CN103397282B - The preparation method of nano zircite coating aluminium borate whisker/aluminum matrix composite - Google Patents
The preparation method of nano zircite coating aluminium borate whisker/aluminum matrix composite Download PDFInfo
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- CN103397282B CN103397282B CN201310351427.1A CN201310351427A CN103397282B CN 103397282 B CN103397282 B CN 103397282B CN 201310351427 A CN201310351427 A CN 201310351427A CN 103397282 B CN103397282 B CN 103397282B
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- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 39
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000011159 matrix material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000576 coating method Methods 0.000 title claims abstract description 15
- 239000011248 coating agent Substances 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000007864 aqueous solution Substances 0.000 claims abstract description 36
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 33
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000002787 reinforcement Effects 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 19
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000000889 atomisation Methods 0.000 claims abstract description 9
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract 3
- 238000001914 filtration Methods 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 229910001008 7075 aluminium alloy Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229910001250 2024 aluminium alloy Inorganic materials 0.000 claims description 3
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims 2
- 238000009413 insulation Methods 0.000 claims 2
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000012856 packing Methods 0.000 claims 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 10
- 238000009716 squeeze casting Methods 0.000 abstract description 5
- 238000010406 interfacial reaction Methods 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 9
- 238000011049 filling Methods 0.000 description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- -1 boric acid Aluminum Chemical compound 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Abstract
纳米氧化锆涂覆硼酸铝晶须/铝基复合材料的制备方法，它涉及一种采用水热合成的方法在陶瓷增强体表面获得纳米氧化锆涂层的制备方法。本发明为了解决高温条件下硼酸铝晶须与铝基体之间存在严重的界面反应，使其力学性能降低的技术问题。方法：将氨水或NaOH溶液与氧氯化锆水溶液以雾化的方式添加到硼酸铝晶须水溶液中，过滤，然后将过滤后所得的增强体倒入水热釜中保温，冷却，压制，得到增强体的预制件，将增强体的预制件保温后放入模具中加热，将熔融的铝或铝合金浇入模具中同时加压，保压，即得。本发明用挤压铸造的方法得到的增强体制备纳米氧化锆涂覆硼酸铝晶须/铝基复合材料抗拉强度可达540MPa，相比现有复合材料抗拉强度提高了40%以上。
The invention discloses a preparation method of nano-zirconia coated aluminum borate whisker/aluminum matrix composite material, which relates to a preparation method of obtaining nano-zirconia coating on the surface of a ceramic reinforcement by adopting a hydrothermal synthesis method. The invention aims to solve the technical problem that there is a serious interfacial reaction between the aluminum borate whisker and the aluminum matrix under high temperature conditions, which reduces its mechanical properties. Method: Ammonia water or NaOH solution and zirconium oxychloride aqueous solution are added to aluminum borate whisker aqueous solution in the form of atomization, filtered, and then the reinforced body obtained after filtration is poured into a hydrothermal kettle to keep warm, cooled, and pressed to obtain The prefabricated part of the reinforced body is obtained by heating the prefabricated part of the reinforced body in a mold after being kept warm, and pouring molten aluminum or aluminum alloy into the mold while pressurizing and maintaining the pressure. The invention uses the reinforced body obtained by the squeeze casting method to prepare the nano-zirconia coated aluminum borate whisker/aluminum matrix composite material, which has a tensile strength of up to 540MPa, which is more than 40% higher than that of the existing composite material.
Description
技术领域technical field
本发明涉及一种采用水热合成的方法在陶瓷增强体表面获得纳米氧化锆涂层的制备方法。The invention relates to a preparation method for obtaining a nano-zirconia coating on the surface of a ceramic reinforcement by using a hydrothermal synthesis method.
