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CN108085575A - Interior raw nanometer TiB in a kind of refinement pottery aluminium composite material2The method of particle - Google Patents

Interior raw nanometer TiB in a kind of refinement pottery aluminium composite material2The method of particle Download PDF

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Publication number
CN108085575A
CN108085575A CN201711274156.9A CN201711274156A CN108085575A CN 108085575 A CN108085575 A CN 108085575A CN 201711274156 A CN201711274156 A CN 201711274156A CN 108085575 A CN108085575 A CN 108085575A
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Prior art keywords
powder
grams
tib
copper
particles
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Inventor
邱丰
董柏欣
常芳
姜启川
查敏
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Jilin University
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Jilin University
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Abstract

本发明涉及了一种细化陶铝复合材料中内生纳米TiB2颗粒的方法，包括以下步骤:(1)硼粉球磨预处理；(2)含有细化元素的Al‑Ti‑B‑M反应体系的混合制备；(3)含有细化元素的Al‑Ti‑B‑M反应体系球磨均匀化及粉体压坯致密化；(4)压坯原位反应制备并细化处理TiB2颗粒；本发明中的合金元素添加细化陶铝复合材料中内生纳米TiB2颗粒可以用于陶瓷颗粒的细化和尺寸控制，有利于制备纳米尺寸TiB2颗粒，TiB2颗粒是铝合金重要的细化剂和强化剂，纳米尺寸TiB2颗粒可大幅提高合金组织的细化效果，大幅减少TiB2颗粒使用量，降低细化铝合金的成本。The present invention relates to a kind of method of endogenous nanometer TiB2 particle in refinement pottery-aluminum composite material, comprises the following steps: (1) boron powder ball milling pretreatment; (2) Al-Ti-B-M containing refinement element Mixed preparation of the reaction system; (3) Al-Ti-B-M reaction system containing refinement elements, ball milling homogenization and powder compact compaction; (4) In-situ reaction of the compact to prepare and refine TiB 2 particles ; The alloying element in the present invention adds endogenous nanometer TiB in the pottery-aluminum composite material of refinement 2 particles can be used for the refinement and size control of ceramic particles, which is conducive to the preparation of nano-sized TiB 2 particles, TiB 2 particles are important for aluminum alloys As a refiner and strengthener, nano-sized TiB 2 particles can greatly improve the refinement effect of the alloy structure, greatly reduce the amount of TiB 2 particles used, and reduce the cost of refining aluminum alloys.

Description

一种细化陶铝复合材料中内生纳米TiB2颗粒的方法A method for refining endogenous nano-TiB2 particles in ceramic-aluminum composite materials

技术领域technical field

本发明涉及铝合金和陶瓷复合加工和制备领域，具体涉及一种细化陶铝复合材料中内生纳米TiB2颗粒的方法。The invention relates to the field of composite processing and preparation of aluminum alloy and ceramics, in particular to a method for refining endogenous nanometer TiB2 particles in ceramic-aluminum composite materials.

背景技术Background technique

目前，颗粒增强铝基复合材料的增强体主要是微米尺寸颗粒。尽管微米尺寸颗粒能够明显提高复合材料的强度和弹性模量，但是它同时会降低塑性和韧性，且高温性能提高不明显，这极大地限制了其在一些高端领域的应用。纳米陶瓷颗粒增强金属基复合具有较高的比强度、较低的密度、较高的硬度、较好的热稳定性以及良好的耐磨损性能等，广泛应用与结构件和功能件中，例如航空航天、汽车制造等领域。且对于陶瓷金属复合来说，较低的陶瓷颗粒含量即可获得很好的强化效果，这也使得制备过程简便，成本易于控制。此外，纳米颗粒还可以作为α-Al的异质核心，促进α-Al形核，细化铝合金组织。内生纳米TiB2颗粒陶铝复合材料中的纳米TiB2陶瓷颗粒作为一种纳米级的增强相，可以通过细晶强化、奥罗万强化、钉扎晶界、热错配强化等强化铝合金。大量的实验结果表明，陶瓷颗粒的含量相同时，颗粒尺寸越细小，其对材料性能的改善越好。由于纳米颗粒的尺寸越小，提高复合材料的屈服强度、抗拉强度、延伸率的效果越好，因此有必要考虑一种纳米颗粒的细化方法；通过加入一定质量分数的合金元素，在不生成其他中间产物的基础上，进一步减小纳米颗粒的尺寸。At present, the reinforcements of particle-reinforced aluminum matrix composites are mainly micron-sized particles. Although micron-sized particles can significantly improve the strength and elastic modulus of composite materials, they will reduce plasticity and toughness at the same time, and the high-temperature performance is not significantly improved, which greatly limits its application in some high-end fields. Nano-ceramic particles reinforced metal matrix composites have high specific strength, low density, high hardness, good thermal stability and good wear resistance, etc., and are widely used in structural and functional parts, such as Aerospace, automobile manufacturing and other fields. And for ceramic-metal composites, a relatively low content of ceramic particles can achieve a good strengthening effect, which also makes the preparation process simple and the cost easy to control. In addition, nanoparticles can also serve as the heterogeneous core of α-Al, promote the nucleation of α-Al, and refine the structure of aluminum alloy. Nano-TiB 2 ceramic particles in endogenous nano-TiB 2 ceramic-aluminum composites, as a nanoscale reinforcement phase, can strengthen aluminum alloys through fine-grain strengthening, Orowan strengthening, pinning grain boundaries, and thermal mismatch strengthening. . A large number of experimental results show that when the content of ceramic particles is the same, the finer the particle size, the better the improvement of the material properties. Since the smaller the size of the nanoparticles, the better the effect of improving the yield strength, tensile strength, and elongation of the composite material, so it is necessary to consider a method of refining the nanoparticles; by adding a certain mass fraction of alloy elements, in different On the basis of generating other intermediate products, the size of nanoparticles is further reduced.

发明内容Contents of the invention

本发明的目的是提供一种细化陶铝复合材料中内生纳米TiB2颗粒的方法。The purpose of the present invention is to provide a method for refining endogenous nano- TiB2 particles in ceramic-aluminum composite materials.

