles in the preparation process of the material, so that the dispersion strengthening effect is optimized, the mechanical property of the material is greatly improved, and the conductivity is maintained at a higher level. In general, the composition design and the preparation process of the invention realize the excellent comprehensive properties of high strength and high conductivity of the copper-based material.
Drawings
FIG. 1 is a composite Cu-4 wt% (Si) 3 N 4 -Y 2 O 3 ) SEM images of (2);
FIG. 2 is a composite Cu-4 wt% (Si) 3 N 4 -Y 2 O 3 ) Is an EDS map of (2);
FIG. 3 is a composite Cu-4 wt% (Si) 3 N 4 -Y 2 O 3 ) Is a stretch break topography of (c).
Detailed Description
The invention is further illustrated below with reference to specific examples.
Example 1
Cu- (Si) in this example 3 N 4 -Y 2 O 3 ) The composite material is prepared by salt solidification crystallization, nitriding calcination, atomic level alloying and direct current pulse hot-pressing sintering, wherein Si 3 N 4 -Y 2 O 3 The mass fraction of (2%).
Cu- (Si) in this example 3 N 4 -Y 2 O 3 ) The preparation method of the composite material comprises the following steps:
(1) Crystallization of solid salt, yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 O) powder was dissolved in deionized water, and after sufficient stirring, pure Si powder was added to the solution in an amount of 2.97. 2.97 g, yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 Adding O) 27.03-g, heating and stirring in magnetic stirrer until the solution is evaporated, completely precipitating yttrium salt, and grinding in mortar to obtain Si-Y (NO) with uniform dispersion 3 ) 3 Precursor powder;
(2) Nitriding and calcining: putting the precursor powder into a high-temperature tube furnace, nitriding and calcining in nitrogen atmosphere to obtain Si 3 N 4 -Y 2 O 3 The composite powder, the temperature is raised to 300 ℃ at the rate of 10 ℃ per minute from room temperature and then kept for 1 hour to ensure that yttrium nitrate is completely decomposed, then raised to 1000 ℃ at the rate of 10 ℃ per minute, then raised to 1300 ℃ at the rate of 5 ℃ per minute and kept for 2 hours, then the temperature is lowered to 1000 ℃ at the rate of 5 ℃ per minute, finally the temperature is lowered to 500 ℃ at the rate of 10 ℃ per minute and then cooled with a furnace, finally Si is obtained 3 N 4 -Y 2 O 3 A powder;
(3) Atomic level alloying: si obtained in the previous step 3 N 4 -Y 2 O 3 Placing the powder and copper powder in a ball milling tank, si 3 N 4 -Y 2 O 3 The powder accounts for 2% of the mass ratio, the ball milling rotating speed (autorotation speed) is 200 rpm, the ball milling time is 12 hours, the ball material ratio is 7:1, the assembly of a ball milling tank is completed under the argon atmosphere in a vacuum glove box, the ball milling process is ensured to be carried out under the protection of the argon atmosphere so as to reduce the influence of oxygen oxidation powder in air in the atomic level alloying process, the ball milling tank and the ball milling medium are made of hard alloy, after the assembly is completed, the ball milling tank is placed in a planetary ball mill for ball milling, and after the ball milling tank is taken out, the ball milling tank is milled, and finally dispersed Cu-2%wt (Si) is obtained 3 N 4 -Y 2 O 3 ) A composite powder;
(4) Direct current pulse hot-pressing sintering: cu-2% wt (Si 3 N 4 -Y 2 O 3 ) Putting the composite powder into a graphite mold, wrapping the surface of the powder with carbon paper, putting the mold into a Labox (TM) -300 direct current pulse hot-pressing sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃, preserving heat for 5min, and setting the pre-pressing pressure to 10 MPa; heating to 750 ℃ and preserving heat for 5min, manually pressurizing to the final pressure of 50 MPa in the heating process, wherein the heating rate is 100 ℃/min; cooling to room temperature after heat preservation is finished, wherein the cooling rate is 100 ℃/min, and the Cu-2%wt (Si) is obtained 3 N 4 -Y 2 O 3 ) Composite materialAnd (5) material.
Example 2
Cu- (Si) in this example 3 N 4 -Y 2 O 3 ) The composite material is prepared by salt solidification crystallization, nitriding calcination, atomic level alloying and direct current pulse hot-pressing sintering, wherein Si 3 N 4 -Y 2 O 3 Is 4% by mass.