背景技术Background technique
晶须增强铝基复合材料具有良好的比刚度、比强度等一系列的优异性能，同时在价格上也颇具竞争力。硼酸铝晶须增强铝基复合材料具有广泛的应用前景，但是高温条件下硼酸铝晶须与铝基体之间存在严重的界面反应，破坏了晶须的完整性，同时在界面处生成脆性相，降低了界面结合强度，使其力学性能降低。为了改善复合材料的性能，往往通过通过增强体表面涂覆来调整界面结构。适当的涂层引入不仅能提高基体与增强体之间的润湿性、还能抑制基体与增强体间的界面反应，从而大幅度改善复合材料的性能。Whisker-reinforced aluminum matrix composites have a series of excellent properties such as good specific stiffness and specific strength, and are also quite competitive in price. Aluminum borate whisker-reinforced aluminum matrix composites have broad application prospects, but severe interfacial reactions exist between aluminum borate whiskers and the aluminum matrix under high temperature conditions, which destroys the integrity of the whiskers and generates brittle phases at the interface. The interfacial bonding strength is reduced and its mechanical properties are reduced. In order to improve the performance of composite materials, the interfacial structure is often adjusted by coating the reinforcement surface. Appropriate coating introduction can not only improve the wettability between the matrix and the reinforcement, but also inhibit the interfacial reaction between the matrix and the reinforcement, thereby greatly improving the performance of the composite material.
发明内容Contents of the invention
本发明是为了解决高温条件下硼酸铝晶须与铝基体之间存在严重的界面反应，在界面处生成脆性相，降低了界面结合强度，使其力学性能降低的技术问题，提供了一种纳米氧化锆涂覆硼酸铝晶须/铝基复合材料的制备方法。The present invention aims to solve the technical problem that serious interfacial reaction exists between aluminum borate whiskers and aluminum matrix under high temperature conditions, and a brittle phase is formed at the interface, which reduces the interfacial bonding strength and reduces its mechanical properties, and provides a nano Zirconia-coated aluminum borate whisker/aluminum matrix composites.
纳米氧化锆涂覆硼酸铝晶须/铝基复合材料的制备方法如下：The preparation method of nanometer zirconia coated aluminum borate whisker/aluminum matrix composite material is as follows:
一、将硼酸铝晶须倒入水中，水与硼酸铝晶须的质量比为40～80:1，充分搅拌后超声分散，得到硼酸铝晶须水溶液；1. Pour aluminum borate whiskers into water, the mass ratio of water to aluminum borate whiskers is 40-80:1, stir thoroughly and ultrasonically disperse to obtain an aqueous solution of aluminum borate whiskers;
二、将氧氯化锆溶解到水中，得到浓度为0.00001～0.2mol/L的氧氯化锆水溶液；2. Dissolving zirconium oxychloride into water to obtain an aqueous zirconium oxychloride solution with a concentration of 0.00001 to 0.2 mol/L;
三、配制浓度为0.001～1mol/L的氨水或NaOH溶液；3. Prepare ammonia water or NaOH solution with a concentration of 0.001-1mol/L;
四、按照氧化锆与硼酸铝晶须的质量比为1:10～80的比例，将氧氯化锆水溶液以雾化的方式添加到硼酸铝晶须水溶液中，同时将氨水或NaOH溶液以雾化的方式添加到硼酸铝晶须水溶液中调节体系的pH值为6～12，搅拌，静置1～5h，过滤，然后将过滤后所得的增强体倒入水热釜中，填充比为70%～80%，在100～300℃保温1～24h，自然冷却；4. According to the mass ratio of zirconia and aluminum borate whiskers in the ratio of 1:10 to 80, the zirconium oxychloride aqueous solution is added to the aluminum borate whisker aqueous solution by atomization, and the ammonia water or NaOH solution is sprayed Add it to the aqueous solution of aluminum borate whiskers to adjust the pH of the system to 6-12, stir, let it stand for 1-5 hours, filter, and then pour the filtered reinforcement into a hydrothermal kettle with a filling ratio of 70 %~80%, keep warm at 100~300℃ for 1~24h, and cool naturally;
五、将步骤四所得产物从水热釜中倒入模具中压制，得到增强体的预制件；5. Pour the product obtained in step 4 from the hydrothermal kettle into the mold and press it to obtain the prefabricated part of the reinforcement;
六、将增强体的预制件在400～1100℃的温度下保温30～120min；6. Heat the prefabricated part of the reinforcement at a temperature of 400-1100°C for 30-120 minutes;
七、将经过步骤六处理的增强体的预制件放入模具中加热至450～550℃，将熔融的铝或铝合金浇入模具中同时加压，压力为80～200MPa，保压15～30min，即得纳米氧化锆涂覆硼酸铝晶须/铝基复合材料。7. Put the prefabricated part of the reinforced body processed in step 6 into the mold and heat it to 450-550°C, pour the molten aluminum or aluminum alloy into the mold and pressurize at the same time, the pressure is 80-200MPa, and the pressure is kept for 15-30min , that is, the nano-zirconia coated aluminum borate whisker/aluminum matrix composite material.