本发明的目的可以通过以下技术方案实现：The purpose of the present invention can be achieved through the following technical solutions:

一种细化陶铝复合材料中内生纳米TiB2颗粒的方法，包括以下步骤：A kind of endogenous nanometer TiB in thinning pottery-aluminum composite The method of particle , comprises the following steps:

(1)硼粉球磨预处理：将硼粉放入球磨罐中，用球磨机将硼粉以200～300r/min的速度球磨处理1～3h；(1) Boron powder ball milling pretreatment: put boron powder into a ball mill tank, and use a ball mill to mill the boron powder at a speed of 200-300r/min for 1-3 hours;

(2)含有细化元素的Al-Ti-B-M反应体系的混合制备，具体如下：(2) The mixed preparation of the Al-Ti-B-M reaction system containing refinement elements is as follows:

(2a)称取粒度13～48μm的铝粉、球磨处理后粒度为0.5～1μm的硼粉、粒度为13～45μm的钛粉、粒度为45μm的铜粉以及粒度为45μm的镁粉备用；(2a) Weigh aluminum powder with a particle size of 13-48 μm, boron powder with a particle size of 0.5-1 μm after ball milling, titanium powder with a particle size of 13-45 μm, copper powder with a particle size of 45 μm and magnesium powder with a particle size of 45 μm for subsequent use;

(2b)将铝粉、钛粉、硼粉、铜粉、镁粉按以下几种配比配制成100g混合粉末制成Al-Ti-B-M压坯，其中，M代表铜粉、镁粉，Ti/B质量比为2.22:1；Ti/B摩尔比为1:2；铝粉的含量为65～85wt.％；钛粉含量为6.88～20.64wt.％；硼粉含量为3.12～9.36wt.％铜粉的含量为0～5wt.％，镁粉的含量为0～5wt.％，上述各组分具体如下；(2b) Aluminum powder, titanium powder, boron powder, copper powder, and magnesium powder are formulated into 100g mixed powder according to the following proportions to make Al-Ti-B-M compact, wherein, M represents copper powder, magnesium powder, and Ti The /B mass ratio is 2.22:1; the Ti/B molar ratio is 1:2; the content of aluminum powder is 65-85wt.%; the content of titanium powder is 6.88-20.64wt.%; the content of boron powder is 3.12-9.36wt. The content of % copper powder is 0～5wt.%, the content of magnesium powder is 0～5wt.%, above-mentioned each component is specific as follows;

①Al-Ti-B–Cu体系中反应生成纳米TiB2陶瓷颗粒的质量分数为10wt.％，体系中铜元素的含量为5wt.％，其中，Ti/B质量比为2.22:1；Ti/B摩尔比为1:2；体系中铝粉、钛粉、硼粉、铜粉、镁粉各自重量分别为：铝粉：85克；钛粉：6.88克；硼粉：3.12克；铜粉：5克；镁粉：0克；配制成100克混合粉末；①In the Al-Ti-B–Cu system, the mass fraction of nano-TiB 2 ceramic particles produced by the reaction is 10wt.%, and the content of copper element in the system is 5wt.%. Among them, the mass ratio of Ti/B is 2.22:1; Ti/B The molar ratio is 1:2; the respective weights of aluminum powder, titanium powder, boron powder, copper powder, and magnesium powder in the system are: aluminum powder: 85 grams; titanium powder: 6.88 grams; boron powder: 3.12 grams; copper powder: 5 grams; magnesium powder: 0 grams; formulated into 100 grams of mixed powder;

②Al-Ti-B–Cu体系中反应生成纳米TiB2陶瓷颗粒的质量分数为20wt.％，体系中铜元素的含量为5wt.％，其中，Ti/B质量比为2.22:1；Ti/B摩尔比为1:2；体系中铝粉、钛粉、硼粉、铜粉、镁粉各自重量分别为：铝粉：75克；钛粉：13.77克；硼粉：6.23克；铜粉：5克；镁粉：0克；配制成100克混合粉末；②In the Al-Ti-B–Cu system, the mass fraction of nano-TiB 2 ceramic particles produced by the reaction is 20wt.%, and the content of copper element in the system is 5wt.%. Among them, the mass ratio of Ti/B is 2.22:1; Ti/B The molar ratio is 1:2; the respective weights of aluminum powder, titanium powder, boron powder, copper powder, and magnesium powder in the system are: aluminum powder: 75 grams; titanium powder: 13.77 grams; boron powder: 6.23 grams; copper powder: 5 grams; magnesium powder: 0 grams; formulated into 100 grams of mixed powder;

③Al-Ti-B–Cu体系中反应生成纳米TiB2陶瓷颗粒的质量分数为30wt.％，体系中铜元素的含量为5wt.％，其中，Ti/B质量比为2.22:1；Ti/B摩尔比为1:2；体系中铝粉、钛粉、硼粉、铜粉、镁粉各自重量分别为：铝粉：65克；钛粉：20.64克；硼粉：9.36克；铜粉：5克；镁粉：0克；配制成100克混合粉末；③In the Al-Ti-B–Cu system, the mass fraction of nano-TiB 2 ceramic particles produced by the reaction is 30wt.%, and the content of copper element in the system is 5wt.%. Among them, the mass ratio of Ti/B is 2.22:1; Ti/B The molar ratio is 1:2; the respective weights of aluminum powder, titanium powder, boron powder, copper powder and magnesium powder in the system are: aluminum powder: 65 grams; titanium powder: 20.64 grams; boron powder: 9.36 grams; copper powder: 5 grams; magnesium powder: 0 grams; formulated into 100 grams of mixed powder;

④Al-Ti-B-Mg体系中反应生成纳米TiB2陶瓷颗粒的质量分数为20wt.％，体系中镁元素的含量为5wt.％，其中，Ti/B质量比为2.22:1；Ti/B摩尔比为1:2；体系中铝粉、钛粉、硼粉、铜粉、镁粉各自重量分别为：铝粉：75克；钛粉：13.77克；硼粉：6.23克；铜粉：0克；镁粉：5克；配制成100克混合粉末；④In the Al-Ti-B-Mg system, the mass fraction of nano -TiB2 ceramic particles produced by the reaction is 20wt.%, and the content of magnesium element in the system is 5wt.%. Among them, the mass ratio of Ti/B is 2.22:1; Ti/B The molar ratio is 1:2; the respective weights of aluminum powder, titanium powder, boron powder, copper powder, and magnesium powder in the system are: aluminum powder: 75 grams; titanium powder: 13.77 grams; boron powder: 6.23 grams; copper powder: 0 grams; magnesium powder: 5 grams; formulated into 100 grams of mixed powder;

(3)含有细化元素的Al-Ti-B-M反应体系球磨均匀化及粉体压坯致密化：(3) Ball milling homogenization of Al-Ti-B-M reaction system containing refining elements and densification of powder compacts:

(3a)将将步骤(2)中配制好的不同组分的粉料与氧化锆磨球放入混料机中，罐中盛有直径分别为5mm、7mm、11mm、15mm、20mm、22mm的ZrO2球，每种10个，ZrO2球质量共800g；混料机以30～60r/min的速度均匀混合8～32h；其中氧化锆磨球和混合粉末的质量比是8:1；(3a) Put the powders and zirconia grinding balls of different components prepared in step (2) into the mixer, and the tanks are filled with 5mm, 7mm, 11mm, 15mm, 20mm, and 22mm diameters respectively. ZrO 2 balls, 10 of each type, the total mass of ZrO 2 balls is 800g; the mixer is uniformly mixed at a speed of 30-60r/min for 8-32h; the mass ratio of zirconia grinding balls to mixed powder is 8:1;