Cu- (Si) in this example 3 N 4 -Y 2 O 3 ) The preparation method of the composite material comprises the following steps:
(1) Salt fixation crystallization: yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 O) powder was dissolved in deionized water, and after sufficient stirring, pure Si powder was added to the solution in an amount of 2.97. 2.97 g, yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 Adding O) 27.03-g, heating and stirring in magnetic stirrer until the solution is evaporated, completely precipitating yttrium salt, and grinding in mortar to obtain Si-Y (NO) with uniform dispersion 3 ) 3 Precursor powder;
(2) Nitriding and calcining: putting the precursor powder into a high-temperature tube furnace, nitriding and calcining in nitrogen atmosphere to obtain Si 3 N 4 -Y 2 O 3 The composite powder, the temperature is raised to 300 ℃ at the rate of 10 ℃ per minute from room temperature and then is kept for 1 hour to ensure that yttrium nitrate is completely decomposed, then is raised to 1000 ℃ at the rate of 10 ℃ per minute, is raised to 1350 ℃ at the rate of 5 ℃ per minute and is kept for 2.5 hours, then is lowered to 1000 ℃ at the rate of 5 ℃ per minute, finally is lowered to 500 ℃ at the rate of 10 ℃ per minute and then is cooled along with the furnace, and finally Si is obtained 3 N 4 -Y 2 O 3 A powder;
(3) Atomic level alloying: si obtained in the previous step 3 N 4 -Y 2 O 3 Placing the powder and copper powder in a ball milling tank, si 3 N 4 -Y 2 O 3 The powder accounts for 4 percent of the mass ratio, the ball milling rotating speed (autorotation speed) is 250 rpm, the ball milling time is 15 hours, the ball material ratio is 7:1, and the ball milling rotating speed is in a vacuum glove boxThe assembly of the ball milling tank is completed under the argon atmosphere, the ball milling process is ensured to be carried out under the protection of the argon atmosphere so as to reduce the influence of oxygen in air to oxidize powder in the atomic level alloying process, the ball milling tank and the ball milling medium are both made of hard alloy, after the assembly is completed, the ball milling tank is placed in a planetary ball mill for ball milling, and after the ball milling tank is taken out, the dispersed Cu-4%wt (Si) is finally obtained 3 N 4 -Y 2 O 3 ) A composite powder;
(4) Direct current pulse hot-pressing sintering: cu-4% wt (Si 3 N 4 -Y 2 O 3 ) Putting the composite powder into a graphite mold, wrapping the surface of the powder with carbon paper, putting the mold into a Labox (TM) -300 direct current pulse hot-pressing sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃, preserving heat for 5min, and setting the pre-pressing pressure to 10 MPa; heating to 800 ℃ and preserving heat for 5min, manually pressurizing to the final pressure of 50 MPa in the heating process, wherein the heating rate is 100 ℃/min; cooling to room temperature after heat preservation is finished, wherein the cooling rate is 100 ℃/min, and the Cu-4%wt (Si) is obtained 3 N 4 -Y 2 O 3 ) A composite material.
Example 3
Cu- (Si) in this example 3 N 4 -Y 2 O 3 ) The composite material is prepared by salt solidification crystallization, nitriding calcination, atomic level alloying and direct current pulse hot-pressing sintering, wherein Si 3 N 4 -Y 2 O 3 Is 6% by mass.
Cu- (Si) in this example 3 N 4 -Y 2 O 3 ) The preparation method of the composite material comprises the following steps:
(1) Salt fixation crystallization: yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 O) powder was dissolved in deionized water, and after sufficient stirring, pure Si powder was added to the solution in an amount of 2.97. 2.97 g, yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 Adding O) 27.03-g, heating and stirring in magnetic stirrer until the solution is evaporated, completely precipitating yttrium salt, and grinding in mortar to obtain Si-Y (NO) with uniform dispersion 3 ) 3 Precursor powder;
(2) Nitriding and calcining: putting the precursor powder into a high-temperature tube furnace, nitriding and calcining in nitrogen atmosphere to obtain Si 3 N 4 -Y 2 O 3 The composite powder, the temperature is raised to 300 ℃ at the rate of 10 ℃ per minute from room temperature and then kept for 1 hour to ensure that yttrium nitrate is completely decomposed, then raised to 1000 ℃ at the rate of 10 ℃ per minute, then raised to 1400 ℃ at the rate of 5 ℃ per minute and kept for 3 hours, then the temperature is lowered to 1000 ℃ at the rate of 5 ℃ per minute, finally the temperature is lowered to 500 ℃ at the rate of 10 ℃ per minute and then cooled with a furnace, finally Si is obtained 3 N 4 -Y 2 O 3 A powder;