步骤七中所述的铝合金为2024铝合金、6061铝合金或7075铝合金。The aluminum alloy described in step seven is 2024 aluminum alloy, 6061 aluminum alloy or 7075 aluminum alloy.
本发明制备涂层的无机盐原料廉价，涂覆工艺简单，涂层的引入能够有效阻止界面反应的发生，提高界面结合强度。本发明用挤压铸造的方法得到的增强体制备纳米氧化锆涂覆硼酸铝晶须/铝基复合材料抗拉强度可达540MPa，相比现有复合材料抗拉强度提高了40%以上。In the present invention, the inorganic salt raw material for preparing the coating is cheap, the coating process is simple, and the introduction of the coating can effectively prevent the occurrence of interface reaction and improve the interface bonding strength. The invention uses the reinforced body obtained by the squeeze casting method to prepare the nano-zirconia coated aluminum borate whisker/aluminum matrix composite material, which has a tensile strength of up to 540MPa, which is more than 40% higher than that of the existing composite material.
附图说明Description of drawings
图1是实验一制备的纳米氧化锆涂覆硼酸铝晶须/铝基复合材料中涂覆后晶须表面的扫描电镜照片；Fig. 1 is the scanning electron micrograph of the whisker surface after coating in the nano zirconia coated aluminum borate whisker/aluminum matrix composite material that experiment one prepares;
图2是实验一制备的纳米氧化锆涂覆硼酸铝晶须/铝基复合材料中涂覆后晶须的XRD衍射图谱，图中●表示ZrO2。Fig. 2 is the XRD diffraction pattern of the coated whiskers in the nano-zirconia-coated aluminum borate whiskers/aluminum matrix composite material prepared in Experiment 1, in which ● represents ZrO 2 .
具体实施方式Detailed ways
本发明技术方案不局限于以下所列举具体实施方式，还包括各具体实施方式间的任意组合。The technical solution of the present invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.
具体实施方式一：本实施方式中纳米氧化锆涂覆硼酸铝晶须/铝基复合材料的制备方法如下：Embodiment 1: In this embodiment, the preparation method of nano-zirconia coated aluminum borate whisker/aluminum-based composite material is as follows:
一、将硼酸铝晶须倒入水中，水与硼酸铝晶须的质量比为40～80:1，充分搅拌后超声分散，得到硼酸铝晶须水溶液；1. Pour aluminum borate whiskers into water, the mass ratio of water to aluminum borate whiskers is 40-80:1, stir thoroughly and ultrasonically disperse to obtain an aqueous solution of aluminum borate whiskers;
二、将氧氯化锆溶解到水中，得到浓度为0.00001～0.2mol/L的氧氯化锆水溶液；2. Dissolving zirconium oxychloride into water to obtain an aqueous zirconium oxychloride solution with a concentration of 0.00001 to 0.2 mol/L;
三、配制浓度为0.001～1mol/L的氨水或NaOH溶液；3. Prepare ammonia water or NaOH solution with a concentration of 0.001-1mol/L;
四、按照氧化锆与硼酸铝晶须的质量比为1:10～80的比例，将氧氯化锆水溶液以雾化的方式添加到硼酸铝晶须水溶液中，同时将氨水或NaOH溶液以雾化的方式添加到硼酸铝晶须水溶液中调节体系的pH值为6～12，搅拌，静置1～5h，过滤，然后将过滤后所得的增强体倒入水热釜中，填充比为70%～80%，在100～300℃保温1～24h，自然冷却；4. According to the mass ratio of zirconia and aluminum borate whiskers in the ratio of 1:10 to 80, the zirconium oxychloride aqueous solution is added to the aluminum borate whisker aqueous solution by atomization, and the ammonia water or NaOH solution is sprayed Add it to the aqueous solution of aluminum borate whiskers to adjust the pH of the system to 6-12, stir, let it stand for 1-5 hours, filter, and then pour the filtered reinforcement into a hydrothermal kettle with a filling ratio of 70 %~80%, keep warm at 100~300℃ for 1~24h, and cool naturally;