(3b)将球磨混料的粉料取出，将球磨混好的粉料用铝箔包好，在液压机上冷压制成Φ30圆柱形压坯，高35～45mm；致密度为60～75％；(3b) Take out the ball-milled powder, wrap the ball-milled powder with aluminum foil, and cold-press it on a hydraulic press to make a Φ30 cylindrical compact with a height of 35-45mm and a density of 60-75%;

(4)压坯原位反应制备并细化处理TiB2颗粒：(4) Preparation and refinement of TiB 2 particles by in-situ reaction of the green compact:

(4a)用石墨纸将步骤(3b)中制得的Φ30圆柱形压坯包裹好放入到石墨模具中；(4a) Wrap the Φ30 cylindrical compact made in step (3b) with graphite paper and put it into a graphite mould;

(4b)将石墨模具和Φ30圆柱形压坯放入到真空热爆炉中，关闭炉门，后抽真空至炉内压力低于10Pa；(4b) Put the graphite mold and Φ30 cylindrical compact into the vacuum thermal explosion furnace, close the furnace door, and then evacuate until the pressure in the furnace is lower than 10Pa;

(4c)开始加热，加热速度设置为25～40K/min；加热升温至1183K，然后将温度降到1073K后保温10min，保温过程中同时对圆柱形压坯施加轴向25～55MPa压力，保压时间20～60s；反应后并经轴向压力致密化的圆柱形陶铝复合材料随炉在真空中冷却至室温。(4c) Start heating, and set the heating rate to 25-40K/min; heat up to 1183K, then lower the temperature to 1073K and keep warm for 10 minutes. During the heat-keeping process, apply an axial pressure of 25-55MPa to the cylindrical compact at the same time, and keep the pressure The time is 20-60s; after the reaction, the cylindrical ceramic-aluminum composite material densified by axial pressure is cooled to room temperature in vacuum with the furnace.

优选的，步骤(2)中的Al-Ti-B-Cu体系中反应生成纳米TiB2陶瓷颗粒的质量分数为10wt.％，体系中铜元素的含量为5wt.％，其中，Ti/B质量比为2.22:1；Ti/B摩尔比为1:2。Preferably, in the Al-Ti-B-Cu system in step (2), the reaction generates nano-TiB 2 The mass fraction of ceramic particles is 10wt.%, and the content of copper element in the system is 5wt.%, wherein, Ti/B mass The ratio is 2.22:1; the Ti/B molar ratio is 1:2.

该发明的有益效果在于：本发明中的细化陶铝复合材料中内生纳米TiB2颗粒的方法，包括以下步骤:(1)硼粉球磨预处理；(2)含有细化元素的Al-Ti-B-M反应体系的混合制备；(3)含有细化元素的Al-Ti-B-M反应体系球磨均匀化及粉体压坯致密化；(4)压坯原位反应制备并细化处理TiB2颗粒。本发明通过在反应体系内加入一定质量分数的合金元素将TiB2颗粒反应制备和细化一步完成，进一步减小纳米颗粒的尺寸。本发明中的合金元素添加细化陶铝复合材料中内生纳米TiB2颗粒可以用于陶瓷颗粒的细化和尺寸控制，有利于制备纳米尺寸TiB2颗粒，TiB2颗粒是铝合金重要的细化剂和强化剂，纳米尺寸TiB2颗粒可大幅提高合金组织的细化效果，大幅减少TiB2颗粒使用量，降低细化铝合金的成本，具有重要的实际应用价值。The beneficial effects of the invention are: the method of endogenous nano- TiB2 particles in the refinement pottery-aluminum composite material in the present invention comprises the following steps: (1) boron powder ball milling pretreatment; (2) Al- Mixed preparation of Ti-BM reaction system; (3) Al-Ti-BM reaction system containing refining elements for ball milling homogenization and powder compact compaction; (4) In-situ reaction preparation and refinement treatment of TiB 2 particles. The invention completes the reaction preparation and refinement of TiB2 particles in one step by adding a certain mass fraction of alloy elements in the reaction system, and further reduces the size of nano particles. The addition of alloying elements in the present invention refines the endogenous nano- TiB2 particles in the ceramic-aluminum composite material, which can be used for the refinement and size control of ceramic particles, which is beneficial to the preparation of nano-sized TiB2 particles. TiB2 particles are important fine particles of aluminum alloys. Nano-sized TiB2 particles can greatly improve the refining effect of the alloy structure, greatly reduce the amount of TiB2 particles used, and reduce the cost of refining aluminum alloys, which has important practical application value.

附图说明Description of drawings

图1为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为10wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图。Fig. 1 is that the mass fraction of the nano- TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 10wt.%, in the system When the content of copper element is 5wt.%, the X-ray diffraction pattern of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles.

图2为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为10wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Fig. 2 is that the mass fraction of the nanometer TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 10wt.%, in the system When the content of copper element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

图3为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图；Fig. 3 is that the mass fraction of the nano-TiB 2 ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 20wt.%. When the content of copper element is 5wt.%, the X-ray diffraction pattern of the ceramic-aluminum composite containing endogenous nano- TiB2 particle that makes;

图4为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Fig. 4 is that the mass fraction of the nano- TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 20wt.%, in the system When the content of copper element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

图5为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为30wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图。Fig. 5 is that the mass fraction of the nano- TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 30wt.%, in the system When the content of copper element is 5wt.%, the X-ray diffraction pattern of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles.

图6为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为30wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Fig. 6 is that the mass fraction of the nano-TiB 2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Cu system is 30wt.%. When the content of copper element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

图7为Al-Ti-B-Mg体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中镁元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图。Figure 7 shows that the mass fraction of nano- TiB2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Mg system is 20wt.%. When the content of magnesium element is 5wt.%, the X-ray diffraction pattern of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles.

图8为Al-Ti-B-Mg体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中镁元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Figure 8 shows that the mass fraction of nano- TiB2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Mg system is 20wt.%. When the content of magnesium element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

具体实施方式Detailed ways

为使本发明实现的技术手段、创新特征、达成目的易于明白了解，下面结合具体实施方式，进一步阐述本发明。In order to make the technical means, innovative features, and goals achieved by the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.