(3) Atomic level alloying: si obtained in the previous step 3 N 4 -Y 2 O 3 Placing the powder and copper powder in a ball milling tank, si 3 N 4 -Y 2 O 3 The mass ratio of the powder is 6%, the ball milling rotating speed (autorotation speed) is 300 rpm, the ball milling time is 18 hours, the ball material ratio is 7:1, the assembly of the ball milling tank is completed under the argon atmosphere in a vacuum glove box, and the ball milling process is ensured to be carried out under the protection of the argon atmosphere so as to reduce the influence of oxygen in the air to oxidize the powder in the atomic level alloying process. The ball tank and the ball milling medium are made of hard alloy, after the assembly is completed, the ball milling tank is put into a planetary ball mill for ball milling, and after the ball milling tank is taken out, the ball milling medium is ground, and finally the dispersed Cu-6%wt (Si) is obtained 3 N 4 -Y 2 O 3 ) A composite powder;
(4) Direct current pulse hot-pressing sintering: cu-6% wt. (Si 3 N 4 -Y 2 O 3 ) Putting the composite powder into a graphite mold, wrapping the surface of the powder with carbon paper, putting the mold into a Labox (TM) -300 direct current pulse hot-pressing sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃, preserving heat for 5min, and setting the pre-pressing pressure to 10 MPa; heating to 850 ℃ and preserving heat for 5min, manually pressurizing to the final pressure of 50 MPa in the heating process, wherein the heating rate is 100 ℃/min; cooling to room temperature after heat preservation is finished, wherein the cooling rate is 100 ℃/min, and the Cu-6%wt (Si) is obtained 3 N 4 -Y 2 O 3 ) A composite material.
For Cu- (Si) in examples 1 to 3 3 N 4 -Y 2 O 3 ) The composite material was tested for electrical conductivity and mechanical properties, and the test results are shown in table 1:
table 1 Cu- (Si) in examples 1 to 3 3 N 4 -Y 2 O 3 ) Conductivity and mechanical properties of the composite material
As can be seen from table 1, the addition of another nonmetallic ceramic phase to cooperate with the dispersion-strengthened particles significantly improves the overall performance of the composite material as compared with the conventional single oxide dispersion-strengthened particles.
As can be seen from fig. 1, the second phase is mainly and uniformly distributed at the grain boundary, and can generate pinning effect on dislocation and grain boundary movement, thereby being beneficial to improving the mechanical properties of the composite material.
As can be seen from FIG. 2, Y 2 O 3 The particles are mainly attached to Cu particles, si 3 N 4 In Cu matrix and Y 2 O 3 Segregation on the interfaces between particles can effectively reduce the interface energy and inhibit Y 2 O 3 Coarsening of the particles.
As can be seen from fig. 3, the fracture of the specimen after the tensile test exhibits a ductile pit and a quasi-cleaved morphology, and second phase particles are observed at the bottom of the ductile pit. And small particles are distributed in the tear ridge and act to transfer load during stretching.
Unlike the traditional contradiction between the mechanical property and conductivity of copper alloy, the present invention obtains composite powder with homogeneous dispersion through salt fixing crystallization and nitriding calcination, and adds the composite powder into copper matrix through atomic level alloying process to reach the dispersion strengthening effect. Traditionally added single hard phase Y 2 O 3 It has an undesirable reinforcing effect when added alone due to coarsening at high temperature. The dispersion strengthening effect can be further improved by adding another nonmetallic ceramic phase to be matched with the nonmetallic ceramic phaseAnd (5) fruits. Si (Si) 3 N 4 The material has the characteristics of high hardness, high strength, wear resistance and the like, and can inhibit coarsening of yttrium oxide particles in the preparation process of the material, so that the dispersion strengthening effect is optimized. The mechanical property of the material is greatly improved and the conductivity is maintained at a higher level; in general, the composition design and the preparation process of the invention realize the excellent comprehensive properties of high strength and high conductivity of the copper-based material.
The above examples merely illustrate specific embodiments of the disclosure, but the embodiments of the disclosure are not limited by the foregoing. Any changes, modifications, substitutions, combinations, and simplifications that may be made without materially departing from the spirit and principles of the inventive concepts of the present disclosure are intended to be equivalent substitutes and are intended to be included within the scope of protection as defined by the claims.