五、将步骤四所得产物从水热釜中倒入模具中压制，得到增强体的预制件；5. Pour the product obtained in step 4 from the hydrothermal kettle into the mold and press it to obtain the prefabricated part of the reinforcement;
六、将增强体的预制件在400～1100℃的温度下保温30～120min；6. Heat the prefabricated part of the reinforcement at a temperature of 400-1100°C for 30-120 minutes;
七、将经过步骤六处理的增强体的预制件放入模具中加热至450～550℃，将熔融的铝或铝合金浇入模具中同时加压，压力为80～200MPa，保压15～30min，即得纳米氧化锆涂覆硼酸铝晶须/铝基复合材料。7. Put the prefabricated part of the reinforced body processed in step 6 into the mold and heat it to 450-550°C, pour the molten aluminum or aluminum alloy into the mold and pressurize at the same time, the pressure is 80-200MPa, and the pressure is kept for 15-30min , that is, the nano-zirconia coated aluminum borate whisker/aluminum matrix composite material.
本实施方式步骤四中所述的雾化是将氨水或NaOH溶液与氧氯化锆水溶液分别采用喷雾的方式同时添加到硼酸铝晶须水溶液中。The atomization described in step 4 of this embodiment is to add ammonia water or NaOH solution and zirconium oxychloride aqueous solution to the aluminum borate whisker aqueous solution at the same time by spraying respectively.
具体实施方式二：本实施方式与具体实施方式一不同的是步骤一中将硼酸铝晶须倒入水中，水与硼酸铝晶须的质量比为45～75:1。其它与具体实施方式一相同。Embodiment 2: This embodiment differs from Embodiment 1 in that in Step 1, aluminum borate whiskers are poured into water, and the mass ratio of water to aluminum borate whiskers is 45-75:1. Others are the same as in the first embodiment.
具体实施方式三：本实施方式与具体实施方式一或二之一不同的是步骤一中将硼酸铝晶须倒入水中，水与硼酸铝晶须的质量比为50:1。其它与具体实施方式一或二之一不相同。Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that in step 1, aluminum borate whiskers are poured into water, and the mass ratio of water to aluminum borate whiskers is 50:1. Others are different from the first or second specific embodiment.
具体实施方式四：本实施方式与具体实施方式一至三之一不同的是步骤二中将氧氯化锆溶解到水中，得到浓度为0.0001～0.15mol/L的氧氯化锆水溶液。其它与具体实施方式一至三之一相同。Embodiment 4: This embodiment differs from Embodiments 1 to 3 in that in Step 2, zirconium oxychloride is dissolved in water to obtain an aqueous solution of zirconium oxychloride with a concentration of 0.0001-0.15 mol/L. Others are the same as those in the first to third specific embodiments.
具体实施方式五：本实施方式与具体实施方式一至四之一不同的是步骤二中将氧氯化锆溶解到水中，得到浓度为0.001～0.1mol/L的氧氯化锆水溶液。其它与具体实施方式一至四之一相同。Embodiment 5: This embodiment differs from Embodiments 1 to 4 in that in Step 2, zirconium oxychloride is dissolved in water to obtain an aqueous solution of zirconium oxychloride with a concentration of 0.001-0.1 mol/L. Others are the same as one of the specific embodiments 1 to 4.