实施例1：Example 1:

本实施例中的一种细化陶铝复合材料中内生纳米TiB2颗粒的方法，包括以下步骤：A kind of refinement in the ceramic aluminum composite material in the present embodiment endogenous nanometer TiB 2The method for particle, comprises the following steps:

(1)硼粉球磨预处理：将硼粉放入球磨罐中，用球磨机将硼粉以300r/min的速度球磨处理1h；(1) Boron powder ball milling pretreatment: put boron powder into a ball mill tank, and use a ball mill to mill the boron powder at a speed of 300r/min for 1 hour;

(2)含有细化元素的Al-Ti-B-M反应体系的混合制备：(2) Mixing preparation of Al-Ti-B-M reaction system containing refinement elements:

(2a)称取一定量所需的粒度13μm的铝粉，球磨处理后粒度为0.5μm的硼粉以及粒度为13μm的钛粉，粒度为45μm的铜粉备用；(2a) Weighing a certain amount of required aluminum powder with a particle size of 13 μm, boron powder with a particle size of 0.5 μm and titanium powder with a particle size of 13 μm after ball milling, and copper powder with a particle size of 45 μm for subsequent use;

(2b)将铝粉、钛粉、硼粉、铜粉按以下几种配比配制成100g混合粉末制成Al-Ti-B-Cu试样:其中Al-Ti-B-Cu体系中反应生成纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1，Ti/B摩尔比为1:2)的质量分数为10wt.％，体系中铜元素的含量为5wt.％：体系中铝粉、钛粉、硼粉、铜粉各自重量分别为：铝粉：85克；钛粉：6.88克；硼粉：3.12克；铜粉：5克；配制成100克混合粉末；(2b) Aluminum powder, titanium powder, boron powder, and copper powder are formulated into 100g of mixed powder according to the following ratios to make Al-Ti-B-Cu sample: wherein the Al-Ti-B-Cu system reacts to form The mass fraction of nanometer TiB2 ceramic particles (Ti/B mass ratio is 2.22:1, Ti/B molar ratio is 1:2) is 10wt.%, and the content of copper element in the system is 5wt.%.In the system, aluminum powder, The respective weights of titanium powder, boron powder, and copper powder are: aluminum powder: 85 grams; titanium powder: 6.88 grams; boron powder: 3.12 grams; copper powder: 5 grams; mixed into 100 grams of powder;

(3)含有细化元素的Al-Ti-B-M反应体系球磨均匀化及粉体压坯致密化：(3) Ball milling homogenization of Al-Ti-B-M reaction system containing refining elements and densification of powder compacts:

(3a)将将将步骤(2)中配制好的不同组分的粉料与氧化锆磨球放入混料机中，罐中盛有直径分别为5mm、7mm、11mm、15mm、20mm、22mm的ZrO2球，每种10个，ZrO2球质量共800g。混料机以60r/min的速度均匀混合8h；其中氧化锆磨球和混合粉末的质量比是8:1；(3a) Put the powders and zirconia balls of different components prepared in step (2) into the mixer, and the tanks are filled with 5mm, 7mm, 11mm, 15mm, 20mm, and 22mm diameters respectively. ZrO 2 balls, 10 of each kind, the total mass of ZrO 2 balls is 800g. The mixer is uniformly mixed at a speed of 60r/min for 8 hours; the mass ratio of zirconia balls to mixed powder is 8:1;

(3b)将球磨混料的粉料取出，将球磨混好的粉料用铝箔包好，在液压机上冷压制成Φ30圆柱形压坯，高45mm；致密度为60％；(3b) Take out the powder material mixed by ball mill, wrap the powder material mixed by ball mill with aluminum foil, and cold press it on a hydraulic press to make a Φ30 cylindrical compact with a height of 45mm; the density is 60%;

(4)压坯原位反应制备并细化处理TiB2颗粒：(4) Preparation and refinement of TiB 2 particles by in-situ reaction of the green compact:

(4a)用石墨纸将步骤(3)中制得的Φ30圆柱形压坯包裹好放入到石墨模具中；(4a) wrap the Φ30 cylindrical compact made in step (3) with graphite paper and put it into a graphite mould;

(4b)将石墨模具和Φ30圆柱形压坯放入到真空热爆炉中，关闭炉门，后抽真空至炉内压力低于10Pa；(4b) Put the graphite mold and Φ30 cylindrical compact into the vacuum thermal explosion furnace, close the furnace door, and then evacuate until the pressure in the furnace is lower than 10Pa;

(4c)开始加热，加热速度设置为40K/min；加热升温至1183K，然后将温度降到1073K后保温10min，保温过程中同时对圆柱形压坯施加轴向55MPa压力，保压时间20s；反应后并经轴向压力致密化的圆柱形陶铝复合材料随炉在真空中冷却至室温。(4c) Start heating, and set the heating rate to 40K/min; heat up to 1183K, then lower the temperature to 1073K and keep warm for 10 minutes. During the keep warm process, apply an axial pressure of 55MPa to the cylindrical compact at the same time, and hold the pressure for 20s; Afterwards, the cylindrical ceramic-aluminum composite material densified by axial pressure is cooled to room temperature in vacuum with the furnace.

其中，步骤(2)中以铝粉、钛粉、硼粉、铜粉按配比配制成的Al-Ti-B-Cu试样，其中Al-Ti-B-Cu体系中反应生成纳米TiB2陶瓷颗粒的质量分数为10wt.％，体系中铜元素的含量为5wt.％：Wherein, in the step (2), the Al-Ti-B-Cu sample prepared by proportioning with aluminum powder, titanium powder, boron powder and copper powder, wherein the reaction in the Al-Ti-B-Cu system generates nanometer TiB ceramics The mass fraction of particles is 10wt.%, and the content of copper element in the system is 5wt.%:

当Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为10wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射如图1所示，所制备的含有内生纳米TiB2颗粒的陶瓷铝复合主要由TiB2陶瓷相和α-Al相组成，制得的TiB2颗粒尺寸最小，其平均尺寸为106.5nm。未加入Cu元素时，TiB2纳米颗粒含量为10wt.％的颗粒平均尺寸为177.9nm，加入5wt.％Cu元素后相比于未添加Cu元素时TiB2陶瓷颗粒的尺寸减小了40％，TiB2纳米颗粒得到了显著细化；如图2所示。When the mass fraction of the nano- TiB2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Cu system is 10wt.%, the copper element in the system %, the X-ray diffraction of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is shown in Figure 1, and the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is mainly composed of TiB 2 Composed of ceramic phase and α-Al phase, the prepared TiB 2 particle size is the smallest, with an average size of 106.5nm. When no Cu element was added, the average particle size of the TiB 2 nanoparticle content of 10wt.% was 177.9nm. After adding 5wt.% Cu element, the size of TiB 2 ceramic particles was reduced by 40% compared with that without Cu element. The TiB2 nanoparticles were significantly refined; as shown in Fig. 2.