Claims (10)

1. Cu- (Si) with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: the method specifically comprises the following steps:
(one) solid salt crystallization
(1) Yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 O) dissolving the powder in deionized water, fully stirring, and adding pure Si powder into the solution;
(2) Heating and stirring the mixture in a magnetic stirrer until the solution is evaporated, and completely precipitating yttrium salt for crystallization to obtain a precursor;
(3) Fully grinding the precursor obtained in the step (2) in a mortar to finally obtain the Si-Y (NO) with uniform dispersion 3 ) 3 Precursor powder;
(II) high temperature nitriding calcination
Putting the precursor powder prepared in the step (one) into a high-temperature tube furnace, and nitriding and calcining in a nitrogen atmosphere to obtain Si 3 N 4 -Y 2 O 3 The composite powder was incubated for 1 hour after the temperature had been raised from room temperature to 300 ℃ at a rate of 10 ℃ per minute to ensure complete decomposition of yttrium nitrate, then raised to 1000 ℃ at a rate of 10 ℃ per minute, then raised to 5 °Raising the temperature to 1300-1400 ℃ per minute, maintaining for 2-3 hours, lowering the temperature to 1000 ℃ at 5 ℃ per minute, lowering the temperature to 500 ℃ at 10 ℃ per minute, and cooling with a furnace to obtain Si 3 N 4 -Y 2 O 3 A powder;
(III) atomic level alloying
Si obtained in the step (II) 3 N 4 -Y 2 O 3 Placing the powder and copper powder in a ball milling tank, si 3 N 4 -Y 2 O 3 The powder accounts for 2% -6% of the mass ratio, the ball milling rotating speed (autorotation speed) is 200-300 rpm, the ball milling time is 12-18 hours, the assembly of a ball milling tank is completed under the argon atmosphere in a vacuum glove box, the ball milling process is ensured to be carried out under the protection of the argon atmosphere so as to reduce the influence of oxygen oxidation powder in air in the atomic level alloying process, the ball milling tank and the ball milling medium are made of hard alloy, after the assembly is completed, the ball milling tank is placed in a planetary ball mill for ball milling, and after the ball milling tank is taken out for grinding, the dispersed Cu- (Si) is finally obtained 3 N 4 -Y 2 O 3 ) A composite powder;
(IV) direct-current pulse hot-pressing sintering
(1) Cu- (Si) obtained in the step (III) 3 N 4 -Y 2 O 3 ) Loading the composite powder into a graphite mold, prepressing, then placing the mold into a direct current pulse hot-pressing sintering furnace, vacuumizing the furnace chamber at room temperature, heating to 600 ℃ and preserving heat for 5 min;
(2) Heating to 750-850 deg.C, maintaining for 5min, and cooling to room temperature to obtain Cu- (Si) 3 N 4 -Y 2 O 3 ) A composite material.
2. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: in the step (one), yttrium nitrate (Y (NO) 3 ) 3 ·6H 2 The purity of O) and silicon powder is 99 percent.
3. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: and (3) in the step (II), the model GSL-1200X of the tube furnace has the temperature rising rate of 5-10 ℃ per minute and the temperature reducing rate of 5-10 ℃ per minute.
4. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: si in the step (II) 3 N 4 And Y 2 O 3 The mass ratio of (2) is 1:1.
5. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: the copper powder in step (three) had a purity of 99.5% and a particle size of 25 μm and was purchased from Chengdu Kogyo Co.
6. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: in the step (III), the model of a vacuum glove box is ZKX, the planetary ball mill is a QM-QX4 omnibearing planetary ball mill, the ball-material ratio is 7:1, the ball milling rotating speed (autorotation speed) is 200-300 rpm, the ball milling time is 12-18 hours, the assembly of a ball milling tank is completed in the vacuum glove box, the pure ball milling environment is ensured, the ball milling medium and the pellets are all hard alloy, and the hard alloy component is WC-Co.
7. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: the graphite mold diameter in the step (four) is 20 mm.
8. A process according to claim 1, wherein the composition is excellentCu- (Si) of the Performance 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: in the step (IV), the temperature rising rate is 100 ℃ per minute, and the temperature reducing rate is 100 ℃ per minute.
9. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: the type of the sintering furnace for direct current pulse hot-pressing sintering in the step (IV) is Labox (TM) -300, the pre-pressing pressure is 10 MPa, the sintering temperature is 750-850 ℃, the heat preservation time is 5min, and the final pressure is 50 MPa.
10. A Cu- (Si) composition having excellent overall properties as claimed in claim 1 3 N 4 -Y 2 O 3 ) The preparation method of the composite material is characterized by comprising the following steps: and (3) in the step (IV), the heating rate of the direct current pulse hot-pressing sintering is 100 ℃/min, the temperature is kept at 600 ℃ for 5min in the heating process, and the process from pre-pressing to final pressing is completed in the heating process from 600 ℃ to the sintering temperature.
CN202311353839.9A 2023-10-19 2023-10-19 Cu- (Si) with excellent comprehensive performance 3 N 4 -Y 2 O 3 ) Preparation method of composite material Pending CN117385223A (en)

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