具体实施方式六：本实施方式与具体实施方式一至五之一不同的是步骤三中配制浓度为0.01～0.5mol/L的氨水或NaOH溶液。其它与具体实施方式一至五之一相同。Embodiment 6: This embodiment differs from Embodiment 1 to Embodiment 5 in that in step 3, ammonia water or NaOH solution with a concentration of 0.01-0.5 mol/L is prepared. Others are the same as one of the specific embodiments 1 to 5.
具体实施方式七：本实施方式与具体实施方式一至六之一不同的是步骤四中在200℃保温15h。其它与具体实施方式一至六之一相同。Embodiment 7: The difference between this embodiment and one of Embodiments 1 to 6 is that in Step 4, the temperature is kept at 200° C. for 15 hours. Others are the same as one of the specific embodiments 1 to 6.
具体实施方式八：本实施方式与具体实施方式一至七之一不同的是步骤六中将增强体的预制件在400～1100℃的温度下保温30～120min。其它与具体实施方式一至七之一相同。Embodiment 8: This embodiment differs from Embodiments 1 to 7 in that in Step 6, the prefabricated part of the reinforcing body is kept at a temperature of 400-1100° C. for 30-120 minutes. Others are the same as one of the specific embodiments 1 to 7.
具体实施方式九：本实施方式与具体实施方式一至八之一不同的是步骤七中压力为100MPa。其它与具体实施方式一至八之一相同。Embodiment 9: This embodiment is different from one of Embodiments 1 to 8 in that the pressure in step 7 is 100 MPa. Others are the same as one of the specific embodiments 1 to 8.
具体实施方式十：本实施方式与具体实施方式一至九之一不同的是步骤七中所述的铝合金为2024铝合金、6061铝合金或7075铝合金。其它与具体实施方式一至九之一相同。Embodiment 10: This embodiment is different from Embodiment 1 to Embodiment 9 in that the aluminum alloy mentioned in step 7 is 2024 aluminum alloy, 6061 aluminum alloy or 7075 aluminum alloy. Others are the same as one of the specific embodiments 1 to 9.
采用下述实验验证本发明效果：Adopt following experiment verification effect of the present invention:
实验一：experiment one:
纳米氧化锆涂覆硼酸铝晶须/铝基复合材料的制备方法如下：The preparation method of nanometer zirconia coated aluminum borate whisker/aluminum matrix composite material is as follows:
一、将硼酸铝晶须倒入水中，水与硼酸铝晶须的质量比为40:1，充分搅拌后超声分散，得到硼酸铝晶须水溶液；1. Pour the aluminum borate whiskers into water, the mass ratio of water to aluminum borate whiskers is 40:1, and after fully stirring, ultrasonically disperse to obtain an aqueous solution of aluminum borate whiskers;
二、将氧氯化锆溶解到水中，得到浓度为0.0001mol/L的氧氯化锆水溶液；2. Dissolving zirconium oxychloride in water to obtain a zirconium oxychloride aqueous solution with a concentration of 0.0001mol/L;
三、配制浓度为0.001mol/L的氨水或NaOH溶液；3. Prepare ammonia water or NaOH solution with a concentration of 0.001mol/L;
四、按照氧化锆与硼酸铝晶须的质量比为1:50的比例，将氧氯化锆水溶液以雾化的方式添加到硼酸铝晶须水溶液中，同时将氨水或NaOH溶液以雾化的方式添加到硼酸铝晶须水溶液中调节体系的pH值为6，搅拌，静置1h，过滤，然后将过滤后所得的增强体倒入水热釜中，填充比为70%，在100℃保温1h，自然冷却；Four, according to the mass ratio of zirconium oxide and aluminum borate whisker is the ratio of 1:50, the aqueous solution of zirconium oxychloride is added in the aqueous solution of aluminum borate whisker in the mode of atomization, ammoniacal water or NaOH solution are atomized at the same time Add to the aluminum borate whisker aqueous solution to adjust the pH of the system to 6, stir, let stand for 1 hour, filter, then pour the filtered reinforcement into a hydrothermal kettle with a filling ratio of 70%, and keep it warm at 100°C 1h, natural cooling;
五、将步骤四所得产物从水热釜中倒入模具中压制，得到增强体的预制件；5. Pour the product obtained in step 4 from the hydrothermal kettle into the mold and press it to obtain the prefabricated part of the reinforcement;
六、将增强体的预制件在400℃的温度下保温30min；6. Heat the prefabricated part of the reinforcement at a temperature of 400°C for 30 minutes;
七、将经过步骤六处理的增强体的预制件放入模具中加热至450℃，将熔融的铝浇入模具中同时加压，压力为80MPa，保压15min，即得纳米氧化锆涂覆硼酸铝晶须/铝基复合材料。7. Put the prefabricated part of the reinforced body processed in step 6 into the mold and heat it to 450°C, pour the molten aluminum into the mold and pressurize at the same time, the pressure is 80MPa, and the pressure is maintained for 15min to obtain nano-zirconia-coated boric acid Aluminum whisker/aluminum matrix composites.