实施例2：Example 2:

本实施例中的一种细化陶铝复合材料中内生纳米TiB2颗粒的方法，包括以下步骤：A kind of refinement in the ceramic aluminum composite material in the present embodiment endogenous nanometer TiB 2The method for particle, comprises the following steps:

(1)硼粉球磨预处理：将硼粉放入球磨罐中，用球磨机将硼粉以200r/min的速度球磨处理3h；(1) Boron powder ball milling pretreatment: put boron powder in a ball mill tank, and use a ball mill to mill the boron powder at a speed of 200r/min for 3 hours;

(2)含有细化元素的Al-Ti-B-M反应体系的混合制备：(2) Mixing preparation of Al-Ti-B-M reaction system containing refinement elements:

(2a)称取一定量所需的粒度48μm的铝粉，球磨处理后粒度为1μm的硼粉以及粒度为45μm的钛粉，粒度为45μm的铜粉备用；(2a) Weighing a certain amount of required aluminum powder with a particle size of 48 μm, boron powder with a particle size of 1 μm and titanium powder with a particle size of 45 μm after ball milling, and copper powder with a particle size of 45 μm for subsequent use;

(2b)将铝粉、钛粉、硼粉、铜粉按以下几种配比配制成100g混合粉末制成Al-Ti-B-Cu试样:其中Al-Ti-B-Cu体系中反应生成纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1，Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中铜元素的含量为5wt.％：体系中铝粉、钛粉、硼粉、铜粉各自重量分别为：铝粉：75克；钛粉：13.77克；硼粉：6.23克；铜粉：5克；配制成100克混合粉末；(2b) Aluminum powder, titanium powder, boron powder, and copper powder are formulated into 100g of mixed powder according to the following ratios to make Al-Ti-B-Cu sample: wherein the Al-Ti-B-Cu system reacts to form The mass fraction of nano -TiB2 ceramic particles (Ti/B mass ratio is 2.22:1, Ti/B molar ratio is 1:2) is 20wt.%, and the content of copper element in the system is 5wt.%.In the system, aluminum powder, The respective weights of titanium powder, boron powder and copper powder are: aluminum powder: 75 grams; titanium powder: 13.77 grams; boron powder: 6.23 grams; copper powder: 5 grams; mixed into 100 grams of powder;

(3)含有细化元素的Al-Ti-B-M反应体系球磨均匀化及粉体压坯致密化：(3) Ball milling homogenization of Al-Ti-B-M reaction system containing refining elements and densification of powder compacts:

(3a)将步骤(2)中配制好的不同组分的粉料与氧化锆磨球放入混料机中，罐中盛有直径分别为5mm、7mm、11mm、15mm、20mm、22mm的ZrO2球，每种10个，ZrO2球质量共800g。混料机以30r/min的速度均匀混合32h；其中氧化锆磨球和混合粉末的质量比是8:1；(3a) Put the powders and zirconia balls of different components prepared in step (2) into the mixer, and the tanks are filled with ZrO powders with diameters of 5mm, 7mm, 11mm, 15mm, 20mm, and 22mm respectively. 2 balls, 10 of each kind, the total mass of ZrO 2 balls is 800g. The mixer is uniformly mixed at a speed of 30r/min for 32h; the mass ratio of zirconia balls to mixed powder is 8:1;

(3b)将球磨混料的粉料取出，将球磨混好的粉料用铝箔包好，在液压机上冷压制成Φ30圆柱形压坯，高40mm；致密度为65％；(3b) Take out the powder material mixed by the ball mill, wrap the powder material mixed by the ball mill with aluminum foil, and cold press it into a Φ30 cylindrical compact with a height of 40mm; the density is 65%;

(4)压坯原位反应制备并细化处理TiB2颗粒：(4) Preparation and refinement of TiB 2 particles by in-situ reaction of the green compact:

(4a)用石墨纸将步骤(3)中制得的Φ30圆柱形压坯包裹好放入到石墨模具中；(4a) wrap the Φ30 cylindrical compact made in step (3) with graphite paper and put it into a graphite mould;

(4b)将石墨模具和Φ30圆柱形压坯放入到真空热爆炉中，关闭炉门，后抽真空至炉内压力低于10Pa；(4b) Put the graphite mold and Φ30 cylindrical compact into the vacuum thermal explosion furnace, close the furnace door, and then evacuate until the pressure in the furnace is lower than 10Pa;

(4c)开始加热，加热速度设置为35K/min；加热升温至1183K，然后将温度降到1073K后保温10min，保温过程中同时对圆柱形压坯施加轴向40MPa压力，保压时间32s；反应后并经轴向压力致密化的圆柱形陶铝复合材料随炉在真空中冷却至室温。(4c) Start heating, and set the heating rate to 35K/min; heat up to 1183K, then lower the temperature to 1073K and keep warm for 10 minutes. During the keep warm process, apply axial 40MPa pressure to the cylindrical compact at the same time, and the holding time is 32s; Afterwards, the cylindrical ceramic-aluminum composite material densified by axial pressure is cooled to room temperature in vacuum with the furnace.

其中，步骤(2)中以铝粉、钛粉、硼粉、铜粉按配比配制成的Al-Ti-B-Cu试样，其中Al-Ti-B-Cu体系中反应生成纳米TiB2陶瓷颗粒的质量分数为20wt.％，体系中铜元素的含量为5wt.％：Wherein, in the step (2), the Al-Ti-B-Cu sample prepared by proportioning with aluminum powder, titanium powder, boron powder and copper powder, wherein the reaction in the Al-Ti-B-Cu system generates nanometer TiB ceramics The mass fraction of particles is 20wt.%, and the content of copper element in the system is 5wt.%:

当Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射如图3所示，所制备的含有内生纳米TiB2颗粒的陶瓷铝复合主要由TiB2陶瓷相和α-Al相组成，制得的TiB2颗粒尺寸较小，其平均尺寸为146nm。未加入Cu元素时，TiB2纳米颗粒含量为20wt.％的颗粒平均尺寸为340.6nm，加入5wt.％Cu元素后相比于未添加Cu元素时TiB2陶瓷颗粒的尺寸减小了57％，TiB2纳米颗粒得到了显著细化，如图4所示。When the mass fraction of the nano- TiB2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Cu system is 20wt.%, the copper element in the system When the content is 5wt.%, the X-ray diffraction of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is shown in Figure 3, and the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is mainly composed of TiB 2 Composed of ceramic phase and α-Al phase, the prepared TiB 2 particle size is small, and its average size is 146nm. When no Cu element was added, the average particle size of the TiB 2 nanoparticle content of 20wt.% was 340.6nm. After adding 5wt.% Cu element, the size of TiB 2 ceramic particles was reduced by 57% compared with that without Cu element. The TiB2 nanoparticles were significantly refined, as shown in Fig. 4.

实施例3：Example 3:

本实施例中的一种细化陶铝复合材料中内生纳米TiB2颗粒的方法，包括以下步骤：A kind of refinement in the ceramic aluminum composite material in the present embodiment endogenous nanometer TiB 2The method for particle, comprises the following steps:

(1)硼粉球磨预处理：将硼粉放入球磨罐中，用球磨机将硼粉以300r/min的速度球磨处理1h；(1) Boron powder ball milling pretreatment: put boron powder into a ball mill tank, and use a ball mill to mill the boron powder at a speed of 300r/min for 1 hour;

(2)含有细化元素的Al-Ti-B-M反应体系的混合制备：(2) Mixing preparation of Al-Ti-B-M reaction system containing refinement elements:

(2a)称取一定量所需的粒度13μm的铝粉，球磨处理后粒度为0.5μm的硼粉以及粒度为25μm的钛粉，粒度为45μm的铜粉备用；(2a) Weighing a certain amount of required aluminum powder with a particle size of 13 μm, boron powder with a particle size of 0.5 μm and titanium powder with a particle size of 25 μm after ball milling, and copper powder with a particle size of 45 μm for subsequent use;

(2b)将铝粉、钛粉、硼粉、铜粉按以下几种配比配制成100g混合粉末制成Al-Ti-B-Cu试样:其中Al-Ti-B-Cu体系中反应生成纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为30wt.％，体系中铜元素的含量为5wt.％：体系中铝粉、钛粉、硼粉、铜粉各自重量分别为：铝粉：65克；钛粉：20.64克；硼粉：9.36克；铜粉：5克；配制成100克混合粉末；(2b) Aluminum powder, titanium powder, boron powder, and copper powder are formulated into 100g of mixed powder according to the following ratios to make Al-Ti-B-Cu sample: wherein the Al-Ti-B-Cu system reacts to form The mass fraction of nano TiB 2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) is 30wt.%, and the content of copper element in the system is 5wt.%.In the system, aluminum powder, The respective weights of titanium powder, boron powder, and copper powder are: aluminum powder: 65 grams; titanium powder: 20.64 grams; boron powder: 9.36 grams; copper powder: 5 grams; mixed into 100 grams of powder;

(3)含有细化元素的Al-Ti-B-M反应体系球磨均匀化及粉体压坯致密化：(3) Ball milling homogenization of Al-Ti-B-M reaction system containing refining elements and densification of powder compacts:

(3a)将步骤(2)中配制好的不同组分的粉料与氧化锆磨球放入混料机中，罐中盛有直径分别为5mm、7mm、11mm、15mm、20mm、22mm的ZrO2球，每种10个，ZrO2球质量共800g。混料机以40r/min的速度均匀混合24h；其中氧化锆磨球和混合粉末的质量比是8:1；(3a) Put the powders and zirconia balls of different components prepared in step (2) into the mixer, and the tanks are filled with ZrO powders with diameters of 5mm, 7mm, 11mm, 15mm, 20mm, and 22mm respectively. 2 balls, 10 of each kind, the total mass of ZrO 2 balls is 800g. The mixer is uniformly mixed at a speed of 40r/min for 24 hours; the mass ratio of zirconia balls to mixed powder is 8:1;

(3b)将球磨混料的粉料取出，将球磨混好的粉料用铝箔包好，在液压机上冷压制成Φ30圆柱形压坯，高40mm；致密度为65％；(3b) Take out the powder material mixed by the ball mill, wrap the powder material mixed by the ball mill with aluminum foil, and cold press it into a Φ30 cylindrical compact with a height of 40mm; the density is 65%;

(4)压坯原位反应制备并细化处理TiB2颗粒：(4) Preparation and refinement of TiB 2 particles by in-situ reaction of the green compact:

(4a)用石墨纸将步骤(3)中制得的Φ30圆柱形压坯包裹好放入到石墨模具中；(4a) wrap the Φ30 cylindrical compact made in step (3) with graphite paper and put it into a graphite mould;

(4b)将石墨模具和Φ30圆柱形压坯放入到真空热爆炉中，关闭炉门，后抽真空至炉内压力低于10Pa；(4b) Put the graphite mold and Φ30 cylindrical compact into the vacuum thermal explosion furnace, close the furnace door, and then evacuate until the pressure in the furnace is lower than 10Pa;

(4c)开始加热，加热速度设置为25K/min；加热升温至1183K，然后将温度降到1073K后保温10min，保温过程中同时对圆柱形压坯施加轴向25MPa压力，保压时间60s；反应后并经轴向压力致密化的圆柱形陶铝复合材料随炉在真空中冷却至室温；(4c) Start heating, and set the heating rate to 25K/min; heat up to 1183K, then lower the temperature to 1073K and keep warm for 10 minutes, and apply axial 25MPa pressure to the cylindrical compact at the same time during the heat preservation process, and the holding time is 60s; Afterwards, the cylindrical ceramic-aluminum composite material densified by axial pressure is cooled to room temperature in vacuum with the furnace;

其中，步骤(2)中以铝粉、钛粉、硼粉、铜粉按配比配制成的Al-Ti-B-Cu试样，其中Al-Ti-B-Cu体系中反应生成纳米TiB2陶瓷颗粒的质量分数为30wt.％，体系中铜元素的含量为5wt.％：Wherein, in the step (2), the Al-Ti-B-Cu sample prepared by proportioning with aluminum powder, titanium powder, boron powder and copper powder, wherein the reaction in the Al-Ti-B-Cu system generates nanometer TiB ceramics The mass fraction of particles is 30wt.%, and the content of copper element in the system is 5wt.%:

当Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为30wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射如图5所示，所制备的含有内生纳米TiB2颗粒的陶瓷铝复合主要由TiB2陶瓷相和α-Al相组成，制得的TiB2颗粒平均尺寸为304nm。未加入Cu元素时，TiB2纳米颗粒含量为30wt.％的颗粒平均尺寸为422.7nm，加入5wt.％Cu元素后相比于未添加Cu元素时TiB2陶瓷颗粒的尺寸减小了28％，TiB2纳米颗粒得到了细化，如图6所示。When the mass fraction of the nano- TiB2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Cu system is 30wt.%, the copper element in the system When the content is 5wt.%, the X-ray diffraction of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is shown in Figure 5, and the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is mainly composed of TiB 2 Composed of ceramic phase and α-Al phase, the average size of the prepared TiB 2 particles is 304nm. When no Cu element was added, the average particle size of the TiB 2 nanoparticles with a content of 30wt.% was 422.7nm. After adding 5wt.% Cu element, the size of TiB 2 ceramic particles was reduced by 28% compared with that without Cu element. The TiB2 nanoparticles were refined, as shown in Fig. 6.

实施例4：Example 4:

本实施例中的一种细化陶铝复合材料中内生纳米TiB2颗粒的方法，包括以下步骤：A kind of refinement in the ceramic aluminum composite material in the present embodiment endogenous nanometer TiB 2The method for particle, comprises the following steps:

(1)硼粉球磨预处理：将硼粉放入球磨罐中，用球磨机将硼粉以200r/min的速度球磨处理3h；(1) Boron powder ball milling pretreatment: put boron powder in a ball mill tank, and use a ball mill to mill the boron powder at a speed of 200r/min for 3 hours;

(2)含有细化元素的Al-Ti-B-M反应体系的混合制备：(2) Mixing preparation of Al-Ti-B-M reaction system containing refinement elements:

(2a)称取一定量所需的粒度45μm的铝粉，球磨处理后粒度为1μm的硼粉以及粒度为45μm的钛粉，粒度为45μm的镁粉备用；(2a) Weighing a certain amount of required aluminum powder with a particle size of 45 μm, boron powder with a particle size of 1 μm and titanium powder with a particle size of 45 μm after ball milling, and magnesium powder with a particle size of 45 μm for subsequent use;