本实验采用挤压铸造的方法制备的增强体体积分数为20%的复合材料抗拉强度可达510MPa，相比现有复合材料抗拉强度提高了40%以上。In this experiment, the tensile strength of the composite material with a reinforcement volume fraction of 20% prepared by squeeze casting method can reach 510MPa, which is more than 40% higher than that of the existing composite material.
实验二：Experiment 2:
纳米氧化锆涂覆硼酸铝晶须/铝基复合材料的制备方法如下：The preparation method of nanometer zirconia coated aluminum borate whisker/aluminum matrix composite material is as follows:
一、将硼酸铝晶须倒入水中，水与硼酸铝晶须的质量比为60:1，充分搅拌后超声分散，得到硼酸铝晶须水溶液；1. Pour the aluminum borate whiskers into water, the mass ratio of water to aluminum borate whiskers is 60:1, and after fully stirring, ultrasonically disperse to obtain an aqueous solution of aluminum borate whiskers;
二、将氧氯化锆溶解到水中，得到浓度为0.001mol/L的氧氯化锆水溶液；2. Dissolving zirconium oxychloride in water to obtain a zirconium oxychloride aqueous solution with a concentration of 0.001mol/L;
三、配制浓度为0.01mol/L的氨水或NaOH溶液；3. Prepare ammonia water or NaOH solution with a concentration of 0.01mol/L;
四、按照氧化锆与硼酸铝晶须的质量比为1:60的比例，将氧氯化锆水溶液以雾化的方式添加到硼酸铝晶须水溶液中，同时将氨水或NaOH溶液以雾化的方式添加到硼酸铝晶须水溶液中调节体系的pH值为12，搅拌，静置5h，过滤，然后将过滤后所得的增强体倒入水热釜中，填充比为80%，在300℃保温24h，自然冷却；Four, according to the mass ratio of zirconium oxide and aluminum borate whisker is the ratio of 1:60, the aqueous solution of zirconium oxychloride is added in the aqueous solution of aluminum borate whisker in the mode of atomization, ammoniacal water or NaOH solution are atomized at the same time Add to the aqueous solution of aluminum borate whiskers to adjust the pH of the system to 12, stir, let stand for 5 hours, filter, then pour the filtered reinforcement into a hydrothermal kettle with a filling ratio of 80%, and keep it warm at 300°C 24h, natural cooling;
五、将步骤四所得产物从水热釜中倒入模具中压制，得到增强体的预制件；5. Pour the product obtained in step 4 from the hydrothermal kettle into the mold and press it to obtain the prefabricated part of the reinforcement;
六、将增强体的预制件在450℃的温度下保温50min；Sixth, heat the prefabricated part of the reinforcement at a temperature of 450°C for 50 minutes;
七、将经过步骤六处理的增强体的预制件放入模具中加热至480℃，将熔融的7075铝合金浇入模具中同时加压，压力为90MPa，保压20min，即得纳米氧化锆涂覆硼酸铝晶须/铝基复合材料。7. Put the prefabricated part of the reinforced body processed in step 6 into the mold and heat it to 480°C, pour the molten 7075 aluminum alloy into the mold and pressurize at the same time, the pressure is 90MPa, and the pressure is maintained for 20min to obtain nano-zirconia coating. Aluminum borate-coated whiskers/aluminum matrix composites.
本实验采用挤压铸造的方法制备的增强体（硼酸铝晶须与氧化锆涂层的质量比为60:1）体积分数为20%的复合材料抗拉强度可达528MPa。In this experiment, the reinforcement (the mass ratio of aluminum borate whiskers to zirconia coating is 60:1) prepared by squeeze casting method has a tensile strength of 20% composite material with a tensile strength of 528MPa.
实验三：Experiment three:
纳米氧化锆涂覆硼酸铝晶须/铝基复合材料的制备方法如下：The preparation method of nanometer zirconia coated aluminum borate whisker/aluminum matrix composite material is as follows:
一、将硼酸铝晶须倒入水中，水与硼酸铝晶须的质量比为60:1，充分搅拌后超声分散，得到硼酸铝晶须水溶液；1. Pour the aluminum borate whiskers into water, the mass ratio of water to aluminum borate whiskers is 60:1, and after fully stirring, ultrasonically disperse to obtain an aqueous solution of aluminum borate whiskers;
二、将氧氯化锆溶解到水中，得到浓度为0.01mol/L的氧氯化锆水溶液；2. Dissolving zirconium oxychloride in water to obtain a zirconium oxychloride aqueous solution with a concentration of 0.01mol/L;
三、配制浓度为0.1mol/L的氨水或NaOH溶液；3. Prepare ammonia water or NaOH solution with a concentration of 0.1mol/L;
四、按照氧化锆与硼酸铝晶须的质量比为1:70的比例，将氧氯化锆水溶液以雾化的方式添加到硼酸铝晶须水溶液中，同时将氨水或NaOH溶液以雾化的方式添加到硼酸铝晶须水溶液中调节体系的pH值为8，搅拌，静置3h，过滤，然后将过滤后所得的增强体倒入水热釜中，填充比为75%，在150℃保温15h，自然冷却；Four, according to the mass ratio of zirconium oxide and aluminum borate whisker is the ratio of 1:70, the zirconium oxychloride aqueous solution is added in the aluminum borate whisker aqueous solution in the mode of atomization, ammoniacal water or NaOH solution is atomized at the same time Add to the aluminum borate whisker aqueous solution to adjust the pH of the system to 8, stir, let stand for 3 hours, filter, then pour the filtered reinforcement into a hydrothermal kettle with a filling ratio of 75%, and keep it warm at 150°C 15h, natural cooling;
五、将步骤四所得产物从水热釜中倒入模具中压制，得到增强体的预制件；5. Pour the product obtained in step 4 from the hydrothermal kettle into the mold and press it to obtain the prefabricated part of the reinforcement;
六、将增强体的预制件在600℃的温度下保温60min；6. Heat the prefabricated part of the reinforcement at a temperature of 600°C for 60 minutes;
七、将经过步骤六处理的增强体的预制件放入模具中加热至500℃，将熔融的铝浇入模具中同时加压，压力为100MPa，保压25min，即得纳米氧化锆涂覆硼酸铝晶须/铝基复合材料。7. Put the prefabricated part of the reinforced body processed in step 6 into the mold and heat it to 500°C, pour the molten aluminum into the mold and pressurize at the same time, the pressure is 100MPa, and the pressure is maintained for 25min to obtain nano-zirconia-coated boric acid Aluminum whisker/aluminum matrix composites.
本实验采用挤压铸造的方法制备的增强体（硼酸铝晶须与氧化锆涂层的质量比为70:1）体积分数为20%的复合材料抗拉强度可达540MPa。In this experiment, the reinforcement (the mass ratio of aluminum borate whiskers and zirconia coating is 70:1) prepared by squeeze casting method has a tensile strength of 20% composite material with a tensile strength of 540MPa.
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