(2b)将铝粉、钛粉、硼粉、镁粉按以下几种配比配制成100g混合粉末制成Al-Ti-B-Mg压坯:其中Al-Ti-B-Mg体系中反应生成纳米陶瓷颗粒(Ti/B质量比为2.22:1,Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中镁元素的含量为5wt.％：体系中铝粉、钛粉、硼粉、镁粉各自重量分别为：铝粉：75克；钛粉：13.77克；硼粉：6.23克；镁粉：5克；配制成100克混合粉末；(2b) Aluminum powder, titanium powder, boron powder, and magnesium powder are formulated into 100g of mixed powder according to the following proportions to make Al-Ti-B-Mg compact: wherein the Al-Ti-B-Mg system reacts to form The mass fraction of nano-ceramic particles (Ti/B mass ratio is 2.22:1, Ti/B molar ratio is 1:2) is 20wt.%, and the content of magnesium in the system is 5wt.%. Aluminum powder and titanium powder in the system , boron powder, and magnesium powder are respectively weighted as follows: aluminum powder: 75 grams; titanium powder: 13.77 grams; boron powder: 6.23 grams; magnesium powder: 5 grams; mixed with 100 grams of powder;

(3)含有细化元素的Al-Ti-B-M反应体系球磨均匀化及粉体压坯致密化：(3) Ball milling homogenization of Al-Ti-B-M reaction system containing refining elements and densification of powder compacts:

(3a)将步骤(2)配制好的不同组分的粉料与氧化锆磨球放入混料机中，罐中盛有直径分别为5mm、7mm、11mm、15mm、20mm、22mm的ZrO2球，每种10个，ZrO2球质量共800g。混料机以45r/min的速度均匀混合20h；其中氧化锆磨球和混合粉末的质量比是8:1；(3a) Put the powders and zirconia balls of different components prepared in step (2) into the mixer, and the tank is filled with ZrO2 with diameters of 5mm, 7mm, 11mm, 15mm, 20mm, and 22mm respectively Balls, 10 of each kind, the ZrO 2 balls have a total mass of 800g. The mixer is uniformly mixed at a speed of 45r/min for 20h; the mass ratio of zirconia balls to mixed powder is 8:1;

(3b)将球磨混料的粉料取出，将球磨混好的粉料用铝箔包好，在液压机上冷压制成Φ30圆柱形压坯，高35mm；致密度为75％；(3b) Take out the powder material mixed by ball mill, wrap the powder material mixed by ball mill with aluminum foil, and cold press it into a Φ30 cylindrical compact with a height of 35mm; the density is 75%;

(4)压坯原位反应制备并细化处理TiB2颗粒：(4) Preparation and refinement of TiB 2 particles by in-situ reaction of the green compact:

(4a)用石墨纸将步骤(3)中制得的Φ30圆柱形压坯包裹好放入到石墨模具中；(4a) wrap the Φ30 cylindrical compact made in step (3) with graphite paper and put it into a graphite mould;

(4b)将石墨模具和Φ30圆柱形压坯放入到真空热爆炉中，关闭炉门，后抽真空至炉内压力低于10Pa；(4b) Put the graphite mold and Φ30 cylindrical compact into the vacuum thermal explosion furnace, close the furnace door, and then evacuate until the pressure in the furnace is lower than 10Pa;

(4c)开始加热，加热速度设置为35K/min；加热升温至1183K，然后将温度降到1073K后保温10min，保温过程中同时对圆柱形压坯施加轴向45MPa压力，保压时间25s；反应后并经轴向压力致密化的圆柱形陶铝复合材料随炉在真空中冷却至室温；(4c) Start heating, and set the heating rate to 35K/min; heat up to 1183K, then lower the temperature to 1073K and keep warm for 10 minutes. During the keep warm process, apply axial 45MPa pressure to the cylindrical compact at the same time, and hold the pressure for 25s; Afterwards, the cylindrical ceramic-aluminum composite material densified by axial pressure is cooled to room temperature in vacuum with the furnace;

其中，步骤(2)中以铝粉、钛粉、硼粉、镁粉按一定配比配制成的Al-Ti-B-Mg试样，其中Al-Ti-B-Mg体系中反应生成的纳米陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中镁元素的含量为5wt.％：Among them, the Al-Ti-B-Mg sample prepared by aluminum powder, titanium powder, boron powder, and magnesium powder in a certain proportion in step (2), wherein the nano The mass fraction of ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) is 20wt.%, and the content of magnesium element in the system is 5wt.%:

当Al-Ti-B-Mg体系内生成的纳米陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中镁元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射如图7所示，所制备的含有内生纳米TiB2颗粒的陶瓷铝复合主要由TiB2陶瓷相和α-Al相组成，制得的TiB2颗粒平均尺寸为280.4nm；未加镁元素时，TiB2纳米颗粒含量为20wt.％的颗粒平均尺寸为340.6nm，加入5wt.％Mg元素后相比于未添加Mg元素时TiB2陶瓷颗粒的尺寸减小了17.7％，如图8所示。When the mass fraction of the nano ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Mg system is 20wt.%, the content of magnesium element in the system When it is 5wt.%, the X-ray diffraction of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is shown in Figure 7, and the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles is mainly composed of TiB 2 ceramic phase and α-Al phase, the average particle size of the prepared TiB 2 is 280.4nm; when no magnesium element is added, the average particle size of the TiB 2 nanoparticle content is 20wt.% is 340.6nm, and the phase after adding 5wt.% Mg element The size of the TiB2 ceramic particles was reduced by 17.7% compared to that without adding Mg element, as shown in Fig. 8.

针对上述实施例材料进行X射线分析测试以及颗粒尺寸形貌分析，获得以下数据：Carry out X-ray analysis test and particle size morphology analysis for above-mentioned embodiment material, obtain following data:

图1为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为10wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图。Fig. 1 is that the mass fraction of the nano- TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 10wt.%, in the system When the content of copper element is 5wt.%, the X-ray diffraction pattern of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles.

图2为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为10wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Fig. 2 is that the mass fraction of the nanometer TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 10wt.%, in the system When the content of copper element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

图3为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图；Fig. 3 is that the mass fraction of the nano-TiB 2 ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 20wt.%. When the content of copper element is 5wt.%, the X-ray diffraction pattern of the ceramic-aluminum composite containing endogenous nano- TiB2 particle that makes;

图4为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Fig. 4 is that the mass fraction of the nano- TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 20wt.%, in the system When the content of copper element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

图5为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为30wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图。Fig. 5 is that the mass fraction of the nano- TiB ceramic particle (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) that generates in Al-Ti-B-Cu system is 30wt.%, in the system When the content of copper element is 5wt.%, the X-ray diffraction pattern of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles.

图6为Al-Ti-B-Cu体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为30wt.％，体系中铜元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Fig. 6 is that the mass fraction of the nano-TiB 2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Cu system is 30wt.%. When the content of copper element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

图7为Al-Ti-B-Mg体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中镁元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的X射线衍射图。Figure 7 shows that the mass fraction of nano- TiB2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Mg system is 20wt.%. When the content of magnesium element is 5wt.%, the X-ray diffraction pattern of the prepared ceramic-aluminum composite containing endogenous nano-TiB 2 particles.

图8为Al-Ti-B-Mg体系内生成的纳米TiB2陶瓷颗粒(Ti/B质量比为2.22:1；Ti/B摩尔比为1:2)的质量分数为20wt.％，体系中镁元素的含量为5wt.％时，制得的含有内生纳米TiB2颗粒的陶瓷铝复合的尺寸形貌分析。Figure 8 shows that the mass fraction of nano- TiB2 ceramic particles (Ti/B mass ratio is 2.22:1; Ti/B molar ratio is 1:2) generated in the Al-Ti-B-Mg system is 20wt.%. When the content of magnesium element is 5wt.%, the size and morphology analysis of the ceramic-aluminum composite containing endogenous nano-TiB 2 particles is prepared.

以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也视为本发明的保护范围。The above description is a preferred embodiment of the present invention, and it should be pointed out that for those skilled in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications are also considered Be the protection scope of the present invention.

Claims (2)

1. a kind of interior raw nanometer TiB in refinement pottery aluminium composite material2The method of particle, it is characterised in that：Comprise the following steps：
(1) boron powder ball milling pretreatment：Boron powder is put into ball grinder, with ball mill by boron powder with the speed of 200~300r/min 1~3h of ball-milling treatment；
(2) Al-Ti-B-M reaction systems containing Refining Elements are mixed with, specific as follows：
(2a) weighs the boron powder that granularity after the aluminium powder of 13~48 μm of granularity, ball-milling treatment is 0.5~1 μm, granularity is 13~45 μm Titanium valve, the copper powder that granularity is 45 μm and magnesium powder that granularity is 45 μm it is spare；
Al-Ti- is made by following several 100g mixed-powders that are configured in aluminium powder, titanium valve, boron powder, copper powder, magnesium powder by (2b) B-M green compacts, wherein, M represents copper powder, magnesium powder, and Ti/B mass ratioes are 2.22:1；Ti/B molar ratios are 1:2；The content of aluminium powder is 65 ~85wt.%；Titanium powder content is 6.88~20.64wt.%；Boron powder content be the content of 3.12~9.36wt.% copper powders be 0~ 5wt.%, the content of magnesium powder is 0~5wt.%, and above-mentioned each component is specific as follows；
1. reaction generation nanometer TiB in Al-Ti-B-Cu systems2The mass fraction of ceramic particle is 10wt.%, copper in system Content for 5wt.%, wherein, Ti/B mass ratioes are 2.22:1；Ti/B molar ratios are 1:2；Aluminium powder in system, titanium valve, boron powder, Each weight is respectively for copper powder, magnesium powder：Aluminium powder：85 grams；Titanium valve：6.88 gram；Boron powder：3.12 gram；Copper powder：5 grams；Magnesium powder：0 gram； It is configured to 100 grams of mixed-powders；
2. reaction generation nanometer TiB in Al-Ti-B-Cu systems2The mass fraction of ceramic particle is 20wt.%, copper in system Content for 5wt.%, wherein, Ti/B mass ratioes are 2.22:1；Ti/B molar ratios are 1:2；Aluminium powder in system, titanium valve, boron powder, Each weight is respectively for copper powder, magnesium powder：Aluminium powder：75 grams；Titanium valve：13.77 grams；Boron powder：6.23 gram；Copper powder：5 grams；Magnesium powder：0 gram； It is configured to 100 grams of mixed-powders；
3. reaction generation nanometer TiB in Al-Ti-B-Cu systems2The mass fraction of ceramic particle is 30wt.%, copper in system Content for 5wt.%, wherein, Ti/B mass ratioes are 2.22:1；Ti/B molar ratios are 1:2；Aluminium powder in system, titanium valve, boron powder, Each weight is respectively for copper powder, magnesium powder：Aluminium powder：65 grams；Titanium valve：20.64 grams；Boron powder：9.36 gram；Copper powder：5 grams；Magnesium powder：0 gram； It is configured to 100 grams of mixed-powders；
4. reaction generation nanometer TiB in Al-Ti-B-Mg systems2The mass fraction of ceramic particle is 20wt.%, magnesium elements in system Content for 5wt.%, wherein, Ti/B mass ratioes are 2.22:1；Ti/B molar ratios are 1:2；Aluminium powder in system, titanium valve, boron powder, Each weight is respectively for copper powder, magnesium powder：Aluminium powder：75 grams；Titanium valve：13.77 grams；Boron powder：6.23 gram；Copper powder：0 gram；Magnesium powder：5 grams； It is configured to 100 grams of mixed-powders；
(3) the Al-Ti-B-M reaction systems ball milling containing Refining Elements and the densification of powder green compact：
The powder of prepared different component in step (2) and zirconium oxide balls will be put into batch mixer by (3a), be filled in tank Diameter is respectively the ZrO of 5mm, 7mm, 11mm, 15mm, 20mm, 22mm2Ball, each 10, ZrO2The common 800g of ball quality；Batch mixer 8~32h is uniformly mixed with the speed of 30~60r/min；The mass ratio of wherein zirconium oxide balls and mixed-powder is 8:1；
(3b) takes out the powder of ball mill mixing, and the mixed powder of ball milling is wrapped with aluminium foil, and Φ is made in cold pressing on a hydraulic press 30 cylindrical green compacts, high 35~45mm；Consistency is 60~75%；
(4) green compact reaction in-situ prepares simultaneously micronization processes TiB2Particle：
30 cylindrical green compacts of Φ obtained in step (3b) with graphite paper are wrapped and are put into graphite jig by (4a)；
Graphite jig and 30 cylindrical green compacts of Φ are put into vacuum thermal explosion stove by (4b), close fire door, after be evacuated in stove Pressure is less than 10Pa；
(4c) is begun to warm up, and firing rate is arranged to 25~40K/min；1183K is heated to, is then reduced the temperature to It keeps the temperature 10min after 1073K, applies axial 25~55MPa pressure in insulating process to cylindrical green compact simultaneously, the dwell time 20~ 60s；Cylindrical pottery aluminium composite material after reaction and through axial compressive force densification is cooled to room temperature in a vacuum with stove.
2. interior raw nanometer TiB in refinement pottery aluminium composite material according to claim 12The method of particle, it is characterised in that： Reaction generation nanometer TiB in Al-Ti-B-Cu systems in the step 22The mass fraction of ceramic particle be 10wt.%, system The content of middle copper is 5wt.%, wherein, Ti/B mass ratioes are 2.22:1；Ti/B molar ratios are 1:2.
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